CN103205823B - Preparation method of hydrophilic polyacrylonitrile fiber - Google Patents
Preparation method of hydrophilic polyacrylonitrile fiber Download PDFInfo
- Publication number
- CN103205823B CN103205823B CN201310152671.5A CN201310152671A CN103205823B CN 103205823 B CN103205823 B CN 103205823B CN 201310152671 A CN201310152671 A CN 201310152671A CN 103205823 B CN103205823 B CN 103205823B
- Authority
- CN
- China
- Prior art keywords
- polyacrylonitrile
- polypropylene nitrile
- preparation
- hydrophilic polypropylene
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a preparation method of a hydrophilic polyacrylonitrile fiber. The preparation method is characterized by comprising the following steps to obtain the fiber: (1) carrying out hydrolysis treatment on an acrylonitrile copolymer by using an aqueous solution of an alkaline metal salt; (2) precipitating the obtained hydrolysate using a solvent, filtering the resulting product, and regulating the pH value of the filtered product to 4-7 by adding acid; (3) preparing the obtained polyacrylonitrile hydrolysate to a hydrolyzed polyacrylonitrile raw liquid by using a spinning solvent; (4) regulating the temperature of the hydrolyzed polyacrylonitrile raw liquid, sufficiently and uniformly mixing the temperature reduced hydrolyzed polyacrylonitrile raw liquid with the polyacrylonitrile raw liquid produced by using a conventional method according to a certain mass ratio to prepare a hydrophilic polyacrylonitrile raw liquid; and (5) subjecting the raw liquid to extrusion solidification molding, pre-drawing, washing, hot drawing, densification-crosslinking, shape fixing, oiling, and drying procedures in a polyacrylonitrile wet spinning production line to obtain the hydrophilic polyacrylonitrile fiber. The hydrophilic polyacrylonitrile fiber prepared by the method provided by the invention not only has good moisture adsorption performance, but also is good in uniformity and durability, as well as is not limited by size and length of the fiber, and the preparation method is high in production efficiency.
Description
Technical field
The invention belongs to chemical fibre manufacturing technology field, be specifically related to a kind of manufacture method of hydrophilic polypropylene nitrile fiber.
Background technology
Polyacrylonitrile fibre is one of three large synthetic fiber, has the features such as good warmth retention property, dyeability and simulate wool, has the title of artificial wool, in the fields of taking such as knitted underwear, woollen blanket, Fake Furss, is widely used.But along with growing with clothing design of improving constantly of people's living standard, warming is no longer the unitary request of clothes, people to its comfort level, functional and security requirement is more and more higher.The gender gap comfortable and easy to wear of different fibrous material clothes is relevant with the moisture pick-up properties of fiber, and moisture pick-up properties can represent with official regain.The official regain of natural fabric is about 8～15%, and polyacrylonitrile fibre is only 2%, in the performance relevant to human body skin-friendly such as hygroscopicity, poisture-penetrability, show serious defect, make its clothing dress of making have feeling of oppression and heat, sweat to be difficult for being absorbed and distributing, static behaviour is strong, often need to spin blend ratio after additional functionality processing or minimizing, not only increase processing cost, and the durability for the treatment of effect is lower, thereby greatly reduce the wearability of polyacrylonitrile fibre, the field application that more has antistatic behaviour to require at some is limited.
