CN114592253A - Polylactic acid filament and preparation method thereof - Google Patents
Polylactic acid filament and preparation method thereof Download PDFInfo
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- CN114592253A CN114592253A CN202210130466.8A CN202210130466A CN114592253A CN 114592253 A CN114592253 A CN 114592253A CN 202210130466 A CN202210130466 A CN 202210130466A CN 114592253 A CN114592253 A CN 114592253A
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 97
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000009987 spinning Methods 0.000 claims abstract description 66
- 239000000835 fiber Substances 0.000 claims abstract description 60
- 239000000155 melt Substances 0.000 claims abstract description 35
- 238000007664 blowing Methods 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 239000004595 color masterbatch Substances 0.000 claims abstract description 11
- 238000009998 heat setting Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 41
- 239000004576 sand Substances 0.000 claims description 16
- 238000007602 hot air drying Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 230000006855 networking Effects 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000009835 boiling Methods 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 5
- 239000004753 textile Substances 0.000 abstract description 4
- 239000004745 nonwoven fabric Substances 0.000 abstract description 3
- 238000004804 winding Methods 0.000 description 16
- 239000008041 oiling agent Substances 0.000 description 12
- 238000010998 test method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 5
- 238000004043 dyeing Methods 0.000 description 4
- 238000002074 melt spinning Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000005489 elastic deformation Effects 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000013520 petroleum-based product Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 241001589086 Bellapiscis medius Species 0.000 description 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 229920006240 drawn fiber Polymers 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
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Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
- D01D1/00—Treatment of filament-forming or like material
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/106—Filtering
-
- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- 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
- D01D5/08—Melt spinning methods
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
- D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/08—Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Fluid Mechanics (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention provides a polylactic acid filament and a preparation method thereof. The preparation method comprises the following steps: extruding and melting the dried polylactic acid slices and the optional color master batches by using a screw extruder to form a melt; filtering and spinning the melt by a spinning assembly in a spinning box to form melt filaments; cooling and molding the melt filament by using a circular blowing device, and simultaneously extracting monomers and oligomers by using a monomer suction device to form nascent fiber; oiling the nascent fiber, and then carrying out network treatment to obtain a pre-oriented polylactic acid filament; or oiling the as-spun fiber, and then sequentially carrying out network treatment and drawing heat setting to obtain the fully drawn polylactic acid filament. The polylactic acid filament provided by the invention has the advantages of low linear density deviation, high breaking strength, high yarn evenness and low boiling water shrinkage, and can be applied to the fields of textiles, non-woven fabrics, decorative materials, clothes and the like.
Description
Technical Field
The invention belongs to the technical field of polylactic acid spinning, and particularly relates to a polylactic acid filament and a preparation method thereof.
Background
Green textiles, biodegradable materials have become a focus of attention all over the world today. Polylactic acid (PLA) is used as a biodegradable high molecular polymer and is widely applied to the fields of medical treatment, medicine, agriculture, packaging, clothing industry and the like to replace the traditional materials. Polylactic acid is also a low energy consumption product, and the energy consumption is 30-50% lower than that of the polymer produced by using a substitute petroleum product as a raw material. Before the exhaustion period of the non-renewable petroleum resources comes, the market price of petroleum and derivatives thereof is soaring, and renewable products are bound to become a worldwide tense consumer product.
The polylactic acid fiber combines the excellent performances of natural fiber and synthetic fiber, and is a novel ecological fiber. Polylactic acid can be made into fibers by solution spinning and melt spinning. At present, dichloromethane, trichloromethane and toluene are commonly used as solvents for solution spinning, but the solvents are toxic, the spinning environment is severe, the process is complex, the solvent is difficult to recover, and the industrial production of the solvent is limited. Polylactic acid can also be melt-spun using melt-spinning equipment, and therefore, melt-spinning is more promising and becomes the mainstream of industrial production. The research on the polylactic acid spinning is earlier in foreign countries, and in contrast, the domestic polylactic acid production technology still belongs to the starting stage. At present, the production line for producing polylactic acid fiber in China is basically modified and perfected by key process equipment and flow on the basis of the original polyester fiber production line. However, the characteristics of the polylactic acid chip are significantly different from those of the polyester chip, which determines that the melt spinning process of polylactic acid and polyester is significantly different.
