CN101070634A - Method for preparing hydrophilic polymerized acrylonitrile fiber - Google Patents
Method for preparing hydrophilic polymerized acrylonitrile fiber Download PDFInfo
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- CN101070634A CN101070634A CNA2007100575992A CN200710057599A CN101070634A CN 101070634 A CN101070634 A CN 101070634A CN A2007100575992 A CNA2007100575992 A CN A2007100575992A CN 200710057599 A CN200710057599 A CN 200710057599A CN 101070634 A CN101070634 A CN 101070634A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
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Abstract
The invention relates to the hydrophilic acrylonitrile copolymer fiber and the processing method. The processing method: 1. Process the acrylonitrile copolymer by the aqueous precipitation polymerization. Using the acrylonitrile with the percentage of quality (the same below) is 76%-85% and the vinyl acetate with 9%-10% as monomer, using the Acrylic -2 - Hydroxyl propyl with 5%-15% as potential crosslinker, triggered by the initiator sodium chlorate with 0.2%, reductant it by the reductant sodium sulfite with 0.6%, ph 2+-0.1. the monomer quality is 25%-40% of water quality, we can get Acrylonitrile copolymer after Copolymerization in 1-1.5h. 2. Mix the Acrylonitrile copolymer and the cellulose acetate in the proportion of 85-95:15-5 after dry them. Using N,N-dimethyl acetamide as solvent, preparing the spinning solution with the concentration is 15%-25%, making the acrylonitrile copolymer fiber by the way of wet spinning after vacuum defoaming in 1.5-2h. 3. We can get the hydrophilic acrylonitrile copolymer fiber after this art. The art of this invention is aqueous precipitation polymerization. The art has simple process, and simple adjustments of the hydrolysis conditions, the absorbent of fibers can be easily controlled, and also it has a low cost.
Description
Technical field
The present invention relates to the chemical fibre manufacturing technology, be specially a kind of preparation method of hydrophilic polymerized acrylonitrile fiber, international Patent classificating number intends being Int.Cl D01M 15/00 (2006.01).
Background technology
The preparation method of hydrophilic fibre mainly contains two kinds at present:
1. hydrophilic polymer spin processes: for example: U.S. Arco chemical technology (ARCO) company adopts NaOH neutralization (degree of neutralization 55%) maleic acid-isobutylene copolymers aqueous solution, obtain the as-spun fibre that fiber number was 2～3 dawn through the dry spinning shaping, obtain the method for hydrophilic fibre after 10 minutes 180 ℃ of crosslinking Treatment, its commodity are called " Fibersorb (" adsorbing fiber ") " (Le-Khac, high polymer and adsorbing fiber, United States Patent (USP) 5026784,1991.6.25); It is comonomer with acrylic acid, sodium acrylate, acrylamide, hydroxy propyl methacrylate that people such as China Textile Academy grandson Yushan have studied a kind of, causes through polymerization initiator, and polymerization obtains aqueous copolymers solution in the aqueous solution; With described aqueous copolymers solution is cortex or sandwich layer, with the polyvinyl alcohol water solution is sandwich layer or cortex, through the method (Sun Yushan etc. that the sheath-core type composite spinneret is extruded, dry spinning and heat cross-linking obtain superabsorbent fiber, the manufacture method of superabsorbent fiber and fiber thereof, CN 1407147,2003.4.2) etc.But the hydrophilic fibre that this method obtains tends to reduce the mechanical and physical performance and the heat resistance of fiber, and suction back fiber is difficult to keep original shape.