In order to improve the hygroscopicity of acrylic fibers, improve the wearing comfort of acrylic fibers, researcher has adopted several different methods to carry out modification to the moisture pick-up properties of acrylic fibers.For example CN1900413A provides a kind of employing acrylic fiber surface graft protein to carry out modification, first under certain condition acrylic fiber is hydrolyzed, then hydrolysis fiber is reacted to obtain to chloride fiber with thionyl chloride, again with protein grafting, making superficial layer is phytoprotein grafting cover layer, core is the modified fibre of acrylic fiber, has improved the hygroscopicity of acrylic fibers.But due to grafting limited amount, make the hygroscopic raising of acrylic fibers limited, modified effect is not obvious.Abroad adopt chemical modification method carry out moisture absorption polyacrylonitrile prepare aspect research early.As Japan discloses polyacrylonitrile fibre is hydrolyzed and compound crosslink is processed and prepared the method for water absorbent fiber in the patent such as CN1239775C, CN1247849C, CN1230585C, CN101023212B and CN101914852A of China application, and in fibre whiteness and fire resistance, improve respectively.The durability of these methods is better, but shortcoming be due to hydrolysis and crosslinked chemical treatment time longer, can only be applied to spin batch processing process after staple fibre, belong to a kind of off-line and produce the manufacture method of water absorbent fiber, thereby the inhomogeneity of the moisture absorption of fiber treatment and fibrous physics mechanical performance is higher, production efficiency is low.
In addition, also have by adding the monomer of hydrophilic radical or the method for latent crosslinker to prepare the report of similar hydrophily polyacrylonitrile fibre in polymerization formula, but due to the change of the copolymerization process impact on polymerization production control and polymerizate performance, and the follow-up basic hydrolysis processing of spinning the long period indispensable in journey, make these class methods not have the condition of online production moisture absorption polyacrylonitrile fibre.
Summary of the invention
The present invention is directed to the above-mentioned state of the art, from meeting the requirement of taking of polyacrylonitrile fibre, provide a kind of online production method that obtains hydrophilic polypropylene nitrile fiber in conventional polyacrylonitrile fibre manufacture process.Do not changing under the prerequisite of polymerization technique, adopting polyacrylonitrile basic hydrolysis solution and the conventional polyacrylonitrile matrix obtaining of producing to carry out a certain proportion of blend spinning, thereby prepare hydrophilic polypropylene nitrile fiber.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber of the present invention, comprises the steps:
(1) acrylonitrile copolymer hydrolysis
With the aqueous solution of alkaline metal salt to the polymer processing that is hydrolyzed;
The mass ratio of acrylonitrile copolymer and alkaline metal salt is 1:0.5～1:2.0, and hydrolysising reacting temperature is 80～110 ℃, and hydrolysis time is 1～10 hour;
Cyano group in acrylonitrile copolymer has greater activity, and cyano group reacts under the effect of alkalinous metal saline solution, can be hydrolyzed hydrophilic radicals such as generating amide groups, carboxyl;
(2) precipitating
In order to improve the concentration of hydrolysate polyacrylonitrile in hydrolyzate, by the hydrolyzate solvent precipitation of described hydrolysis process gained, polyacrylonitrile hydrolyzed liquid after filtering shows as alkalescence, adds acid for adjusting pH value to 4～7, obtains hydrolysate polyacrylonitrile;
(3) preparation hydrolyzed polyacrylonitrile stoste
For the ease of adding, further realize and the even blend of conventional stoste, hydrolysate polyacrylonitrile need be mixed with to solution.Described hydrolysate polyacrylonitrile is deployed into hydrolyzed polyacrylonitrile stoste with spin solvent, and adjusting solid content is 10～40wt%;
(4) preparation hydrophilic polypropylene nitrile stoste
The molecular weight and molecular weight of polyacrylonitrile after hydrolysis, water-solublely improves greatly, cannot meet wet spinning requirement, and hydrolyzed polyacrylonitrile stoste and conventional polyacrylonitrile matrix can be obtained to stable and uniform, meet the stoste of spinning fibre requirement with certain proportion blend.
