CN103668530B - Utilize acrylonitrile and methyl methacrylate to prepare the method for anti-pilling acrylic fiber - Google Patents
Utilize acrylonitrile and methyl methacrylate to prepare the method for anti-pilling acrylic fiber Download PDFInfo
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Abstract
A kind of method of utilizing acrylonitrile and methyl methacrylate to prepare anti-pilling acrylic fiber, comprise step 1. by acrylonitrile content 85%~95%, methyl methacrylate content is 5%~10%, methylpropene sodium sulfonate content is less than 1%, and the viscosity average molecular weigh of polyacrylonitrile is dissolved in concentration at 4.5 ten thousand~6.5 ten thousand polyacrylonitrile condensate by dissolving machine be in 40%~60% sodium thiocyanate water solution; 2. spinning solution, by after deaeration and filtering, by spinneret orifice is extruded after being measured by spinning pump; 3. after clamp-oning coagulating bath, spinneret forms as-spun fibre; 4. fiber enters secondary coagulating bath shaping, then carries out cold drawing-off, washing and hot drawing-off, and total draft multiplying power is less than or equal to 12; 5. fiber carries out heat oven dry densification; 6. fiber carries out thermal finalization. Acrylic fiber prepared by the inventive method has high resistance to fracture, anti-pilling.
Description
Technical field
The present invention relates to a kind of production method of wet method Antipilling nitrilon, particularly relate to a kind of method of utilizing acrylonitrile and methyl methacrylate to prepare anti-pilling acrylic fiber.
Background technology
Most of synthetic fibers all exist in use " balling-up " this phenomenon. Because the brute force of acrylic fibers is higher than natural fiber, on its product surface, the formation speed of fiber spherolite is greater than exfoliation rates, therefore in the situation that frictional force cannot be eliminated fiber spherolite, these fiber spherolites that form will be retained in fabric face for a long time, thereby affect outward appearance and the snugness of fit of fabric. Exploitation patent documentation both domestic and external about anti-pill fibre is also many, as<publication number>relate to the polyacrylonitrile condensate blend that adopts two kinds of different molecular weights and two single content in 1948567 Antipilling nitrilon production method, and to be made into polymer content be 13.5%~14% thick stoste, obtain spinning solution through deaeration, after filtering and carry out spinning. This method has reduced two single content in polymer and has increased intermolecular density, reduces the activity of molecule segment, increases fiber rigidity and the fragility for shear action, makes the fiber powder in fabric be difficult for being wound in knot, obtains good anti pilling effect. But the production method complex procedures of this Antipilling nitrilon, first polymerization technique regulates, and need to produce the condensate of different viscosity average molecular weighs, and changes two single content. Two kinds of polymeric proportionings that its less important control mixes. Also to solve two kinds of condensate compatibilities and mixing uniformity. Due to different molecular weight condensate compatibility difference, and after dissolving mobility difference to cause solution to mix inhomogeneous, finally easily cause producing unstable, affect fiber quality. And for example<publication number>adopt textile impregnation in finishing agent, to improve anti pilling effect in the method for 1737246 reduction balling-up property of acrylic fibre. But this method has increased operation on the one hand, has increased the blowdown for the treatment of fluid. This method is that fabric is carried out to impregnation process on the other hand, therefore fabric is had certain selective. And it is not clearly that the anti pilling effect of fabric improves after repeatedly washing. Also have United States Patent (USP)<3,975,486>it is 50%-70% in spinning solution that the Antipilling nitrilon of describing is controlled sodium sulfocyanate concentration in coagulating bath in producing, and this concentration range sovent diffusion in spinning technique is excessively slow, and fibre forming causes normally spinning excessively slowly. United States Patent (USP)<4, the mode of 205,037>description employing drawing-off is for the second time carried out the production of anti-pill fibre, but very fast owing to spinning at present speed, designs such draft apparatus more difficult, and inconvenient operation, and expense is higher.
Summary of the invention
The object of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of method of utilizing acrylonitrile and methyl methacrylate to prepare anti-pilling acrylic fiber is provided, produce the acrylic fibers with anti pilling characteristic by the quantity that regulates fiber Hole.
