CN102086535B - Method for preparing polyvinyl alcohol coarse denier monofilament fiber - Google Patents
Method for preparing polyvinyl alcohol coarse denier monofilament fiber Download PDFInfo
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- CN102086535B CN102086535B CN200910188649.XA CN200910188649A CN102086535B CN 102086535 B CN102086535 B CN 102086535B CN 200910188649 A CN200910188649 A CN 200910188649A CN 102086535 B CN102086535 B CN 102086535B
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Abstract
The invention discloses a method for preparing polyvinyl alcohol coarse denier monofilament fiber. The method comprises the steps of: mixing a polyvinyl alcohol raw material and water uniformly, and fully swelling; adding the swelled polyvinyl alcohol raw material into a single screw extruder, fully melting, extruding through a metering pump and a spinning pack, and freeze-forming in a coagulating bath to obtain polyvinyl alcohol fiber; and performing drying by a hot air dryer, multistage stretching, and tension hot-air setting on the obtained polyvinyl alcohol fiber to obtain the polyvinyl alcohol coarse denier monofilament fiber. The method for preparing the polyvinyl alcohol coarse denier monofilament fiber is simple in production technology and low in production cost; and the polyvinyl alcohol coarse denier monofilament fiber prepared by the method has the advantages of high denier, high strength and high modulus.
Description
Technical field
The present invention relates to a kind of method preparing polyvinyl alcohol monofilament fiber, particularly relate to the method that one prepares polyvinyl alcohol coarse denier monofilaments fiber (fiber number >=1000D).
Background technology
At present, the vinal that civil engineering concrete field is conventional adopts wet-formed method to prepare mostly.Adopt vinal prepared by the method, its fiber number can not be greater than 20D, and its filament diameter is comparatively thin, dispersed not strong with enhancing effect.
The patent No. be 200620047142.4 Chinese utility model patent description disclose a kind of polyvinyl alcohol monofilament adopting gel spinning method to be prepared from, the fiber number of this polyvinyl alcohol monofilament is larger.But it is longer that gel spinning method has technological process, the shortcoming that production cost is higher.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of method utilizing low temperature to solidify spinning technique to prepare polyvinyl alcohol coarse denier monofilaments fiber.The production technology of the method is simple, and production cost is low.The polyvinyl alcohol coarse denier monofilaments fiber adopting the method to prepare has the advantage of high fiber number, high strength, high-modulus, can be widely used in civil engineering concrete field.
For solving the problem, the method preparing polyvinyl alcohol coarse denier monofilaments fiber of the present invention, comprises the following steps:
Raw material swelling step: by weight ratio be 2 ~ 7: 3 polyvinyl alcohol raw material and water mix, fully swelling under 20 ~ 60 DEG C of conditions;
Freezing fusing spinning step: will add in single screw extrusion machine through swelling polyvinyl alcohol raw material, abundant melting, extrude through measuring pump, filament spinning component, through the freezing shaping of coagulating bath, obtained vinal, described single screw extrusion machine comprises following district and each district temperature is: feed zone 80 ~ 160 DEG C, 100 ~ 170 DEG C, compression section, metering section 90 ~ 170 DEG C, coagulating bath-30 ~-15 DEG C;
Dry drawing and setting step: obtained vinal is dry through hot-air oven, three grades of stretchings, nervous hot air shapings make polyvinyl alcohol coarse denier monofilaments fiber, described hot-air oven baking temperature is 120 ~ 150 DEG C, in described three grades of stretchings, the draw ratio that one-level stretches is 1.5 ~ 4.8 times, draft temperature is 40 ~ 150 DEG C, the draw ratio of secondary drawing is 1.8 ~ 6 times, draft temperature is 80 ~ 180 DEG C, three grades of draw ratios stretched are 2 ~ 5 times, draft temperature is 150 ~ 220 DEG C, and the temperature of described nervous hot air shaping is 110 ~ 230 DEG C.
Further, described polyvinyl alcohol raw material is pva powder or pellet.
Further, the aperture of the spinneret orifice of described filament spinning component is 0.5 ~ 6mm.