At present, the spinning technology of the domestic polylactic acid fiber is less researched, and the industrialized production method of the polylactic acid fiber still needs to be developed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a polylactic acid filament and a preparation method thereof. The polylactic acid filament provided by the invention has the advantages of low linear density deviation, high breaking strength, high yarn evenness and low boiling water shrinkage.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a polylactic acid filament, comprising the steps of:
(1) drying the polylactic acid slices;
(2) extruding and melting the dried polylactic acid slices and the optional color master batches by using a screw extruder to form a melt;
(3) filtering and spinning the melt by a spinning assembly in a spinning box to form melt filaments;
(4) cooling and molding the melt filament by using a circular blowing device, and simultaneously extracting monomers and oligomers by using a monomer suction device to form nascent fiber;
(5) oiling the nascent fiber, and then sequentially carrying out network treatment through a pre-network device, a godet roller and a main network device to obtain a pre-oriented (POY) polylactic acid filament;
or oiling the nascent fiber, sequentially carrying out network treatment by a pre-network device, a godet roller and a main network device, and sequentially carrying out drafting and heat setting by a first hot roller, a second hot roller and a third hot roller to obtain Fully Drawn (FDY) polylactic acid filament.
It should be noted that, the "optional color masterbatch" in step (2) means the presence or absence of color masterbatch.
The invention adopts a circular blowing system and a monomer suction device to cool and form melt filaments. Compared with a side blowing system, the filament produced by the circular blowing system has lower evenness (more uniform thickness degree in the longitudinal direction of the filament) and is more favorable for the subsequent processing. The monomer suction system can be used for sucking the degraded small monomers or oligomers away from the spinneret surface at any time, so that the phenomenon of filament breakage or filament floating in the spinning process due to the existence of the monomers is prevented.
In some embodiments of the invention, the drying method in step (1) is: drying with a drum dryer, and continuously drying with a hot air drying tower.
In some embodiments of the present invention, the drum dryer adopts a step drying manner, and the drum dryer is firstly dried at 95-100 ℃ for 3h, then dried at 100-105 ℃ for 3h, and finally dried at 105-110 ℃ for 3 h.
In some embodiments of the present invention, the water content of the polylactic acid chip after drying by the drum dryer is less than or equal to 100 ppm.
In some embodiments of the invention, the temperature of the hot air drying tower is 95-105 ℃, for example, 95 ℃, 96 ℃, 98 ℃, 100 ℃, 102 ℃, 103 ℃ or 105 ℃ and the like; the drying time is 8-10h, for example, 8h, 8.5h, 9h, 9.5h or 10 h.
In some embodiments of the present invention, the water content of the polylactic acid slices after drying in the hot air drying tower is less than or equal to 20 ppm.
According to the invention, the rotary drum dryer is firstly used for drying, polylactic acid slices with different water contents can be dried to the same water content level, and then the hot air drying tower is used for continuous drying, so that the primarily dried polylactic acid slices can be simultaneously dried on the same water content level, each polylactic acid slice can simultaneously reach the water content required by the process, and the drying time is shortened.
In some embodiments of the present invention, the temperature of the extrusion melting in step (2) is 220-240 ℃; for example, the temperature may be 220 ℃, 222 ℃, 225 ℃, 228 ℃, 230 ℃, 232 ℃, 235 ℃, 238 ℃, 240 ℃ or the like.
In some embodiments of the present invention, in the filtering in step (3), 5 layers of filter screen layers are used in the assembly, the filter screen mesh number is 50-200 meshes, and the filtering sand is mixed metal sand of 60 meshes and 80 meshes.
In some embodiments of the invention, the pressure of the spin pack assembly is 6 to 16 Mpa.
When a melt passes through micropores of a spinneret orifice after being melted and extruded by a screw extruder, if the melt contains gel particles, impurities and other particles with larger sizes, the micropores can be blocked, so that the micropores are abnormal, thick threads and defects are generated, and the product quality is seriously influenced. The polylactic acid spinning temperature is lower than the polyester spinning temperature, and the high requirements of polylactic acid filament fibers on the quality uniformity and purity of a melt are met by selecting the filtering conditions, so that the stable product quality is ensured, and the service cycle of the assembly is ideal.
In some embodiments of the present invention, the temperature of the spinning beam in step (3) is 220-240 ℃; for example, the temperature may be 220 ℃, 222 ℃, 225 ℃, 228 ℃, 230 ℃, 232 ℃, 235 ℃, 238 ℃, 240 ℃ or the like.