By described hydrolyzed polyacrylonitrile stoste temperature adjustment to 70～80 ℃, the polyacrylonitrile matrix of producing with routine fully mixes, and prepares hydrophilic polypropylene nitrile stoste; Wherein, described hydrolyzed polyacrylonitrile stoste accounts for 5～40wt% of described hydrophilic polypropylene nitrile stoste.More conventional stoste, the hydrolysising original liquid that hydrophilic polypropylene nitrile stoste contains a large amount of hydrophilic radicals due to blend molecular structure, thus there is water suction moisture pick-up properties;
(5) spinning solidification forming
Spinning solution is extruded from spinnerets, forms as-spun fibre in coagulating bath;
(6) preliminary draft
1.0～4.0 times of as-spun fibre preliminary drafts after coagulation forming;
(7) washing
As-spun fibre after preliminary draft washes away spin solvent, and water temperature is 45～65 ℃;
(8) hot drawing-off
In the hot water of 98～100 ℃, carry out the water-bath drawing-off of 3.0～10.0 times;
(9) densification-crosslinked
Fiber after hot drawing-off is carried out at 105～145 ℃ to thermal crosslinking treatment;
(10) curling and sizing
Adopt hot bath or decatize mode preheating tow to carry out machine crimp, the fiber after curling carries out the processing of saturated vapor HEAT SETTING, and heat setting temperature is 120～135 ℃;
(11) oil and dry
After HEAT SETTING, fiber floods and oils, and concentration of oil trough is 1.0～3.0%, afterwards, in temperature, is lax oven dry in second drying machine of 90～120 ℃.
As preferred technical scheme:
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described alkaline metal salt is alkali metal hydroxide, alkaline earth metal hydroxide or alkali carbonate; The concentration of aqueous solution of described alkaline metal salt is 1～40wt%.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described alkali metal hydroxide is NaOH or potassium hydroxide; Described alkaline earth metal hydroxide is magnesium hydroxide or calcium hydroxide; Described alkali carbonate is sodium bicarbonate or saleratus.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described acrylonitrile copolymer is the copolymer of acrylonitrile monemer and other the second comonomer and/or the 3rd comonomer; Described other second comonomer is a kind of in acrylate monomer, methacrylate monomers or vinyl acetate, and the 3rd comonomer is a kind of in methylpropene sodium sulfonate, Sodium styrene sulfonate, sodium vinyl sulfonate or 2-acrylamide-2-methylpro panesulfonic acid.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described acrylate monomer is methyl acrylate, ethyl acrylate or butyl acrylate; Described methacrylate monomers is methyl methacrylate, ethyl methacrylate or butyl methacrylate.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described acid is inorganic acid or the organic acid aqueous solution; Described inorganic acid is nitric acid, hydrochloric acid or sulfuric acid, and described organic acid is formic acid, acetic acid or ethanedioic acid.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described spin solvent is organic solvent or inorganic solvent; Described organic solvent is dimethyl formamide, dimethyl sulfoxide (DMSO) or dimethylacetylamide, and described inorganic solvent is sodium thiocyanate water solution or solder(ing)acid.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described solvent is absolute ethyl alcohol, acetone or methyl alcohol.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, described hydrophilic polypropylene nitrile fiber is endless tow or staple fibre.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, in described hydrophilic polypropylene nitrile stoste, acrylonitrile copolymer main chain is C-C singly-bound, contains carboxyl, amide groups and a large amount of cyano group in the large molecule of acrylonitrile copolymer simultaneously.Described hydrophilic polypropylene nitrile stoste is by conventional polyacrylonitrile matrix, the 5～40wt% hydrolyzed polyacrylonitrile stoste of 60～95wt%, and while adopting inorganic solvent, wherein polyacrylonitrile is 10～24.4wt%, and solvent is 38～45wt%, and water is 30.6～52wt%; While adopting organic solvent, wherein polyacrylonitrile is 20～30wt%, and solvent is 70～80wt%.
