CN103668531B - Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl chloride - Google Patents

Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl chloride Download PDF

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Publication number
CN103668531B
CN103668531B CN201210359087.2A CN201210359087A CN103668531B CN 103668531 B CN103668531 B CN 103668531B CN 201210359087 A CN201210359087 A CN 201210359087A CN 103668531 B CN103668531 B CN 103668531B
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acrylonitrile
fiber
vinyl chloride
content
spinning solution
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CN103668531A (en
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杨雪红
俞玉芳
黄翔宇
沈喜宾
沈志明
章毅
马正升
潘建国
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China Petroleum and Chemical Corp
Sinopec Shanghai Petrochemical Co Ltd
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China Petroleum and Chemical Corp
Sinopec Shanghai Petrochemical Co Ltd
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Abstract

The invention relates to a method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl chloride, which comprises the following steps: (1) dissolving a polyacrylonitrile polymer in a 40-60% sodium thiocyanate water solution through a dissolver, wherein in the polyacrylonitrile polymer, the acrylonitrile content is 85-95%, the vinyl chloride content is 5-10%, the sodium methylallyl sulfonate content is less than 1%, and the viscosity-average molecular weight of polyacrylonitrile is 45-65 thousand; (2) after debubbling and filtering a spinning solution, metering through a spinning metering pump, and extruding through spinneret orifices; (3) extruding into a coagulation bath through a spinneret plate to form nascent fibers; (4) sending the fibers into a secondary coagulation bath to form, and carrying out cold drawing, water washing and hot drawing, wherein the total drawing magnification is less than or equal to 12; (5) carrying out hot drying and compaction treatment on the fibers; and (6) thermoforming the fibers. The acrylic fibers prepared by the method have the advantages of high fracture resistance and high pilling resistance.