Further, described three grades of total drawing ratios (i.e. the product of every grade of draw ratio) stretched are 10 ~ 16 times.
The beneficial effect preparing the method for polyvinyl alcohol coarse denier monofilaments fiber of the present invention is, coarse denier monofilaments fiber is prepared owing to have employed solidification forming under lower coagulation bath temperature, greatly can reduce the degree of primary crystallization in large molecule, and reduce because moisture content volatilizees the bubble formed in the fibre, make the fiber obtained have better tensility, thus obtain the polyvinyl alcohol coarse denier monofilaments fiber with high fiber number, high strength, high-modulus.The production technology of the method is simple, and production cost is low.Adopt the polyvinyl alcohol coarse denier monofilaments fiber prepared of the method can be widely used in civil engineering concrete field, for improve concrete toughness reinforcing, strengthen, cracking resistance.
Detailed description of the invention
The method preparing polyvinyl alcohol (PVA) coarse denier monofilaments fiber (fiber number >=1000D) of the present invention, comprises the following steps:
(1) raw material swelling step: raw material adopts polyvinyl alcohol (PVA) powder or the pellet that the degree of polymerization is 1750 ~ 8000, alcoholysis degree is 99%, through washing and processed.In pva powder or pellet, add a certain amount of water, mix, fully swelling at 20 ~ 60 DEG C, wherein the weight ratio of polyvinyl alcohol and water is (2 ~ 7): 3.
(2) freezing fusing spinning step: by adding in single screw extrusion machine through swelling pva powder or pellet, fully melt, extrudes through measuring pump, filament spinning component, forms vinal through coagulating bath in cryogenic freezing liquid.Single screw extrusion machine comprises following district and each district temperature is: feed zone 80 ~ 160 DEG C, 100 ~ 170 DEG C, compression section, metering section 90 ~ 170 DEG C, coagulating bath :-30 ~-15 DEG C.Filament spinning component adopts larger spinneret orifice, and aperture is 0.5 ~ 6mm.
(3) dry drawing and setting step: the vinal that step (2) is formed forms polyvinyl alcohol (PVA) the coarse denier monofilaments fiber of high strength, high-modulus through hot-air oven drying, multistage stretching and nervous hot air shaping.Wherein:
Hot-air oven baking temperature is 120 ~ 150 DEG C.Multistage stretching is specially three poles and stretches, and every one-level extensograph parameter is as follows: one-level stretches, and draw ratio is 1.5 ~ 4.8 times, and draft temperature is 40 ~ 150 DEG C, and draw speed is 10 ~ 30 ms/min; Secondary drawing, draw ratio is 1.8 ~ 6 times, and draft temperature is 80 ~ 180 DEG C, and draw speed is 18 ~ 180 ms/min; Three grades of stretchings, draw ratio is 2 ~ 5 times, and draft temperature is 150 ~ 220 DEG C, and draw speed is 48 ~ 900 ms/min.The draw ratio (i.e. the product of every grade of draw ratio) that three poles stretch total is 10 ~ 16 times.The temperature of nervous hot air shaping is 110 ~ 230 DEG C, and the time is 5 ~ 20 minutes.
(4) post-processing step: polyvinyl alcohol (PVA) coarse denier monofilaments fiber step (3) can also prepared needs to cut into certain length by difference, and general shearing length is 6mm ~ 40mm.
Adopt polyvinyl alcohol (PVA) coarse denier monofilaments fiber prepared by said method, its diameter is 0.1mm ~ 2mm; Intensity is 600 ~ 1000MPa, modulus 20 ~ 35Ga, can be used as toughness reinforcing, reinforcing material and is widely used in civil engineering concrete, comprise structural concrete, concrete of basement, gunite concrete, dam concrete, bridge tunnel section of jurisdiction concrete etc.