The preparation method of a kind of hydrophilic polypropylene nitrile fiber as above, the water absorption rate of described hydrophilic polypropylene nitrile fiber records with the following method: a kind of hydrophilic polypropylene nitrile fiber sample (approximately 5g) is dried to constant weight and weighs its weight in the electric drying oven with forced convection of 105 ℃ is W1(g), then sample is dipped in enough distilled water to 30 minutes, taking-up allows it naturally dangle to drip after 30 minutes, and the weight that weighs sample is W2(g).By formula below, calculate sample water absorption rate:
Water absorption rate (g water/g fiber)=(W2-W1)/W1
Beneficial effect:
The preparation method of a kind of hydrophilic polypropylene nitrile fiber provided by the present invention obtains hydrophilic polypropylene nitrile fiber in conventional polyacrylonitrile fibre manufacture process.The hydrophilic polypropylene nitrile fiber being obtained by the present invention not only has good moisture pick-up properties, and good uniformity, and durability is good, is not subject to the restriction of fibre number, length, and production efficiency is high.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
The acrylonitrile compolymer body being comprised of acrylonitrile, methyl acrylate and methylpropene sodium sulfonate is hydrolyzed in 1wt% sodium hydrate aqueous solution, the mass ratio of acrylonitrile copolymer and NaOH is 1:0.5, hydrolysis temperature is 90 ℃, hydrolysis time is 2 hours, then by the hydrolyzate of hydrolysis process gained absolute ethyl alcohol precipitating, after filtering, with nitre acid for adjusting pH value to 4, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 13wt% with sodium thiocyanate water solution.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 5wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 1.5 times of preliminary drafts, afterwards through 45 ℃ of washings, through carrying out the hot water drawing-off of 4.0 times in the hot water of 98 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 105 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 120 ℃, and the oil concentration oiling is 1.2%, and bake out temperature is 100 ℃.Obtain hydrophilic polypropylene nitrile fiber.This fiber can be cut off on request, make the hydrophilic polypropylene nitrile staple fibre of different length.The water absorption rate that obtains fiber of surveying is 24.
Embodiment 2
The acrylonitrile compolymer body being comprised of acrylonitrile and methyl methacrylate is hydrolyzed in 8wt% potassium hydroxide aqueous solution, the mass ratio of acrylonitrile copolymer and potassium hydroxide is 1:0.8, hydrolysis temperature is 100 ℃, hydrolysis time is 3 hours, then by the hydrolyzate of hydrolysis process gained absolute ethyl alcohol precipitating, after filtering, with first acid for adjusting pH value to 5, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 12wt% with dimethyl sulfoxide (DMSO).By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 15wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 1.0 times of preliminary drafts, afterwards through 50 ℃ of washings, through carrying out the hot water drawing-off of 5 times in the hot water of 100 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 120 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 125 ℃, and the oil concentration oiling is 1.0%, and bake out temperature is 110 ℃.Obtain hydrophilic polypropylene nitrile fiber.This fiber can be cut off on request, make the hydrophilic polypropylene nitrile staple fibre of different length.The water absorption rate that obtains fiber of surveying is 33.
Embodiment 3
The acrylonitrile compolymer body being comprised of acrylonitrile and ethyl acrylate is hydrolyzed in 10wt% sodium hydrate aqueous solution, the mass ratio of acrylonitrile copolymer and NaOH is 1:1.0, hydrolysis temperature is 105 ℃, hydrolysis time is 1 hour, then by the hydrolyzate of hydrolysis process gained acetone precipitating, after filtering, with salt acid for adjusting pH value to 5, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 15wt% with solder(ing)acid.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 10wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 2.3 times of preliminary drafts, afterwards through 58 ℃ of washings, through carrying out the hot water drawing-off of 4.0 times in the hot water of 99 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 110 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 120 ℃, and the oil concentration oiling is 2.3%, and bake out temperature is 110 ℃.Obtain hydrophilic polypropylene nitrile fiber.The water absorption rate that obtains fiber of surveying is 40.
Embodiment 4
By acrylonitrile, ethyl acrylate and vinyl sulfonic acid, receive formed acrylonitrile compolymer body is hydrolyzed in 12wt% magnesium hydroxide aqueous solution, the mass ratio of acrylonitrile copolymer and magnesium hydroxide is 1:1.2, hydrolysis temperature is 95 ℃, hydrolysis time is 2 hours, then by the hydrolyzate of hydrolysis process gained acetone precipitating, after filtering, with sulphur acid for adjusting pH value to 6, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 15wt% with dimethylacetylamide.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 5wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 2.5 times of preliminary drafts, afterwards through 53 ℃ of washings, through carrying out the hot water drawing-off of 3.0 times in the hot water of 99 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 130 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 120 ℃, and the oil concentration oiling is 3.0%, and bake out temperature is 90 ℃.Obtain hydrophilic polypropylene nitrile fiber.The water absorption rate that obtains fiber of surveying is 25.
