WO2016188274A1 - Matte high-strength, low-stretch viscose fiber and manufacturing method therefor - Google Patents
Matte high-strength, low-stretch viscose fiber and manufacturing method therefor Download PDFInfo
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- WO2016188274A1 WO2016188274A1 PCT/CN2016/079847 CN2016079847W WO2016188274A1 WO 2016188274 A1 WO2016188274 A1 WO 2016188274A1 CN 2016079847 W CN2016079847 W CN 2016079847W WO 2016188274 A1 WO2016188274 A1 WO 2016188274A1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/12—Addition of delustering agents to the spinning solution
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
Definitions
- the invention relates to viscose fiber and preparation thereof, in particular to a matting type high-strength low-stretch viscose fiber and a preparation method thereof, and belongs to the technical field of textile fiber processing.
- textile fiber raw materials are mainly classified into natural fiber raw materials represented by cotton and hemp, petroleum-based fiber raw materials represented by polyester and acrylic fibers, and bio-based materials such as viscose fiber which is regenerated from natural cellulose materials.
- Fiber raw materials At present, with the scarcity of land resources and the shortage of human resources, the cotton planting area is declining year by year, and cotton products will not meet the growing needs of people's living standards. With the decreasing oil reserves and people's comfort for textiles, Functional and environmentally conscious awareness continues to increase, and viscose fibers produced from renewable resources are increasingly valued. As viscose fiber, as a natural recycled fiber, it has both natural fiber quality and excellent processability. Its structural composition is similar to that of cotton.
- Patent document CN102296373A (a method for producing ultra-fine high-strength high-mode viscose fiber, 2011.12.28) discloses a viscose fiber having a uniform structure, a fiber strength and a modulus higher than that of a conventional variety of 50% or more.
- the viscose fiber has a fiber strength of 0.44 to 0.78 dtex, a dry strength of ⁇ 3.1 cN/dtex (centimeter/denier), a wet strength of ⁇ 2.1 cN/dtex, a wet modulus of ⁇ 0.5 cN/dtex, and a whiteness of ⁇ 82.0%. .
- Patent document CN1632189 (a high-white strong fine-density viscose staple fiber and its production process, 2005.06.29) discloses a fine-density, high-strength viscose staple fiber, which is processed by an ordinary viscose fiber. In terms of high strength, strong abrasion resistance, fine hand feeling, anti-pleatability, resistance to multiple deformations, etc., it can also be used for textile high count yarn woven products.
- Patent document CN102251301A (a superfine denier high-strength viscose fiber production process, 2011.11.23) discloses a preparation method of viscose fiber with low fineness and high strength, which can obtain a fineness of 1.11 dtex and a strength of more than 2.9 cN/ Dtex viscose fiber.
- the patent document CN101130885 discloses a viscose fiber produced by using a hemp material plant and a preparation process thereof, and the process is simple and the material consumption is Low, and the produced ramie viscose fiber has excellent whiteness, strength and fiber elongation.
- the ramie viscose fiber prepared by the process meets the dry rupture strength ⁇ 1.820cN/dtex, and the wet rupture strength ⁇ 1.12 cN/dtex, dry elongation at break ⁇ 15.4%, linear density deviation rate ⁇ 6.00%, length deviation rate ⁇ 6.00%, ultra-long fiber rate ⁇ 1.0%, long fiber ⁇ 18.0mg/100g, defect point ⁇ 11mg/100g , residual sulfur ⁇ 18.0mg / 100g.
- Modal fiber is made from European eucalyptus wood and made into a wood slurry and then made by a special spinning process. It is the same natural fiber material as cotton, and the modal fiber is not produced in the whole production process. Any pollution, its dry strength is close to polyester, the wet strength is much higher than ordinary viscose fiber, no matter the gloss, softness, hygroscopicity, dyeing, dyeing fastness is better than pure cotton products, use it to do The finished fabric not only exhibits a silky luster, but also has a pleasant soft touch feeling and drape, as well as excellent wear resistance. It is an ideal environmentally friendly cellulose fiber. However, due to the high cost of modal fiber textile technology, the market modal modal is basically a blend of modal and cotton, or directly take the viscose (human cotton) fiber to impersonate Modal.
- the object of the present invention is to provide a matting type high-strength low-stretch viscose fiber which is different from the traditional viscose fiber product and cotton fiber, and is a novel fiber type realized by technological innovation, which is different from ordinary viscose.
- the index system of fiber and modal fiber not only exhibits the high-strength, low-stretch fiber characteristics of modal fiber, but also exhibits better skin-friendly properties than cotton fiber and modal, and can effectively replace existing modal fiber, and Production costs are lower than Modal and have good economic and social benefits.
- a matting type high-strength low-stretch viscose fiber which is a slurry raw material which is sequentially impregnated, ground, pressed, crushed, smashed, depolymerized, yellowed, dissolved, filtered, taken off. After the foaming, aging, spinning drafting and post-treatment, the matting type high-strength low-stretch viscose fiber meets the following technical indexes:
- the strength required to produce 5% elongation in wet state is ⁇ 0.55 cN/dtex
- Dry elongation at break is 11.0 to 19.0%
- the matting agent content is 0.8 to 5%.
- the pulp raw material comprises one or a combination of two or more of cotton pulp, bamboo pulp, wood pulp and hemp pulp.
- cotton pulp, bamboo pulp, wood pulp and hemp pulp can be carried out in any ratio. Mixing, wide source of raw materials, and low requirements on the content of fiber, can effectively reduce the cost of raw materials.
- the degree of polymerization of the pulp raw material is 650 to 1200, and the advantage is that the length of the softwood pulp fiber is 2 to 3 mm, and the strength is higher.
- the viscose fiber further satisfies the following technical indicators:
- Double fiber ⁇ 4.0mg/100g
- the defect point is ⁇ 4.0mg/100g.
- Another object of the present invention is to provide a method for preparing a matting type high-strength low-stretch viscose fiber, which comprises pulp as a raw material for production, viscose fiber by viscose preparation, spinning process and post-treatment, During the production process, the cross-sectional area of the secondary reaction microscope is still retained, and the ratio of the inner and outer layers of the interface is significantly different from the secondary reaction traces of the modal fiber and the ordinary viscose fiber, ensuring that the product has the characteristics of high strength and low elongation. It also has suitable water absorption and significant fiber skin-friendly properties.
- the pulp raw material is immersed in a dipping bucket containing alkali solution, and ground by a grinder to prepare a slurry of porridge having a concentration of 3 to 6%.
- the pulp raw material is first placed on the feeder. After setting a certain feeding speed (such as 40kg/min), it is added to the dip tank, and the purpose of the grinding is to open and disperse the fiber by mechanical action, thereby increasing the alkalization speed and alkalization rate of the cellulose;
- the porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a crucible, and the concentration is 30-40% after treatment.
- Pulp porridge, in this step, the press can remove excess lye, and the excess lye can be recycled.
- the treatment method is to remove the lye by using a filter with a filter of 60-120 mesh and a vacuum of -0.4 to -0.1 MPa.
- the alkali cellulose is recovered, and the twin-screw equipment is used to make the fiber separate and smelt, thereby breaking the cell wall of the cellulose fiber, removing small molecules in the cellulose, thereby improving the cellulose reaction performance. , to increase the content of cellulose-bound alkali, reaching 6 to 8% (mass percentage);
- the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor to obtain an alkali fiber having a degree of polymerization of 400-600 and a purity of 98.0-98.5%.
- the purpose of adding pure oxygen is oxidative depolymerization. After depolymerization, the degree of polymerization of alkali cellulose is reduced from 650 to 1200 to 400 to 600.
- step C The alkali cellulose obtained in step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent to obtain a concentration of 9.0 to 10.0% cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the lye is a sodium hydroxide solution having a concentration of 110 to 240 g/L
- the temperature of the immersion alkali solution is 30 to 60 ° C
- the immersion time is 50 to 90 minutes.
- the concentration of lye is too high, the solubility of the obtained cellulose sulfonate will decrease, and the viscosity of the viscose will be difficult to filter;
- the concentration of the alkali solution is too low, the degree of expansion of the pulp material is too high, and the pressing is difficult; the temperature is too high, and the cellulose is lowered. Gather quickly, accelerate side reactions, affect viscose filtration; temperature is too low, pulp pulping is high, and pressing is difficult.
- the grinder is disposed in a pipe connecting the dip tank and the press.
- the temperature of the porridge is 30 to 60 ° C, and the grinding time of the mill is 10 to 40 s.
- the material pressed by the press by the press can be divided into two parts, one part is an excess alkali solution mixed with fibers and impurities, and the other part is a mixture of solid and liquid which is pressed out of excess water. That is, alkali cellulose, in the above step B, the press has a press temperature of 57 to 63 ° C and a press ratio of 2.2 to 2.8.
- Pressing is to impregnate the pulp with excess lye, hemicellulose and impurities to increase the purity of the alkali cellulose.
- the degree of pressing is the pressure after pressing with the pulp and the quality of the pulp and the quality of the pre-impregnated dry pulp and quality.
- the ratio indicates that the pressed alkali cellulose is very tight, the plate is hard, and the surface area is small, which is not conducive to the later processing.
- the purpose of the pulverization is to make the alkali cellulose into fine and loose scraps, which increases the surface area and is beneficial to the later stage.
- the uniformity of the process and the expression of the degree of pulverization which is a fixed weight of alkali cellulose, is simply referred to as the degree of pulverization in the present invention, and refers to the weight per unit volume after pulverization of alkali cellulose, generally expressed in g/L, and alkali.
- the porridge is pressed and sent to a pulverizer for pulverization.
- the pulverization degree of the pulverizer is 120-180 g/L, and the post-processing can be improved by adjusting the pressing ratio and the pulverization degree.
- the uniformity of the performance of the alkali cellulose in the process prevents the local from receiving strong extrusion, thereby hindering the entry of oxygen and reducing the speed of the depolymerization step; the content of the alkali fiber obtained by the pulverization is 29 to 31%, and the alkali content It is 15 to 17%, and the content of the half fiber in the lye is controlled within 10 g/L.
- the lye is a sodium hydroxide solution having a concentration of 140 to 200 g/l, and the pure oxygen is added in an amount of 2 to 10% of the reactor volume, and the depolymerization reaction time is controlled at 30. ⁇ 60min.
- the amount of carbon disulfide added is 25 to 37% of the content of the methyl cellulose in the alkali cellulose obtained in the step B.
- the amount of carbon disulfide added is too small, the yellowing reaction is incomplete, and the filtration is difficult.
- the amount of carbon disulfide added is too high, the yellowing reaction is excessive, and the by-products are more.
- the yellowing reaction time is controlled at 45 to 50 minutes, and the yellowing reaction temperature is 20 to 30 °C.
- the dissolving is mixing, stirring and grinding the cellulose sulfonate with a solvent
- the solvent comprises a sodium hydroxide solution having a concentration of 25 to 45 g/L, and the concentration is 5-10 g/L aqueous sodium sulfite solution.
- the dissolution temperature is 10 to 20 ° C, and the dissolution time is 30 to 50 minutes.
- the matting agent is titanium dioxide.
- the present invention also improves the spinning drafting process, including a low acid and high salt moderate acid bath process and a high stretch spinning process, etc., specifically, the spinning
- the wire drawing steps are as follows:
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified.
- the bath comprises 90-120 g/L of sulfuric acid, 220-280 g/L of sodium sulfate and 8-15 g/L of zinc sulfate;
- the present invention adopts the three-bath wet spinning technique, and the viscose is formed into a tow after the spinning and drawing process, thereby ensuring multiple reactions of the fiber, in which the fiber cross section can form a clear secondary reaction.
- the microscope interface has the characteristics of improving the fiber strength, increasing the water absorption rate of the fiber, and increasing the water retention property of the fiber.
- the tow is stretched by a drafting machine, a two-way drafting machine, and a three-way drafting machine. It is more conducive to improving the brittleness of the fiber and improving the elongation of the fiber.
- the post-treatment includes desulfurization, bleaching and oiling of the tow formed by the spinning draft, and the desulfurizing agent used in the desulfurization is composed of sodium sulfide having a concentration of 4 to 8 g/L and a concentration of 1 to 4 g/L.
- the sodium carbonate composition; the bleaching agent used for the bleaching is a hydrogen peroxide concentration of 0.3-0.6 g/L; the oiling agent used for the oiling is 7-9 g/L, and the pH of the tow after oiling is 6.5. ⁇ 7.
- the invention adopts a mild desulfurization process to reduce the damage of product strength and elongation.
- the desulfurizing agent composed of sodium sulfide and sodium carbonate is milder than the existing sodium hydroxide and sodium sulfite, and the sodium carbonate can be used.
- the sulfuric acid brought by the tow from the acid bath, after the desulfurization process the pH of the adjustable tow is 8-11; the hydrogen peroxide bleach is milder than the bleach such as sodium hypochlorite, and the pH of the viscose fiber prepared by the invention should be
- the control is in the range of 6.5 to 7, and the pH value can also be adjusted by means of water washing and polyfunctional acid (organic acid). Within this range, the strength of the finished viscose fiber is not affected, and the elongation is high.
- the desulfurization temperature is 50 to 55 ° C, the desulfurization time is 2 to 3 min; the bleaching temperature is 50 to 55 ° C, the bleaching time is 1 to 2 min; and the temperature of the oil agent is 50 to 55 ° C. .
- the post-treatment further includes drying, the drying is performed on the tow formed by the spinning draft, the desulfurization, bleaching and the tow obtained after the oiling are dried using a dryer.
- the drying temperature is 75-115 ° C. After drying, high-strength low-stretch viscose fiber products are obtained, and the moisture regain rate of the product is controlled at 11 to 13.5%.
- the invention has the following beneficial effects:
- the viscose fiber according to the present invention is a novel fiber type realized through technological innovation, and belongs to a major innovation in the production technology of viscose staple fiber and cellulose fiber, which is different from the traditional viscose fiber product and Cotton fiber, which has an index system different from ordinary viscose fiber and modal fiber, has a fiber strength of 3.1 cN/dtex or more, which is about 30% higher than that of ordinary bio-based short fiber, close to modal, and has high strength of modal fiber. Low elongation and degradable characteristics make the fabric not easy to be deformed. It also has better moisture absorption and gas permeability than cotton fiber and modal, and it is soft, smooth and bright in appearance, and can effectively replace the existing differential viscosity. Glue fiber can improve the downstream processing performance of viscose fiber, and promote the development and industrial upgrading of downstream new textiles, with good economic and social benefits.
- the viscose fiber of the present invention has lower cost than the modal with higher performance index, and the price is lower than the modal fiber by 4000-5000 yuan/ton, and the viscose fiber of the invention is mainly reduced in the following aspects.
- the raw material of the viscose fiber of the invention has wide source and low requirement, and the raw material with lower content of methyl cellulose can be selected (the higher the content of methyl cellulose, the higher the price), the cotton pulp, bamboo pulp, One or a combination of two or more of wood pulp and hemp pulp, no proportion requirement; b. the amount of alkali used in the process of the invention is lower than that of conventional products; c.
- the spinning speed of the spinning machine is 45-55m/min, which is faster than 30m/min in the production process of Modal.
- the optimized acid bath composition and drafting process can comprehensively balance the control of each process parameter, and the production efficiency is high. Low energy consumption, which reduces production costs.
- the invention adopts the three-bath wet spinning technology, the coagulation bath adopts low acid and high salt, the reaction condition is mild, and the viscose is formed into a tow after the spinning and drawing process, thereby ensuring multiple reactions of the fiber.
- the viscose fiber of the present invention has a secondary reaction interface different from that of ordinary viscose fiber and modal fiber. It should be noted that the secondary reaction interface is formed according to the difference in fiber dyeing ability of the fiber cross section, that is, the cortex of the fiber and The core layer and the skin layer have small color absorption ability and dyeing, and the core layer has a large color absorption ability for the dye, the color is deep, and the skin layer has a high degree of orientation.
- the more the skin layer, the higher the breaking strength, and the more the core layer The water swelling degree is higher; the fiber of the present invention is dyed and then subjected to fiber slicing, and the fiber slice of the viscose fiber according to the present invention exhibits a clear and obvious cross-sectional area of the secondary reaction microscope, and the "area" of the core layer and the skin layer.
- the ratio is (40-70): (30-60), the ratio is moderate, and the ratio of the "area" of the core layer and the cortex of ordinary viscose fiber is (90-95): (5-10), the ratio is biased to the inner layer, so Viscose fiber and ordinary viscose fiber of the invention Compared with high strength and low elongation, it also has proper water absorption, and fiber skin-friendliness has obvious advantages.
- the viscose fiber of the invention After modal fiber dyeing, it is made into fiber section, observed under microscope, no secondary reaction interface, and the adhesive of the invention
- the fiber and the modal fiber under the same dyeing condition, the viscose fiber of the invention has a darker color absorption than the modal, the dyeing rate is higher, the uniformity is better, and the color fastness of the finished product is good.
- the present invention proceeds from the process technology to improve the acid bath process, such as reducing the sulfuric acid concentration, slow reaction, and increasing the thickness of the skin layer;
- the viscose index such as viscose ripeness, nail fiber content, alkali content and the like, are changed to ensure high breaking strength of the viscose fiber of the present invention.
- the alkali cellulose hemicellulose content obtained by the invention is low, and is controlled within 10 g/L.
- hemicellulose refers to a polymerization degree of 50-200.
- ⁇ cellulose and ⁇ cellulose with a degree of polymerization ⁇ 50 the effect of hemicellulose is as follows: a. affecting the uniformity of alkali cellulose; b. prolonging the age of the old; c. yellowing of hemicellulose The speed is faster than that of the fiber, and a certain amount of carbon disulfide is consumed, resulting in a decrease in alkali cellulose esterification and a decrease in the solubility of the sulfonate; d.
- the metal ions in the carboxyl group and the ash such as: ferrous ion, manganese ion, calcium ion, magnesium ion, form a highly viscous complex, which leads to difficulty in filtering the viscose and low yield; e. the more hemicellulose, the viscose The poorer the physical and mechanical properties of the fiber.
- the invention can grind the porridge fed into the press in advance by a grinding machine, and the grinding time is 10-40 s.
- the milled porridge After the milled porridge is pressed by a press, the mixed lye and alkali cellulose are separated and mixed.
- the lye contains hemicellulose and other impurities, and is crushed by a pulverizer.
- the multiple of the pressing is 2.2 to 2.8, and the pulverization degree is 120-180 g/L.
- the reaction performance of the porridge is improved to ensure the production of viscose fiber. Smooth progress.
- the pulp raw material used in the present invention may be selected from any one or a mixture of two or more of cotton pulp, bamboo pulp, wood pulp and hemp pulp, and may be prepared in any ratio, and the raw material range is applicable widely, and the technical requirements are relatively prepared. Lower, lower raw material costs.
- the lye is a sodium hydroxide solution having a concentration of 110 to 240 g/L, the temperature of the immersion alkali solution is 30 to 60 ° C, and the immersion time is 50 to 90 minutes.
- the pressing and filtration can be smoothly carried out; if the concentration of lye is too high, the solubility of the obtained cellulose sulfonate will decrease, the filtration of the viscose will be difficult; the concentration of the lye is too low, the pulping degree of the pulp is too high, and the pressing Difficult; the temperature is too high, cellulose depolymerization is fast, accelerate the side reaction, affect the viscose filtration; the temperature is too low, the pulp has a high degree of puffing and the pressing is difficult.
- the invention adopts multi-stage purification, such as grinding, pressing and pulverizing, mashing, lye step utilization, for example, adding lye before and after the immersion stage, respectively, not only mentioning the cellulose-bound alkali content, but also increasing the alkali
- the purpose of the comprehensive utilization of the liquid, at the same time, can also effectively reduce the input cost of the auxiliary lye and reduce the production cost of the viscose fiber.
- the invention can obtain alkali cellulose having a fiber content of 29 to 31% and an alkali content of 15 to 17% after grinding and pressing, and the alkali cellulose can be directly fed into the viscose fiber after being subjected to hydrazine oxidation and polycondensation.
- Production system, viscose fiber production process can be carried out by conventional techniques, such as yellowing to obtain viscose, then filtered, matured, defoamed, and spun to obtain viscose fiber.
- the alkali cellulose fiber is treated by a twin-screw equipment to separate the fibers, thereby decomposing the fibers, thereby breaking the cell wall of the cellulose fibers, removing small molecules in the cellulose, thereby increasing the cellulose.
- the reaction performance improves the cellulose-bound alkali content to 6 to 8% by mass.
- the F-step directional depolymerization of the present invention the alkali cellulose obtained in the step D is mixed with the lye having a concentration of 140-200 g/L to form a porridge having a concentration of 4 to 8%, and the porridge is transported to the directional drop.
- the polyreactor has a reaction time of 30 to 60 min. After depolymerization, the degree of polymerization of alkali cellulose is reduced from 650 to 1200 to 400 to 600, and the purity of the fiber is 98.0 to 98.5%, which is 2 to 3% higher than the conventional process.