2. to conventional fibre chemical modification processing method: for example: Japanese Exlan company has reported that a kind of employing chemical method carries out surface treatment to polyacrylonitrile fibre, make fiber surface contain the method (Sawanishi that granular high hydroscopic resin layer is made hydrophilic fibre, Shigeru, Wakitani, Mitruru, the acrylic acid water-absorption fiber, United States Patent (USP) 4562114,1985.12.31).Water absorbing properties is not high on the one hand for the hydrophilic fibre that this method obtains, and coat is very not water-fast on the other hand washes, and in use can reduce water absorption rate gradually; Again for example, people such as Deo have studied a kind of with KMnO
4-HNO
3Cause acrylonitrile and cotton fiber graft copolymerization, obtain the method (H.T.Deo of hydrophilic fibre after the hydrolysis, V.D.Gotmare, gray cotton grafting acrylonitrile monemer improves its water imbibition, journal of applied, 1999,72:887～894), but because copolymerization conditions limits, can only grafting in the polymer on hydrophilic monomer on a small quantity, restricted its water imbibition; Again for example, people such as Lin Kunhua have introduced a kind of energy with common commercially available polyacrylonitrile fibre (3.33dtex, 65mm) immersion contains in the certain density ethylene glycol solution, oil bath is cooled to room temperature after being heated to uniform temperature and being incubated 40 minutes, take out fiber and be washed till neutrality with distilled water immersion repeatedly, centrifuge dripping, vacuumize, can get the golden yellow fiber of the degree of cross linking about 2.5%, again by the hydrolysis of NAOH solution, neutralization, make method (Lin Kunhua, Cai Dongmei, a kind of hydrophilic fibre and with its high blotting paper of making of hydrophilic fibre after the dried, chemical research and application 2000,12 (3): 339～342).But this method preparation process more complicated, the polyacrylonitrile macromolecules cross-linking degree that obtains is less, fully not keeping fibrous substantially after the hydrolysis, has lost the physical-mechanical property of fiber, is difficult to be effective as fibrous material and uses.
Summary of the invention
At the deficiencies in the prior art, the technical problem that quasi-solution of the present invention is determined is that a kind of preparation method of hydrophilic polymerized acrylonitrile fiber is provided.It is simple relatively that this preparation method has technology, but the controlled serialization preparation of fiber water absorbent rate, characteristics such as production cost is lower, the gained hydrophilic polymerized acrylonitrile fiber having also that suction back keeps fibre morphology, good physical-mechanical performance, reusability is good and characteristics such as recyclable utilization when having good water absorbing properties.
The technical scheme that the present invention solves described preparation method's technical problem is: design a kind of preparation method of hydrophilic polymerized acrylonitrile fiber, this preparation method comprises
(1) preparation copolymerized acrylonitrile, this copolymerization process is an aqueous precipitation polymerization, with mass percent concentration is that 76～85% acrylonitrile and mass percent concentration are that 9～10% vinylacetates are monomer, with mass percent concentration is that acrylic acid-2-hydroxypropyl acrylate of 5～15% is a latent crosslinker, initator sodium chlorate through mass percent concentration 0.2% causes, mass percent concentration is 0.6%, pH is 2 ± 0.1 reductant sodium sulfite reduction, described monomer mass is 25～40% of a quality, copolyreaction 1～1.5h can obtain copolymerized acrylonitrile;
(2) spinning polymerized acrylonitrile fiber, after the copolymerized acrylonitrile drying with gained, with cellulose acetate in 85～95: 15～5 ratio blend is even, with N, the N-dimethylacetylamide is a solvent, and the spinning solution of configuration 15～25% concentration is behind vacuum defoamation 1.5～2h, through wet spinning, can make polymerized acrylonitrile fiber;
(3) aftertreatment technology, the gained polymerized acrylonitrile fiber can make described hydrophilic polymerized acrylonitrile fiber after crosslinked, hydrolysis, neutralization, removing alkali and dehydration and drying process processing.
Compared with prior art, hydrophilic polymerized acrylonitrile fiber preparation method of the present invention has adopted aqueous precipitation polymerization, preparation copolymerized acrylonitrile technology is simple relatively, and hydrolysising condition is adjusted easy, be easy to the controlling fiber water absorbing properties, therefore have properties of product and easily control, production cost is lower, but characteristics such as serialization preparation.Preparation method of the present invention is owing to adopted the technology of crosslinked hydrolysis after the first spinning, the crosslinking degree height, therefore the gained hydrophilic polymerized acrylonitrile fiber is when having good water absorbing properties, can also after suction, keep fibre morphology, and have good physical-mechanical property, can reuse characteristics with recyclable utilization.