Embodiment 5
The acrylonitrile compolymer body being comprised of acrylonitrile, butyl acrylate and Sodium styrene sulfonate is hydrolyzed in 15wt% calcium hydroxide aqueous solution, the mass ratio of acrylonitrile copolymer and calcium hydroxide is 1:1.5, hydrolysis temperature is 95 ℃, hydrolysis time is 4 hours, then by the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, after filtering, with second acid for adjusting pH value to 6, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 13wt% with sodium thiocyanate water solution.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 20wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 3.5 times of preliminary drafts, afterwards through 55 ℃ of washings, through carrying out the hot water drawing-off of 2.6 times in the hot water of 100 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 145 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 130 ℃, and the oil concentration oiling is 2.0%, and bake out temperature is 110 ℃.Obtain hydrophilic polypropylene nitrile fiber.The water absorption rate that obtains fiber of surveying is 30.
Embodiment 6
The acrylonitrile compolymer body being comprised of acrylonitrile, butyl acrylate and 2-acrylamide-2-methylpro panesulfonic acid is hydrolyzed in 30wt% sodium bicarbonate aqueous solution, the mass ratio of acrylonitrile copolymer and sodium bicarbonate is 1:1.8, hydrolysis temperature is 110 ℃, hydrolysis time is 5 hours, then by the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, after filtration, with ethanedioic acid, regulate pH value to 7, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 40wt% with dimethyl formamide.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 25wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 2.8 times of preliminary drafts, afterwards through 65 ℃ of washings, through carrying out the hot water drawing-off of 10 times in the hot water of 100 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 145 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 135 ℃, and the oil concentration oiling is 2.5%, and bake out temperature is 110 ℃.Obtain hydrophilic polypropylene nitrile fiber.The water absorption rate that obtains fiber of surveying is 29.
Embodiment 7
The acrylonitrile compolymer body being comprised of acrylonitrile, vinyl acetate and methylpropene sodium sulfonate is hydrolyzed in 40wt% potassium bicarbonate aqueous solution, the mass ratio of acrylonitrile copolymer and saleratus is 1:2.0, hydrolysis temperature is 80 ℃, hydrolysis time is 10 hours, then by the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, after filtering, with salt acid for adjusting pH value to 7, then resulting hydrolysate polyacrylonitrile is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 20wt% with dimethyl formamide.By this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, with the conventional polyacrylonitrile matrix of producing, fully mix, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 40wt% of described hydrophilic polypropylene nitrile stoste.Hydrophilic polypropylene nitrile stoste is extruded from spinnerets, in coagulating bath, solidify formation as-spun fibre, then as-spun fibre is through 1.8 times of preliminary drafts, afterwards through 50 ℃ of washings, through carrying out the hot water drawing-off of 6 times in the hot water of 98 ℃, the fiber after hot drawing-off carries out thermal crosslinking treatment at 125 ℃ again.Then carry out curling, shape, oil, dry.Heat setting temperature is 120 ℃, and the oil concentration oiling is 2.3%, and bake out temperature is 120 ℃.Obtain hydrophilic polypropylene nitrile fiber.The water absorption rate that obtains fiber of surveying is 36.