- the directional depolymerization reduces the loss of the fiber by 3 to 5% compared with the conventional aging, improves the utilization rate of raw materials, saves the production cost, and the molecular degradation is more uniform, sufficient and effective.
- the drafting process of the present invention adopts a step-by-step high drafting technique, a drawing ratio of 50 to 100%, a high draft, a high number of filaments, a low draft, and a low strength; and a second draft ratio. 40 ⁇ 60%; three drafting rate is 5 ⁇ 15%, the drafting is too high, the wool is much, the drafting is too low, the strength is decreased, and the brittleness of the fiber is improved and the fiber strength is improved by the reasonable drafting rate control. And reduce the amount of wool, improving the appearance of the product.
- the desulfurizing agent composed of sodium sulfide and sodium carbonate in the desulfurization process of the present invention is milder than the sodium hydroxide and sodium sulfite currently used, and can reduce the damage of the strength and elongation of the fiber product, and the sodium carbonate can be neutralized.
- the tow brought from the acid bath to the sulfuric acid, after the desulfurization process, can be adjusted The pH of the tow is between 8 and 11.
- the bleaching agent used in the invention is mild, and the hydrogen peroxide bleaching agent is milder than the bleaching agent such as sodium hypochlorite.
- the pH of the viscose fiber prepared by the invention should be controlled within the range of 6.5 to 7, and can also be washed with water and palatable acid. The pH is adjusted in the manner of (organic acid), within which the strength of the finished viscose fiber is not affected and the elongation is high.
- the invention has reasonable design, comprehensively reduces the production cost of viscose fiber products in the production process of the same viscose fiber product, comprehensively selects the above raw materials, and improves the production cost of the viscose fiber product, and the price thereof is compared with the modal fiber phase.
- the ratio is 4,000-5,000 yuan/ton, which can greatly reduce the cost of downstream raw materials. It can be used in home textiles, non-woven fabrics, etc., especially underwear, masks, wet wipes, etc., bringing higher profits to downstream enterprises such as spinning and weaving. The added value and broad market prospects significantly enhance the market competitiveness of enterprises.
- Figure 1 is a cross section of a fiber section of the matte type high strength low stretch viscose fiber of the present invention
- Figure 2 is a cross section of a fiber section of Modal
- Figure 3 is a cross-section of a fiber section of Tencel.
- Fiber raw materials such as Tencel, Modal, copper ammonia fiber and viscose fiber are bio-based fiber raw materials regenerated from natural cellulose materials.
- viscose fiber has the highest market share, but with recent years The scale of viscose fiber of ordinary varieties has expanded rapidly, the supply of raw materials has been tight, and the development of downstream new textiles and industrial upgrading have been gradually restricted.
- a series of differential viscose fibers are exemplified by patent documents CN102296373A, CN1632189 and CN102251301A. It is proposed that the disclosed patented technology can be realized by changing the production process, but for the increasingly fierce market competition, the differentiated viscose fiber is not bigger.
- the limit meets the development and industrial upgrading of downstream new textiles, especially the development of fiber materials such as Tencel, Modal, and Cuminous fiber, which are also recycled from natural cellulose materials, which makes the market share of viscose fiber decrease.
- the present invention proposes a high-strength low-stretch viscose fiber which has high-strength, low-stretch product characteristics and high absorption characteristics, and the skin-friendly property of the product is far superior to that of modal fiber. Better than cotton fiber.
- the high-strength low-stretch viscose fiber of the invention maintains a unique fiber structure during the fiber formation process, and has the characteristics of high strength, and the dry breaking strength and the wet breaking strength are improved by about 25% compared with the ordinary viscose fiber. It is also obviously different from the differentiated viscose fiber.
- the product index of high strength and low elongation viscose fiber meets: fineness 0.88 ⁇ 1.67dtex, dry breaking strength ⁇ 3.10cN/dtex, wet breaking strength ⁇ 1.60 cN/dtex, and the differentiated viscose fiber is exemplified by the patent documents CN102296373A, CN1632189, CN102251301A, and its product specifications are as follows: CN102296373A satisfies the fineness of 0.44 ⁇ 0.78dtex, dry breaking strength ⁇ 3.10cN/dtex, wet breaking strength ⁇ 2.1cN /dtex;CN1632189 meets the fineness of 0.90 ⁇ 1.40dtex, dry rupture strength ⁇ 2.50cN/dtex, wet rupture strength ⁇ 1.20cN/dtex; CN102251301A meets the fineness of 1.11dtex, strength ⁇ 2.9cN/dtex, as can be seen from the above indicators, this The fiber strength of the high-strength low
- the high-strength low-stretch viscose fiber according to the present invention is separately compared with the modal fiber and the tencel, and the comparison manner is as follows:
- the high-strength low-stretch viscose fiber, the modal fiber, and the tencel were respectively dyed and then subjected to fiber slicing, and the fiber sections were observed under a microscope for 2000 times, as shown in Figs. 1 to 3, and Fig. 1 is a high-strength and low-stretching adhesive of the present invention.
- the cortex is shallow, the core layer is obviously deep, and there is a clear secondary reaction interface, and the proportion is moderate, which ensures that the product has the characteristics of high strength and low elongation, and also has appropriate water absorption, and the fiber skin-friendly property has significant advantages.
- the core layer the "area" ratio of the skin layer is 40 to 70:30 to 60.
- Figure 2 is a cross-sectional view of the fiber section of the modal fiber. As shown in Fig. 2, after the dyeing of the modal fiber, the color of the fiber skin layer and the core layer are deep and shallow, and there is no obvious secondary interface. The product features enhance the fiber. Hydrophobic, poor water absorption, which makes it less skin-friendly.
- Figure 3 is a cross-sectional view of the fiber section of Tencel. As shown in Figure 3, after the dyeing process, the fiber skin layer and the core layer are dark and light in color, and there is no obvious secondary interface. The product features both common types.
- the viscose fiber has the advantages of excellent hygroscopicity, smoothness and smoothness, and comfort. It overcomes the defects of ordinary viscose fiber, such as low strength, especially low wet strength. Its strength is almost similar to that of polyester.
- the strength required to produce 5% elongation in wet state is ⁇ 0.55 cN/dtex
- the dry elongation at break is 11.0 to 19.0%, and the wet elongation at break is 16.0 to 21.0%.
- the matting agent content is 0.8-5%, the whiteness is ⁇ 85%, and the radial water swelling degree is 22-26%.
- the linear density deviation rate is ⁇ 11.0%, and the residual sulfur is ⁇ 12.0mg/100g.
- the length deviation rate is ⁇ 11.0%, and the ultra-long fiber rate is ⁇ 0.5%.
- the above indicators are applicable to the determination of high strength and low elongation viscose fiber with a linear density ranging from 0.8 dtex to 1.67 dtex.
- the method for determining the dry rupture strength is GB/T 14337, and the method for determining the wet rupture strength is GB/T 14337.
- the strength required to produce 5% elongation is achieved by GB/T14337.
- the method for determining the dry elongation at break is GB/T 14337.
- the method for determining the wet elongation at break is GB/T 14337.
- the method for determining the rate is GB/T 14335
- the method for determining residual sulfur is FZ/T 50014
- the method for measuring the length deviation rate is GB/T 14336
- the method for measuring the ultra-long fiber ratio is GB/T 14336, which is a long fiber.
- the measurement method is GB/T 14336
- the measurement method of the defect is GB/T 14339
- the measurement method of whiteness is FZ/T 50013
- the measurement method of radial water swelling degree is GB/T 6503.
- the high-strength low-stretch viscose fiber according to the embodiment is sequentially impregnated, ground, pressed, pulverized, depolymerized, yellowed, dissolved, filtered, defoamed, matured, spun drawn and post-treated from pulp raw materials. And obtained, determined that the high-strength low-stretch viscose fiber meets:
- the strength required to produce 5% elongation in wet state is ⁇ 0.55 cN/dtex
- Dry elongation at break is 11.0 to 19.0%
- the matting agent content is 0.8 to 5%.
- the high-strength low-stretch viscose fiber according to the embodiment also satisfies:
- Double fiber ⁇ 4.0mg/100g
- the defect point is ⁇ 4.0mg/100g.
- a method for preparing a matting type high-strength low-stretch viscose fiber the steps are as follows:
- the purpose is to open and disperse the fiber by mechanical action, thereby increasing the alkalization speed and alkalization rate of the cellulose;
- step B The porridge obtained in step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 30% after the treatment.
- the press can remove excess lye, and the excess lye can be recycled.
- the treatment method is to remove excess hemicellulose from the lye by using a filter with a mesh size of 60 mesh and a vacuum of -0.4 MPa.
- Alkali cellulose the use of twin-screw equipment, the fiber can be divided into filaments, deuterated, to break the cell wall of cellulose fibers, remove small molecules in cellulose, thereby improving the cellulose reaction performance, increasing the cellulose-bound alkali content , reaching 6%;
- the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 400 and a purity of the corn fiber of 98.0% is obtained.
- the purpose of adding pure oxygen is oxidative depolymerization.
- step C The alkali cellulose obtained in step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent to obtain a concentration of 9.0% cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is cotton pulp.
- a method for preparing a matting type high-strength low-stretch viscose fiber the steps are as follows:
- the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 3.5%;
- step B The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 32% after the treatment. ;
- step C The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 450 and a purity of 98.5% of the methyl fiber is obtained;
- step D The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 10.0. % cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, the mixing ratio is 3:2:1:1; the alkali liquid is sodium hydroxide, The concentration was 120 g/L, the immersion temperature was 35 ° C, and the immersion time was 65 min.
- the grinding machine was placed in a pipe connecting the dip tank and the press. The temperature of the porridge after grinding was 35 ° C, and the grinding time was 35 s.
- the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
- step B The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 35% after the treatment. ;
- step C The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 500 and a purity of the fiber of 98.2% is obtained;
- step D The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.5. % cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is a mixture of wood pulp and hemp pulp, the mixing ratio is 3:1, and the degree of polymerization is 1000.
- the alkali solution is sodium hydroxide
- the concentration is 110 g/L
- the immersion temperature is 30 ° C
- the immersion time is 50 min.
- a method for preparing a matting type high-strength low-stretch viscose fiber the steps are as follows:
- the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
- step B The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 38% after the treatment. ;
- the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 550 and a purity of 98.3% of the methyl fiber is obtained;
- step D The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.6. % cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is a mixture of bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 900, the mixing ratio is 3:1:1; the alkali liquid is sodium hydroxide, and the concentration thereof is 240 g/L.
- the immersion temperature is 60 ° C and the immersion time is 90 min; the grinding machine is arranged in a pipe connecting the dip tank and the press, and the temperature of the porridge after grinding is 30 ° C, and the grinding time is 10 s.
- a method for preparing matt high-strength low-stretch viscose fiber the steps are as follows
- the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 6%;
- step B The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 40% after the treatment. ;
- the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor to obtain an alkali cellulose having a degree of polymerization of 600 and a purity of 98.5%.
- step D The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 10.0. % cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is bamboo pulp
- the degree of polymerization is 800.
- the alkali liquid is sodium hydroxide
- the concentration is 200 g/L
- the immersion temperature is 40 ° C
- the immersion time is 60 min
- the grinding machine is arranged in a pipe connecting the dipping bucket and the press, The temperature of the porridge after grinding was 60 ° C, and the grinding time was 40 s.
- the pressing temperature of the press was 57 ° C
- the pressing ratio was 2.2 times
- the pulverizing degree of the pulverizer was 120 g / L.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1200, and the mixing ratio is 2:3:1:1;
- the press had a press temperature of 63 ° C and a press multiple of 2.8.
- step C the lye is a sodium hydroxide solution having a concentration of 140 g/L, and the amount of pure oxygen in the reactor is 2%, and the polymerization reaction time is Controlled at 30min.
- a method for preparing a matt high-strength low-stretch viscose fiber comprising the following steps:
- the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
- step B The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 32% after the treatment. ;
- the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 600 and a purity of the corn fiber of 98.0% is obtained;
- step D The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.6. % cellulose sulfonate solution;
- step E After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, the mixing ratio is 3:2:1:1; the alkali liquid is sodium hydroxide, The concentration is 180g / L, the immersion temperature is 50 ° C, the immersion time is 55min; the grinding machine is arranged in the pipe connecting the dipping bucket and the press, the temperature of the porridge after grinding is 45 ° C, the grinding time is 20 s;
- the pressing temperature of the press is 60 ° C, the pressing multiple is 2.6 times, the pulverization degree of the pulverizer is 160 g / L;
- the alkali liquid is sodium hydroxide having a concentration of 200 g / L
- the solution, the pure oxygen in the reactor was added in an amount of 10%, and the depolymerization reaction time was controlled at 60 min.
- the amount of carbon disulfide added is 25% of the content of the methyl fiber in the alkali cellulose obtained in the step B; the yellowing reaction time is controlled at 45 minutes, and the yellowing reaction temperature is 20 ° C.
- the dissolution is carried out by mixing, stirring and grinding the cellulose sulfonate with a solvent comprising a sodium sulfite solution having a concentration of 25 g/L sodium hydroxide solution and a concentration of 5 g/L, and the dissolution temperature is 10 ° C.
- the dissolution time is 30 min.
- the lye is a sodium hydroxide solution having a concentration of 140 g/L
- the amount of pure oxygen in the reactor is 5%
- the depolymerization reaction time is controlled at 45 min. .
- the amount of carbon disulfide added is 37% of the content of the methyl fiber in the alkali cellulose obtained in the step B; the yellowing reaction time is controlled at 50 min, and the yellowing reaction temperature is 30 ° C.
- the solution is to mix, stir and grind the cellulose sulfonate with a solvent comprising a sodium sulfite solution having a concentration of 45 g/L sodium hydroxide solution and a concentration of 10 g/L, and the dissolution temperature is 20 ° C.
- the dissolution time is 50 min.
- the alkali liquid is a sodium hydroxide solution having a concentration of 160 g/L
- the carbon disulfide is added in the amount of the alkali cellulose obtained in the step B. 30% of the fiber content
- the yellowing reaction time is controlled at 48 minutes, and the yellowing reaction temperature is 26 ° C.
- the dissolution is mixing, stirring and grinding the cellulose sulfonate with a solvent, and the solvent includes
- the concentration was 30 g/L sodium hydroxide solution and a sodium sulfite aqueous solution having a concentration of 8 g/L.
- the dissolution temperature was 15 ° C and the dissolution time was 44 min.
- titanium dioxide is used as a matting agent.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1000, and the mixing ratio is 4:2:1:1.
- step E the specific steps of the spinning draft are as follows:
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified.
- the bath comprises 90 g/L of sulfuric acid, 220 g/L of sodium sulfate and 8 g/L of zinc sulfate;
- the alkali solution is a sodium hydroxide solution having a concentration of 190 g/L
- the amount of pure oxygen in the reactor is 3%
- the depolymerization reaction time is controlled at 50 min. .
- step E the specific steps of the spinning draft are as follows:
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified.
- the bath comprises 120 g/L of sulfuric acid, 280 g/L of sodium sulfate and 15 g/L of zinc sulfate;
- the one bath temperature is 40 ° C
- the two bath temperature is 80 ° C
- the three bath temperature is 80 ° C.
- the post-process includes desulfurization, bleaching and oiling, and the desulfurizing agent used in the desulfurization has a concentration of 4 g/L of sodium sulfide and a concentration of 4 g/L.
- the sodium carbonate composition is used; the bleaching agent used for the bleaching is hydrogen peroxide at a concentration of 0.3 g/L; the oil used for the oiling is added in an amount of 7 g/L, and the pH of the tow after oiling is 6.5.
- the spinning drafting steps are as follows:
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified.
- the bath comprises 100 g/L of sulfuric acid, 250 g/L of sodium sulfate and 10 g/L of zinc sulfate;
- the one bath temperature was 50 ° C
- the two bath temperature was 85 ° C
- the three bath temperature was 80 ° C.
- the difference between this embodiment and the embodiment 12 is that in the spinning drafting step, the bath temperature is 44 ° C, the two bath temperature is 90 ° C, and the three bath temperature is 90 ° C; the desulfurization is used.
- the desulfurizing agent is composed of sodium sulfide having a concentration of 8 g/L and sodium carbonate having a concentration of 1 g/L; the bleaching agent used for the bleaching is hydrogen peroxide at a concentration of 0.6 g/L; and the amount of the oil used for the oiling is 9 g.
- the pH of the tow after oiling is 7; the desulfurization temperature is 50 ° C, the desulfurization time is 3 min; the bleaching temperature is 50 ° C, the bleaching time is 2 min; the temperature of the oil agent is 50 °C.
- a method for preparing a matt high-strength low-stretch viscose fiber comprising the following steps:
- the pulp raw material is immersed in a dipping bucket containing a lye, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, and the mixing ratio is 3:2: 1:1; the concentration of the lye is 180g / L, the temperature is 50 ° C, the immersion time is 55min; after immersion, grinding by a grinder, the grinding time is 20s, after grinding, the slurry is prepared at a concentration of 4% and a temperature of 45 ° C Porridge
- the porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, and the pulverization degree is 120 g/L to obtain alkali cellulose.
- the alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 35% is obtained;
- step C The porridge obtained in the step B is mixed with the lye having a concentration of 190 g/L and sent to the reactor, and 2% pure oxygen is added to the reactor, and the degree of polymerization is 450, and the purity of the fiber is obtained after 50 minutes of depolymerization. 98.1% alkali cellulose;
- the alkali cellulose obtained in the step C is sent to a yellowing machine, and 35% of carbon disulfide in the alkali cellulose obtained in the step B is added to the yellowing machine, and after being yellowed at 20 ° C for 45 minutes,
- the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 25 g/L and an aqueous solution of sodium sulfite having a concentration of 5 g/L, the dissolution temperature is 10 ° C, and the dissolution time is 30 min. , obtaining a cellulose sulfonate solution having a concentration of 9.5%;
- step E after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 42 ° C, the coagulation bath used comprises 120 g / L of sulfuric acid, 280 g / L of sodium sulfate and 15 g / L of zinc sulfate;
- the post treatment of this example includes desulfurization, bleaching, and oiling and drying.
- the desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 5 g/L and sodium carbonate having a concentration of 2 g/L, the desulfurization temperature is 55 ° C, the desulfurization time is 3 min; and the bleaching agent used for the bleaching is a concentration of 0.5 g.
- a method for preparing a matt high-strength low-stretch viscose fiber comprising the following steps:
- the pulp raw material is immersed in an immersion tank containing an alkali solution, the concentration of the alkali liquid is 120 g/L, the temperature is 40 ° C, and the immersion time is 60 min; after immersion, it is ground by a grinder, and the grinding time is 15 s, after grinding Preparing a porridge having a concentration of 4% and a temperature of 45 ° C;
- the porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, and the pulverization degree is 180 g/L to obtain alkali cellulose.
- the alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 32% is obtained;
- step C The porridge obtained in the step B is mixed with the lye having a concentration of 150 g/L, and then sent to the reactor, 10% pure oxygen is added to the reactor, and the degree of polymerization is 600, and the purity of the fiber is obtained after 40 minutes of depolymerization. 98% alkali cellulose;
- the alkali cellulose obtained in the step C is sent to a yellowing machine, and 32% of the carbon fiber content of the alkali fiber in the alkali cellulose obtained in the step B is added to the yellowing machine, and after 48 minutes of yellowing at 26 ° C,
- the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 35 g/L and an aqueous solution of sodium sulfite having a concentration of 8 g/L, the dissolution temperature is 15 ° C, and the dissolution time is 40 min. , obtaining a cellulose sulfonate solution having a concentration of 9.6%;
- step E after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 40 ° C, the coagulation bath used comprises 120 g / L of sulfuric acid, 280 g / L of sodium sulfate and 15 g / L of zinc sulfate;
- the post treatment of this example includes desulfurization, bleaching, and oiling and drying.
- the desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 6 g/L and sodium carbonate having a concentration of 3 g/L, the desulfurization temperature is 52 ° C, the desulfurization time is 2.5 min; and the bleaching agent used for the bleaching is a concentration of 0.5.
- bleaching temperature is 50 ° C, bleaching time is 2 min; the oil used in the oiling is 9 g / L, the pH of the tow after oiling is 7, the temperature of the oil is 53 ° C
- the post-treatment drying is to perform desulfurization, bleaching and tow obtained after spinning the tow, and the tow obtained after oiling is dried by a dryer, the drying temperature is 75 ° C, and after drying, Matte type high strength low stretch viscose fiber products.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1200, and the mixing ratio is 1:2:4:1.
- a method for preparing a matt high-strength low-stretch viscose fiber comprising the following steps:
- the pulp raw material is immersed in an immersion tank containing an alkali solution, the concentration of the alkali liquid is 120 g/L, the temperature is 40 ° C, and the immersion time is 60 min; after immersion, it is ground by a grinder, and the grinding time is 15 s, after grinding Preparing a porridge having a concentration of 4% and a temperature of 45 ° C;
- the porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, the pulverization degree is 130 g/L, and alkali cellulose is obtained.