Description

The method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride
Technical field
The present invention relates to a kind of production method of wet method Antipilling nitrilon, more particularly to one kind utilize acrylonitrile and chloroethene The method that alkene prepares anti-pilling acrylic fiber.
Background technology
Most of synthetic fibers all have " balling-up " this phenomenon in use.Because the strength of acrylon is than natural Fiber is high, and on its product surface, the synthesis speed of fiber spherolite is more than exfoliation rates, therefore cannot eliminate fibrous nodules in frictional force In the case of grain, these fiber spherolites being formed will be retained in fabric face for a long time, thus affecting the outward appearance of fabric and wearing Comfortableness.Exploitation patent documentation both domestic and external with regard to anti-pill fibre is also relatively more, as resisting of<publication number>1948567 It is related to the polyacrylonitrile polymer blending using two kinds of different molecular weights and two single contents in ball acrylic fiber production process method, and be made into Polymer content is 13.5%~14% thick stock solution, obtains spinning solution and carry out spinning after deaeration, filtration.This method subtracts Having lacked in polymer two single contents increases intermolecular density, reduces the activeness of molecule segment, increase fiber rigidity and for The fragility of shear action, makes the fiber powder in fabric be difficult to be wound in knot, obtains preferable anti pilling effect.But this anti pilling The production method complex procedures of acrylon, polymerization technique first is adjusted, and needs to produce the polymer of different viscosity-average molecular weights, and And change two single contents.Two kinds of polymeric proportionings of its secondary control mixing.Two kinds of polymerization compatability also to be solved and mix Close uniformity.Because different molecular weight polymerization compatability is different, and mobility difference leads to solution mixing uneven after dissolving Even, finally it is easily caused and produce unstable, impact fiber quality.The and for example reduction acrylic fiber pilling tendency of<publication number>1737246 In the method for energy, raising anti pilling effect in finishing agent be impregnated in using fabric.But this method one side increased operation, increase Add the blowdown for the treatment of fluid.On the other hand this method is that fabric is carried out with impregnation process, therefore has certain selection to fabric Property.And it is not apparent that the anti pilling effect of fabric improves after multiple washing.United States Patent (USP)<3,975,486>is also had to retouch The Antipilling nitrilon stated controls 50% 70% that sodium rhodanate concentration in coagulating bath is in spinning liquid in producing, and this concentration model It is trapped among solvent diffuse in spinning technique excessively slow, fibre forming leads to not normal spinning excessively slowly.United States Patent (USP)<4,205,037>is retouched The production carrying out anti-pill fibre by the way of second drawing-off stated, but because current speed of spinning is very fast, design is such again Draft apparatus are relatively difficult, and inconvenient operation, costly.
Content of the invention
It is an object of the invention to overcoming above-mentioned the deficiencies in the prior art, provide a kind of producer of anti-pilling acrylic fiber Method, produces the acrylon with anti pilling characteristic by the quantity adjusting fiber Hole.
The technical solution of the present invention is as follows:
A kind of method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride, its feature is, the method includes Step is as follows:
1. by acrylonitrile content 85%~95%, 5%~10%, methylpropene sodium sulfonate content is less than content of vinylchloride 1%, the viscosity-average molecular weight of polyacrylonitrile is dissolved in concentration by dissolving machine and is in 4.5 ten thousand~6.5 ten thousand polyacrylonitrile polymer In 40%~60% sodium thiocyanate water solution;
2. spinning solution, after deaeration and filtering, is extruded by spinneret orifice by after spinning measuring pump-metered, spray orifice is permissible It is alternatively other shapes for circular;
3. clamp-on formation as-spun fibre after coagulating bath through spinneret, adjust coagulating bath export orientation roller speed and spinneret Extruded velocity, makes spinning solution extruded velocity and the ratio of guide roller hauling speed be less than or equal to 5;
4. fiber enters secondary coagulating bath and shapes, then carries out cold drawing-off, washing and hot gas spring, and total draft multiplying power is less than etc. In 12, fiber baking the affected part after applying some drugs are done total contraction and are less than or equal to 20%;
5. fiber carries out the dry densification of baking the affected part after applying some drugs, 60 DEG C~80 DEG C of wet bulb temperature, 120 DEG C~150 DEG C of dry-bulb temperature;
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C.
Described step 2. in middle spinning solution polyacrylonitrile polymer content be 7wt % ~ 11wt%, spinning solution temperature At 30 DEG C~50 DEG C.More excellent, in spinning solution, polyacrylonitrile polymer content is 8wt % ~ 10wt%.
Described step 3. in middle coagulating bath sodium rhodanate concentration be 10%~15%, be conducive to the diffusion of nascn in fiber, And the generation of fiber hole, the temperature of coagulating bath is -2 DEG C ~ 5 DEG C..
3. middle spinning solution extruded velocity and the ratio of guide roller hauling speed are less than or equal to 4.5 to described step.
Compared with prior art, resist the invention has the beneficial effects as follows producing to have by the quantity adjusting fiber Hole The acrylon of ball characteristic.
Specific embodiment
With reference to embodiment, the invention will be further described, but should not be limited the scope of the invention with this.
A kind of method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride, comprises the following steps that
1. with 40%~60% nascn solution, more precisely concentration passes through at a high speed in 50%~60% nascn solution 85%~95%, 5%~10%, methylpropene sodium sulfonate content is less than 1% to content of vinylchloride to dissolving machine dissolving acrylonitrile content, The viscosity-average molecular weight of polyacrylonitrile 4.5 ten thousand~6.5 ten thousand polyacrylonitrile polymer.For ensureing more preferable solute effect, sulfur cyanogen Sour sodium solvent need to be heated to more than 75 DEG C.Primarily serving the purpose of of vinyl chloride reduces macromolecular chain regularity, reduces molecular rigidity, increases Plus fabric hand.The effect of methylpropene sodium sulfonate is mainly to increase dyeing position, makes fiber be easier to dye.
2. it is configured to the spinning liquid in 7wt%~12wt% for the polymer content after dissolving, for improving fiber Hole body Long-pending, in spinning liquid, polymer preferably ranges from 8wt%~11wt%, because polymer content is higher, leads to structure in fiber to compare Closely, therefore fibre strength is high, easy balling-up.Spinning liquid delivers to spinning measuring pump inlet after deaeration, filtration and temperature-adjustment pressure-adjustment, Extruded from spinneret orifice after metering by dosing pump.
Due to the difference of polymer concentration, the therefore viscosity of solution and mobility all different it is therefore desirable to solution temperature Carry out suitable adjustment, make spinning solution temperature control at 30 DEG C~50 DEG C.We are to the solution of variable concentrations in different temperatures Under carry out the test of rheological characteristic.Result is as shown in the table:
Note: flow graph model mcr301
3. clamp-on coagulating bath through spinneret, as-spun fibre carries out double diffusion shaping in coagulating tank.For ensureing to shape effect Fruit and holding fiber hole, coagulating bath concentration range is arranged between 10%~15%, and temperature range is -2 DEG C~5 DEG C.For reducing Fiber is sagging and ensures fiber Hole, adjusts coagulating bath export orientation roller speed and spinneret extruded velocity, makes spinning molten The ratio of liquid extruded velocity and guide roller hauling speed is less than or equal to 5, more preferably less than 4.5 times.
4. fiber, after coagulating bath shaping, enters secondary coagulating bath and shapes, enter back into cold drawing-off, washing and heat and lead Stretch.For ensureing fiber hole, total draft multiple requires to be less than or equal to 12.
5. fiber enters lax densification after hot gas spring and dries, and wherein wet bulb temperature sets 60 DEG C~80 DEG C, dry bulb Temperature sets 120 DEG C~150 DEG C.
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C.For ensure fiber have softness feel, reduce The generation of yarn filoplume afterwards, the selection to oil preparation has certain requirement.Being stretched due to the strong knot of knot is certain weight of anti-pill fibre Want index, for ensureing the anti pilling effect of the hole number in fiber and fiber it is desirable to total contraction of fiber is less than 20%.
The fiber obtaining is carried out with the test of characteristic index, and fiber spinning be made into cloth after carry out the survey of anti pilling series Examination.Test result is as follows:
As seen from table, the acrylic fiber through the inventive method preparation has high resistance to fracture, anti-pilling.