Claims (9)
1. a preparation method for hydrophilic polypropylene nitrile fiber, is characterized in that comprising the steps:
(1) acrylonitrile copolymer hydrolysis;
With the aqueous solution of alkaline metal cpds to the polymer processing that is hydrolyzed; Described alkaline metal cpds is alkali metal hydroxide, alkaline earth metal hydroxide or alkali carbonate;
The mass ratio of acrylonitrile copolymer and alkaline metal cpds is 1:0.5～1:2.0, and hydrolysising reacting temperature is 80～110 ℃, and hydrolysis time is 1～10 hour;
(2) precipitating;
Hydrolyzate solvent precipitation by described hydrolysis process gained, adds acid for adjusting pH value to 4～7 after filtration, the hydrolysate polyacrylonitrile obtaining;
(3) preparation hydrolyzed polyacrylonitrile stoste;
Described hydrolysate polyacrylonitrile is deployed into hydrolyzed polyacrylonitrile stoste with spin solvent, and adjusting solid content is 10～40wt%;
(4) preparation hydrophilic polypropylene nitrile stoste;
By described hydrolyzed polyacrylonitrile stoste temperature adjustment to 70～80 ℃, the polyacrylonitrile matrix of producing with routine fully mixes, and prepares hydrophilic polypropylene nitrile stoste; Wherein, described hydrolyzed polyacrylonitrile stoste accounts for 5～40wt% of described hydrophilic polypropylene nitrile stoste;
(5) spinning solidification forming;
Described hydrophilic polypropylene nitrile stoste is extruded from spinnerets, through coagulating bath, formed as-spun fibre;
(6) preliminary draft;
By 1.0～3.5 times of as-spun fibre preliminary drafts;
(7) washing;
Then wash away spin solvent, washing temperature is 45～65 ℃;
(8) hot drawing-off;
In the hot water of 98～100 ℃, carry out the water-bath drawing-off of 2.5～5.0 times;
(9) densification-crosslinked;
Fiber after hot drawing-off is carried out at 105～145 ℃ to thermal crosslinking treatment;
(10) curling and sizing;
Adopt hot bath or decatize mode preheating tow to carry out machine crimp, the fiber after curling carries out the processing of saturated vapor HEAT SETTING, and heat setting temperature is 120～135 ℃;
(11) oil and dry;
After HEAT SETTING, fiber floods and oils, and concentration of oil trough is 1.0～2.5%, afterwards, in temperature, is lax oven dry in second drying machine of 90～120 ℃;
Obtain hydrophilic polypropylene nitrile fiber.
2. the preparation method of the flat polyacrylonitrile matrix of a kind of moisture absorption according to claim 1, is characterized in that, the concentration of aqueous solution of described alkaline metal cpds is 1～40wt%.
3. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described alkali metal hydroxide is NaOH or potassium hydroxide; Described alkaline earth metal hydroxide is magnesium hydroxide or calcium hydroxide; Described alkali carbonate is sodium bicarbonate or saleratus.
4. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described acrylonitrile copolymer is the copolymer of acrylonitrile monemer and other the second comonomer and/or the 3rd comonomer; Described other second comonomer is a kind of in acrylate monomer, methacrylate monomers or vinyl acetate, and the 3rd comonomer is a kind of in methylpropene sodium sulfonate, Sodium styrene sulfonate, sodium vinyl sulfonate or 2-acrylamide-2-methylpro panesulfonic acid.
5. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 4, is characterized in that, described acrylate monomer is methyl acrylate, ethyl acrylate or butyl acrylate; Described methacrylate monomers is methyl methacrylate, ethyl methacrylate or butyl methacrylate.
6. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described acid is inorganic acid or the organic acid aqueous solution; Described inorganic acid is nitric acid, hydrochloric acid or sulfuric acid, and described organic acid is formic acid, acetic acid or ethanedioic acid.
7. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described spin solvent is organic solvent or inorganic solvent; Described organic solvent is dimethyl formamide, dimethyl sulfoxide (DMSO) or dimethylacetylamide, and described inorganic solvent is sodium thiocyanate water solution or solder(ing)acid.
8. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described solvent is absolute ethyl alcohol, acetone or methyl alcohol.