- the alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 35% is obtained;
- step C The porridge obtained in the step B is mixed with the lye having a concentration of 150 g/L and sent to the reactor, and 5% pure oxygen is added to the reactor, and the degree of polymerization is 450, and the purity of the fiber is obtained after 40 minutes of depolymerization. 98.1% alkali cellulose;
- the alkali cellulose obtained in the step C is sent to a yellowing machine, and 35% of carbon disulfide in the alkali cellulose obtained in the step B is added to the yellowing machine, and after being yellowed at 26 ° C for 48 minutes,
- the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 35 g/L and an aqueous solution of sodium sulfite having a concentration of 8 g/L, the dissolution temperature is 15 ° C, and the dissolution time is 40 min. , obtaining a cellulose sulfonate solution having a concentration of 9.5%;
- step E after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
- the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 42 ° C, the coagulation bath used comprises 100 g / L of sulfuric acid, 230 g / L of sodium sulfate and 10 g / L of zinc sulfate;
- the post treatment of this example includes desulfurization, bleaching, and oiling and drying.
- the desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 5 g/L and sodium carbonate having a concentration of 2 g/L, the desulfurization temperature is 55 ° C, the desulfurization time is 2 min; and the bleaching agent used for the bleaching is a concentration of 0.5 g.
- the post-treatment drying is obtained after desulfurization, bleaching and oiling of the tow formed by the spinning drafting.
- the tow is dried by a dryer, and the drying temperature is 95 ° C. After drying, a matt high-strength low-stretch viscose fiber product is obtained.
- the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 650, and the mixing ratio is 1:1:2:1.
- the viscose fibers obtained in Examples 3 to 18 were tested, and the index statistics were as follows, wherein Examples 3 to 10 are shown in Table 1, Examples 11 to 18 are shown in Table 2, and the index values of the viscose fibers of Examples 3 to 18 were taken.
- the average value and the average value are compared with the test indexes of the modal fiber, the differentiated viscose fiber (CN102296373A comparison document 1, CN1632189 comparison document 2, CN102251301A comparison document 3) and ordinary viscose fiber, respectively, as shown in Table 3.
- the viscose fiber products prepared in Examples 4, 5 and 6 are mainly used in the field of compact siro spinning, producing sorghum and high count yarn products, and are suitable for sorghum, etc. with high product strength.
- the field demand is characterized; the viscose fiber products obtained by the preparation of the examples 10, 11, 12, 13, 14, 15, 16, 17, 18 are mainly used in the production of underwear and high-grade woven fabrics, and the products are silky and soft to the touch.
- the comfort and skin-friendly, as well as the dimensional stability of the finished fabric are good;
- the viscose fiber products prepared in Examples 8, 9, and 10 are mainly used in the field of denim fabric, and are characterized by being bright, soft, and characterized by a small variation of the finished fabric. .
- the matte type high-strength low-stretch viscose fiber product prepared in Examples 3 to 18 was arbitrarily selected, and as shown in Example 16, the fiber section was subjected to microscopic screenshots, and it was found that the cross section retained clear reaction traces and the fiber cortex
- the color of the core layer shows a shallow and deep difference, the skin layer is obviously shallow, and the core layer is deep.
- (Inner layer + middle layer): The ratio of the "area" of the outer layer is 60:37, belonging to the core layer: cortex (40 to 70): Within the range of (30 to 60).
- the high-strength low-stretch viscose fiber of the present invention has an index system different from ordinary viscose fiber, differentiated viscose fiber and modal fiber, and the dry breaking strength and wet breaking strength of the viscose fiber of the present invention. It is obviously higher than ordinary viscose fiber, and the elongation is obviously lower than that of ordinary viscose fiber.
- the viscose fiber of the invention has obvious secondary reaction interface, thereby ensuring high strength and low elongation equivalent to modal.
- the characteristic is that the radial water swelling degree is higher than that of the modal fiber, and has higher hygroscopicity than the modal, so the skin-friendly property is better than the modal fiber;
- the viscose fiber of the invention is a novel viscose fiber capable of It effectively replaces existing modal fibers and ordinary viscose fibers, and has lower production cost and good economic and social benefits.
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Abstract
The present invention relates to the technical field of textile fiber processing. Disclosed is a matte high-strength, low-stretch viscose fiber. he viscose fiber is produced from a pulp raw material that sequentially undergoes impregnation, grinding, pressing and crushing, rubbing, degradation, xanthation, dissolution, filtration, defoaming, aging, spinning and drafting, and aftertreatment. The viscose fiber of the present invention has the following technical indicators: dry tensile strength ≥ 3.10 cN/dtex, wet tensile strength ≥ 1.60 cN/dtex, strength required to produce 5% elongation in a wet state ≥ 0.55 cN/dtex, dry breaking elongation 11.0-19.0%, wet breaking elongation 16.0-21.0%, radial water swelling capacity 22-26%, and matting agent content 0.8-5%. The viscose fiber of the present invention is a novel viscose fiber and has lower production costs compared with an existing modal, thus providing great economic and social benefits.
Description
本发明涉及粘胶纤维及制备,尤其涉及一种消光型高强低伸粘胶纤维及其制备方法,属于纺织纤维加工技术领域。The invention relates to viscose fiber and preparation thereof, in particular to a matting type high-strength low-stretch viscose fiber and a preparation method thereof, and belongs to the technical field of textile fiber processing.
目前纺织纤维原料主要分为以棉、麻等为代表的天然纤维原料,以涤纶、腈纶等为代表的石油基纤维原料,以及以天然纤维素材料为原料再生而成的粘胶纤维等生物基纤维原料。目前,随着土地资源的稀缺及人力资源的紧张,棉花种植面积呈逐年下降趋势,棉花产品将不能满足人们生活水平日益增长的需要;而随着石油储量的日渐减少和人们对纺织品舒适性、功能性、环保型意识的不断增强,以可再生性资源为原料生产的粘胶纤维越来越多的受到重视。对于粘胶纤维而言,作为天然再生纤维,它既有天然纤维的品质,又具有优良的可加工性,其结构组成与棉相似,不仅具有吸湿性高、透气性好、穿着舒适、易染色、耐高温性强等多种特性,同时,又具有棉花所没有的悬垂性和柔软性,当然,由于粘胶纤维具备的这些优异性能,近年来发展十分迅速,特别是普通品种的粘胶纤维规模正在急剧的膨胀,这一现象造成了原材料供应紧张,市场恶性竞争激烈,与此同时,更限制了下游新型纺织品的开发和产业升级。At present, textile fiber raw materials are mainly classified into natural fiber raw materials represented by cotton and hemp, petroleum-based fiber raw materials represented by polyester and acrylic fibers, and bio-based materials such as viscose fiber which is regenerated from natural cellulose materials. Fiber raw materials. At present, with the scarcity of land resources and the shortage of human resources, the cotton planting area is declining year by year, and cotton products will not meet the growing needs of people's living standards. With the decreasing oil reserves and people's comfort for textiles, Functional and environmentally conscious awareness continues to increase, and viscose fibers produced from renewable resources are increasingly valued. As viscose fiber, as a natural recycled fiber, it has both natural fiber quality and excellent processability. Its structural composition is similar to that of cotton. It has high hygroscopicity, good gas permeability, comfortable wearing and easy dyeing. High temperature resistance and other characteristics, at the same time, it has the drape and softness that cotton does not have. Of course, due to these excellent properties of viscose fiber, it has developed very rapidly in recent years, especially the viscose fiber of common varieties. The scale is exploding rapidly. This phenomenon has caused a tight supply of raw materials and fierce competition in the market. At the same time, it has restricted the development of new downstream textiles and industrial upgrading.
基于上述情况,为促进粘胶纤维行业的持续发展,生产差别化、功能化的粘胶纤维已成为目前行业新标。专利文献CN102296373A(一种超细高强高模粘胶纤维的生产方法,2011.12.28)公开了一种结构均匀、纤维强度和模量高出常规品种50%以上的一种粘胶纤维,制得的粘胶纤维的纤维强度为0.44~0.78dtex、干强≥3.1cN/dtex(厘牛/分特)、湿强≥2.1cN/dtex、湿模量≥0.5cN/dtex、白度≥82.0%。Based on the above situation, in order to promote the sustainable development of the viscose fiber industry, the production of differentiated and functional viscose fiber has become a new standard in the industry. Patent document CN102296373A (a method for producing ultra-fine high-strength high-mode viscose fiber, 2011.12.28) discloses a viscose fiber having a uniform structure, a fiber strength and a modulus higher than that of a conventional variety of 50% or more. The viscose fiber has a fiber strength of 0.44 to 0.78 dtex, a dry strength of ≥3.1 cN/dtex (centimeter/denier), a wet strength of ≥2.1 cN/dtex, a wet modulus of ≥0.5 cN/dtex, and a whiteness of ≥82.0%. .
专利文献CN1632189(一种高白强力细旦粘胶短纤维及其生产工艺,2005.06.29)公开了一种纤度细、强度高的粘胶短纤,由其加工的服装面料较普通粘胶纤维而言具有强度高、耐磨性强、手感细腻、抗褶皱性、耐多次变形等优点,还可用于纺织高支纱织制品。Patent document CN1632189 (a high-white strong fine-density viscose staple fiber and its production process, 2005.06.29) discloses a fine-density, high-strength viscose staple fiber, which is processed by an ordinary viscose fiber. In terms of high strength, strong abrasion resistance, fine hand feeling, anti-pleatability, resistance to multiple deformations, etc., it can also be used for textile high count yarn woven products.
专利文献CN102251301A(一种超细旦高强粘胶纤维生产工艺,2011.11.23)公开了一种纤度低、强度高的粘胶纤维的制备方法,可获得纤度为1.11分特和强度大于2.9cN/dtex的粘胶纤维。Patent document CN102251301A (a superfine denier high-strength viscose fiber production process, 2011.11.23) discloses a preparation method of viscose fiber with low fineness and high strength, which can obtain a fineness of 1.11 dtex and a strength of more than 2.9 cN/ Dtex viscose fiber.
仅上述公开的专利文献可以获知,为制得差别化、功能化的粘胶纤维,现有技术均是通过改变生产工艺的方式来实现的,其中,涉及有原材料、粘胶成型及其工艺参数的改变等等,获得的粘胶纤维较普通粘胶纤维均在纤度和强度上进行了适当优化,但对于日益激烈的市场竞争来说,差别化的粘胶纤维并没有更大限度的满足下游新型纺织品的开发和产业升级,尤其是同样以天然纤维素材料为原料再生而成的天丝、莫代尔、铜氨纤维等纤维原料的发展,使得粘胶纤维的市场占有率日趋降低。如:专利文献CN101130885(麻材粘胶纤维的制备方法及制备的麻材粘胶纤维,2008.02.27)公开了一种利用麻材植物生产的粘胶纤维及其制备工艺,工艺简单,物料消耗低,而且生产的麻材粘胶纤维具有优良的白度、强度和纤维伸长等性能,通过该工艺制备获得的麻材粘胶纤维满足干断裂强度≥1.820cN/dtex,湿断裂强度≥1.12cN/dtex,干断裂伸长率≥15.4%,线密度偏差率±6.00%,长度偏差率±6.00%,超长纤维率≤1.0%,倍长纤维≤18.0mg/100g,疵点≤11mg/100g,残硫≤18.0mg/100g。It is only known from the above-disclosed patent documents that in order to produce differentiated, functionalized viscose fibers, the prior art is achieved by changing the production process, in which raw materials, viscose molding and process parameters are involved. The change of viscose fiber is better optimized in terms of fineness and strength than ordinary viscose fiber, but for the increasingly fierce market competition, the differentiated viscose fiber does not meet the downstream limit to a greater extent. The development of new textiles and industrial upgrading, especially the development of fiber materials such as Tencel, Modal, and Cuminous fiber, which are also recycled from natural cellulose materials, have led to a decline in the market share of viscose fibers. For example, the patent document CN101130885 (the preparation method of the sesame viscose fiber and the prepared sesame viscose fiber, 2008.02.27) discloses a viscose fiber produced by using a hemp material plant and a preparation process thereof, and the process is simple and the material consumption is Low, and the produced ramie viscose fiber has excellent whiteness, strength and fiber elongation. The ramie viscose fiber prepared by the process meets the dry rupture strength ≥1.820cN/dtex, and the wet rupture strength ≥1.12 cN/dtex, dry elongation at break ≥15.4%, linear density deviation rate ±6.00%, length deviation rate ±6.00%, ultra-long fiber rate ≤1.0%, long fiber ≤18.0mg/100g, defect point ≤11mg/100g , residual sulfur ≤ 18.0mg / 100g.
以莫代尔纤维为例,我们知道,莫代尔纤维是以欧洲榉木为原料,制成木质浆液后经过专门的纺丝工艺制作而成的,与棉一样同属天然纤维原料,莫代尔纤维的整个生产过程中没有任何污染,它的干强接近于涤纶,湿强要比普通粘胶纤维提高了许多,不论是光泽、柔软性、吸湿性、染色性、染色牢度均优于纯棉产品,用它所做成的面料,不仅展示了一种丝面光泽,更具有宜人的柔软触摸感觉和悬垂感以及极好的耐穿性能,是一种理想的环保型纤维素纤维。但由于莫代尔纤维纺织技术成本昂贵,市面上流通的莫代尔基本上属于莫代尔和棉混纺,或者直接拿粘胶(人棉)纤维来冒充莫代尔。Taking Modal fiber as an example, we know that Modal fiber is made from European eucalyptus wood and made into a wood slurry and then made by a special spinning process. It is the same natural fiber material as cotton, and the modal fiber is not produced in the whole production process. Any pollution, its dry strength is close to polyester, the wet strength is much higher than ordinary viscose fiber, no matter the gloss, softness, hygroscopicity, dyeing, dyeing fastness is better than pure cotton products, use it to do The finished fabric not only exhibits a silky luster, but also has a pleasant soft touch feeling and drape, as well as excellent wear resistance. It is an ideal environmentally friendly cellulose fiber. However, due to the high cost of modal fiber textile technology, the market modal modal is basically a blend of modal and cotton, or directly take the viscose (human cotton) fiber to impersonate Modal.
为此,我们需要找到一种区别于天然纤维原料和石油基纤维原料,性能又优于差别化粘胶纤维的新型粘胶纤维,不仅能满足人们对天然产品(如:莫代尔纤维)的要求,还能适用于工业化的持续生产,为企业带来较大的经济效益,当然,这也是粘胶纤维行业能持续发展的必然趋势。To this end, we need to find a new viscose fiber that is different from natural fiber raw materials and petroleum-based fiber raw materials and has better performance than differentiated viscose fiber, which not only meets the requirements of natural products (such as modal fiber). It can also be applied to the continuous production of industrialization, bringing greater economic benefits to the enterprise. Of course, this is also an inevitable trend for the viscose fiber industry to continue to develop.
发明内容Summary of the invention
本发明的目的在于提供一种消光型高强低伸粘胶纤维,该粘胶纤维有别于传统粘胶纤维产品和棉纤,是通过技术创新而实现的新型纤维品种,具有区别于普通粘胶纤维和莫代尔纤维的指标体系,其产品不仅表现出了莫代尔纤维高强、低伸的纤维特征,还表现出了较棉纤和莫代尔更好的亲肤性,能有效地替代现有莫代尔纤维,且生产成本较莫代尔低,具有良好的经济和社会效益。The object of the present invention is to provide a matting type high-strength low-stretch viscose fiber which is different from the traditional viscose fiber product and cotton fiber, and is a novel fiber type realized by technological innovation, which is different from ordinary viscose. The index system of fiber and modal fiber not only exhibits the high-strength, low-stretch fiber characteristics of modal fiber, but also exhibits better skin-friendly properties than cotton fiber and modal, and can effectively replace existing modal fiber, and Production costs are lower than Modal and have good economic and social benefits.
本发明是通过下述技术方案实现的:一种消光型高强低伸粘胶纤维,它是浆粕原料依次经浸渍、研磨、压榨粉碎、搓揉、降聚、黄化、溶解、过滤、脱泡、熟成、纺丝牵伸和后处理后得到的,所述消光型高强低伸粘胶纤维满足以下技术指标:The invention is realized by the following technical scheme: a matting type high-strength low-stretch viscose fiber, which is a slurry raw material which is sequentially impregnated, ground, pressed, crushed, smashed, depolymerized, yellowed, dissolved, filtered, taken off. After the foaming, aging, spinning drafting and post-treatment, the matting type high-strength low-stretch viscose fiber meets the following technical indexes:
干断裂强度≥3.10cN/dtex;
Dry breaking strength ≥ 3.10cN/dtex;
湿断裂强度≥1.60cN/dtex;Wet breaking strength ≥ 1.60cN / dtex;
湿状态下产生5%伸长率所需的强度≥0.55cN/dtex,The strength required to produce 5% elongation in wet state is ≥0.55 cN/dtex,
干断裂伸长率11.0~19.0%;Dry elongation at break is 11.0 to 19.0%;
湿断裂伸长率16.0~21.0%;Wet elongation at break is 16.0 to 21.0%;
径向水膨润度22~26%;Radial water swelling degree 22 to 26%;
结晶度40.0~45.0%;Crystallinity 40.0 to 45.0%;
消光剂含量0.8~5%。The matting agent content is 0.8 to 5%.
所述的浆粕原料包括棉浆、竹浆、木浆、麻浆中的一种或者两种以上的组合,在实际应用时,棉浆、竹浆、木浆、麻浆可按任意比例进行混合,原料来源广,且对甲纤含量要求不高,可有效降低原料成本。The pulp raw material comprises one or a combination of two or more of cotton pulp, bamboo pulp, wood pulp and hemp pulp. In practical application, cotton pulp, bamboo pulp, wood pulp and hemp pulp can be carried out in any ratio. Mixing, wide source of raw materials, and low requirements on the content of fiber, can effectively reduce the cost of raw materials.
所述浆粕原料的聚合度为650~1200,优点在于:针叶浆纤维长度2~3mm,强度更高。The degree of polymerization of the pulp raw material is 650 to 1200, and the advantage is that the length of the softwood pulp fiber is 2 to 3 mm, and the strength is higher.
进一步优选,所述的粘胶纤维还满足以下技术指标:Further preferably, the viscose fiber further satisfies the following technical indicators:
白度≥85%;Whiteness ≥ 85%;
线密度偏差率≤±11.0%;Linear density deviation rate ≤ ± 11.0%;
残硫≤12.0mg/100g;Residual sulfur ≤ 12.0mg / 100g;
长度偏差率≤±11.0%;Length deviation rate ≤ ± 11.0%;
超长纤维率≤0.5%;Ultra-long fiber rate ≤0.5%;
倍长纤维≤4.0mg/100g;Double fiber ≤4.0mg/100g;
疵点≤4.0mg/100g。The defect point is ≤4.0mg/100g.
本发明的另一目的在于提供一种消光型高强低伸粘胶纤维的制备方法,该制备方法以浆粕作为生产原料,通过粘胶制备、纺丝工艺和后处理后制得粘胶纤维,生产过程中,仍保留了二次反应显微镜截面积,且该界面的内外层面积比例明显区别于莫代尔纤维和普通粘胶纤维的二次反应痕迹,确保了该产品具有高强、低伸的特点,同时还具有适当的吸水性以及显著的纤维亲肤性。Another object of the present invention is to provide a method for preparing a matting type high-strength low-stretch viscose fiber, which comprises pulp as a raw material for production, viscose fiber by viscose preparation, spinning process and post-treatment, During the production process, the cross-sectional area of the secondary reaction microscope is still retained, and the ratio of the inner and outer layers of the interface is significantly different from the secondary reaction traces of the modal fiber and the ordinary viscose fiber, ensuring that the product has the characteristics of high strength and low elongation. It also has suitable water absorption and significant fiber skin-friendly properties.