The specific embodiment
The present invention is further elaborated below in conjunction with specific embodiment:
The described fiber of preparation method (hereinafter to be referred as the preparation method) of hydrophilic polymerized acrylonitrile fiber of the present invention (hereinafter to be referred as fiber) is pressed following mass percent prescription copolymerization gained by materials such as acrylonitrile, vinylacetate and latent crosslinkers:
The content of acrylonitrile in comonomer is 76～85%;
The content of vinylacetate in comonomer is 9～10%;
The content of latent crosslinker in comonomer is 5～15%;
The content of initator in comonomer is 0.2%;
The content of reductant in comonomer is 0.6%,
Described latent crosslinker is acrylic acid-2-hydroxypropyl acrylate, and described initator is sodium chlorate (NaClO
3), reductant is sodium sulfite (Na
2SO
3);
Its copolymerization process is: adopt aqueous precipitation polymerization, cause through initator sodium chlorate, reductant is a sodium sulfite, and pH is 24 ± 0.1 times, and copolyreaction 1～1.5h can obtain copolymerized acrylonitrile; After the copolymerized acrylonitrile drying with gained, with cellulose acetate in 85～95: 15～5 ratio blend, with N, the N-dimethylacetylamide is a solvent, the spinning solution of configuration 15～25% concentration behind vacuum defoamation 1.5～2h, can make polymerized acrylonitrile fiber through wet spinning; Heat cross-linking 20～40min in 160～180 ℃ hot-air then, through concentration be 5～20% the NaOH aqueous solution at 65～95 ℃ of following hydrolysis 2～30min, again through neutralization, remove alkali and dehydration, drying process promptly can be made into described hydrophilic polymerized acrylonitrile fiber.
In the described mass percent prescription of preparation method of the present invention, the selection of latent crosslinker and use are one of key problem in technology of the present invention.Described latent crosslinker is selected foundation or is required: 1. under 130-200 ℃ of temperature, can carry out self-crosslinking reaction, give hydrophilic fibre and have certain tridimensional network; 2. before spinning technique, crosslinked action can not take place in latent crosslinker, has the favorable linearity structure to guarantee the big molecule of fibre-forming polymer, and spinning solution has better spinnability; 3. the fiber to final shaping does not have physics damage and chemical damage.In view of the above, the preferential latent crosslinker of selecting of the embodiment of the invention is acrylic acid-2-hydroxypropyl acrylate.It can satisfy the selection requirement about latent crosslinker of the present invention, but does not get rid of other latent crosslinkers that other can satisfy described specification requirement.And be in polymerisation, to make the big molecule of product take place crosslinked the latent crosslinker that common process uses (as the N-N` methylene-bisacrylamide etc.), the big molecule of the product of gained does not possess linear structure, both be insoluble to solvent, there is not melt temperature yet, can't satisfy spinning requirement, therefore all not be suitable for the present invention.
The fiber production method of the present invention design is a foundation with the mass percent prescription of described hydrophilic polymerized acrylonitrile fiber, adopts following processing step to finish:
1. preparation copolymerized acrylonitrile: the mass percent prescription with described copolymerized acrylonitrile is a foundation, adopts aqueous precipitation polymerization, causes through initator NaClO3, and reductant is Na
2SO3, pH are 2 ± 0.1 times, can obtain copolymerized acrylonitrile, and wherein monomer mass is 25～40% of a quality, and the copolyreaction time is 1～1.5h;
2. spinning polymerized acrylonitrile fiber: after the copolymerized acrylonitrile drying with gained, with the ratio blend of cellulose acetate in 85-95: 15-5, with N, the N-dimethylacetylamide is a solvent, the spinning solution of configuration 15～25% concentration, behind vacuum defoamation 1.5～2h, can make polymerized acrylonitrile fiber through wet spinning.