Claims (4)

1. a kind of using acrylonitrile and vinyl chloride prepare anti-pilling acrylic fiber method it is characterised in that the method include walk Suddenly as follows:
1. by acrylonitrile content 85%~95%, 5%~10%, methylpropene sodium sulfonate content is less than content of vinylchloride 1%, the viscosity-average molecular weight of polyacrylonitrile is dissolved in concentration by dissolving machine and is in 4.5 ten thousand~6.5 ten thousand polyacrylonitrile polymer In 40%~60% sodium thiocyanate water solution;
2. spinning solution, after deaeration and filtering, is extruded by spinneret orifice by after spinning measuring pump-metered;
Described step 2. in middle spinning solution polyacrylonitrile polymer content be 7wt%~12wt%, spinning solution temperature exists 30 DEG C~50 DEG C;
3. clamp-on formation as-spun fibre after coagulating bath through spinneret, adjust coagulating bath export orientation roller speed and spinneret extrusion Speed, makes spinning solution extruded velocity and the ratio of guide roller hauling speed be less than or equal to 5;
4. fiber enters secondary coagulating bath and shapes, then carries out cold drawing-off, washing and hot gas spring, and total draft multiplying power is less than or equal to 12;
5. fiber carries out the dry densification of baking the affected part after applying some drugs, 60 DEG C~80 DEG C of wet bulb temperature, 120 DEG C~150 DEG C of dry-bulb temperature;
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C.
2. the method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride according to claim 1, its feature exists In in described spinning solution, polyacrylonitrile polymer content is 8wt%~10wt%.
3. the method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride according to claim 1, its feature exists In, described step 3. middle coagulating bath, sodium rhodanate concentration is 10%~15%, and the temperature of coagulating bath is -2 DEG C~5 DEG C.
4. the method preparing anti-pilling acrylic fiber using acrylonitrile and vinyl chloride according to claim 1, its feature exists In 3. middle spinning solution extruded velocity and the ratio of guide roller hauling speed are less than or equal to 4.5 to described step.
CN201210359087.2A 2012-09-25 2012-09-25 Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl chloride Active CN103668531B (en)

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KR101913970B1 (en) * 2014-08-27 2018-10-31 미쯔비시 케미컬 주식회사 Glossy pilling-resistant acrylic fiber, method for producing same, and spun yarn and knitted fabric including said acrylic fiber
CN107419351A (en) * 2017-07-27 2017-12-01 合肥远科服装设计有限公司 A kind of preparation technology of acrylic fiber

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JPH0823083B2 (en) * 1985-11-26 1996-03-06 日本エクスラン工業株式会社 Acrylic fiber manufacturing method
CN1298902C (en) * 2005-03-14 2007-02-07 东华大学 Plant protein/polyurethane/polyacrylonitrile blended composite fiber and preparing process
CN100445438C (en) * 2005-12-22 2008-12-24 中国石化上海石油化工股份有限公司 Process of producing polyacrylic fiber dyeable with both cationic dye and acid dye
CN1807712A (en) * 2006-02-09 2006-07-26 东华大学 Process for preparing antibacterial polyacrylonitrile fiber
ZA200901737B (en) * 2006-09-21 2010-05-26 Kaneka Corp Fiber for artificial hair with improved processability and hair accessory using the same
CN100540760C (en) * 2006-12-12 2009-09-16 新华锦集团有限公司 A kind of modified polyacrylonitrile fiber and manufacture method thereof and purposes
CN101748498B (en) * 2008-12-12 2011-10-05 中国石化上海石油化工股份有限公司 Method for producing anti-pilling acrylic fiber

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