所述的消光型高强低伸粘胶纤维的制备方法具体步骤如下:The specific steps of the preparation method of the matting type high-strength low-stretch viscose fiber are as follows:
A.将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为3~6%的浆粥,在实际生产时,将浆粕原料首先放在喂机粕上,设定一定的投料速度(如40kg/min)后,再加入至浸渍桶中,研磨的目的是通过机械作用对纤维进行开松和分散,从而提高纤维素的碱化速度及碱化率;A. The pulp raw material is immersed in a dipping bucket containing alkali solution, and ground by a grinder to prepare a slurry of porridge having a concentration of 3 to 6%. In actual production, the pulp raw material is first placed on the feeder. After setting a certain feeding speed (such as 40kg/min), it is added to the dip tank, and the purpose of the grinding is to open and disperse the fiber by mechanical action, thereby increasing the alkalization speed and alkalization rate of the cellulose;
B.将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为30~40%的浆粥,在该步骤中,压榨机能除去多余的碱液,多余的碱液能够回收利用,处理方式是使用滤网60~120目、真空度–0.4~–0.1MPa的过滤机去除碱液中多余的半纤维素后回收碱纤维素,揉搓机使用双螺杆设备,可使纤维分丝、帚化,达到破坏纤维素纤维细胞壁的作用,去除纤维素中的小分子,从而提高纤维素反应性能,提高纤维素结合碱含量,达到6~8%(质量百分比);B. The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a crucible, and the concentration is 30-40% after treatment. Pulp porridge, in this step, the press can remove excess lye, and the excess lye can be recycled. The treatment method is to remove the lye by using a filter with a filter of 60-120 mesh and a vacuum of -0.4 to -0.1 MPa. After the excess hemicellulose is recovered, the alkali cellulose is recovered, and the twin-screw equipment is used to make the fiber separate and smelt, thereby breaking the cell wall of the cellulose fiber, removing small molecules in the cellulose, thereby improving the cellulose reaction performance. , to increase the content of cellulose-bound alkali, reaching 6 to 8% (mass percentage);
C、将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为400~600、甲纤纯度为98.0~98.5%的碱纤维素,在该步骤中,加入纯氧的目的是氧化降聚,经降聚后,碱纤维素聚合度由650~1200降为400~600。C. The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor to obtain an alkali fiber having a degree of polymerization of 400-600 and a purity of 98.0-98.5%. In this step, the purpose of adding pure oxygen is oxidative depolymerization. After depolymerization, the degree of polymerization of alkali cellulose is reduced from 650 to 1200 to 400 to 600.
D.将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.0~10.0%的纤维素磺酸酯溶液;D. The alkali cellulose obtained in step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent to obtain a concentration of 9.0 to 10.0% cellulose sulfonate solution;
E.将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E. After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
在所述的步骤A中,所述的碱液为浓度110~240g/L的氢氧化钠溶液,浸渍碱液的温度为30~60℃,浸渍时间为50~90min。在实际使用时,碱液浓度过高,所得纤维素磺酸脂溶解度会降低,粘胶过滤困难;碱液浓度过低,浆粕原料膨化度过高,压榨困难;温度过高,纤维素降聚快,加速副反应,影响粘胶过滤;温度过低,浆粕膨化度高,压榨困难。In the above step A, the lye is a sodium hydroxide solution having a concentration of 110 to 240 g/L, the temperature of the immersion alkali solution is 30 to 60 ° C, and the immersion time is 50 to 90 minutes. In actual use, if the concentration of lye is too high, the solubility of the obtained cellulose sulfonate will decrease, and the viscosity of the viscose will be difficult to filter; the concentration of the alkali solution is too low, the degree of expansion of the pulp material is too high, and the pressing is difficult; the temperature is too high, and the cellulose is lowered. Gather quickly, accelerate side reactions, affect viscose filtration; temperature is too low, pulp pulping is high, and pressing is difficult.
为更好的实现本发明,在所述的步骤A中,所述的研磨机设于连接浸渍桶与压榨机的管道内。In order to better implement the present invention, in the step A described, the grinder is disposed in a pipe connecting the dip tank and the press.
为达到更好的碱化率,在所述的步骤A中,所述浆粥的温度为30~60℃,所述研磨机的研磨时间为10~40s。In order to achieve a better alkalization rate, in the step A, the temperature of the porridge is 30 to 60 ° C, and the grinding time of the mill is 10 to 40 s.
在粘胶纤维的制备领域,浆粥通过压榨机压榨后的物质可分为两部分,一部分是夹杂着纤维和杂质的多余碱液,另一部分是压出了多余水分的固态和液态的混合物,即碱纤维素,在所述的步骤B中,所述压榨机的压榨温度为57~63℃、压榨倍数为2.2~2.8。In the field of preparation of viscose fiber, the material pressed by the press by the press can be divided into two parts, one part is an excess alkali solution mixed with fibers and impurities, and the other part is a mixture of solid and liquid which is pressed out of excess water. That is, alkali cellulose, in the above step B, the press has a press temperature of 57 to 63 ° C and a press ratio of 2.2 to 2.8.
压榨是将浆粕经浸渍后把多余的碱液、半纤维素、杂质压出,提高碱纤维素纯度,压榨的程度用压榨倍数即用浆粕压榨后的质量和浸渍前干浆和质量之比值表示;经压榨后的碱纤维素十分紧密、板硬、表面积变小,不利于后期的加工,粉碎的目的是使碱纤维素成为细小、松散的屑状,增大了表面积,有利于后期工序加工的均匀性,粉碎程度的表示方式之一碱纤维素的定积重量,本发明中简称为粉碎度,是指碱纤维素粉碎后,单位体积的重量,一般以g/L表示,碱纤维素粉碎效果越好,则定积重量越小,其表面积越
大。Pressing is to impregnate the pulp with excess lye, hemicellulose and impurities to increase the purity of the alkali cellulose. The degree of pressing is the pressure after pressing with the pulp and the quality of the pulp and the quality of the pre-impregnated dry pulp and quality. The ratio indicates that the pressed alkali cellulose is very tight, the plate is hard, and the surface area is small, which is not conducive to the later processing. The purpose of the pulverization is to make the alkali cellulose into fine and loose scraps, which increases the surface area and is beneficial to the later stage. The uniformity of the process and the expression of the degree of pulverization, which is a fixed weight of alkali cellulose, is simply referred to as the degree of pulverization in the present invention, and refers to the weight per unit volume after pulverization of alkali cellulose, generally expressed in g/L, and alkali. The better the cellulose pulverization effect, the smaller the fixed weight and the larger the surface area.
Big.
在所述的步骤B中,浆粥经压榨后被送至粉碎机进行粉碎,所述粉碎机的粉碎度为120~180g/L,通过合理的压榨倍数和粉碎度的调整,能够提高后期加工工序中碱纤维素的性能均匀性,防止局部收到强挤压,从而阻碍了氧气进入,降低降聚步骤的速度;粉碎后获得的碱纤维素的甲纤含量为29~31%、碱含量为15~17%,碱液中半纤含量控制在10g/L以内。In the step B, the porridge is pressed and sent to a pulverizer for pulverization. The pulverization degree of the pulverizer is 120-180 g/L, and the post-processing can be improved by adjusting the pressing ratio and the pulverization degree. The uniformity of the performance of the alkali cellulose in the process prevents the local from receiving strong extrusion, thereby hindering the entry of oxygen and reducing the speed of the depolymerization step; the content of the alkali fiber obtained by the pulverization is 29 to 31%, and the alkali content It is 15 to 17%, and the content of the half fiber in the lye is controlled within 10 g/L.
进一步的,在所述的步骤C中,所述的碱液为浓度140~200g/l的氢氧化钠溶液,纯氧的加入量反应器容积的2~10%,降聚反应时间控制在30~60min。Further, in the step C, the lye is a sodium hydroxide solution having a concentration of 140 to 200 g/l, and the pure oxygen is added in an amount of 2 to 10% of the reactor volume, and the depolymerization reaction time is controlled at 30. ~60min.
在所述的步骤D中,二硫化碳的加入量为步骤B制得的碱纤维素中甲纤含量的25~37%,在实际应用时,二硫化碳加入量过少,黄化反应不完全,过滤困难;二硫化碳加入量过高,黄化反应过度,副产物较多。In the step D, the amount of carbon disulfide added is 25 to 37% of the content of the methyl cellulose in the alkali cellulose obtained in the step B. In practical application, the amount of carbon disulfide added is too small, the yellowing reaction is incomplete, and the filtration is difficult. The amount of carbon disulfide added is too high, the yellowing reaction is excessive, and the by-products are more.
进一步的,在所述的步骤D中,所述的黄化反应时间控制在45~50min,黄化反应温度为20~30℃。Further, in the step D, the yellowing reaction time is controlled at 45 to 50 minutes, and the yellowing reaction temperature is 20 to 30 °C.
进一步的,在所述的步骤D中,所述的溶解是将纤维素磺酸酯与溶剂进行混合、搅拌和研磨,所述的溶剂包括浓度为25~45g/L氢氧化钠溶液和浓度为5~10g/L的亚硫酸钠水溶液。Further, in the step D, the dissolving is mixing, stirring and grinding the cellulose sulfonate with a solvent, the solvent comprises a sodium hydroxide solution having a concentration of 25 to 45 g/L, and the concentration is 5-10 g/L aqueous sodium sulfite solution.
在所述的步骤D中,所述的溶解温度为10~20℃,溶解时间为30~50min。In the step D described, the dissolution temperature is 10 to 20 ° C, and the dissolution time is 30 to 50 minutes.
在所述的步骤D中,所述的消光剂为钛白粉。In the step D described, the matting agent is titanium dioxide.
为进一步的提高粘胶纤维的产品特性,本发明还对纺丝牵伸工艺进行了改进,包括低酸高盐缓和酸浴工艺和高拉伸纺塑工艺等,具体表现在,所述的纺丝牵伸步骤如下:In order to further improve the product characteristics of the viscose fiber, the present invention also improves the spinning drafting process, including a low acid and high salt moderate acid bath process and a high stretch spinning process, etc., specifically, the spinning The wire drawing steps are as follows:
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴使用的凝固浴包括90~120g/L的硫酸、220~280g/L的硫酸钠和8~15g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified. The bath comprises 90-120 g/L of sulfuric acid, 220-280 g/L of sodium sulfate and 8-15 g/L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴使用的凝固浴包括18~22g/L的硫酸,所述一道牵伸机的牵伸率为50~100%;G: The tow after one bath is fed into the two bath by a drafting machine, the coagulation bath used in the two baths comprises 18-22 g/L of sulfuric acid, and the drafting ratio of the one drafting machine is 50-100. %;
H:经二浴后的丝束由二道牵伸机送入三浴,所述三浴使用的凝固浴包括pH值为1~3的硫酸,所述二道牵伸机的牵伸率为40~60%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, and the coagulation bath used in the three baths includes sulfuric acid having a pH of 1 to 3, and the draft ratio of the two drafting machines is 40 to 60%;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为5~15%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 5 to 15%.
如上所述,本发明采用三浴湿法纺丝技术,粘胶经纺丝拉伸工艺后形成丝束,保证了纤维的多次反应,在此过程中,纤维截面能形成清晰的二次反应显微镜界面,具有提高纤维强度、增加纤维吸水速率及加大纤维保水性的特性,在纺丝工艺中,丝束通过一道牵伸机、二道牵伸机、三道牵伸机进行拉伸,更有利于改善纤维的脆性,使纤维的伸度得到提高。As described above, the present invention adopts the three-bath wet spinning technique, and the viscose is formed into a tow after the spinning and drawing process, thereby ensuring multiple reactions of the fiber, in which the fiber cross section can form a clear secondary reaction. The microscope interface has the characteristics of improving the fiber strength, increasing the water absorption rate of the fiber, and increasing the water retention property of the fiber. In the spinning process, the tow is stretched by a drafting machine, a two-way drafting machine, and a three-way drafting machine. It is more conducive to improving the brittleness of the fiber and improving the elongation of the fiber.
所述的后处理包括对纺丝牵伸形成的丝束进行的脱硫、漂白和上油,所述脱硫使用的脱硫剂由浓度为4~8g/L的硫化钠和浓度为1~4g/L的碳酸钠组成;所述漂白使用的漂白剂为浓度0.3~0.6g/L的双氧水;所述上油使用的油剂加入量为7~9g/L,上油后丝束的pH值为6.5~7。The post-treatment includes desulfurization, bleaching and oiling of the tow formed by the spinning draft, and the desulfurizing agent used in the desulfurization is composed of sodium sulfide having a concentration of 4 to 8 g/L and a concentration of 1 to 4 g/L. The sodium carbonate composition; the bleaching agent used for the bleaching is a hydrogen peroxide concentration of 0.3-0.6 g/L; the oiling agent used for the oiling is 7-9 g/L, and the pH of the tow after oiling is 6.5. ~7.
本发明采用温和的脱硫工艺,使产品强度、伸度的损伤减小,在实际使用时,硫化钠和碳酸钠组成的脱硫剂较现有使用的氢氧化钠、亚硫酸钠更加温和,碳酸钠能中和丝束从酸浴中带来的硫酸,脱硫工艺后,可调节丝束的pH值在8~11;双氧水漂白剂较次氯酸钠等漂白剂更加温和,本发明制备的粘胶纤维的pH值应控制在6.5~7范围内,还可通过水洗、多效酸(有机酸)的方式调节pH值,在该范围内,粘胶纤维成品的强伸度不会受到影响,强伸度高。The invention adopts a mild desulfurization process to reduce the damage of product strength and elongation. In actual use, the desulfurizing agent composed of sodium sulfide and sodium carbonate is milder than the existing sodium hydroxide and sodium sulfite, and the sodium carbonate can be used. And the sulfuric acid brought by the tow from the acid bath, after the desulfurization process, the pH of the adjustable tow is 8-11; the hydrogen peroxide bleach is milder than the bleach such as sodium hypochlorite, and the pH of the viscose fiber prepared by the invention should be The control is in the range of 6.5 to 7, and the pH value can also be adjusted by means of water washing and polyfunctional acid (organic acid). Within this range, the strength of the finished viscose fiber is not affected, and the elongation is high.
进一步的,所述的脱硫温度为50~55℃,脱硫时间为2~3min;所述的漂白温度为50~55℃,漂白时间为1~2min;所述油剂的温度为50~55℃。Further, the desulfurization temperature is 50 to 55 ° C, the desulfurization time is 2 to 3 min; the bleaching temperature is 50 to 55 ° C, the bleaching time is 1 to 2 min; and the temperature of the oil agent is 50 to 55 ° C. .
在本发明中,所述的后处理还包括烘干,所述的烘干是对纺丝牵伸形成的丝束进行的脱硫、漂白和上油后获得的丝束使用烘干机烘干,烘干温度为75~115℃,烘干后,得到高强低伸粘胶纤维产品,产品回潮率控制在11~13.5%。In the present invention, the post-treatment further includes drying, the drying is performed on the tow formed by the spinning draft, the desulfurization, bleaching and the tow obtained after the oiling are dried using a dryer. The drying temperature is 75-115 ° C. After drying, high-strength low-stretch viscose fiber products are obtained, and the moisture regain rate of the product is controlled at 11 to 13.5%.
本发明与现有技术相比,具有以下有益效果:Compared with the prior art, the invention has the following beneficial effects:
(1)本发明涉及的粘胶纤维是通过技术创新而实现的新型纤维品种,属于粘胶短纤维及纤维素纤维生产技术领域的重大创新,该粘胶纤维有别于传统粘胶纤维产品和棉纤,具有区别于普通粘胶纤维和莫代尔纤维的指标体系,纤维的强度达到3.1cN/dtex以上,比普通生物基短纤维强度高30%左右,接近于莫代尔,具有莫代尔纤维的高强度,低伸长率,可降解的特点,使得织物不易变形,还具有较棉纤、莫代尔更好的吸湿性和透气性,且手感柔软,平滑,外观亮丽,能有效地替代现有的差别化粘胶纤维,在提高粘胶纤维下游工序加工性能的同时,还能促进下游新型纺织品的开发和产业升级,具有良好的经济效益和社会效益。(1) The viscose fiber according to the present invention is a novel fiber type realized through technological innovation, and belongs to a major innovation in the production technology of viscose staple fiber and cellulose fiber, which is different from the traditional viscose fiber product and Cotton fiber, which has an index system different from ordinary viscose fiber and modal fiber, has a fiber strength of 3.1 cN/dtex or more, which is about 30% higher than that of ordinary bio-based short fiber, close to modal, and has high strength of modal fiber. Low elongation and degradable characteristics make the fabric not easy to be deformed. It also has better moisture absorption and gas permeability than cotton fiber and modal, and it is soft, smooth and bright in appearance, and can effectively replace the existing differential viscosity. Glue fiber can improve the downstream processing performance of viscose fiber, and promote the development and industrial upgrading of downstream new textiles, with good economic and social benefits.
(2)本发明的粘胶纤维与性能指标较高的莫代尔相比,成本更低,导致售价比莫代尔纤维低4000~5000元/吨,主要有以下几个方面降低了本发明粘胶纤维的生产成本:a.于本发明粘胶纤维的原材料来源广泛,要求低,可选择甲纤维素含量较低的原料(甲纤维素含量越高,价格越高),可用棉浆、竹浆、
木浆、麻浆中的一种或两种以上的组合,无比例要求;b.本发明工艺过程中,碱的用量较常规产品更低;c.本发明工艺步骤中的纺丝过程中,纺丝机的纺速为45~55m/min,比莫代尔生产过程中的30m/min更快,且优化的酸浴组成和牵伸工艺,能够做到综合平衡各个工序参数的控制,生产效率高,能耗低,从而降低生产成本。(2) The viscose fiber of the present invention has lower cost than the modal with higher performance index, and the price is lower than the modal fiber by 4000-5000 yuan/ton, and the viscose fiber of the invention is mainly reduced in the following aspects. Production cost: a. The raw material of the viscose fiber of the invention has wide source and low requirement, and the raw material with lower content of methyl cellulose can be selected (the higher the content of methyl cellulose, the higher the price), the cotton pulp, bamboo pulp,
One or a combination of two or more of wood pulp and hemp pulp, no proportion requirement; b. the amount of alkali used in the process of the invention is lower than that of conventional products; c. during the spinning process in the process step of the present invention, The spinning speed of the spinning machine is 45-55m/min, which is faster than 30m/min in the production process of Modal. The optimized acid bath composition and drafting process can comprehensively balance the control of each process parameter, and the production efficiency is high. Low energy consumption, which reduces production costs.
(3)本发明采用三浴湿法纺丝技术,凝固浴采用的是低酸高盐,反应条件温和,且粘胶经纺丝拉伸工艺后形成丝束,保证了纤维的多次反应,本发明的粘胶纤维具有与普通粘胶纤维和莫代尔纤维不同的二次反应界面,需要说明的是,二次反应界面是根据纤维横截面对染料吸色能力不同形成的,即纤维的皮层和芯层,皮层对染料吸色能力小,染色偏浅,芯层对染料吸色能力大,颜色偏深,皮层具有较高的取向度,皮层越多,断裂强度越高,而芯层越多,水膨润度越高;将本发明纤维经染色后做纤维切片,本发明涉及的粘胶纤维的纤维切片表现出了清晰、明显的二次反应显微镜截面积,芯层、皮层“面积”比例为(40~70):(30~60),比例适中,而普通粘胶纤维的芯层和皮层“面积”比例为(90~95):(5~10),比例偏内层,故本发明的粘胶纤维与普通粘胶纤维相比,具有高强、低伸的特点,同时还具有适当的吸水性,纤维亲肤性具有显著优势;莫代尔纤维染色后做纤维切片,在显微镜下观察,无二次反应界面,本发明的粘胶纤维与莫代尔纤维在同等染色条件下,本发明的粘胶纤维比莫代尔吸色深,上染率高,均匀性更好,且成品的色牢度好。(3) The invention adopts the three-bath wet spinning technology, the coagulation bath adopts low acid and high salt, the reaction condition is mild, and the viscose is formed into a tow after the spinning and drawing process, thereby ensuring multiple reactions of the fiber. The viscose fiber of the present invention has a secondary reaction interface different from that of ordinary viscose fiber and modal fiber. It should be noted that the secondary reaction interface is formed according to the difference in fiber dyeing ability of the fiber cross section, that is, the cortex of the fiber and The core layer and the skin layer have small color absorption ability and dyeing, and the core layer has a large color absorption ability for the dye, the color is deep, and the skin layer has a high degree of orientation. The more the skin layer, the higher the breaking strength, and the more the core layer The water swelling degree is higher; the fiber of the present invention is dyed and then subjected to fiber slicing, and the fiber slice of the viscose fiber according to the present invention exhibits a clear and obvious cross-sectional area of the secondary reaction microscope, and the "area" of the core layer and the skin layer. The ratio is (40-70): (30-60), the ratio is moderate, and the ratio of the "area" of the core layer and the cortex of ordinary viscose fiber is (90-95): (5-10), the ratio is biased to the inner layer, so Viscose fiber and ordinary viscose fiber of the invention Compared with high strength and low elongation, it also has proper water absorption, and fiber skin-friendliness has obvious advantages. After modal fiber dyeing, it is made into fiber section, observed under microscope, no secondary reaction interface, and the adhesive of the invention The fiber and the modal fiber under the same dyeing condition, the viscose fiber of the invention has a darker color absorption than the modal, the dyeing rate is higher, the uniformity is better, and the color fastness of the finished product is good.
(4)为确保高强低伸粘胶纤维二次反应界面具有适宜的皮层、芯层比例,本发明从工艺技术出发,做到了改进酸浴工艺,如降低硫酸浓度,反应缓慢,提高皮层厚度;改变粘胶指标,如粘胶熟成度、甲纤含量、碱含量等指标,从而保证了本发明粘胶纤维的断裂强度高。(4) In order to ensure a suitable skin layer and core layer ratio at the secondary reaction interface of the high-strength and low-stretch viscose fiber, the present invention proceeds from the process technology to improve the acid bath process, such as reducing the sulfuric acid concentration, slow reaction, and increasing the thickness of the skin layer; The viscose index, such as viscose ripeness, nail fiber content, alkali content and the like, are changed to ensure high breaking strength of the viscose fiber of the present invention.