The described wet spinning process of preparation method of the present invention comprises: 1. copolymerized acrylonitrile and cellulose acetate are in 85-95: the blend of 15-5 ratio; 2. controlling coagulating bath concentration is the N,N-dimethylacetamide aqueous solution of 30-50%; 3. adopt multiple tracks to stretch the gained polymerized acrylonitrile fiber is carried out 4～6 times stretching in boiling water bath; 4. make the gained polymerized acrylonitrile fiber under relaxed state, carry out relaxation heat setting through 100 ℃ of water-baths.Described boiling water relaxation heat setting technology plays an important role to the retentivity of the DIMENSIONAL STABILITY of fiber in the heat cross-linking process.
3. the aftertreatment technology of polymerized acrylonitrile fiber: aftertreatment technology comprises crosslinked, hydrolysis, neutralization, remove technologies such as alkali, dehydration, drying promptly can be made into described hydrophilic polymerized acrylonitrile fiber; Wherein, described crosslinking process is meant the heat cross-linking 20-40min in 160～180 ℃ hot-air of the polymerized acrylonitrile fiber behind the relaxation heat setting; Described hydrolysis process is meant the polymerized acrylonitrile fiber behind the heat cross-linking in concentration is 5～20% NaOH (NaOH) aqueous solution, hydrolysis 2～20min under 65～95 ℃ of temperature.
The hydrolysising condition that the suction of preparation method's gained fiber of the present invention and water retention property depend on fiber.Hydrolysis process or process mainly are to make that hydrophobic cyano group is converted into the stronger amide groups of hydrophily, carboxyl and carboxylate groups on the big molecule of copolymerized acrylonitrile.Hydrolysising condition is determining the number of the contained hydrophilic radical of fiber.Obviously, appropriateness improves hydrolysis temperature, hydrolysis time and hydrolysis (NaOH) concentration, can make fiber contain hydrophilic radical as much as possible, helps improving the suction and the water retention property of fiber.After the described fiber hydrolysis, remove alkali through the neutralization of 2% concentration watery hydrochloric acid again, common process processes such as washing, dehydration, drying promptly can be made into hydrophilic polymerized acrylonitrile fiber of the present invention.
Preparation method of the present invention is a comonomer with acrylonitrile, vinylacetate, latent crosslinker etc., adopt the former liquid preparing process of aqueous phase precipitation polymerization, solid blend, vacuum defoamation, wet spinning makes fiber and makes described fiber through post processings such as heat cross-linking, basic hydrolysis, neutralization, washing, dryings.Wherein, design is separated to produce micropore, stretched to improve the mechanical property of fiber, make fiber in the heat cross-linking process, keep good DIMENSIONAL STABILITY by relaxation heat setting, and technical process such as described heat cross-linking, hydrolysis, neutralization, washing and drying etc. all can realize the serialization preparation of described hydrophilic fibre.
Can make hydrophilic polymerized acrylonitrile fiber of the present invention according to fiber prescription of the present invention and preparation method thereof.This fiber has stronger suction and water retention property, has suction conformality and good physical and mechanical properties simultaneously again, can be processed into textiles or non-woven product.These textiless or non-woven product have characteristics such as the good and recyclable utilization of reusability, meet environment protection requirement, are suitable for modern actual applying.
What need supplementary notes is that the applicant also relates to the hydrophilic polymerized acrylonitrile fiber technology in the patent (CN1743517) of first to file.This technology has mainly solved the technical problem of the crosslinked hydrolysis of polymerized acrylonitrile fiber, but this technology is to prepare copolymerized acrylonitrile with solution polymerization process, and some condition is not suitable for domestic and international enterprise production status.Fiber of the present invention is different with the technological invention point of patent formerly, it has adopted the aqueous phase precipitation legal system to be equipped with the method for copolymerized acrylonitrile, mainly solved latent crosslinker with polyacrylonitrile and vinyl acetate polyisocyanate polyaddition after hot crosslinked technical problem, can be applicable to enterprise's production application better.