As the micropores of the spinneret plate of the spinning manifold are fine, the flow resistance of the melt in the component is increased and the flow performance is poor due to the increase of the layer number and the mesh number of the filter screen of the component. Further, the melt quality is required to satisfy the requirements of viscosity uniformity and reduction of the generation of agglomerated particles, and therefore, the control of the spinning temperature is very important. In the invention, the temperature of the screw and the box body is controlled to be 220-240 ℃, the formed melt has good fluidity, the high elastic deformation relaxation time can be shortened, the melt expansion effect can be reduced, and the melt fracture can be prevented. However, the spinning temperature should not be too high, otherwise the melt is easily degraded seriously, and the normal spinning can not be ensured.
In some embodiments of the present invention, the spinning rate in step (3) is 2800-3600 m/min; for example, 2800m/min, 2900m/min, 3000m/min, 3100m/min, 3200m/min, 3300m/min, 3400m/min, 3500m/min, 3600m/min, or the like can be used. The spinning rate is related to the fiber orientation crystallization rate, affecting the elongation at break and tenacity of the fiber.
In some embodiments of the present invention, the circular blowing device in the step (4) is a double-row circular blowing device. Double ring blast apparatus reforms transform on single ring blast apparatus's basis, compares single ring blast apparatus, and double ring blast apparatus can arrange more spinning positions in limited space, helps improving production efficiency.
In some embodiments of the present invention, the air pressure of the circular blowing device in step (4) is 300-650pa (for example, 300pa, 350pa, 400pa, 450pa, 500pa, 550pa, 600pa, 650pa, etc.), the air temperature is 20-22 ℃ (for example, 20 ℃, 20.2 ℃, 20.5 ℃, 20.8 ℃, 21 ℃, 21.2 ℃, 21.5 ℃, 21.8 ℃, or 22 ℃, etc.), and the air speed is 0.3-0.7m/s (for example, 0.3m/s, 0.35m/s, 0.4m/s, 0.45m/s, 0.5m/s, 0.55m/s, 0.6m/s, 0.65m/s, or 0.7m/s, etc.).
In the invention, the high or low wind speed can cause high section unevenness (DVC) of the protofilament. If the wind speed is too low, the cooling and solidifying speed difference on the section of the nascent fiber is small, and the self-rolling effect is poor; if the wind speed is too high, the yarn strip disturbance is big, is unfavorable for spinning, draft, and too high wind speed can make the nascent fibre pre-orientation degree on the high side moreover to produce transition draft in the draft, lead to broken filament, broken end, kinking roller to increase, the draft process can not normally go on, still can lead to macromolecule contractility to reduce, is unfavorable for the coiling.
In some embodiments of the invention, the pre-network has a pressure of 0.05-0.1MPa (e.g., 0.05MPa, 0.06MPa, 0.07MPa, 0.08MPa, 0.09MPa, 0.1MPa, etc.), and the main network has a pressure of 0.15-0.2MPa (e.g., 0.15MPa, 0.16MPa, 0.17MPa, 0.18MPa, 0.19MPa, 0.2MPa, etc.).
The pre-network device and the main network device are collectively called as the network device, have similar functions and are used for adding the network to a bundle of scattered filaments. A plurality of filaments are arranged in one bundle of filaments, the bundle of filaments is fluffy and loose under the condition of no twisting, a holding point is formed on the bundle of filaments at a certain distance by using compressed air, and the holding point is a network point. According to different air pressures of network points, the network is divided into a pre-network device and a main network device.
In some embodiments of the present invention, the temperature of the drawing heat setting in the step (5) is 70-110 ℃ (for example, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃ or 110 ℃ can be adopted).
When the nascent fiber is stretched at low temperature, large tensile stress can be generated, and the stretching temperature is far lower than TgStress relaxation can not take place, and stress makes the molecule mobility strengthen, and the high-elastic deformation of force leads to the fibre orientation degree high, and excessive orientation can reduce the contractility that macromolecule stress relaxes, influences the coiling shaping effect, also makes fluffiness decline simultaneously, can produce broken filaments and broken ends even. And when the fiber is stretched at high temperature, the tensile stress is small, the plastic deformation of the fiber is increased, the high elastic deformation is reduced, the tensile property of the whole fiber is consistent, the internal stress difference and the molecular structure difference are reduced, and the effect of inhibiting the network is achieved. Therefore, the drawing temperature is controlled to be higher than the glass transition temperature of the polylactic acid fiber, and the drawing temperature is controlled to be 70-110 ℃ in the invention.