(5)与现有技术中的粘胶工艺相比,本发明制得的碱纤维素半纤维素含量低,控制在10g/L以内,我们知道:半纤维素是指聚合度在50~200的β纤维素和聚合度<50的γ纤维素,半纤维素的影响只要有以下几个方面:a.影响碱纤维素的均匀性;b.延长老成时间;c.半纤维素的黄化速度比甲纤快,消耗一定量的二硫化碳,导致碱纤维素酯化减少,磺酸酯的溶解度降低;d.影响粘胶的过滤,磺酸酯的溶解度降低,其末端潜在的醛基氧化成羧基与灰分中的金属离子如:亚铁离子,锰离子,钙离子,镁离子,形成粘性极强的络合物,导致粘胶过滤困难,产量低;e.半纤维素越多,粘胶纤维的物理机械性能越差。本发明通过碾磨机,可提前对送入压榨机的浆粥进行研磨,研磨时间为10~40s,将研磨后的浆粥用压榨机压榨后,分离获得混合碱液和碱纤维素,混合碱液中含有半纤维素以及其他杂质,经粉碎机粉碎,压榨的倍数为2.2~2.8,粉碎度为120-180g/L,通过机械作用,以提高浆粥的反应性能,保证粘胶纤维生产的顺利进行。(5) Compared with the prior art viscose process, the alkali cellulose hemicellulose content obtained by the invention is low, and is controlled within 10 g/L. We know that hemicellulose refers to a polymerization degree of 50-200. β cellulose and γ cellulose with a degree of polymerization <50, the effect of hemicellulose is as follows: a. affecting the uniformity of alkali cellulose; b. prolonging the age of the old; c. yellowing of hemicellulose The speed is faster than that of the fiber, and a certain amount of carbon disulfide is consumed, resulting in a decrease in alkali cellulose esterification and a decrease in the solubility of the sulfonate; d. affecting the filtration of the viscose, the solubility of the sulfonate is lowered, and the potential aldehyde group is oxidized at the end. The metal ions in the carboxyl group and the ash, such as: ferrous ion, manganese ion, calcium ion, magnesium ion, form a highly viscous complex, which leads to difficulty in filtering the viscose and low yield; e. the more hemicellulose, the viscose The poorer the physical and mechanical properties of the fiber. The invention can grind the porridge fed into the press in advance by a grinding machine, and the grinding time is 10-40 s. After the milled porridge is pressed by a press, the mixed lye and alkali cellulose are separated and mixed. The lye contains hemicellulose and other impurities, and is crushed by a pulverizer. The multiple of the pressing is 2.2 to 2.8, and the pulverization degree is 120-180 g/L. By mechanical action, the reaction performance of the porridge is improved to ensure the production of viscose fiber. Smooth progress.
(6)本发明使用的浆粕原料可选取棉浆、竹浆、木浆、麻浆中的任意一种或两者以上的混合物可按任意比例进行制备,原材料范围适用广泛,技术要求制备相对较低,原材料成本较低。(6) The pulp raw material used in the present invention may be selected from any one or a mixture of two or more of cotton pulp, bamboo pulp, wood pulp and hemp pulp, and may be prepared in any ratio, and the raw material range is applicable widely, and the technical requirements are relatively prepared. Lower, lower raw material costs.
(7)本发明步骤A中,碱液为浓度110~240g/L的氢氧化钠溶液,浸渍碱液的温度为30~60℃,浸渍时间为50~90min。通过合理的参数设置,保证压榨和过滤的顺利进行;碱液浓度过高,所得纤维素磺酸脂溶解度会降低,粘胶过滤困难;碱液浓度过低,浆粕原料膨化度过高,压榨困难;温度过高,纤维素降聚快,加速副反应,影响粘胶过滤;温度过低,浆粕膨化度高,压榨困难。(7) In the step A of the present invention, the lye is a sodium hydroxide solution having a concentration of 110 to 240 g/L, the temperature of the immersion alkali solution is 30 to 60 ° C, and the immersion time is 50 to 90 minutes. Through reasonable parameter setting, the pressing and filtration can be smoothly carried out; if the concentration of lye is too high, the solubility of the obtained cellulose sulfonate will decrease, the filtration of the viscose will be difficult; the concentration of the lye is too low, the pulping degree of the pulp is too high, and the pressing Difficult; the temperature is too high, cellulose depolymerization is fast, accelerate the side reaction, affect the viscose filtration; the temperature is too low, the pulp has a high degree of puffing and the pressing is difficult.
(8)本发明采用多级提纯,如研磨、压榨粉碎、揉搓,碱液梯级利用,如分别在浸渍阶段前、揉搓阶段后加入碱液,不仅能提到纤维素结合碱含量,达到提高碱液的综合利用率的目的,同时,还能有效的降低辅料碱液的投入成本,降低粘胶纤维的生产成本。(8) The invention adopts multi-stage purification, such as grinding, pressing and pulverizing, mashing, lye step utilization, for example, adding lye before and after the immersion stage, respectively, not only mentioning the cellulose-bound alkali content, but also increasing the alkali The purpose of the comprehensive utilization of the liquid, at the same time, can also effectively reduce the input cost of the auxiliary lye and reduce the production cost of the viscose fiber.
(9)本发明经研磨、压榨粉碎后可获得甲纤含量29~31%、碱含量15~17%的碱纤维素,该碱纤维素经揉搓、氧化降聚后可直接送入粘胶纤维生产系统,粘胶纤维生产工艺可采用常规工艺,如黄化获得粘胶后,再经过过滤、熟成、脱泡、纺丝以获得粘胶纤维。(9) The invention can obtain alkali cellulose having a fiber content of 29 to 31% and an alkali content of 15 to 17% after grinding and pressing, and the alkali cellulose can be directly fed into the viscose fiber after being subjected to hydrazine oxidation and polycondensation. Production system, viscose fiber production process can be carried out by conventional techniques, such as yellowing to obtain viscose, then filtered, matured, defoamed, and spun to obtain viscose fiber.
(10)在本发明中,碱纤维素纤维经搓揉机双螺杆设备进行处理,使纤维分丝、帚化,达到破坏纤维素纤维的细胞壁,去除纤维素中的小分子,从而提高纤维素反应性能,提高纤维素结合碱含量,达到6~8%(质量百分比)。(10) In the present invention, the alkali cellulose fiber is treated by a twin-screw equipment to separate the fibers, thereby decomposing the fibers, thereby breaking the cell wall of the cellulose fibers, removing small molecules in the cellulose, thereby increasing the cellulose. The reaction performance improves the cellulose-bound alkali content to 6 to 8% by mass.
(11)本发明的F步骤定向降聚:将步骤D得到的碱纤维素与浓度为140~200g/L的碱液混合形成浓度为4~8%的浆粥,将浆粥输送至定向降聚反应器,反应时间为30~60min,经降聚后,使碱纤维素聚合度由650~1200降为400~600,甲纤纯度达到98.0~98.5%,比传统工艺可提高2~3%,定向降聚比传统老成降聚减少甲纤损失3~5%,提高了原材料利用率,节约了生产成本,且分子降聚更加均匀、充分、有效。(11) The F-step directional depolymerization of the present invention: the alkali cellulose obtained in the step D is mixed with the lye having a concentration of 140-200 g/L to form a porridge having a concentration of 4 to 8%, and the porridge is transported to the directional drop. The polyreactor has a reaction time of 30 to 60 min. After depolymerization, the degree of polymerization of alkali cellulose is reduced from 650 to 1200 to 400 to 600, and the purity of the fiber is 98.0 to 98.5%, which is 2 to 3% higher than the conventional process. The directional depolymerization reduces the loss of the fiber by 3 to 5% compared with the conventional aging, improves the utilization rate of raw materials, saves the production cost, and the molecular degradation is more uniform, sufficient and effective.
(12)本发明的牵伸工艺,采用逐级高牵伸技术,一牵伸率为50~100%,牵伸过高,毛丝多,牵伸过低,强度低;二牵伸率为40~60%;三牵伸率为5~15%牵伸过高,毛丝多,牵伸过低,强度下降,通过合理的牵伸率的控制,改善了纤维的脆性,提高了纤维强度,且减少毛丝的量,提高了产品的外观性能。(12) The drafting process of the present invention adopts a step-by-step high drafting technique, a drawing ratio of 50 to 100%, a high draft, a high number of filaments, a low draft, and a low strength; and a second draft ratio. 40~60%; three drafting rate is 5~15%, the drafting is too high, the wool is much, the drafting is too low, the strength is decreased, and the brittleness of the fiber is improved and the fiber strength is improved by the reasonable drafting rate control. And reduce the amount of wool, improving the appearance of the product.
(13)本发明的脱硫工艺中硫化钠和碳酸钠组成的脱硫剂较现有使用的氢氧化钠、亚硫酸钠更加温和,能使纤维产品强度、伸度的损伤减小,并且碳酸钠能中和丝束从酸浴中带来的硫酸,脱硫工艺后,可调节
丝束的pH值在8~11。(13) The desulfurizing agent composed of sodium sulfide and sodium carbonate in the desulfurization process of the present invention is milder than the sodium hydroxide and sodium sulfite currently used, and can reduce the damage of the strength and elongation of the fiber product, and the sodium carbonate can be neutralized. The tow brought from the acid bath to the sulfuric acid, after the desulfurization process, can be adjusted
The pH of the tow is between 8 and 11.
(14)本发明使用的漂白剂温和,采用双氧水漂白剂较次氯酸钠等漂白剂更加温和,本发明制备的粘胶纤维的pH值应控制在6.5~7范围内,还可通过水洗、多效酸(有机酸)的方式调节pH值,在该范围内,粘胶纤维成品的强伸度不会受到影响,强伸度高。(14) The bleaching agent used in the invention is mild, and the hydrogen peroxide bleaching agent is milder than the bleaching agent such as sodium hypochlorite. The pH of the viscose fiber prepared by the invention should be controlled within the range of 6.5 to 7, and can also be washed with water and palatable acid. The pH is adjusted in the manner of (organic acid), within which the strength of the finished viscose fiber is not affected and the elongation is high.
(15)本发明设计合理,在相同粘胶纤维产品的生产过程中,综合上述原料选取、制备工艺改进等方面,极大程度的降低粘胶纤维产品的生产成本,其售价与莫代尔纤维相比低4000~5000元/吨,能大幅度降低下游原料使用成本,可用于家纺、无纺布等,特别是内衣以及面膜、湿纸巾等,为纺纱、织布等下游企业带来更高附加值及广阔的市场前景,显著提升企业的市场竞争力。(15) The invention has reasonable design, comprehensively reduces the production cost of viscose fiber products in the production process of the same viscose fiber product, comprehensively selects the above raw materials, and improves the production cost of the viscose fiber product, and the price thereof is compared with the modal fiber phase. The ratio is 4,000-5,000 yuan/ton, which can greatly reduce the cost of downstream raw materials. It can be used in home textiles, non-woven fabrics, etc., especially underwear, masks, wet wipes, etc., bringing higher profits to downstream enterprises such as spinning and weaving. The added value and broad market prospects significantly enhance the market competitiveness of enterprises.
图1为本发明所述消光型高强低伸粘胶纤维的纤维切片横截面;Figure 1 is a cross section of a fiber section of the matte type high strength low stretch viscose fiber of the present invention;
图2为莫代尔的纤维切片横截面;Figure 2 is a cross section of a fiber section of Modal;
图3为天丝的纤维切片横截面。Figure 3 is a cross-section of a fiber section of Tencel.
下面将本发明的发明目的、技术方案和有益效果作进一步详细的说明。The object, technical solution and advantageous effects of the present invention will be further described in detail below.
应该指出,以下详细说明都是示例性的,旨在对所要求的本发明提供进一步的说明,除非另有说明,本文使用的所有技术和科学术语具有与本发明所属技术领域的普通技术人员通常理解的相同含义。It is to be understood that the following detailed description is intended to be illustrative of the invention, and the claims of the invention The same meaning of understanding.
天丝、莫代尔、铜氨纤维、粘胶纤维等纤维原料均是以天然纤维素材料为原料再生而成的生物基纤维原料,其中,以粘胶纤维的市场占有率最高,但随着近年来普通品种的粘胶纤维规模急剧膨胀,原材料供应紧张,下游新型纺织品的开发和产业升级逐步受到限制,为克服这一现象,以专利文献CN102296373A、CN1632189、CN102251301A为例的一系列差别化粘胶纤维被提出,由其公开的专利技术可知,这类差别化粘胶纤维均是通过改变生产工艺的方式来实现的,但对于日益激烈的市场竞争来说,差别化的粘胶纤维并没有更大限度的满足下游新型纺织品的开发和产业升级,尤其是同样以天然纤维素材料为原料再生而成的天丝、莫代尔、铜氨纤维等纤维原料的发展,使得粘胶纤维的市场占有率日趋降低。在此基础上,本发明提出了一种高强低伸粘胶纤维,该粘胶纤维产品具有高强、低伸的产品特性,同时还具有高吸收特性,产品亲肤性远胜于莫代尔纤维,略优于棉纤维。Fiber raw materials such as Tencel, Modal, copper ammonia fiber and viscose fiber are bio-based fiber raw materials regenerated from natural cellulose materials. Among them, viscose fiber has the highest market share, but with recent years The scale of viscose fiber of ordinary varieties has expanded rapidly, the supply of raw materials has been tight, and the development of downstream new textiles and industrial upgrading have been gradually restricted. To overcome this phenomenon, a series of differential viscose fibers are exemplified by patent documents CN102296373A, CN1632189 and CN102251301A. It is proposed that the disclosed patented technology can be realized by changing the production process, but for the increasingly fierce market competition, the differentiated viscose fiber is not bigger. The limit meets the development and industrial upgrading of downstream new textiles, especially the development of fiber materials such as Tencel, Modal, and Cuminous fiber, which are also recycled from natural cellulose materials, which makes the market share of viscose fiber decrease. . On the basis of this, the present invention proposes a high-strength low-stretch viscose fiber which has high-strength, low-stretch product characteristics and high absorption characteristics, and the skin-friendly property of the product is far superior to that of modal fiber. Better than cotton fiber.
本发明涉及的高强低伸粘胶纤维在纤维形成过程中,保持了独有的纤维结构,具有高强力的特点,其干断裂强度和湿断裂强度与普通粘胶纤维相比提高了25%左右,与差别化粘胶纤维也具有明显区别,从产品指标可以看出,高强低伸粘胶纤维的产品指标满足:纤度0.88~1.67dtex,干断裂强度≥3.10cN/dtex,湿断裂强度≥1.60cN/dtex,而差别化粘胶纤维以专利文献记载CN102296373A、CN1632189、CN102251301A为例,其产品指标如下:CN102296373A满足纤度0.44~0.78dtex、干断裂强度≥3.10cN/dtex、湿断裂强度≥2.1cN/dtex;CN1632189满足纤度0.90~1.40dtex、干断裂强度≥2.50cN/dtex、湿断裂强度≥1.20cN/dtex;CN102251301A满足纤度1.11dtex、强度≥2.9cN/dtex,从上述指标可以看出,本发明涉及的高强低伸粘胶纤维的纤维强度明显优于现有的差别化粘胶纤维。The high-strength low-stretch viscose fiber of the invention maintains a unique fiber structure during the fiber formation process, and has the characteristics of high strength, and the dry breaking strength and the wet breaking strength are improved by about 25% compared with the ordinary viscose fiber. It is also obviously different from the differentiated viscose fiber. It can be seen from the product index that the product index of high strength and low elongation viscose fiber meets: fineness 0.88~1.67dtex, dry breaking strength≥3.10cN/dtex, wet breaking strength≥1.60 cN/dtex, and the differentiated viscose fiber is exemplified by the patent documents CN102296373A, CN1632189, CN102251301A, and its product specifications are as follows: CN102296373A satisfies the fineness of 0.44~0.78dtex, dry breaking strength≥3.10cN/dtex, wet breaking strength≥2.1cN /dtex;CN1632189 meets the fineness of 0.90~1.40dtex, dry rupture strength ≥2.50cN/dtex, wet rupture strength ≥1.20cN/dtex; CN102251301A meets the fineness of 1.11dtex, strength ≥2.9cN/dtex, as can be seen from the above indicators, this The fiber strength of the high-strength low-stretch viscose fiber involved in the invention is significantly superior to the existing differential viscose fiber.
将本发明涉及的高强低伸粘胶纤维再分别与莫代尔纤维、天丝进行比对,比对方式如下:The high-strength low-stretch viscose fiber according to the present invention is separately compared with the modal fiber and the tencel, and the comparison manner is as follows:
将高强低伸粘胶纤维、莫代尔纤维、天丝分别染色后做纤维切片,将其纤维切片在显微镜下放大2000倍进行观察,如图1~3所示,图1为本发明高强低伸粘胶纤维的纤维切片横截面,如图1所示,本发明涉及的高强低伸粘胶纤维经染色处理后,其纤维皮层、芯层的颜色分别表现出了浅、深的差异,差异较大,皮层偏浅,芯层明显偏深,存在清晰的二次反应界面,比例适中,确保了该产品具有高强、低伸的特点,同时还具有适当的吸水性,纤维亲肤性具有显著优势,其中,芯层:皮层的“面积”比例为40~70:30~60。The high-strength low-stretch viscose fiber, the modal fiber, and the tencel were respectively dyed and then subjected to fiber slicing, and the fiber sections were observed under a microscope for 2000 times, as shown in Figs. 1 to 3, and Fig. 1 is a high-strength and low-stretching adhesive of the present invention. The cross-section of the fiber section of the rubber fiber, as shown in Fig. 1, after the dyeing treatment of the high-strength low-stretch viscose fiber of the present invention, the color of the fiber skin layer and the core layer respectively show a difference between shallow and deep, and the difference is large. The cortex is shallow, the core layer is obviously deep, and there is a clear secondary reaction interface, and the proportion is moderate, which ensures that the product has the characteristics of high strength and low elongation, and also has appropriate water absorption, and the fiber skin-friendly property has significant advantages. Among them, the core layer: the "area" ratio of the skin layer is 40 to 70:30 to 60.
图2为莫代尔纤维的纤维切片截面图,如图2所示,莫代尔纤维经染色处理后,其纤维皮层和芯层的颜色深、浅一致,无明显二次界面,该产品特点增强了纤维的疏水性,吸水率差,从而使其亲肤性变差。Figure 2 is a cross-sectional view of the fiber section of the modal fiber. As shown in Fig. 2, after the dyeing of the modal fiber, the color of the fiber skin layer and the core layer are deep and shallow, and there is no obvious secondary interface. The product features enhance the fiber. Hydrophobic, poor water absorption, which makes it less skin-friendly.
图3为天丝的纤维切片截面图,如图3所示,天丝经染色处理后,其纤维皮层和芯层的颜色深、浅一致,无明显二次界面,该产品特点兼具普通型粘胶纤维优良的吸湿性、柔滑飘逸性、舒适性等优点外,克服了普通粘胶纤维强力低,尤其是湿强低的缺陷,它的强力几乎与涤纶相近。Figure 3 is a cross-sectional view of the fiber section of Tencel. As shown in Figure 3, after the dyeing process, the fiber skin layer and the core layer are dark and light in color, and there is no obvious secondary interface. The product features both common types. The viscose fiber has the advantages of excellent hygroscopicity, smoothness and smoothness, and comfort. It overcomes the defects of ordinary viscose fiber, such as low strength, especially low wet strength. Its strength is almost similar to that of polyester.
正是由于产品的上述特性,决定了本发明涉及的消光型高强低伸粘胶纤维满足以下指标:It is precisely because of the above characteristics of the product that the matting type high-strength low-stretch viscose fiber according to the present invention satisfies the following indexes:
干断裂强度≥3.10cN/dtex,湿断裂强度≥1.60cN/dtex,Dry breaking strength ≥ 3.10cN/dtex, wet breaking strength ≥ 1.60cN/dtex,
湿状态下产生5%伸长率所需的强度≥0.55cN/dtex,The strength required to produce 5% elongation in wet state is ≥0.55 cN/dtex,
干断裂伸长率11.0~19.0%,湿断裂伸长率16.0~21.0%,The dry elongation at break is 11.0 to 19.0%, and the wet elongation at break is 16.0 to 21.0%.
消光剂含量0.8~5%,白度≥85%,径向水膨润度22~26%,The matting agent content is 0.8-5%, the whiteness is ≥85%, and the radial water swelling degree is 22-26%.
线密度偏差率≤±11.0%,残硫≤12.0mg/100g,The linear density deviation rate is ≤±11.0%, and the residual sulfur is ≤12.0mg/100g.
长度偏差率≤±11.0%,超长纤维率≤0.5%,The length deviation rate is ≤±11.0%, and the ultra-long fiber rate is ≤0.5%.