Embodiment 1:
Abundant washing and dry remove excessive moisture after PVA1799 and water respectively get 50 parts by weight, mix, at 30 DEG C swelling 2 hours, swelling rear Single screw extrusion spinning, feed zone temperature 150 DEG C, compression section temperature 160 DEG C, metering section temperature 160 DEG C, coagulation bath temperature-15 DEG C, spinneret orifice footpath 1.8mm, hot-air oven 140 DEG C of dryings 2 hours, one-level stretching is carried out at 100 DEG C, draw ratio is 3 times, secondary drawing is carried out at 150 DEG C, draw ratio is 2 times, three grades of stretchings are carried out at 220 DEG C, draw ratio is 2 times, total drawing ratio multiple is 12 times, nervous hot air shaping temperature 230 DEG C.The diameter of obtained polyvinyl alcohol coarse denier monofilaments fiber is 0.5mm, and fibre strength is 700MPa, and fiber modulus is 30GPa.
Embodiment 2:
By weight, abundant washing and dry remove excessive moisture after PVA1799 get 60 parts, water gets 40 parts, mix, at 40 DEG C swelling 2 hours, swelling rear Single screw extrusion spinning, feed zone temperature 160 DEG C, compression section temperature 170 DEG C, metering section temperature 170 DEG C, coagulation bath temperature-15 DEG C, spinneret orifice footpath 1.5mm, hot-air oven 140 DEG C of dryings 2 hours, one-level stretching is carried out at 120 DEG C, draw ratio is 2 times, secondary drawing is carried out at 150 DEG C, draw ratio is 3 times, at 220 DEG C, carry out three grades of draw ratio multiples is 2.5 times, total draw ratio is 15 times, nervous hot air shaping temperature 230 DEG C.The diameter of obtained polyvinyl alcohol coarse denier monofilaments fiber is 0.35mm, and fibre strength is 800MPa, and fiber modulus is 32GPa.
Embodiment 3:
Abundant washing and dry remove excessive moisture after PVA2699 and water respectively get 50 parts by weight, mix, at 50 DEG C swelling 2 hours, swelling rear Single screw extrusion spinning, charging degree temperature 160 DEG C, compression section temperature 170 DEG C, metering section temperature 170 DEG C, coagulation bath temperature-20 DEG C, spinneret orifice footpath 1.8mm, hot-air oven 140 DEG C of dryings 2 hours, one-level stretching is carried out at 140 DEG C, draw ratio is 2 times, secondary drawing is carried out at 180 DEG C, draw ratio is 3 times, at 220 DEG C, carry out three grades of draw ratios is 2.5 times, total drawing ratio multiple is 15 times, nervous hot air shaping temperature 230 DEG C.The diameter of obtained polyvinyl alcohol coarse denier monofilaments fiber is 0.4mm, and fibre strength is 1000MPa, and fiber modulus is 35GPa.
The method preparing polyvinyl alcohol coarse denier monofilaments fiber of the present invention, be characterized in adopting and carry out spinning under the plasticising of suitable quantity of water, adopt larger spinneret orifice to extrude, under lower coagulation bath temperature, solidification forming prepares coarse denier monofilaments fiber.The degree of primary crystallization in large molecule can be reduced because lower temperature is shaped, and reduce because moisture content volatilizees the bubble formed in the fibre, make the fiber obtained have better tensility, thus obtain the polyvinyl alcohol coarse denier monofilaments fiber with high strength, high-modulus.It is simple that the method also has production technology, the advantage that production cost is low.Adopt polyvinyl alcohol coarse denier monofilaments fiber prepared by the inventive method, its fiber number (dawn number) can reach more than 1000D.
The above is preferred embodiment of the present invention, is not limited to the present invention, and all amendments, equivalent replacement or improvement etc. done in the present invention's spirit and principle, all should be included in protection scope of the present invention.