9. the preparation method of a kind of hydrophilic polypropylene nitrile fiber according to claim 1, is characterized in that, described hydrophilic polypropylene nitrile fiber is endless tow or staple fibre.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310152671.5A CN103205823B (en) | 2013-04-27 | 2013-04-27 | Preparation method of hydrophilic polyacrylonitrile fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310152671.5A CN103205823B (en) | 2013-04-27 | 2013-04-27 | Preparation method of hydrophilic polyacrylonitrile fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103205823A CN103205823A (en) | 2013-07-17 |
| CN103205823B true CN103205823B (en) | 2014-11-26 |
Family
ID=48753223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310152671.5A Expired - Fee Related CN103205823B (en) | 2013-04-27 | 2013-04-27 | Preparation method of hydrophilic polyacrylonitrile fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103205823B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826764B (en) * | 2020-07-28 | 2021-10-15 | 吴忠德悦纺织科技有限公司 | Preparation method of modified multi-component composite yarn |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752302A (en) * | 2004-09-23 | 2006-03-29 | 中国石化上海石油化工股份有限公司 | Wet spinning method for polyacryl-nitrile fibre |
-
2013
- 2013-04-27 CN CN201310152671.5A patent/CN103205823B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1752302A (en) * | 2004-09-23 | 2006-03-29 | 中国石化上海石油化工股份有限公司 | Wet spinning method for polyacryl-nitrile fibre |
Non-Patent Citations (1)
| Title |
|---|
| P.Bajaj、叶明超.丙烯腈三元共聚物和其水解产物之混抽纤维的物理机械性能.《国外纺织技术（化纤、染整、环境保护分册）》.1989,第1989年卷(第6期),第6-10页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103205823A (en) | 2013-07-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103233291B (en) | Preparation method of moisture-absorption polyacrylonitrile fiber | |
| CN103205821B (en) | Preparation method of moisture-absorption flat polyacrylonitrile fiber | |
| CN103266381B (en) | Preparation method for moisture-absorbing and heat-radiating polyacrylonitrile yarn | |
| CN107237004B (en) | Crosslinked acrylate fiber and fiber structure containing the same | |
| CN102493016B (en) | Porous superfine polyamide 6 fully-drawn yarn, preparation method thereof, and equipment thereof | |
| CN102174720B (en) | Compound protein fiber and preparation method thereof | |
| WO2016127833A1 (en) | Acetic nitrile fibre and preparation method therefor | |
| CN101696517B (en) | Method for manufacturing adsorption transfer fiber | |
| CN103498208A (en) | Thermal storage fiber and preparation method thereof | |
| TW201816211A (en) | Modified acrylonitrile-based fiber, method for manufacturing fiber of the same, and fiber structure containing fiber thereof | |
| CN111334880B (en) | Photochromic lyocell fibers and method for making same | |
| CN101392456A (en) | Method for preparing super absorbent fiber by modification of polyvinyl alcohol fiber | |
| CN100368608C (en) | Method for preparing copolymerized acrylonitrile high water-absorption fiber | |
| WO2020238543A1 (en) | Functional protein fiber imitating human hair and wet spinning method therefor | |
| CN103205823B (en) | Preparation method of hydrophilic polyacrylonitrile fiber | |
| CN1294305C (en) | Acrylic fiber-crosslinking plant protein composite fiber and method for manufacturing the same | |
| CN102864521B (en) | Cortex-core protein and polyacrylonitrile compound fiber and method for wigs | |
| CN106283224A (en) | A kind of wet method has greatly the preparation method of light acrylon | |
| CN103205822A (en) | Preparation method for hydrophilic polyacrylonitrile stoste | |
| CN108342786B (en) | Acrylic fiber with magnet physiotherapy health-care function and preparation method thereof | |
| CN108532065A (en) | A kind of spinning process of modified cotton fiber and modified flax fiber blending yarn | |
| CN107419351A (en) | A kind of preparation technology of acrylic fiber | |
| CN101240462B (en) | Method for preparing acrylics-protein-copper salt composite antistatic fiber | |
| CN110453311A (en) | A kind of warming chitin fiber and preparation method thereof | |
| CN109577021A (en) | A kind of good wig preparation method of simulated effect |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141126 Termination date: 20200427 |