倍长纤维≤4.0mg/100g,疵点≤4.0mg/100g。
The long fiber ≤ 4.0 mg / 100 g, 疵 point ≤ 4.0 mg / 100g.
上述指标适用于线密度范围为0.8dtex~1.67dtex的高强低伸的粘胶纤维的测定,干断裂强度的测定方法是GB/T 14337,湿断裂强度的测定方法是GB/T 14337,湿状态下产生5%伸长率所需的强度是通过GB/T14337完成的,干断裂伸长率的测定方法是GB/T 14337,湿断裂伸长率的测定方法是GB/T 14337,线密度偏差率的测定方法是GB/T 14335,残硫的测定方法是FZ/T 50014,长度偏差率的测定方法是GB/T 14336,超长纤维率的测定方法是GB/T 14336,倍长纤维的测定方法是GB/T 14336,疵点的测定方法是GB/T 14339,白度的测定方法是FZ/T 50013,径向水膨润度的测定方法是GB/T 6503。The above indicators are applicable to the determination of high strength and low elongation viscose fiber with a linear density ranging from 0.8 dtex to 1.67 dtex. The method for determining the dry rupture strength is GB/T 14337, and the method for determining the wet rupture strength is GB/T 14337. The strength required to produce 5% elongation is achieved by GB/T14337. The method for determining the dry elongation at break is GB/T 14337. The method for determining the wet elongation at break is GB/T 14337. The method for determining the rate is GB/T 14335, the method for determining residual sulfur is FZ/T 50014, the method for measuring the length deviation rate is GB/T 14336, and the method for measuring the ultra-long fiber ratio is GB/T 14336, which is a long fiber. The measurement method is GB/T 14336, the measurement method of the defect is GB/T 14339, the measurement method of whiteness is FZ/T 50013, and the measurement method of radial water swelling degree is GB/T 6503.
下面以几个典型实施例来列举说明本发明的具体实施方式,当然,本发明的保护范围并不局限于以下实施例。The specific embodiments of the present invention are illustrated by the following exemplary embodiments. Of course, the scope of the present invention is not limited to the following embodiments.
实施例1Example 1
本实施例涉及的高强低伸粘胶纤维是由浆粕原料依次经浸渍、研磨、压榨粉碎、搓揉、降聚、黄化、溶解、过滤、脱泡、熟成、纺丝牵伸和后处理后而得到的,经测定,该高强低伸粘胶纤维满足:The high-strength low-stretch viscose fiber according to the embodiment is sequentially impregnated, ground, pressed, pulverized, depolymerized, yellowed, dissolved, filtered, defoamed, matured, spun drawn and post-treated from pulp raw materials. And obtained, determined that the high-strength low-stretch viscose fiber meets:
干断裂强度≥3.10cN/dtex;Dry breaking strength ≥ 3.10cN/dtex;
湿断裂强度≥1.60cN/dtex;Wet breaking strength ≥ 1.60cN / dtex;
湿状态下产生5%伸长率所需的强度≥0.55cN/dtex,The strength required to produce 5% elongation in wet state is ≥0.55 cN/dtex,
干断裂伸长率11.0~19.0%;Dry elongation at break is 11.0 to 19.0%;
湿断裂伸长率16.0~21.0%;Wet elongation at break is 16.0 to 21.0%;
径向水膨润度22~26%;Radial water swelling degree 22 to 26%;
消光剂含量0.8~5%。The matting agent content is 0.8 to 5%.
实施例2Example 2
本实施例与实施例1的区别在于:本实施例涉及的高强低伸粘胶纤维还满足:The difference between this embodiment and the embodiment 1 is that the high-strength low-stretch viscose fiber according to the embodiment also satisfies:
白度≥85%;Whiteness ≥ 85%;
线密度偏差率≤±11.0%;Linear density deviation rate ≤ ± 11.0%;
残硫≤12.0mg/100g;Residual sulfur ≤ 12.0mg / 100g;
长度偏差率≤±11.0%;Length deviation rate ≤ ± 11.0%;
超长纤维率≤0.5%;Ultra-long fiber rate ≤0.5%;
倍长纤维≤4.0mg/100g;Double fiber ≤4.0mg/100g;
疵点≤4.0mg/100g。The defect point is ≤4.0mg/100g.
实施例3Example 3
一种消光型高强低伸粘胶纤维的制备方法,步骤如下:A method for preparing a matting type high-strength low-stretch viscose fiber, the steps are as follows:
A.将浆粕原料首先放在喂机粕上,设定投料速度为40kg/min后,将原料加入到浸渍桶中,经研磨机研磨后制成浓度为3%的浆粥,其中,研磨的目的是通过机械作用对纤维进行开松和分散,从而提高纤维素的碱化速度及碱化率;A. Put the pulp raw material on the feeding machine first, set the feeding speed to 40kg/min, add the raw material to the dipping bucket, and grind it to make the porridge with the concentration of 3%. The purpose is to open and disperse the fiber by mechanical action, thereby increasing the alkalization speed and alkalization rate of the cellulose;
B.将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为30%的浆粥,在该步骤中,压榨机能除去多余的碱液,多余的碱液能够回收利用,处理方式是使用滤网60目、真空度–0.4MPa的过滤机去除碱液中多余的半纤维素后回收碱纤维素,揉搓机使用双螺杆设备,可使纤维分丝、帚化,达到破坏纤维素纤维细胞壁的作用,去除纤维素中的小分子,从而提高纤维素反应性能,提高纤维素结合碱含量,达到6%;B. The porridge obtained in step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 30% after the treatment. In this step, the press can remove excess lye, and the excess lye can be recycled. The treatment method is to remove excess hemicellulose from the lye by using a filter with a mesh size of 60 mesh and a vacuum of -0.4 MPa. Alkali cellulose, the use of twin-screw equipment, the fiber can be divided into filaments, deuterated, to break the cell wall of cellulose fibers, remove small molecules in cellulose, thereby improving the cellulose reaction performance, increasing the cellulose-bound alkali content , reaching 6%;
C、将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为400、甲纤纯度为98.0%的碱纤维素,在该步骤中,加入纯氧的目的是氧化降聚。C. The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 400 and a purity of the corn fiber of 98.0% is obtained. In the step, the purpose of adding pure oxygen is oxidative depolymerization.
D.将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.0%的纤维素磺酸酯溶液;D. The alkali cellulose obtained in step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent to obtain a concentration of 9.0% cellulose sulfonate solution;
E.将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E. After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
本实施例中,浆粕原料为棉浆。In this embodiment, the pulp raw material is cotton pulp.
实施例4Example 4
一种消光型高强低伸粘胶纤维的制备方法,步骤如下:A method for preparing a matting type high-strength low-stretch viscose fiber, the steps are as follows:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为3.5%的浆粥;A: the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 3.5%;
B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为32%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 32% after the treatment. ;
C:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为450、甲纤纯度为98.5%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 450 and a purity of 98.5% of the methyl fiber is obtained;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄花反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为10.0%的纤维素磺酸酯溶液;
D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 10.0. % cellulose sulfonate solution;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
上述步骤A中,浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1100,混合比例为3:2:1:1;所述的碱液为氢氧化钠,其浓度为120g/L,浸渍温度为35℃,浸渍时间为65min;所述的研磨机设于连接浸渍桶和压榨机的管道内,研磨后浆粥的温度为35℃,研磨的时间为35s。In the above step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, the mixing ratio is 3:2:1:1; the alkali liquid is sodium hydroxide, The concentration was 120 g/L, the immersion temperature was 35 ° C, and the immersion time was 65 min. The grinding machine was placed in a pipe connecting the dip tank and the press. The temperature of the porridge after grinding was 35 ° C, and the grinding time was 35 s.
实施例5Example 5
A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为4%的浆粥;A: the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为35%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 35% after the treatment. ;
C:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为500、甲纤纯度为98.2%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 500 and a purity of the fiber of 98.2% is obtained;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄花反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.5%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.5. % cellulose sulfonate solution;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
本实施例步骤A中,浆粕原料为木浆和麻浆的混合物,混合比例为3:1,聚合度为1000。In the step A of the present embodiment, the pulp raw material is a mixture of wood pulp and hemp pulp, the mixing ratio is 3:1, and the degree of polymerization is 1000.
本实施例步骤A中,所述的碱液为氢氧化钠,其浓度为110g/L,浸渍温度为30℃,浸渍时间为50min。In the step A of the present embodiment, the alkali solution is sodium hydroxide, the concentration is 110 g/L, the immersion temperature is 30 ° C, and the immersion time is 50 min.
实施例6Example 6
一种消光型高强低伸粘胶纤维的制备方法,步骤如下:A method for preparing a matting type high-strength low-stretch viscose fiber, the steps are as follows:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为4%的浆粥;A: the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为38%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 38% after the treatment. ;
C:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为550、甲纤纯度为98.3%的碱纤维素;C: the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 550 and a purity of 98.3% of the methyl fiber is obtained;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄花反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.6%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.6. % cellulose sulfonate solution;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
上述步骤A中,浆粕原料为竹浆、木浆和麻浆的混合物,聚合度为900,混合比例为3:1:1;所述的碱液为氢氧化钠,其浓度为240g/L,浸渍温度为60℃,浸渍时间为90min;所述的研磨机设于连接浸渍桶和压榨机的管道内,研磨后浆粥的温度为30℃,研磨的时间为10s。In the above step A, the pulp raw material is a mixture of bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 900, the mixing ratio is 3:1:1; the alkali liquid is sodium hydroxide, and the concentration thereof is 240 g/L. The immersion temperature is 60 ° C and the immersion time is 90 min; the grinding machine is arranged in a pipe connecting the dip tank and the press, and the temperature of the porridge after grinding is 30 ° C, and the grinding time is 10 s.
实施例7Example 7
一种消光型高强低伸粘胶纤维的制备方法,步骤如下A method for preparing matt high-strength low-stretch viscose fiber, the steps are as follows
A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为6%的浆粥;A: the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 6%;
B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为40%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 40% after the treatment. ;
C:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为600、甲纤纯度为98.5%的碱纤维素;C: the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor to obtain an alkali cellulose having a degree of polymerization of 600 and a purity of 98.5%.
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄花反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为10.0%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 10.0. % cellulose sulfonate solution;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
本实施例中,浆粕原料为竹浆,其聚合度为800。In this embodiment, the pulp raw material is bamboo pulp, and the degree of polymerization is 800.
上述步骤A中,所述的碱液为氢氧化钠,其浓度为200g/L,浸渍温度为40℃,浸渍时间为60min;所述的研磨机设于连接浸渍桶和压榨机的管道内,研磨后浆粥的温度为60℃,研磨的时间为40s。In the above step A, the alkali liquid is sodium hydroxide, the concentration is 200 g/L, the immersion temperature is 40 ° C, and the immersion time is 60 min; the grinding machine is arranged in a pipe connecting the dipping bucket and the press, The temperature of the porridge after grinding was 60 ° C, and the grinding time was 40 s.
上述步骤B中,压榨机的压榨温度57℃,压榨倍数为2.2倍,粉碎机的粉碎度为120g/L。In the above step B, the pressing temperature of the press was 57 ° C, the pressing ratio was 2.2 times, and the pulverizing degree of the pulverizer was 120 g / L.
实施例8Example 8
本实施例与实施例4的区别在于:在步骤A中,浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1200,混合比例为2:3:1:1;在步骤B中,所述压榨机的压榨温度为63℃、压榨倍数为2.8。通过合理的压榨倍数和粉碎度的调整,能够提高后期加工工序中碱纤维素的性能均匀性,防止局部收到强挤压,从而阻碍了氧气进入,降低降聚步骤的速度。The difference between this embodiment and the embodiment 4 is that, in the step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1200, and the mixing ratio is 2:3:1:1; In the step B, the press had a press temperature of 63 ° C and a press multiple of 2.8. Through reasonable adjustment of the pressing ratio and the degree of pulverization, the performance uniformity of the alkali cellulose in the post-processing step can be improved, and the strong extrusion can be prevented from being locally received, thereby hindering the entry of oxygen and reducing the speed of the depolymerization step.
步骤C中,所述的碱液为浓度140g/L的氢氧化钠溶液,反应器中纯氧的加入量为2%,降聚反应时间
控制在30min。In step C, the lye is a sodium hydroxide solution having a concentration of 140 g/L, and the amount of pure oxygen in the reactor is 2%, and the polymerization reaction time is
Controlled at 30min.
实施例9Example 9
一种消光型高强低伸粘胶纤维的制备方法,包括以下步骤:A method for preparing a matt high-strength low-stretch viscose fiber, comprising the following steps:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为4%的浆粥;A: the pulp raw material is immersed in a dipping bucket containing a lye, and ground by a grinder to prepare a porridge having a concentration of 4%;
B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为32%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a mashing machine to obtain a porridge having a concentration of 32% after the treatment. ;
C:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为600、甲纤纯度为98.0%的碱纤维素;C: the porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor, and after depolymerization, alkali cellulose having a degree of polymerization of 600 and a purity of the corn fiber of 98.0% is obtained;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄花反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.6%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellow flower reaction is dissolved in a solvent to obtain a concentration of 9.6. % cellulose sulfonate solution;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming and aging the cellulose sulfonate solution prepared in step D, a matting agent is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscose. fiber.
上述步骤A中,浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1100,混合比例为3:2:1:1;所述的碱液为氢氧化钠,其浓度为180g/L,浸渍温度为50℃,浸渍时间为55min;所述的研磨机设于连接浸渍桶和压榨机的管道内,研磨后浆粥的温度为45℃,研磨的时间为20s;在步骤B中,所述压榨机的压榨温度为60℃、压榨倍数为2.6倍,粉碎机的粉碎度为160g/L;步骤C中,所述的碱液为浓度200g/L的氢氧化钠溶液,反应器中纯氧的加入量为10%,降聚反应时间控制在60min。In the above step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, the mixing ratio is 3:2:1:1; the alkali liquid is sodium hydroxide, The concentration is 180g / L, the immersion temperature is 50 ° C, the immersion time is 55min; the grinding machine is arranged in the pipe connecting the dipping bucket and the press, the temperature of the porridge after grinding is 45 ° C, the grinding time is 20 s; In the step B, the pressing temperature of the press is 60 ° C, the pressing multiple is 2.6 times, the pulverization degree of the pulverizer is 160 g / L; in the step C, the alkali liquid is sodium hydroxide having a concentration of 200 g / L The solution, the pure oxygen in the reactor was added in an amount of 10%, and the depolymerization reaction time was controlled at 60 min.
本实施例的步骤D中,二硫化碳的加入量为步骤B制得的碱纤维素中甲纤含量的25%;所述的黄化反应时间控制在45min,黄化反应温度为20℃,所述的溶解是将纤维素磺酸酯与溶剂进行混合、搅拌和研磨,所述的溶剂包括浓度为25g/L氢氧化钠溶液和浓度为5g/L的亚硫酸钠水溶液,所述的溶解温度为10℃,溶解时间为30min。In the step D of the present embodiment, the amount of carbon disulfide added is 25% of the content of the methyl fiber in the alkali cellulose obtained in the step B; the yellowing reaction time is controlled at 45 minutes, and the yellowing reaction temperature is 20 ° C. The dissolution is carried out by mixing, stirring and grinding the cellulose sulfonate with a solvent comprising a sodium sulfite solution having a concentration of 25 g/L sodium hydroxide solution and a concentration of 5 g/L, and the dissolution temperature is 10 ° C. The dissolution time is 30 min.
实施例10Example 10
本实施例与实施例9的区别在于:步骤C中,所述的碱液为浓度140g/L的氢氧化钠溶液,反应器中纯氧的加入量为5%,降聚反应时间控制在45min。The difference between this embodiment and the embodiment 9 is that in the step C, the lye is a sodium hydroxide solution having a concentration of 140 g/L, the amount of pure oxygen in the reactor is 5%, and the depolymerization reaction time is controlled at 45 min. .
本实施例的步骤D中,二硫化碳的加入量为步骤B制得的碱纤维素中甲纤含量的37%;所述的黄化反应时间控制在50min,黄化反应温度为30℃,所述的溶解是将纤维素磺酸酯与溶剂进行混合、搅拌和研磨,所述的溶剂包括浓度为45g/L氢氧化钠溶液和浓度为10g/L的亚硫酸钠水溶液,所述的溶解温度为20℃,溶解时间为50min。In the step D of the present embodiment, the amount of carbon disulfide added is 37% of the content of the methyl fiber in the alkali cellulose obtained in the step B; the yellowing reaction time is controlled at 50 min, and the yellowing reaction temperature is 30 ° C. The solution is to mix, stir and grind the cellulose sulfonate with a solvent comprising a sodium sulfite solution having a concentration of 45 g/L sodium hydroxide solution and a concentration of 10 g/L, and the dissolution temperature is 20 ° C. The dissolution time is 50 min.
实施例11Example 11
本实施例与实施例8的区别在于:步骤C中,所述的碱液为浓度160g/L的氢氧化钠溶液;步骤D中,二硫化碳的加入量为步骤B制得的碱纤维素中甲纤含量的30%;所述的黄化反应时间控制在48min,黄化反应温度为26℃,所述的溶解是将纤维素磺酸酯与溶剂进行混合、搅拌和研磨,所述的溶剂包括浓度为30g/L氢氧化钠溶液和浓度为8g/L的亚硫酸钠水溶液,所述的溶解温度为15℃,溶解时间为44min。The difference between this embodiment and the embodiment 8 is that in the step C, the alkali liquid is a sodium hydroxide solution having a concentration of 160 g/L; in the step D, the carbon disulfide is added in the amount of the alkali cellulose obtained in the step B. 30% of the fiber content; the yellowing reaction time is controlled at 48 minutes, and the yellowing reaction temperature is 26 ° C. The dissolution is mixing, stirring and grinding the cellulose sulfonate with a solvent, and the solvent includes The concentration was 30 g/L sodium hydroxide solution and a sodium sulfite aqueous solution having a concentration of 8 g/L. The dissolution temperature was 15 ° C and the dissolution time was 44 min.
本实施例选用钛白粉作消光剂。In this embodiment, titanium dioxide is used as a matting agent.
实施例12Example 12
本实施例与实施例9的区别在于:步骤A中,浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1000,混合比例为4:2:1:1。The difference between this embodiment and the embodiment 9 is that in the step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1000, and the mixing ratio is 4:2:1:1.
步骤E中,所述的纺丝牵伸具体步骤如下:In step E, the specific steps of the spinning draft are as follows:
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴使用的凝固浴包括90g/L的硫酸、220g/L的硫酸钠和8g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified. The bath comprises 90 g/L of sulfuric acid, 220 g/L of sodium sulfate and 8 g/L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴使用的凝固浴包括18g/L的硫酸,所述一道牵伸机的牵伸率为50%;G: the tow after one bath is fed into the two bath by a drafting machine, the coagulation bath used in the two baths comprises 18 g/L of sulfuric acid, and the drafting ratio of the one drafting machine is 50%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述三浴使用的凝固浴包括pH值为1的硫酸,所述二道牵伸机的牵伸率为40%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, the coagulation bath used in the three baths includes sulfuric acid having a pH of 1, and the drafting ratio of the two drafting machines is 40%. ;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为5%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 5%.
实施例13Example 13
本实施例与实施例9的区别在于:步骤C中,所述的碱液为浓度190g/L的氢氧化钠溶液,反应器中纯氧的加入量为3%,降聚反应时间控制在50min。The difference between this embodiment and the embodiment 9 is that in the step C, the alkali solution is a sodium hydroxide solution having a concentration of 190 g/L, the amount of pure oxygen in the reactor is 3%, and the depolymerization reaction time is controlled at 50 min. .
步骤E中,所述的纺丝牵伸具体步骤如下:In step E, the specific steps of the spinning draft are as follows:
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴使用的凝固浴包括120g/L的硫酸、280g/L的硫酸钠和15g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified. The bath comprises 120 g/L of sulfuric acid, 280 g/L of sodium sulfate and 15 g/L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴使用的凝固浴包括18~22g/L的硫酸,所述一道牵伸机的牵伸率为60%;
G: the tow after one bath is fed into the two bath by a drafting machine, the coagulation bath used in the two baths comprises 18-22 g/L of sulfuric acid, and the drafting ratio of the one drafting machine is 60%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述三浴使用的凝固浴包括pH值为3的硫酸,所述二道牵伸机的牵伸率为45%;H: The tow after the two baths is sent to the three baths by a two-way drafting machine, and the coagulation bath used in the three baths includes sulfuric acid having a pH of 3, and the drafting ratio of the two drafting machines is 45%. ;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为8%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 8%.
本实施例中,所述的一浴温度为40℃、二浴温度为80℃、三浴温度为80℃。In this embodiment, the one bath temperature is 40 ° C, the two bath temperature is 80 ° C, and the three bath temperature is 80 ° C.