Technical solution of the present invention is as follows:
Utilize acrylonitrile and methyl methacrylate to prepare a method for anti-pilling acrylic fiber, its feature is, it is as follows that the method comprising the steps of:
1. by acrylonitrile content 85%~95%, methyl methacrylate content is 5%~10%, methylpropene sodium sulfonate content is less than 1%, and the viscosity average molecular weigh of polyacrylonitrile is dissolved in concentration at 4.5 ten thousand~6.5 ten thousand polyacrylonitrile condensate by dissolving machine be in 40%~60% sodium thiocyanate water solution;
2. spinning solution, by after deaeration and filtering, by spinneret orifice is extruded after being measured by spinning pump, and spray orifice can also can be other shape for circle;
3. after spinneret is clamp-oned coagulating bath, form as-spun fibre, regulate coagulating bath export orientation roller speed and spinneret extruded velocity, make 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 shaping, then carries out cold drawing-off, washing and hot drawing-off, and total draft multiplying power is less than or equal to 12, and fiber heat is dried total contraction and is less than or equal to 20%;
5. fiber carries out heat oven dry densification, 60 DEG C~80 DEG C of wet-bulb temperature, 120 DEG C~150 DEG C of dry-bulb temperatures;
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C.
Described step 2. in spinning solution polyacrylonitrile condensate content be 7wt% ~ 11wt%, spinning solution temperature is at 30 DEG C~50 DEG C. More excellent, in spinning solution, polyacrylonitrile condensate content is 8wt% ~ 10wt%.
Described step 3. in coagulating bath sodium sulfocyanate 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. .
Described step 3. middle spinning solution extruded velocity is less than or equal to 4.5 with the ratio of guide roller hauling speed.
Compared with prior art, the invention has the beneficial effects as follows that the quantity production by regulating fiber Hole has the acrylic fibers of anti pilling characteristic.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but should not limit the scope of the invention with this.
Utilize acrylonitrile and methyl methacrylate to prepare a method for anti-pilling acrylic fiber, comprise that step is as follows:
1. use 40%~60% NaSCN solution, more precisely concentration is dissolved acrylonitrile content 85%~95% at 50%~60% NaSCN solution by high speed dissolving machine, methyl methacrylate content is 5%~10%, methylpropene sodium sulfonate content is less than 1%, and the viscosity average molecular weigh of polyacrylonitrile is at 4.5 ten thousand~6.5 ten thousand polyacrylonitrile condensate. For ensureing better solute effect, Sodium Thiocyanate Solvent need be heated to more than 75 DEG C. The Main Function of methyl methacrylate, for reducing macromolecular chain regularity, reduces molecular rigidity, increases fiber feel. The effect of methylpropene sodium sulfonate is mainly to increase dyeing position, and fiber is more easily dyeed.
2. after dissolving, be mixed with the spinning solution of condensate content at 7wt%~12wt%, for improving fiber Hole volume, in spinning solution, condensate scope is preferably 8wt%~11wt%, because condensate content is higher, cause in fiber structure tightr, therefore fibre strength is high, easily balling-up. Spinning solution is delivered to spinning measuring pump inlet after by deaeration, filtration and temperature-adjustment pressure-adjustment, is extruded after metering by measuring pump from spinneret orifice.
Due to the difference of polymer concentration, therefore the viscosity of solution and mobility are all different, therefore need solution temperature to carry out suitable adjustment, make spinning solution temperature be controlled at 30 DEG C~50 DEG C. We carry out the test of rheological characteristic under different temperatures to the solution of variable concentrations. 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 forming effect and keeping fiber hole, coagulating bath concentration range is arranged between 10%~15%, and temperature range is-2 DEG C~5 DEG C. For minimizing fiber is sagging and ensure fiber Hole, regulate coagulating bath export orientation roller speed and spinneret extruded velocity, make spinning solution extruded velocity and the ratio of guide roller hauling speed be less than or equal to 5, be preferably less than 4.5 times.