In some embodiments of the invention, the draw heat-set has a total draw ratio of 1.2 to 2.4 times (e.g., can be 1.2 times, 1.3 times, 1.5 times, 1.6 times, 1.8 times, 2 times, 2.1 times, 2.3 times, or 2.4 times, etc.), and the draw ratio between the first and second heated rolls is 80 to 90% of the total draw ratio (e.g., can be 80%, 82%, 84%, 85%, 86%, 88%, or 90%, etc.).
The draft ratio is selected between the maximum draw ratio of the as-spun fiber and the natural draw ratio. If the draw ratio is less than the natural draw ratio, the thin neck in the drawn fiber does not extend to the whole fiber, and more undrawn yarns are inevitably contained, so that the fiber has no practical value; when the draw ratio reaches the maximum ratio, the fibers are broken. When the drafting multiplying power is smaller, the difference of the microstructure of the fiber section is not enough to be drawn, and the network effect cannot be fully reflected; if the draft magnification is too large, the axial alignment uniformity of macromolecules will be accelerated, and the self-rolling capability will be reduced. In the invention, on the premise of meeting the product quality, the drafting multiplying power is controlled to be 1.2-2.4.
Due to the difference of microstructures in the nascent fibers, after the external force disappears due to macromolecular plastic deformation existing after stretching, the high elastic deformation relaxes to generate different shrinkage effects, so that the tows twist around the axial direction to form a spiral network effect.
In some embodiments of the invention, the temperature of the first hot roll is 88-98 deg.C (e.g., 88 deg.C, 90 deg.C, 92 deg.C, 95 deg.C, or 98 deg.C), the temperature of the second hot roll is 98-108 deg.C (e.g., 98 deg.C, 100 deg.C, 102 deg.C, 105 deg.C, or 108 deg.C), and the temperature of the third hot roll is 108-110 deg.C.
The action of the hot rolls is to further draw and set the tow. The high temperature can make the tows easier to draft, and the drafted tows can be well shaped. The invention can make the temperature rise and the drafting of the filament bundle more uniform by arranging three pairs of hot rollers with gradually increased temperature and rotating speed, and is beneficial to reducing the occurrence of filament breakage.
In some embodiments of the invention, the pre-oriented polylactic acid filaments have an oil content of 0.50 to 0.90 wt%; for example, it may be 0.50 wt%, 0.55 wt%, 0.6 wt%, 0.65 wt%, 0.7 wt%, 0.75 wt%, 0.8 wt%, 0.85 wt%, 0.90 wt%, or the like.
In some embodiments of the invention, the fully drawn polylactic acid filament has an oil content of 1.0 ± 0.2 wt%.
In some embodiments of the invention, the method of making further comprises winding the prepared polylactic acid filament into a cake. For the pre-oriented polylactic acid filament, the winding speed is preferably 2800-3200 m/min; for fully drawn polylactic acid filaments, the winding rate is preferably 3000-3600 m/min.
In the invention, the pre-oriented polylactic acid filament yarn can be further sequentially processed by a yarn cutter, a first roller, a texturing hot box, a cooling plate, a false twister, a second roller, a setting hot box, a network nozzle, a third roller, an oiling roller and winding to prepare a Draw Textured (DTY) polylactic acid filament yarn.
In a second aspect, the present invention provides a polylactic acid filament prepared by the preparation method of the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
the linear density deviation of the POY polylactic acid filament provided by the invention is within +/-0.8%, the breaking strength is more than or equal to 2.2cN/dtex, and the yarn evenness CV value is less than or equal to 1.0%. The provided FDY polylactic acid filament has the linear density deviation within +/-0.7%, the breaking strength of more than or equal to 3.0cN/dtex, the boiling water shrinkage rate of 20-30% and the dyeing uniformity of more than or equal to 4 grade. The polylactic acid filament has the characteristics of environmental protection, no toxicity, antibiosis, flame retardance and degradability, can replace petroleum-based products, and can be widely applied to the fields of textiles, non-woven fabrics, decorative materials, clothes and the like.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The main material sources used in the examples of the invention are as follows:
slicing polylactic acid: FY601 brand of the Anhui Fengyuan Futelai polylactic acid Co., Ltd, the viscosity is 1.4 +/-0.02 dL/g, and the melting point is 170 +/-5 ℃;
oil solution: POY-F-3099# and FDY/DT-F-1768# of Japan bamboo products.