实施例14Example 14
本实施例与实施例13的区别在于:步骤E中,所述的后工序包括脱硫、漂白和上油,所述脱硫使用的脱硫剂由浓度为4g/L的硫化钠和浓度为4g/L的碳酸钠组成;所述漂白使用的漂白剂为浓度0.3g/L的双氧水;所述上油使用的油剂加入量为7g/L,上油后丝束的pH值为6.5。The difference between this embodiment and the embodiment 13 is that in the step E, the post-process includes desulfurization, bleaching and oiling, and the desulfurizing agent used in the desulfurization has a concentration of 4 g/L of sodium sulfide and a concentration of 4 g/L. The sodium carbonate composition is used; the bleaching agent used for the bleaching is hydrogen peroxide at a concentration of 0.3 g/L; the oil used for the oiling is added in an amount of 7 g/L, and the pH of the tow after oiling is 6.5.
所述的纺丝牵伸步骤如下:The spinning drafting steps are as follows:
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴使用的凝固浴包括100g/L的硫酸、250g/L的硫酸钠和10g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified. The bath comprises 100 g/L of sulfuric acid, 250 g/L of sodium sulfate and 10 g/L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴使用的凝固浴包括20g/L的硫酸,所述一道牵伸机的牵伸率为80%;G: the tow after one bath is fed into the two bath by a drafting machine, the coagulation bath used in the two baths comprises 20 g/L of sulfuric acid, and the drafting ratio of the one drafting machine is 80%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述三浴使用的凝固浴包括pH值为2的硫酸,所述二道牵伸机的牵伸率为50%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, the coagulation bath used in the three baths includes sulfuric acid having a pH of 2, and the drafting ratio of the two drafting machines is 50%. ;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为10%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 10%.
所述的一浴温度为50℃、二浴温度为85℃、三浴温度为80℃。The one bath temperature was 50 ° C, the two bath temperature was 85 ° C, and the three bath temperature was 80 ° C.
实施例15Example 15
本实施例与实施例12的区别在于:在所述的纺丝牵伸步骤中,所述的一浴温度为44℃、二浴温度为90℃、三浴温度为90℃;所述脱硫使用的脱硫剂由浓度为8g/L的硫化钠和浓度1g/L的碳酸钠组成;所述漂白使用的漂白剂为浓度0.6g/L的双氧水;所述上油使用的油剂加入量为9g/L,上油后丝束的pH值为7;所述的脱硫温度为50℃,脱硫时间为3min;所述的漂白温度为50℃,漂白时间为2min;所述油剂的温度为50℃。The difference between this embodiment and the embodiment 12 is that in the spinning drafting step, the bath temperature is 44 ° C, the two bath temperature is 90 ° C, and the three bath temperature is 90 ° C; the desulfurization is used. The desulfurizing agent is composed of sodium sulfide having a concentration of 8 g/L and sodium carbonate having a concentration of 1 g/L; the bleaching agent used for the bleaching is hydrogen peroxide at a concentration of 0.6 g/L; and the amount of the oil used for the oiling is 9 g. /L, the pH of the tow after oiling is 7; the desulfurization temperature is 50 ° C, the desulfurization time is 3 min; the bleaching temperature is 50 ° C, the bleaching time is 2 min; the temperature of the oil agent is 50 °C.
实施例16Example 16
一种消光型高强低伸粘胶纤维的制备方法,包括以下步骤:A method for preparing a matt high-strength low-stretch viscose fiber, comprising the following steps:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,所述的浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1100,混合比例为3:2:1:1;碱液的浓度为180g/L,温度为50℃,浸渍时间为55min;浸渍后经研磨机研磨,研磨时间为20s,研磨后制成浓度为4%,温度为45℃的浆粥;A: The pulp raw material is immersed in a dipping bucket containing a lye, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1100, and the mixing ratio is 3:2: 1:1; the concentration of the lye is 180g / L, the temperature is 50 ° C, the immersion time is 55min; after immersion, grinding by a grinder, the grinding time is 20s, after grinding, the slurry is prepared at a concentration of 4% and a temperature of 45 ° C Porridge
B:将步骤A制得的浆粥送至压榨机,压榨温度为60℃,压榨倍数为2.6倍,经压榨后送至粉碎机进行粉碎,粉碎度为120g/L,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为35%的浆粥;B: The porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, and the pulverization degree is 120 g/L to obtain alkali cellulose. The alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 35% is obtained;
C:将步骤B制得的浆粥与浓度为190g/L的碱液混合后送至反应器,在反应器中加2%的纯氧,降聚50min后获得聚合度为450、甲纤纯度为98.1%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye having a concentration of 190 g/L and sent to the reactor, and 2% pure oxygen is added to the reactor, and the degree of polymerization is 450, and the purity of the fiber is obtained after 50 minutes of depolymerization. 98.1% alkali cellulose;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入步骤B制得的碱纤维素中甲纤含量的35%的二硫化碳,在20℃下黄化45min后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,所述的溶剂为浓度为25g/L的氢氧化钠和浓度为5g/L的亚硫酸钠水溶液,溶解的温度为10℃,溶解时间为30min,制得浓度为9.5%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, and 35% of carbon disulfide in the alkali cellulose obtained in the step B is added to the yellowing machine, and after being yellowed at 20 ° C for 45 minutes, The cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 25 g/L and an aqueous solution of sodium sulfite having a concentration of 5 g/L, the dissolution temperature is 10 ° C, and the dissolution time is 30 min. , obtaining a cellulose sulfonate solution having a concentration of 9.5%;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入一定量的消光剂,本实施例的消光剂选用钛白粉,搅拌均匀后得到纺丝原液;E: after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴的温度为42℃,使用的凝固浴包括120g/L的硫酸、280g/L的硫酸钠和15g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 42 ° C, the coagulation bath used comprises 120 g / L of sulfuric acid, 280 g / L of sodium sulfate and 15 g / L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴的温度为80℃,使用的凝固浴包括20g/L的硫酸,所述一道牵伸机的牵伸率为60%;G: The tow after one bath is fed into a two bath by a drafting machine, the temperature of the two baths is 80 ° C, the coagulation bath used includes 20 g / L of sulfuric acid, and the drafting ratio of the one drafting machine 60%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述的三浴的温度为80℃,使用的凝固浴包括pH值为2的硫酸,所述二道牵伸机的牵伸率为45%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, the temperature of the three baths is 80 ° C, and the coagulation bath used includes sulfuric acid having a pH of 2, the two-way drafting machine The drafting rate is 45%;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为8%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 8%.
本实施例的后处理包括脱硫、漂白和上油和烘干。所述的脱硫使用的脱硫剂由浓度为5g/L的硫化钠和浓度为2g/L的碳酸钠组成,脱硫温度为55℃,脱硫时间为3min;所述漂白使用的漂白剂为浓度0.5g/L的双氧水,漂白温度为55℃,漂白时间为1min;所述上油使用的油剂加入量为8g/L,上油后丝束的pH值为7,油剂的温度为55℃;所述的后处理烘干是对纺丝牵伸形成的丝束进行的脱硫、漂白和上油后获得的丝束使用烘干机烘干,烘干温度为115℃,烘干后,得到消光型高强低伸粘胶纤维产品。The post treatment of this example includes desulfurization, bleaching, and oiling and drying. The desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 5 g/L and sodium carbonate having a concentration of 2 g/L, the desulfurization temperature is 55 ° C, the desulfurization time is 3 min; and the bleaching agent used for the bleaching is a concentration of 0.5 g. / L of hydrogen peroxide, bleaching temperature of 55 ° C, bleaching time of 1 min; the oil used to add oil is 8g / L, the pH of the tow after oiling is 7, the temperature of the oil is 55 ° C; The post-treatment drying is to perform desulfurization, bleaching and tow obtained after spinning the tow, and the tow obtained by the oiling is dried by a dryer, the drying temperature is 115 ° C, and after drying, the extinction is obtained. High-strength low-stretch viscose fiber products.
实施例17Example 17
一种消光型高强低伸粘胶纤维的制备方法,包括以下步骤:
A method for preparing a matt high-strength low-stretch viscose fiber, comprising the following steps:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,碱液的浓度为120g/L,温度为40℃,浸渍时间为60min;浸渍后经研磨机研磨,研磨时间为15s,研磨后制成浓度为4%,温度为45℃的浆粥;A: The pulp raw material is immersed in an immersion tank containing an alkali solution, the concentration of the alkali liquid is 120 g/L, the temperature is 40 ° C, and the immersion time is 60 min; after immersion, it is ground by a grinder, and the grinding time is 15 s, after grinding Preparing a porridge having a concentration of 4% and a temperature of 45 ° C;
B:将步骤A制得的浆粥送至压榨机,压榨温度为60℃,压榨倍数为2.6倍,经压榨后送至粉碎机进行粉碎,粉碎度为180g/L,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为32%的浆粥;B: The porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, and the pulverization degree is 180 g/L to obtain alkali cellulose. The alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 32% is obtained;
C:将步骤B制得的浆粥与浓度为150g/L的碱液混合后送至反应器,在反应器中加入10%的纯氧,降聚40min后获得聚合度为600、甲纤纯度为98%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye having a concentration of 150 g/L, and then sent to the reactor, 10% pure oxygen is added to the reactor, and the degree of polymerization is 600, and the purity of the fiber is obtained after 40 minutes of depolymerization. 98% alkali cellulose;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入步骤B制得的碱纤维素中甲纤含量的32%的二硫化碳,在26℃下黄化48min后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,所述的溶剂为浓度为35g/L的氢氧化钠和浓度为8g/L的亚硫酸钠水溶液,溶解的温度为15℃,溶解时间为40min,制得浓度为9.6%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, and 32% of the carbon fiber content of the alkali fiber in the alkali cellulose obtained in the step B is added to the yellowing machine, and after 48 minutes of yellowing at 26 ° C, The cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 35 g/L and an aqueous solution of sodium sulfite having a concentration of 8 g/L, the dissolution temperature is 15 ° C, and the dissolution time is 40 min. , obtaining a cellulose sulfonate solution having a concentration of 9.6%;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入一定量的消光剂,本实施例的消光剂选用钛白粉,搅拌均匀后得到纺丝原液;E: after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴的温度为40℃,使用的凝固浴包括120g/L的硫酸、280g/L的硫酸钠和15g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 40 ° C, the coagulation bath used comprises 120 g / L of sulfuric acid, 280 g / L of sodium sulfate and 15 g / L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴的温度为80℃,使用的凝固浴包括19g/L的硫酸,所述一道牵伸机的牵伸率为60%;G: The tow after one bath is fed into a two bath by a drafting machine, the temperature of the two bath is 80 ° C, the coagulation bath used includes 19 g / L of sulfuric acid, and the drafting ratio of the one drafting machine 60%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述的三浴的温度为80℃,使用的凝固浴包括pH值为2的硫酸,所述二道牵伸机的牵伸率为45%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, the temperature of the three baths is 80 ° C, and the coagulation bath used includes sulfuric acid having a pH of 2, the two-way drafting machine The drafting rate is 45%;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为8%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 8%.
本实施例的后处理包括脱硫、漂白和上油和烘干。所述的脱硫使用的脱硫剂由浓度为6g/L的硫化钠和浓度为3g/L的碳酸钠组成,脱硫温度为52℃,脱硫时间为2.5min;所述漂白使用的漂白剂为浓度0.5g/L的双氧水,漂白温度为50℃,漂白时间为2min;所述上油使用的油剂加入量为9g/L,上油后丝束的pH值为7,油剂的温度为53℃;所述的后处理烘干是对纺丝牵伸形成的丝束进行的脱硫、漂白和上油后获得的丝束使用烘干机烘干,烘干温度为75℃,烘干后,得到消光型高强低伸粘胶纤维产品。The post treatment of this example includes desulfurization, bleaching, and oiling and drying. The desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 6 g/L and sodium carbonate having a concentration of 3 g/L, the desulfurization temperature is 52 ° C, the desulfurization time is 2.5 min; and the bleaching agent used for the bleaching is a concentration of 0.5. g/L of hydrogen peroxide, bleaching temperature is 50 ° C, bleaching time is 2 min; the oil used in the oiling is 9 g / L, the pH of the tow after oiling is 7, the temperature of the oil is 53 ° C The post-treatment drying is to perform desulfurization, bleaching and tow obtained after spinning the tow, and the tow obtained after oiling is dried by a dryer, the drying temperature is 75 ° C, and after drying, Matte type high strength low stretch viscose fiber products.
步骤A中,所述浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为1200,混合比例为1:2:4:1。In the step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 1200, and the mixing ratio is 1:2:4:1.
实施例18Example 18
一种消光型高强低伸粘胶纤维的制备方法,包括以下步骤:A method for preparing a matt high-strength low-stretch viscose fiber, comprising the following steps:
A:将浆粕原料浸渍于装有碱液的浸渍桶中,碱液的浓度为120g/L,温度为40℃,浸渍时间为60min;浸渍后经研磨机研磨,研磨时间为15s,研磨后制成浓度为4%,温度为45℃的浆粥;A: The pulp raw material is immersed in an immersion tank containing an alkali solution, the concentration of the alkali liquid is 120 g/L, the temperature is 40 ° C, and the immersion time is 60 min; after immersion, it is ground by a grinder, and the grinding time is 15 s, after grinding Preparing a porridge having a concentration of 4% and a temperature of 45 ° C;
B:将步骤A制得的浆粥送至压榨机,压榨温度为60℃,压榨倍数为2.6倍,经压榨后送至粉碎机进行粉碎,粉碎度为130g/L,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为35%的浆粥;B: The porridge obtained in the step A is sent to a press, the pressing temperature is 60 ° C, the pressing multiple is 2.6 times, and after being pressed, it is sent to a pulverizer for pulverization, the pulverization degree is 130 g/L, and alkali cellulose is obtained. The alkali cellulose is sent to a crucible, and after treatment, a porridge having a concentration of 35% is obtained;
C:将步骤B制得的浆粥与浓度为150g/L的碱液混合后送至反应器,在反应器中加入5%的纯氧,降聚40min后获得聚合度为450、甲纤纯度为98.1%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye having a concentration of 150 g/L and sent to the reactor, and 5% pure oxygen is added to the reactor, and the degree of polymerization is 450, and the purity of the fiber is obtained after 40 minutes of depolymerization. 98.1% alkali cellulose;
D:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入步骤B制得的碱纤维素中甲纤含量的35%的二硫化碳,在26℃下黄化48min后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,所述的溶剂为浓度为35g/L的氢氧化钠和浓度为8g/L的亚硫酸钠水溶液,溶解的温度为15℃,溶解时间为40min,制得浓度为9.5%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, and 35% of carbon disulfide in the alkali cellulose obtained in the step B is added to the yellowing machine, and after being yellowed at 26 ° C for 48 minutes, The cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent, wherein the solvent is sodium hydroxide having a concentration of 35 g/L and an aqueous solution of sodium sulfite having a concentration of 8 g/L, the dissolution temperature is 15 ° C, and the dissolution time is 40 min. , obtaining a cellulose sulfonate solution having a concentration of 9.5%;
E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入一定量的消光剂,本实施例的消光剂选用钛白粉,搅拌均匀后得到纺丝原液;E: after the cellulose sulfonate solution prepared in the step D is filtered, defoamed, and matured, a certain amount of matting agent is added, and the matting agent of the present embodiment is selected from titanium dioxide, and the spinning dope is obtained after being uniformly stirred;
F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴的温度为42℃,使用的凝固浴包括100g/L的硫酸、230g/L的硫酸钠和10g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine through a bath to form a tow, and the temperature of the one bath is At 42 ° C, the coagulation bath used comprises 100 g / L of sulfuric acid, 230 g / L of sodium sulfate and 10 g / L of zinc sulfate;
G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴的温度为85℃,使用的凝固浴包括20g/L的硫酸,所述一道牵伸机的牵伸率为100%;G: The tow after one bath is fed into a two bath by a drafting machine, the temperature of the two bath is 85 ° C, the coagulation bath used includes 20 g / L of sulfuric acid, and the drafting ratio of the one drafting machine 100%;
H:经二浴后的丝束由二道牵伸机送入三浴,所述的三浴的温度为87℃,使用的凝固浴包括pH值为2的硫酸,所述二道牵伸机的牵伸率为60%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, the temperature of the three baths is 87 ° C, and the coagulation bath used includes sulfuric acid having a pH of 2, the two drafting machines The draw ratio is 60%;
I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为15%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 15%.
本实施例的后处理包括脱硫、漂白和上油和烘干。所述的脱硫使用的脱硫剂由浓度为5g/L的硫化钠和浓度为2g/L的碳酸钠组成,脱硫温度为55℃,脱硫时间为2min;所述漂白使用的漂白剂为浓度0.5g/L的双氧水,漂白温度为52℃,漂白时间为1min;所述上油使用的油剂加入量为8g/L,上油后丝束的pH值为7,油剂的温度为53℃;所述的后处理烘干是对纺丝牵伸形成的丝束进行的脱硫、漂白和上油后获得的
丝束使用烘干机烘干,烘干温度为95℃,烘干后,得到消光型高强低伸粘胶纤维产品。The post treatment of this example includes desulfurization, bleaching, and oiling and drying. The desulfurizing agent used for the desulfurization is composed of sodium sulfide having a concentration of 5 g/L and sodium carbonate having a concentration of 2 g/L, the desulfurization temperature is 55 ° C, the desulfurization time is 2 min; and the bleaching agent used for the bleaching is a concentration of 0.5 g. / L of hydrogen peroxide, bleaching temperature of 52 ° C, bleaching time of 1 min; the oil used to add oil is 8g / L, the pH of the tow after oiling is 7, the temperature of the oil is 53 ° C; The post-treatment drying is obtained after desulfurization, bleaching and oiling of the tow formed by the spinning drafting.
The tow is dried by a dryer, and the drying temperature is 95 ° C. After drying, a matt high-strength low-stretch viscose fiber product is obtained.
步骤A中,所述浆粕原料为棉浆、竹浆、木浆和麻浆的混合物,聚合度为650,混合比例为1:1:2:1。In the step A, the pulp raw material is a mixture of cotton pulp, bamboo pulp, wood pulp and hemp pulp, the degree of polymerization is 650, and the mixing ratio is 1:1:2:1.
将实施例3~18获得的粘胶纤维进行检测,指标统计如下,其中实施例3~10见表1,实施例11~18见表2,实施例3~18的粘胶纤维的指标值取平均值,再将该平均值分别与莫代尔纤维、差别化粘胶纤维(CN102296373A对比文件1、CN1632189对比文件2、CN102251301A对比文件3)以及普通粘胶纤维的测试指标进行比较见表3。The viscose fibers obtained in Examples 3 to 18 were tested, and the index statistics were as follows, wherein Examples 3 to 10 are shown in Table 1, Examples 11 to 18 are shown in Table 2, and the index values of the viscose fibers of Examples 3 to 18 were taken. The average value and the average value are compared with the test indexes of the modal fiber, the differentiated viscose fiber (CN102296373A comparison document 1, CN1632189 comparison document 2, CN102251301A comparison document 3) and ordinary viscose fiber, respectively, as shown in Table 3.
表1Table 1
表2Table 2
表3table 3
从表1、表2可知,实施例4、5、6制备获得的粘胶纤维产品主要运用于紧密赛络纺领域,生产高捻、高支纱产品,并以产品强度高适用于高捻等领域需求为特征;实施例10、11、12、13、14、15、16、17、18制备获得的粘胶纤维产品主要运用于生产内衣、高档梭织面料领域,并以产品手感丝滑柔软、舒适亲肤,以及成品织物尺寸稳定性好为特征;实施例8、9、10制备获得的粘胶纤维产品主要运用于牛仔面料领域,并以光亮、柔软,并以成品织物变型小为特征。It can be seen from Tables 1 and 2 that the viscose fiber products prepared in Examples 4, 5 and 6 are mainly used in the field of compact siro spinning, producing sorghum and high count yarn products, and are suitable for sorghum, etc. with high product strength. The field demand is characterized; the viscose fiber products obtained by the preparation of the examples 10, 11, 12, 13, 14, 15, 16, 17, 18 are mainly used in the production of underwear and high-grade woven fabrics, and the products are silky and soft to the touch. The comfort and skin-friendly, as well as the dimensional stability of the finished fabric are good; the viscose fiber products prepared in Examples 8, 9, and 10 are mainly used in the field of denim fabric, and are characterized by being bright, soft, and characterized by a small variation of the finished fabric. .
任意选取实施例3~18中制备而得的消光型高强低伸粘胶纤维产品,如实施例16,对其纤维切片进行显微镜截图,可发现,其截面保留有清晰的反应痕迹,其纤维皮层、芯层的颜色分别表现出了浅、深的差异,皮层明显偏浅,芯层偏深,(内层+中层):外层的“面积”比例为60:37,属于芯层:皮层=(40~70):(30~60)的范围内。The matte type high-strength low-stretch viscose fiber product prepared in Examples 3 to 18 was arbitrarily selected, and as shown in Example 16, the fiber section was subjected to microscopic screenshots, and it was found that the cross section retained clear reaction traces and the fiber cortex The color of the core layer shows a shallow and deep difference, the skin layer is obviously shallow, and the core layer is deep. (Inner layer + middle layer): The ratio of the "area" of the outer layer is 60:37, belonging to the core layer: cortex = (40 to 70): Within the range of (30 to 60).