The present invention does not address part and is applicable to prior art.
Provide specific embodiments of the invention below, but the present invention is not subjected to the restriction of embodiment:
Embodiment 1
Design copolymerized acrylonitrile mass percent prescription is: acrylonitrile 81.8%, vinylacetate 9.2%, acrylic acid-2-hydroxypropyl acrylate 10% are monomer, sodium chlorate with monomer gross mass 0.2% is initator, the sodium sulfite of monomer gross mass 0.6% is a reductant, the pH that makes mixing material is 2, the aqueous phase precipitation polymerization is carried out in nitrogen protection in water, 45 ℃ times heating, stirring, and wherein monomer mass is 30% of a quality, reaction time is 1h, can obtain copolymerized acrylonitrile; Again copolymerized acrylonitrile and cellulose acetate were pressed 95: 5 respectively, 90: 10,85: 15 ratio blend, with N, the N-dimethylacetylamide is 20% spinning solution for the solvent configuration concentration, behind gained copolymer solution vacuum defoamation 2h, and the N with 40%, the N-dimethylacetylamide aqueous solution is the coagulating agent wet spinning, can obtain polymerized acrylonitrile fiber; Again through 180 ℃ of heat cross-linking 30min, 80 ℃ down with 10%NaOH solution hydrolysis 6min, after the neutralization of 2% concentration watery hydrochloric acid removes alkali, drying at room temperature and handles, promptly can be made into three kinds of hydrophilic polymerized acrylonitrile fibers of the present invention.
Through test, the fracture strength of three kinds of gained fibers is respectively 1.5cN/dtex, 1.9cN/dtex and 1.9cN/dtex; Respectively it is immersed in the pure water, record its saturated water absorption and be respectively 2.3g/g, 3.9g/g and 5.9g/g; Again the fiber after the saturated suction is placed centrifuge, the centrifugal speed rotation 5min with 1000r/min records its water retention rate and is respectively 91.3%, 85.4% and 79.7%.
Embodiment 2
Press embodiment 1 method, under the copolymerized acrylonitrile condition that to be 9: 1 and other preparation process than cellulose acetate identical with embodiment 1, hydrolysis temperature is got 65 ℃, 80 ℃ and 95 ℃ respectively, obtain three kinds of hydrophilic fibres, its fracture strength is respectively 2.2cN/dtex, 1.9cN/dtex and 1.4cN/dtex.The saturated water absorption that records three kinds of hydrophilic fibres is respectively 1.0g/g, 5.9g/g and 20.7g/g; Recording its water retention rate respectively with the method for embodiment 1 is 73.0%, 87.5% and 91.3%.
Embodiment 3
Press embodiment 1 described preparation method, be under 9: 1 the mixed ratio at copolymerized acrylonitrile and cellulose acetate, under the identical condition of other preparation process and embodiment 1, the NaOH concentration of aqueous solution gets 5%, 10%, 15% and 20% respectively in the hydrolytic process, makes four kinds of described fibers.Its fracture strength is respectively 2.4cN/dtex, 1.9cN/dtex, 1.8cN/dtex and 1.8dcN/dtex.The saturated water absorption that records this series fiber with the method for embodiment 1 respectively is 1.0g/g, 5.9g/g, 13.5g/g and 15.7g/g.
Embodiment 4
Press the method for embodiment 1, under the copolymerized acrylonitrile condition that to be 9: 1 and other preparation process than cellulose acetate identical with embodiment 1, hydrolysis time is got 4min, 8min, 12min and 16min respectively, makes four kinds of hydrophilic fibres.Its fracture strength is respectively 2.0cN/dtex, 1.8cN/dtex, 1.5cN/dtex and 1.5cN/dtex.The saturated water absorption that records this series fiber with the method for embodiment 1 respectively is 3.7g/g, 5.9g/g, 15.1g/g and 15.6g/g.