Example 1
This example provides an 84dtex/72f circular cross-section POY polylactic acid filament, its preparation method is as follows:
(1) adding the polylactic acid slices into a drum dryer, firstly drying for 3h at 95 ℃, then drying for 3h at 100 ℃, and finally drying for 3h at 110 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 8 hours at 103 ℃, and the water content of the slices is measured to be less than 20 ppm;
(2) feeding the dried polylactic acid slices into a screw extruder, and extruding and melting at the screw temperature of 220 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtration and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 220 ℃, the diameter of a spinneret plate is 80mm, the diameter of micropores is 0.25mm/72f, and the spinning speed is 25.2 g/min;
(4) the melt filaments enter a double-row circular blowing device for cooling and forming, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fibers;
wherein the wind pressure of the double-row circular blowing device is 300pa, the wind temperature is 22 ℃, and the wind speed is 0.3 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is POY-F-3099#, and the oil content is controlled to be 0.50 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer for network treatment to obtain a POY polylactic acid filament;
wherein each tow contains 72 nascent fiber filaments, the air pressure of the pre-interlacer is 0.05MPa, the air pressure of the main interlacer is 0.15MPa, the rotating speed of the godet roller is 3000m/min, and the tension generated by the godet roller is 12 g;
(7) the POY polylactic acid filament is wound into a spinning cake through a winding device at a winding speed of 3000 m/min.
Example 2
This example provides a 115dtex/72f circular cross-section POY polylactic acid filament, the preparation method is as follows:
(1) adding the polylactic acid slices into a drum dryer, drying for 3.5h at 97 ℃, then drying for 3.5h at 103 ℃, and finally drying for 3.5h at 107 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 10 hours at the temperature of 95 ℃, and the water content of the slices is measured to be less than 20 ppm;
(2) feeding the dried polylactic acid slices into a screw extruder, and extruding and melting at the screw temperature of 240 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtration and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 240 ℃, the diameter of a spinneret plate is 80mm, the diameter of micropores is 0.25mm/72f, and the spinning speed is 34.5 g/min;
(4) the melt filament enters a double-row circular blowing device for cooling and molding, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fiber;
wherein, the wind pressure of the double-row circular blowing device is 650pa, the wind temperature is 20 ℃, and the wind speed is 0.7 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is POY-F-3099#, and the oil content is controlled to be 0.90 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer for network treatment to obtain a POY polylactic acid filament;
wherein each tow contains 72 nascent fiber filaments, the air pressure of the pre-interlacer is 0.1MPa, the air pressure of the main interlacer is 0.2MPa, the rotating speed of the godet roller is 3000m/min, and the tension generated by the godet roller is 17 g;
(7) the POY polylactic acid filament is wound into a spinning cake through a winding device at a winding speed of 3000 m/min.
Example 3
The embodiment provides a 167dtex/48f circular section POY polylactic acid filament, and the preparation method thereof is as follows:
(1) adding the polylactic acid slices into a drum dryer, firstly drying for 3h at 95 ℃, then drying for 3h at 105 ℃, and finally drying for 3h at 110 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 10 hours at the temperature of 100 ℃, and the water content of the slices is measured to be less than 20 ppm; drying the blue color master batch in a color master batch injection machine for 6 hours at 120 ℃;
(2) feeding the dried polylactic acid slices and the blue color master batch into a screw extruder according to the mass ratio of 50:1, and extruding and melting at the screw temperature of 230 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtration and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 220 ℃, the diameter of a spinneret plate is 80mm, the diameter of micropores is 0.3mm/48f, and the spinning speed is 46.8 g/min;
(4) the melt filaments enter a double-row circular blowing device for cooling and forming, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fibers;
wherein the wind pressure of the double-row circular blowing device is 400pa, the wind temperature is 21 ℃, and the wind speed is 0.5 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is POY-F-3099#, and the oil content is controlled to be 0.70 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer for network treatment to obtain a POY polylactic acid filament;
wherein each tow contains 48 nascent fiber filaments, the air pressure of the pre-networking device is 0.08MPa, the air pressure of the main networking device is 0.18MPa, the rotating speed of the godet roller is 2800m/min, and the tension generated by the godet roller is 22 g;
(7) the POY polylactic acid filament is wound into a spinning cake through a winding device at the winding speed of 2800 m/min.