通过对表3数据分析可知,本发明的高强低伸粘胶纤维具有区别于普通粘胶纤维、差别化粘胶纤维和莫代尔纤维的指标体系,本发明粘胶纤维的干断裂强度和湿断裂强度明显高于普通粘胶纤维,而伸长率明显低于普通粘胶纤维,通过工艺参数设置,使得本发明的粘胶纤维具有明显的二次反应界面,从而保证了与莫代尔相当的高强低伸的特性,而其径向水膨润度高于莫代尔纤维,具有比莫代尔更高的吸湿性,故亲肤性较莫代尔纤维好;本发明的粘胶纤维是一种新型的粘胶纤维,能够有效替代现有的莫代尔纤维和普通粘胶纤维,且生产成本更低,具有良好的经济和社会效益。
According to the data analysis of Table 3, the high-strength low-stretch viscose fiber of the present invention has an index system different from ordinary viscose fiber, differentiated viscose fiber and modal fiber, and the dry breaking strength and wet breaking strength of the viscose fiber of the present invention. It is obviously higher than ordinary viscose fiber, and the elongation is obviously lower than that of ordinary viscose fiber. Through the setting of process parameters, the viscose fiber of the invention has obvious secondary reaction interface, thereby ensuring high strength and low elongation equivalent to modal. The characteristic is that the radial water swelling degree is higher than that of the modal fiber, and has higher hygroscopicity than the modal, so the skin-friendly property is better than the modal fiber; the viscose fiber of the invention is a novel viscose fiber capable of It effectively replaces existing modal fibers and ordinary viscose fibers, and has lower production cost and good economic and social benefits.
以上所述,仅是本发明的较佳实施例,并非对本发明做任何形式上的限制,凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化,均落入本发明的保护范围之内。
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications and equivalent changes to the above embodiments in accordance with the technical spirit of the present invention fall within the scope of the present invention. Within the scope of protection.
Claims (21)
- 消光型高强低伸粘胶纤维,其特征在于:将浆粕原料依次经浸渍、研磨、压榨粉碎、搓揉、降聚、黄化、溶解、过滤、脱泡、熟成、纺丝牵伸和后处理后得到高强低伸粘胶纤维,该高强低伸粘胶纤维满足:The matting type high-strength low-stretch viscose fiber is characterized in that the pulp raw material is sequentially impregnated, ground, pressed, crushed, smashed, depolymerized, yellowed, dissolved, filtered, defoamed, matured, spun drawn and post-treated. After obtaining a high-strength low-stretch viscose fiber, the high-strength low-stretch viscose fiber satisfies:干断裂强度≥3.10cN/dtex;Dry breaking strength ≥ 3.10cN/dtex;湿断裂强度≥1.60cN/dtex;Wet breaking strength ≥ 1.60cN / dtex;湿状态下产生5%伸长率所需的强度≥0.55cN/dtex,The strength required to produce 5% elongation in wet state is ≥0.55 cN/dtex,干断裂伸长率11.0~19.0%;Dry elongation at break is 11.0 to 19.0%;湿断裂伸长率16.0~21.0%;Wet elongation at break is 16.0 to 21.0%;结晶度40.0~45.0%;Crystallinity 40.0 to 45.0%;径向水膨润度22~26%;Radial water swelling degree 22 to 26%;消光剂含量0.8~5%。The matting agent content is 0.8 to 5%.
- 根据权利要求1所述的消光型高强低伸粘胶纤维,其特征在于:所述的浆粕原料包括棉浆、竹浆、木浆、麻浆中的一种或者两种以上的组合。The matt high-strength low-extension viscose fiber according to claim 1, wherein the pulp raw material comprises one or a combination of two or more of cotton pulp, bamboo pulp, wood pulp, and hemp pulp.
- 根据权利要求1所述的消光型高强低伸粘胶纤维,其特征在于:所述浆粕原料的聚合度为650~1200。The matt high-strength low-extension viscose fiber according to claim 1, wherein the pulp raw material has a degree of polymerization of from 650 to 1200.
- 根据权利要求1~3任一项所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:该制备方法是将浆粕原料浸渍于碱液中,经研磨、压榨粉碎、搓揉、降聚,除去碱液后获得碱纤维素,将该碱纤维素黄化、溶解后制得纤维素磺酸酯溶液,纤维素磺酸酯溶液再经过滤、脱泡、熟成、纺丝牵伸和后处理后获得高强低伸粘胶纤维。The method for preparing a matting type high-strength low-stretch viscose fiber according to any one of claims 1 to 3, wherein the preparation method comprises immersing the pulp raw material in an alkali solution, grinding, crushing, smashing, smashing After depolymerization, alkali cellulose is obtained after removing the alkali solution, and the alkali cellulose is yellowed and dissolved to obtain a cellulose sulfonate solution, and the cellulose sulfonate solution is filtered, defoamed, matured, and spun. After stretching and post-treatment, high-strength low-stretch viscose fibers are obtained.
- 根据权利要求4所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:所述制备方法的步骤如下:The method for preparing a matting type high-strength low-stretch viscose fiber according to claim 4, wherein the steps of the preparation method are as follows:A:将浆粕原料浸渍于装有碱液的浸渍桶中,由研磨机研磨后制成浓度为3~6%的浆粥;A: immersing the pulp raw material in a dipping bucket containing an alkali solution, and grinding it by a grinder to prepare a porridge having a concentration of 3 to 6%;B:将步骤A制得的浆粥送至压榨机,经压榨后送至粉碎机进行粉碎,获得碱纤维素,将该碱纤维素送至揉搓机,处理后获得浓度为30~40%的浆粥;B: The porridge obtained in the step A is sent to a press, and after being pressed, it is sent to a pulverizer for pulverization to obtain alkali cellulose, and the alkali cellulose is sent to a crucible, and the concentration is 30-40% after the treatment. Pulp porridgeC:将步骤B制得的浆粥与碱液混合后送至反应器,在反应器中加入纯氧,降聚后获得聚合度为400~600、甲纤纯度为98.0~98.5%的碱纤维素;C: The porridge obtained in the step B is mixed with the lye and sent to the reactor, and pure oxygen is added to the reactor to obtain an alkali fiber having a polymerization degree of 400 to 600 and a purity of the fiber of 98.0 to 98.5% after depolymerization. PrimeD:将步骤C制得的碱纤维素送至黄化机,在黄化机中加入二硫化碳,经黄化反应后,将黄化反应得到的纤维素磺酸酯与溶剂溶解,制得浓度为9.0~10.0%的纤维素磺酸酯溶液;D: The alkali cellulose obtained in the step C is sent to a yellowing machine, carbon disulfide is added to the yellowing machine, and after the yellowing reaction, the cellulose sulfonate obtained by the yellowing reaction is dissolved in a solvent to obtain a concentration of 9.0 to 10.0% cellulose sulfonate solution;E:将步骤D制得的纤维素磺酸酯溶液经过滤、脱泡、熟成后,加入的消光剂得到纺丝原液,再将获得的纺丝原液经纺丝牵伸和后处理后制得粘胶纤维。E: After filtering, defoaming, and aging the cellulose sulfonate solution prepared in the step D, the spinning dope is added to obtain a spinning dope, and the obtained spinning dope is subjected to spinning drafting and post-treatment to obtain a viscosity. Glue fiber.
- 根据权利要求5所述的消光型高强低伸粘胶纤维制备方法,其特征在于:在所述的步骤A中,所述的碱液为浓度110~240g/L的氢氧化钠溶液,浸渍碱液的温度为30~60℃,浸渍时间为50~90min。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step A, the alkali liquid is a sodium hydroxide solution having a concentration of 110 to 240 g/L, and the alkali is impregnated. The temperature of the liquid is 30 to 60 ° C, and the immersion time is 50 to 90 minutes.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤A中,所述的研磨机设于连接浸渍桶与压榨机的管道内。The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein in the step A, the grinder is disposed in a pipe connecting the dipping bucket and the press.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤A中,所述浆粥的温度为30~60℃,所述研磨机的研磨时间为10~40s。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step A, the temperature of the porridge is 30 to 60 ° C, and the grinding time of the grinder It is 10 to 40 s.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤B中,所述压榨机的压榨温度为57~63℃、压榨倍数为2.2~2.8。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step B, the pressing temperature of the press is 57 to 63 ° C, and the pressing multiple is 2.2 to 2.8. .
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤B中,所述粉碎机的粉碎度为120~180g/L。The method for producing a matt high-strength low-extension viscose fiber according to claim 5, wherein in the step B, the pulverizer has a pulverization degree of 120 to 180 g/L.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤C中,所述的碱液为浓度140~200g/L的氢氧化钠溶液,反应器中纯氧的加入量为2~10%,降聚反应时间控制在30~60min。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step C, the alkali solution is a sodium hydroxide solution having a concentration of 140 to 200 g/L, and the reaction The amount of pure oxygen added in the device is 2-10%, and the depolymerization reaction time is controlled at 30-60 min.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤D中,二硫化碳的加入量为步骤B制得的碱纤维素中甲纤含量的25~37%。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step D, the amount of carbon disulfide added is 25 in the amount of the methyl cellulose in the alkali cellulose obtained in the step B. ~37%.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤D中,所述的黄化反应时间控制在45~50min,黄化反应温度为20~30℃。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 5, wherein in the step D, the yellowing reaction time is controlled at 45 to 50 minutes, and the yellowing reaction temperature is 20 ~30 ° C.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤D中,所述的溶解是将纤维素磺酸酯与溶剂进行混合、搅拌和研磨,所述的溶剂包括浓度为25~45g/L氢氧化钠溶液和浓度为5~10g/L的亚硫酸钠水溶液。The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein in the step D, the dissolving is mixing, stirring and grinding the cellulose sulfonate with a solvent. The solvent includes a sodium hydroxide solution having a concentration of 25 to 45 g/L and an aqueous sodium sulfite solution having a concentration of 5 to 10 g/L.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤D中,所述的溶解温度为10~20℃,溶解时间为30~50min。The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein in the step D, the dissolution temperature is 10 to 20 ° C, and the dissolution time is 30 to 50 min.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的步骤E中,所述的消光剂为钛白粉。The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein in the step E, the matting agent is titanium dioxide.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:所述的纺丝牵伸步骤 如下:The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein the spinning drafting step as follows:F:将纤维素磺酸酯溶液经过滤、脱泡、熟成后送至纺丝机,由纺丝机的喷头挤出纺丝细流经一浴后形成丝束,所述一浴使用的凝固浴包括90~120g/L的硫酸、220~280g/L的硫酸钠和8~15g/L的硫酸锌;F: the cellulose sulfonate solution is filtered, defoamed, and matured, and then sent to a spinning machine, which is extruded from a nozzle of a spinning machine and passed through a bath to form a tow, and the one bath is solidified. The bath comprises 90-120 g/L of sulfuric acid, 220-280 g/L of sodium sulfate and 8-15 g/L of zinc sulfate;G:经一浴后的丝束由一道牵伸机送入二浴,所述二浴使用的凝固浴包括18~22g/L的硫酸,所述一道牵伸机的牵伸率为50~100%;G: The tow after one bath is fed into the two bath by a drafting machine, the coagulation bath used in the two baths comprises 18-22 g/L of sulfuric acid, and the drafting ratio of the one drafting machine is 50-100. %;H:经二浴后的丝束由二道牵伸机送入三浴,所述三浴使用的凝固浴包括pH值为1~3的硫酸,所述二道牵伸机的牵伸率为40~60%;H: The tow after the two baths is fed into the three baths by a two-way drafting machine, and the coagulation bath used in the three baths includes sulfuric acid having a pH of 1 to 3, and the draft ratio of the two drafting machines is 40 to 60%;I:经三浴后的丝束由三道牵伸机送至后处理部分,所述三道牵伸机的牵伸率为5~15%。I: The tow after three baths was sent to the after-treatment portion by a three-way drafting machine, and the draft ratio of the three-way drafting machine was 5 to 15%.
- 根据权利要求17所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:在所述的纺丝牵伸步骤中,所述的一浴温度为40~50℃、二浴温度为80~90℃、三浴温度为80~90℃。The method for preparing a matting type high-strength low-extension viscose fiber according to claim 17, wherein in the spinning drawing step, the temperature of the one bath is 40 to 50 ° C, and the temperature of the two baths is 80 to 90 ° C, three bath temperature of 80 to 90 ° C.
- 根据权利要求5所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:所述的后处理包括对纺丝牵伸形成的丝束进行的脱硫、漂白和上油,所述脱硫使用的脱硫剂由浓度为4~8g/L的硫化钠和浓度为1~4g/L的碳酸钠组成;所述漂白使用的漂白剂为浓度0.3~0.6g/L的双氧水;所述上油使用的油剂加入量为7~9g/L,上油后丝束的pH值为6.5~7。The method for preparing a matt high-strength low-extension viscose fiber according to claim 5, wherein the post-treatment comprises desulfurization, bleaching and oiling the tow formed by the spinning draft, the desulfurization The desulfurizing agent used is composed of sodium sulfide having a concentration of 4 to 8 g/L and sodium carbonate having a concentration of 1 to 4 g/L; the bleaching agent used for the bleaching is hydrogen peroxide having a concentration of 0.3 to 0.6 g/L; The amount of the oil to be used is 7 to 9 g/L, and the pH of the tow after oiling is 6.5 to 7.
- 根据权利要求19所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:所述的脱硫温度为50~55℃,脱硫时间为2~3min;所述的漂白温度为50~55℃,漂白时间为1~2min;所述油剂的温度为50~55℃。The method for preparing a matt high-strength low-extension viscose fiber according to claim 19, wherein the desulfurization temperature is 50 to 55 ° C, the desulfurization time is 2 to 3 min, and the bleaching temperature is 50 to 55. °C, bleaching time is 1-2 minutes; the temperature of the oil agent is 50-55 °C.
- 根据权利要求19所述的消光型高强低伸粘胶纤维的制备方法,其特征在于:所述的后处理还包括烘干,烘干温度为75~115℃,烘干后,得到所述的消光型高强低伸粘胶纤维产品。 The method for preparing a matting type high-strength low-extension viscose fiber according to claim 19, wherein the post-treatment further comprises drying, the drying temperature is 75 to 115 ° C, and after drying, the obtained Matte type high strength low stretch viscose fiber products.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114481614A (en) * | 2021-12-29 | 2022-05-13 | 山东瑞礼健康科技有限公司 | Seaweed polyester composite fiber and preparation method and application thereof |
CN114540970A (en) * | 2022-03-21 | 2022-05-27 | 赛得利(中国)纤维有限公司 | Refreshing nonwoven cellulose fiber and preparation method thereof |
CN115011639A (en) * | 2022-07-27 | 2022-09-06 | 安徽师范大学 | Method for producing biogas by using wood fiber raw material |
CN116200842A (en) * | 2023-04-23 | 2023-06-02 | 江苏恒力化纤股份有限公司 | Method for spinning ultra-high performance Lyocell fiber by using waste cotton regenerated pulp |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104846459A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength low-elongation viscose fiber and preparation method thereof |
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Citations (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101289761A (en) * | 2008-06-10 | 2008-10-22 | 宜宾长毅浆粕有限责任公司 | Process for preparing dissolved pulp by oxidative decomposition of paper pulp |
CN101602810A (en) * | 2008-06-10 | 2009-12-16 | 宜宾海丝特纤维有限责任公司 | Plant fiber degrading and polymerizing technology |
CN101603210A (en) * | 2008-06-10 | 2009-12-16 | 宜宾海丝特纤维有限责任公司 | String is made the production method of viscose |
CN101851802A (en) * | 2010-05-24 | 2010-10-06 | 杭州奥通科技有限公司 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
CN103215680A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose extinction monofilament |
JP2013256720A (en) * | 2012-03-12 | 2013-12-26 | Daiwabo Holdings Co Ltd | Light ray-shielding regenerated cellulose fiber, method of manufacturing the same, and fiber structure |
CN103556281A (en) * | 2013-11-07 | 2014-02-05 | 唐山三友集团兴达化纤有限公司 | Method for producing high-wet-modulus regenerated cellulose fibers from bamboo pulp |
US20140227504A1 (en) * | 2013-02-08 | 2014-08-14 | Ivy Sau Chun LEE | Metalized yarn and method for making same |
CN104831393A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength viscose fiber and preparation method and application thereof |
CN104831387A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Preparation process of extinction high-strength low-elongation viscose fiber |
CN104831394A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength low-elongation viscose fiber and preparation method and application thereof |
CN104846459A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength low-elongation viscose fiber and preparation method thereof |
CN104846463A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Extinction type low-elongation viscose fiber and preparation method and application thereof |
CN104846454A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Delustering high-strength low-elongation viscose fiber and preparation method thereof |
CN104911726A (en) * | 2015-05-27 | 2015-09-16 | 宜宾丝丽雅集团有限公司 | Extinction superfine high-strength low-elongation viscose fiber and preparation method thereof |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0827620A (en) * | 1994-07-08 | 1996-01-30 | Kanebo Ltd | Production of acrylic synthetic fiber |
KR100601301B1 (en) * | 2000-07-04 | 2006-07-13 | 주식회사 코오롱 | A full dull polyester yarn, and a process of preparing for the same |
CN101024907A (en) * | 2007-03-23 | 2007-08-29 | 山东海龙股份有限公司 | High-wetness modulus adhesive colloid fiber and preparing method |
-
2015
- 2015-05-27 CN CN201510276644.8A patent/CN104846459A/en active Pending
-
2016
- 2016-04-21 WO PCT/CN2016/079847 patent/WO2016188274A1/en active Application Filing
Patent Citations (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101602810A (en) * | 2008-06-10 | 2009-12-16 | 宜宾海丝特纤维有限责任公司 | Plant fiber degrading and polymerizing technology |
CN101603210A (en) * | 2008-06-10 | 2009-12-16 | 宜宾海丝特纤维有限责任公司 | String is made the production method of viscose |
CN101289761A (en) * | 2008-06-10 | 2008-10-22 | 宜宾长毅浆粕有限责任公司 | Process for preparing dissolved pulp by oxidative decomposition of paper pulp |
CN101851802A (en) * | 2010-05-24 | 2010-10-06 | 杭州奥通科技有限公司 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
JP2013256720A (en) * | 2012-03-12 | 2013-12-26 | Daiwabo Holdings Co Ltd | Light ray-shielding regenerated cellulose fiber, method of manufacturing the same, and fiber structure |
US20140227504A1 (en) * | 2013-02-08 | 2014-08-14 | Ivy Sau Chun LEE | Metalized yarn and method for making same |
CN103215680A (en) * | 2013-04-08 | 2013-07-24 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose extinction monofilament |
CN103556281A (en) * | 2013-11-07 | 2014-02-05 | 唐山三友集团兴达化纤有限公司 | Method for producing high-wet-modulus regenerated cellulose fibers from bamboo pulp |
CN104831393A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength viscose fiber and preparation method and application thereof |
CN104831387A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Preparation process of extinction high-strength low-elongation viscose fiber |
CN104831394A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength low-elongation viscose fiber and preparation method and application thereof |
CN104846459A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Extinction type high-strength low-elongation viscose fiber and preparation method thereof |
CN104846463A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Extinction type low-elongation viscose fiber and preparation method and application thereof |
CN104846454A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Delustering high-strength low-elongation viscose fiber and preparation method thereof |
CN104911726A (en) * | 2015-05-27 | 2015-09-16 | 宜宾丝丽雅集团有限公司 | Extinction superfine high-strength low-elongation viscose fiber and preparation method thereof |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114481614A (en) * | 2021-12-29 | 2022-05-13 | 山东瑞礼健康科技有限公司 | Seaweed polyester composite fiber and preparation method and application thereof |
CN114540970A (en) * | 2022-03-21 | 2022-05-27 | 赛得利(中国)纤维有限公司 | Refreshing nonwoven cellulose fiber and preparation method thereof |
CN114540970B (en) * | 2022-03-21 | 2023-10-13 | 赛得利(中国)纤维有限公司 | Fresh non-woven cellulose fiber and preparation method thereof |
CN115011639A (en) * | 2022-07-27 | 2022-09-06 | 安徽师范大学 | Method for producing biogas by using wood fiber raw material |
CN116200842A (en) * | 2023-04-23 | 2023-06-02 | 江苏恒力化纤股份有限公司 | Method for spinning ultra-high performance Lyocell fiber by using waste cotton regenerated pulp |
CN116200842B (en) * | 2023-04-23 | 2023-08-29 | 江苏恒力化纤股份有限公司 | Method for spinning ultra-high performance Lyocell fiber by using waste cotton regenerated pulp |
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