Embodiment 5
Press the method for embodiment 1, under the copolymerized acrylonitrile condition that to be 95: 5 and other preparation process than cellulose acetate identical with embodiment 1, hydrolysis temperature is got 65 ℃, 80 ℃, 95 ℃ respectively, obtains three kinds of hydrophilic fibres.Its fracture strength is respectively 1.9cN/dtex, 1.8cN/dtex and 1.3cN/dtex. and is respectively 2.9g/g, 5.9g/g, 22.5g/g with the saturated water absorption that the method for embodiment 1 records this series hydrophilic fibre.
Embodiment 6
Pressing the method for embodiment 1, is 95: 5 at copolymerized acrylonitrile than cellulose acetate, and under the identical condition of other preparation process and embodiment 1, hydrolysis time is got 4min, 8min, 12min and 16min respectively, obtains hydrophilic fibre.Its fracture strength is respectively 2.0cN/dtex, 1.8cN/dtex, 1.5cN/dtex and 1.5cN/dtex.The saturated water absorption that records this series hydrophilic fibre with the method for embodiment 1 respectively is 1.9g/g, 5.3g/g and 16.2g/g.
Embodiment 7
Press the method for embodiment 1, in copolymerized acrylonitrile than cellulose acetate is 9: 1 the preparation process of polymerized acrylonitrile fiber, respectively to 4,5 and 6 times of this tensile fibers, the gained fiber is handled through the condition identical with embodiment 1, can make three kinds of hydrophilic fibres in boiling water bath.
Through experiment, the fracture strength of this series fiber is respectively 0.8CN/dtex, 1.2CN/dtex and 1.9CN/dtex.The fracture strength of suction back fiber is respectively 0.6CN/dtex, 1.1CN/dtex and 1.85CN/dtex.After repeating suction-dehydration 5 times, marked change does not all take place in the water absorbing properties of gained hydrophilic fibre.Can keep its original mechanical property after the suction of gained hydrophilic fibre is described, and have reusability preferably.
Claims (3)
1. the preparation method of a hydrophilic polymerized acrylonitrile fiber, this preparation method comprises
(1) preparation copolymerized acrylonitrile, this copolymerization process is an aqueous precipitation polymerization, with mass percent concentration is that 76～85% acrylonitrile and mass percent concentration are that 9～10% vinylacetates are monomer, with mass percent concentration is that acrylic acid-2-hydroxypropyl acrylate of 5～15% is a latent crosslinker, initator sodium chlorate through mass percent concentration 0.2% causes, mass percent concentration is 0.6%, pH is 2 ± 0.1 reductant sodium sulfite reduction, described monomer mass is 25～40% of a quality, copolyreaction 1～1.5h can obtain copolymerized acrylonitrile;
(2) spinning polymerized acrylonitrile fiber, after the copolymerized acrylonitrile drying with gained, with cellulose acetate in 85～95: 15～5 ratio blend is even, with N, the N-dimethylacetylamide is a solvent, and the spinning solution of configuration 15～25% concentration is behind vacuum defoamation 1.5～2h, through wet spinning, can make polymerized acrylonitrile fiber;
(3) aftertreatment technology, the gained polymerized acrylonitrile fiber can make described hydrophilic polymerized acrylonitrile fiber after crosslinked, hydrolysis, neutralization, removing alkali and dehydration and drying process processing.
2. according to the preparation method of the described hydrophilic polymerized acrylonitrile fiber of claim 1, it is characterized in that described crosslinking process is meant the heat cross-linking 20-40min in 160～180 ℃ hot-air of the polymerized acrylonitrile fiber behind the relaxation heat setting; Described hydrolysis process is meant the polymerized acrylonitrile fiber behind the heat cross-linking in concentration is 5～20% sodium hydrate aqueous solution, hydrolysis 2～20min under 65～95 ℃ of temperature.
3. a hydrophilic polymerized acrylonitrile fiber is characterized in that this fiber is made by the preparation method of claim 1 or 2 described hydrophilic polymerized acrylonitrile fibers.
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| CN100491608C (en) | 2009-05-27 |
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