Example 4
The embodiment provides an FDY polylactic acid filament with a circular section of 222dtex/36f, and a preparation method thereof is as follows:
(1) adding the polylactic acid slices into a drum dryer, firstly drying for 3h at 95 ℃, then drying for 3h at 105 ℃, and finally drying for 3h at 110 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 10 hours at 103 ℃, and the water content of the slices is measured to be less than 20 ppm;
(2) feeding the dried polylactic acid slices into a screw extruder, and extruding and melting at the screw temperature of 225 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtration and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 225 ℃, the diameter of a spinneret plate is 80mm, the diameter of micropores is 0.3mm/36f, and the spinning speed is 66.6 g/min;
(4) the melt filaments enter a double-row circular blowing device for cooling and forming, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fibers;
wherein the wind pressure of the double-row circular blowing device is 500pa, the wind temperature is 22 ℃, and the wind speed is 0.4 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is FDY/DT-F-1768#, and the oil content is controlled to be 2.0 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer to be subjected to network treatment;
wherein each tow contains 36 nascent fiber filaments, the air pressure of the pre-interlacer is 0.1MPa, the air pressure of the main interlacer is 0.2MPa, the rotating speed of the godet roller is 3000m/min, and the tension generated by the godet roller is 17 g;
(7) the filament bundle after the network treatment is subjected to drawing and heat setting sequentially through a first hot roller, a second hot roller and a third hot roller to obtain an FDY polylactic acid filament;
wherein the temperature of the first hot roller is 90 ℃, and the rotating speed is 2500 m/min; the temperature of the second hot roller is 100 ℃, and the rotating speed is 2700 m/min; the temperature of the third hot roller is 109 ℃, and the rotating speed is 3000 m/min; the total drafting multiplying power is 1.2 times;
(8) the FDY polylactic acid filament is wound into a spinning cake at the winding speed of 3000m/min by a winding device.
Example 5
The embodiment provides an FDY polylactic acid filament with a circular section of 84dtex/72f, and the preparation method comprises the following steps:
(1) adding the polylactic acid slices into a drum dryer, firstly drying for 3h at 95 ℃, then drying for 3h at 105 ℃, and finally drying for 3h at 110 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 10 hours at 103 ℃, and the water content of the slices is measured to be less than 20 ppm;
(2) feeding the dried polylactic acid slices into a screw extruder, and extruding and melting at the screw temperature of 240 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtration and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 230 ℃, the diameter of a spinneret plate is 80mm, the diameter of micropores is 0.25mm/72f, and the spinning speed is 28.6 g/min;
(4) the melt filaments enter a double-row circular blowing device for cooling and forming, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fibers;
wherein, the wind pressure of the double-row circular blowing device is 600pa, the wind temperature is 20 ℃, and the wind speed is 0.6 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is FDY/DT-F-1768#, and the oil content is controlled to be 1.0 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer to be subjected to network treatment;
wherein each tow contains 72 nascent fiber filaments, the air pressure of the pre-interlacer is 0.1MPa, the air pressure of the main interlacer is 0.2MPa, the rotating speed of the godet roller is 3400m/min, and the tension generated by the godet roller is 20 g;
(7) the filament bundle after the network treatment is subjected to drawing and heat setting sequentially through a first hot roller, a second hot roller and a third hot roller to obtain an FDY polylactic acid filament;
wherein the temperature of the first hot roller is 88 ℃, and the rotating speed is 1417 m/min; the temperature of the second hot roller is 98 ℃, and the rotating speed is 2992 m/min; the temperature of the third hot roller is 108 ℃, and the rotating speed is 3400 m/min; the total drafting multiplying power is 2.4 times;
(8) the FDY polylactic acid filament is wound into a spinning cake at the winding speed of 3400m/min by a winding device.