4. fiber, after coagulating bath is shaped, enters secondary coagulating bath and is shaped, then enter cold drawing-off, washing and hot drawing-off. For ensureing fiber hole, total draft multiple requires to be less than or equal to 12.
5. fiber enters lax densified oven dry after overheated drawing-off, and wherein wet-bulb temperature is set 60 DEG C~80 DEG C, and dry-bulb temperature is set 120 DEG C~150 DEG C.
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C. For ensureing that fiber has soft feel, after reducing, the generation of yarn filoplume, has certain requirement to the selection of finish. Stretching due to the strong knot of knot is certain important indicator of anti-pill fibre, for the hole number in guarantee fiber and the anti pilling effect of fiber, requires total contraction of fiber to be less than 20%.
The fiber obtaining is carried out to the test of characteristic index, and fiber spinning is made into the test of carrying out anti pilling progression after cloth. Test result is as following table:
As seen from table, the acrylic fiber of preparing through the inventive method has high resistance to fracture, anti-pilling.
Claims (2)
1. utilize acrylonitrile and methyl methacrylate to prepare a method for anti-pilling acrylic fiber, it is characterized in that, shouldMethod comprises that step is as follows:
1. by acrylonitrile content 85%~95%, methyl methacrylate content is 5%~10%, methylpropene sodium sulfonate containsAmount is less than 1%, and the viscosity average molecular weigh of polyacrylonitrile is dissolved in by dissolving machine at 4.5 ten thousand~6.5 ten thousand polyacrylonitrile condensateConcentration is in 40%~60% sodium thiocyanate water solution;
2. spinning solution, by after deaeration and filtering, by spinneret orifice is extruded after being measured by spinning pump;
3. after spinneret is clamp-oned coagulating bath, form as-spun fibre, regulate coagulating bath export orientation roller speed and spinneret to extrudeSpeed, 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 shaping, then carries out cold drawing-off, washing and hot drawing-off, and total draft multiplying power is less than or equal to12;
5. fiber carries out heat oven dry densification, 60 DEG C~80 DEG C of wet-bulb temperature, 120 DEG C~150 DEG C of dry-bulb temperatures;
6. fiber carries out thermal finalization, and heat setting temperature is 102 DEG C~120 DEG C; Wherein:
Described step 2. in spinning solution polyacrylonitrile condensate content be 8wt%~10wt%, spinning solution temperature exists30℃~50℃;
Described step 3. middle spinning solution extruded velocity is less than or equal to 4.5 with the ratio of guide roller hauling speed.
2. the method for utilizing acrylonitrile and methyl methacrylate to prepare anti-pilling acrylic fiber according to claim 1,It is characterized in that, described step 3. in coagulating bath sodium sulfocyanate concentration be 10%~15%, the temperature of coagulating bath is-2 DEG C~5℃。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4818458A (en) * | 1985-11-26 | 1989-04-04 | Japan Exlan Company Limited | Method of producing acrylic fibers |
CN1986918A (en) * | 2005-12-22 | 2007-06-27 | 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 |
CN101516219A (en) * | 2006-09-21 | 2009-08-26 | 株式会社钟化 | Fiber for artificial hair improved in settability and hair accessories made by using the fiber |
CN101818386A (en) * | 2010-04-28 | 2010-09-01 | 吉林奇峰化纤股份有限公司 | Preparation method of anti-pilling acrylic fiber |
CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
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- 2012-09-25 CN CN201210359060.3A patent/CN103668530B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4818458A (en) * | 1985-11-26 | 1989-04-04 | Japan Exlan Company Limited | Method of producing acrylic fibers |
CN1986918A (en) * | 2005-12-22 | 2007-06-27 | 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 |
CN101516219A (en) * | 2006-09-21 | 2009-08-26 | 株式会社钟化 | Fiber for artificial hair improved in settability and hair accessories made by using the fiber |
CN101818386A (en) * | 2010-04-28 | 2010-09-01 | 吉林奇峰化纤股份有限公司 | Preparation method of anti-pilling acrylic fiber |
CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
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