Claims (3)
1. prepare a method for polyvinyl alcohol coarse denier monofilaments fiber, it is characterized in that, comprise the following steps:
Raw material swelling step: by weight ratio be 2 ~ 7: 3 polyvinyl alcohol raw material and water mix, fully swelling under 20 ~ 60 DEG C of conditions;
Freezing fusing spinning step: will add in single screw extrusion machine through swelling polyvinyl alcohol raw material, abundant melting, extrude through measuring pump, filament spinning component, through the freezing shaping of coagulating bath, obtained vinal, described single screw extrusion machine comprises following district and each district temperature is: feed zone 80 ~ 160 DEG C, 100 ~ 170 DEG C, compression section, metering section 90 ~ 170 DEG C, coagulating bath-30 ~-15 DEG C; Wherein, the aperture of the spinneret orifice of described filament spinning component is 0.5 ~ 6mm;
Dry drawing and setting step: obtained vinal is dry through hot-air oven, three grades of stretchings, nervous hot air shaping makes polyvinyl alcohol coarse denier monofilaments fiber, described hot-air oven baking temperature is 120 ~ 150 DEG C, in described three grades of stretchings, the draw ratio that one-level stretches is 1.5 ~ 4.8 times, draft temperature is 40 ~ 150 DEG C, draw speed is 10 ~ 30 ms/min, the draw ratio of secondary drawing is 1.8 ~ 6 times, draft temperature is 80 ~ 180 DEG C, draw speed is 18 ~ 180 ms/min, three grades of draw ratios stretched are 2 ~ 5 times, draft temperature is 150 ~ 220 DEG C, draw speed is 48 ~ 900 ms/min, the temperature of described nervous hot air shaping is 110 ~ 230 DEG C.
2. prepare the method for polyvinyl alcohol coarse denier monofilaments fiber as claimed in claim 1, it is characterized in that: described polyvinyl alcohol raw material is pva powder or pellet.
3. prepare the method for polyvinyl alcohol coarse denier monofilaments fiber as claimed in claim 1 or 2, it is characterized in that: described three grades of total drawing ratios stretched are 10 ~ 16 times.
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| CN200910188649.XA CN102086535B (en) | 2009-12-02 | 2009-12-02 | Method for preparing polyvinyl alcohol coarse denier monofilament fiber |
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| CN200910188649.XA CN102086535B (en) | 2009-12-02 | 2009-12-02 | Method for preparing polyvinyl alcohol coarse denier monofilament fiber |
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| CN102086535A CN102086535A (en) | 2011-06-08 |
| CN102086535B true CN102086535B (en) | 2015-04-01 |
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| CN104328511A (en) * | 2014-10-08 | 2015-02-04 | 九力绳缆有限公司 | Preparation method for high-strength high-modulus polyvinyl alcohol fibers |
| CN106894109B (en) * | 2017-04-11 | 2019-05-31 | 大连天马可溶制品有限公司 | Low temperature water soluble polyvinyl alcohol filament yarn and preparation method thereof |
| CN110205696B (en) * | 2019-07-15 | 2021-12-07 | 安徽皖维高新材料股份有限公司 | Method for preparing polyvinyl alcohol coarse denier fiber by melt spinning |
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| JPS59163413A (en) * | 1983-03-04 | 1984-09-14 | Asahi Chem Ind Co Ltd | Melt spinning of acrylic polymer composition |
| CN1077923C (en) * | 1999-08-19 | 2002-01-16 | 陈成泗 | Production process of high-strength high-modulus polyethylene fibre |
| US7642307B2 (en) * | 2002-03-12 | 2010-01-05 | E.I. Du Pont De Nemours And Company | Low-color stiff PVB laminates |
| CN100339519C (en) * | 2005-12-13 | 2007-09-26 | 中国石化集团四川维尼纶厂 | Method of preparing high performance polyvinyl alcohel fiber |
| CN101244902A (en) * | 2007-06-15 | 2008-08-20 | 东华大学 | Fluorescence fibre for reinforcing concrete, production and application thereof |
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Effective date of registration: 20160222 Address after: 518040 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan digital city building F3.8, block D, floor seven C Patentee after: SHENZHEN OCEAN POWER MATERIAL TECHNOLOGY Co.,Ltd. Address before: 518040 Guangdong city of Shenzhen province Futian District Che Kung Temple Cheonan digital city building F3.8, block D, floor seven C Patentee before: SHENZHEN OCEANPOWER INDUSTRY Co.,Ltd. Patentee before: SHENZHEN OCEAN POWER ENGINEERING TECHNOLOGY Co.,Ltd. |
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Granted publication date: 20150401 Termination date: 20211202 |