Example 6
The embodiment provides 167dtex/48f FDY (fully drawn yarn) polylactic acid filament with a circular section, and the preparation method comprises the following steps:
(1) adding the polylactic acid slices into a drum dryer, firstly drying for 3h at 95 ℃, then drying for 3h at 105 ℃, and finally drying for 3h at 110 ℃; then the slices are transferred into a hot air drying tower and are continuously dried for 10 hours at 103 ℃, and the water content of the slices is measured to be less than 20 ppm; drying the blue color master batch in a color master batch injection machine for 6 hours at 120 ℃;
(2) feeding the dried polylactic acid slices and the blue color master batch into a screw extruder according to the mass ratio of 50:1, and extruding and melting at the screw temperature of 235 ℃ to form a melt;
(3) the melt is sent into a spinning assembly in a spinning box body through a conveying pipeline for filtering and spinning to form melt filaments;
wherein, the number of the filter screen layers of the component is 5, the mesh number of the filter screen is 200 meshes, the filter sand is mixed with metal sand of 60 meshes and 80 meshes, and the pressure of the component is 16 Mpa;
wherein the temperature of the spinning manifold is 235 ℃, the diameter of a spinneret plate is 80mm, the diameter of a micropore is 0.3mm/48f, and the spinning speed is 53.4 g/min;
(4) the melt filaments enter a double-row circular blowing device for cooling and forming, and simultaneously a monomer suction device is used for pumping out monomers and oligomers to form nascent fibers;
wherein the wind pressure of the double-row circular blowing device is 500pa, the wind temperature is 22 ℃, and the wind speed is 0.5 m/s;
(5) oiling the nascent fiber through an oiling agent nozzle, wherein the oiling agent is FDY/DT-F-1768#, and the oil content is controlled to be 1.5 wt%;
(6) the oiled nascent fiber passes through a tow channel and then sequentially passes through a pre-interlacer, a godet roller and a main interlacer to be subjected to network treatment;
wherein each tow contains 48 nascent fiber filaments, the air pressure of the pre-interlacer is 0.1MPa, the air pressure of the main interlacer is 0.2MPa, the rotating speed of the godet roller is 3200m/min, and the tension generated by the godet roller is 20 g;
(7) the filament bundle after the network treatment is subjected to drawing and heat setting sequentially through a first hot roller, a second hot roller and a third hot roller to obtain an FDY polylactic acid filament;
wherein the temperature of the first hot roller is 98 ℃, and the rotating speed is 1778 m/min; the temperature of the second hot roller is 108 ℃, and the rotating speed is 2800 m/min; the temperature of the third hot roller is 110 ℃, and the rotating speed is 3200 m/min; the total drafting multiplying power is 1.8 times;
(8) the FDY polylactic acid filament is wound into a spinning cake at the winding speed of 3200m/min by a winding device.
Comparative example 1
The difference from example 1 is only that the cooling molding is performed using a side blowing device in step (5).
Comparative example 2
The only difference from example 1 is that in step (1), the polylactic acid chips were directly fed into a hot air drying tower and continuously dried at 103 ℃ for 17 hours. The water content of the sections was found to be >20 ppm.
Comparative example 3
The only difference from example 1 is that in step (1) drying was carried out using only a drum dryer, first for 5h at 95 ℃, then for 6h at 100 ℃ and finally for 6h at 110 ℃. The water content of the sections was found to be >20 ppm.
And (3) performance testing:
the polylactic acid POY/FDY filaments obtained in the above examples and comparative examples were tested for their properties according to the following test criteria:
deviation of linear density: the test method refers to the national standard GB/T14343-2008 chemical fiber filament linear density test method.
Breaking strength: the test method refers to the national standard GB/T14344-2008 chemical fiber filament tensile property test method.
Evenness unevenness: the test method refers to the national standard GB/T14346 2015 test method for the electronic evenness unevenness of chemical fiber filaments.
Shrinkage in boiling water: the test method refers to the national standard GB/T6505-.
Dyeing uniformity (grey card): the test method refers to the national standard GB/T6508-2015 polyester filament dyeing uniformity test method.
Wherein, the performance evaluation indexes of the POY polylactic acid filament are shown in the following table 1:
TABLE 1
The performance evaluation index of the FDY polylactic acid filament executes the standard FZ/T54098-2017 polylactic acid drawing filament, and the standard content is shown in the following table 2:
TABLE 2
The results of the above tests are shown in table 3 below:
TABLE 3
As can be seen from Table 3, the linear density deviation of the polylactic acid POY filament provided by the invention is within +/-0.8%, the breaking strength is more than or equal to 2.2cN/dtex, and the yarn evenness CV value is less than or equal to 1.0%. The linear density deviation of the polylactic acid FDY filament is within +/-0.7%, the breaking strength is more than or equal to 3.0cN/dtex, the boiling water shrinkage is 20-30%, and the dyeing uniformity is more than or equal to 4 level. The polylactic acid POY/FDY filament provided by the invention has the characteristics of environmental protection, no toxicity, antibiosis, flame retardance and degradability, can replace petroleum-based products, and can be widely applied to the fields of textiles, non-woven fabrics, decorative materials, clothes and the like.
Wherein, in comparison with example 1, comparative example 1 was subjected to cooling molding using a side-blowing device, and the water content of the chips of comparative examples 2 and 3 was high, both resulted in a significant increase in the linear density deviation and the evenness unevenness of the obtained polylactic acid POY filaments, and a significant decrease in the breaking strength.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of polylactic acid filament is characterized by comprising the following steps:
(1) drying the polylactic acid slices;
(2) extruding and melting the dried polylactic acid slices and the optional color master batches by using a screw extruder to form a melt;
(3) filtering and spinning the melt by a spinning assembly in a spinning box to form melt filaments;
(4) cooling and forming the melt filaments by using a circular blowing device, and simultaneously pumping out monomers and oligomers by using a monomer suction device to form nascent fibers;
(5) oiling the nascent fiber, and then sequentially carrying out network treatment through a pre-network device, a godet roller and a main network device to obtain a pre-oriented polylactic acid filament;
or oiling the nascent fiber, sequentially performing network treatment by a pre-network device, a yarn guide roller and a main network device, and sequentially performing drafting and heat setting by a first hot roller, a second hot roller and a third hot roller to obtain the fully-drawn polylactic acid filament.
2. The method according to claim 1, wherein the drying in step (1) is performed by: drying by a drum dryer, and then continuously drying by a hot air drying tower;
preferably, the rotary drum dryer adopts a step drying mode, firstly drying at 95-100 ℃ for 3h, then drying at 100-105 ℃ for 3h, and finally drying at 105-110 ℃ for 3 h;
preferably, the water content of the polylactic acid slices dried by the drum dryer is less than or equal to 100 ppm;
preferably, the temperature of the hot air drying tower is 95-105 ℃, and the drying time is 8-10 h;
preferably, the water content of the polylactic acid slices dried by the hot air drying tower is less than or equal to 20 ppm.
3. The method as claimed in claim 1 or 2, wherein the temperature of the extrusion melting in step (2) is 220-240 ℃.
4. The production method according to any one of claims 1 to 3, wherein, in the filtration in the step (3), 5 layers of filter screens are used as a component, the number of the filter screens is 50 to 200 meshes, and the filter sand is mixed metal sand of 60 meshes and 80 meshes;
preferably, the pressure of the spinning assembly is 6-16 Mpa;
preferably, the temperature of the spinning beam in the step (3) is 220-240 ℃;
preferably, the spinning rate in step (3) is 2800 and 3600 m/min.
5. The production method according to any one of claims 1 to 4, wherein the circular blowing device in the step (4) is a double row circular blowing device;
preferably, the air pressure of the circular air blowing device in the step (4) is 300-650pa, the air temperature is 20-22 ℃, and the air speed is 0.3-0.7 m/s.
6. The method according to any one of claims 1 to 5, wherein the pre-networking device has a gas pressure of 0.05 to 0.1MPa and the main networking device has a gas pressure of 0.15 to 0.2 MPa.
7. The production method according to any one of claims 1 to 6, wherein the temperature of the draw heat setting in the step (5) is 70 to 110 ℃;
preferably, the total drafting multiplying factor of the drafting heat setting is 1.2-2.4 times, and the drafting multiplying factor between the first hot roller and the second hot roller is 80-90% of the total drafting multiplying factor;
preferably, the temperature of the first hot roll is 88-98 ℃, the temperature of the second hot roll is 98-108 ℃, and the temperature of the third hot roll is 108-110 ℃.
8. The production method according to any one of claims 1 to 6, wherein the pre-oriented polylactic acid filament has an oil content of 0.50 to 0.90 wt%.
9. The production method according to any one of claims 1 to 7, wherein the oil content of the fully drawn polylactic acid filament is 1.0 ± 0.2 wt%.
10. A polylactic acid filament produced by the production method according to any one of claims 1 to 9.
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