CN103205822A - Preparation method for hydrophilic polyacrylonitrile stoste - Google Patents
Preparation method for hydrophilic polyacrylonitrile stoste Download PDFInfo
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- CN103205822A CN103205822A CN2013101526630A CN201310152663A CN103205822A CN 103205822 A CN103205822 A CN 103205822A CN 2013101526630 A CN2013101526630 A CN 2013101526630A CN 201310152663 A CN201310152663 A CN 201310152663A CN 103205822 A CN103205822 A CN 103205822A
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Abstract
The invention relates to a preparation method for hydrophilic polyacrylonitrile stoste. The method is characterized by comprising the following steps of: (1) hydrolyzing an acrylonitrile copolymer by a basic metal saline liquid; (2) precipitating the obtained hydrolysate, and filtering and adding acid to adjust the pH value to 4-7; (3) preparing the acrylonitrile hydrolysate to the hydrolyzed polyacrylonitrile stoste by the polyacrylonitrile acrylonitrile by a spinning solvent; and (4) adjusting the temperature of the hydrolyzed polyacrylonitrile stoste, and uniformly mixing with normally produced polyacrylonitrile stoste at certain mass ratio adequately to prepare the hydrophilic polyacrylonitrile stoste. The preparation method for hydrophilic polyacrylonitrile stoste provided by the invention based on an original polymerization process can simply prepare the hydrophilic polyacrylonitrile stoste and has the advantages of simple method, good uniformity of stoste, low device requirement, lower cost and the like.
Description
Technical field
The present invention relates to a kind of preparation method of hydrophilic polypropylene nitrile stoste, particularly a kind of polyacrylonitrile stoste that adopts polyacrylonitrile basic hydrolysis solution and conventional production to obtain is carried out the preparation method of the hydrophilic polypropylene nitrile stoste of a certain proportion of blend.
Background technology
Polyacrylonitrile fibre is one of three big synthetic fiber, has characteristics such as good warmth retention property, dyeability and simulate wool, and the title of artificial wool is arranged, and is widely used in the fields of taking such as knitted underwear, woollen blanket, Fake Furss.But along with growing with clothing design of improving constantly of people's living standard, warming no longer is the unitary request of clothes, and people are 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 available standards regain is represented.The regain of natural fabric is about 7～15%, and polyacrylonitrile fibre only is 1.2～2%, show serious defective in performances relevant with the human body skin-friendly such as hygroscopicity, poisture-penetrabilitys, 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 the blend ratio after additional functionality processing or the minimizing, not only increase processing cost, and the durability for the treatment of effect is lower, thereby greatly reduce the wearability of polyacrylonitrile fibre, more use limited in some field that has antistatic behaviour to require.
In order to improve the hygroscopicity of acrylic fibers, improve the wearing comfort of acrylic fibers, the researcher has adopted several different methods that the moisture pick-up properties of acrylic fibers is carried out modification.For example acrylic fibers and native protein or cellulose are carried out grafting or blending and modifying, make fiber with the premium properties of natural fabric and synthetic fiber, this respect is domestic has carried out more research, developed a kind of collagen-polyacrylonitrile composite fiber as CN1243140C, it is to utilize the collagen that separation and Extraction obtains from rawhide or leather industry discarded object, with acrylonitrile and other vinyl monomer graft copolymerization after carry out the modified fibre that spinning obtains with the polyacrylonitrile blended spinning solution that obtains again; CN101240467B has invented a kind of manufacture method of cellulose-polyacrylonitrile composite fiber, it is that the employing ionic liquid is dissolution with solvents cellulose and polyacrylonitrile, carry out the composite fibre that spinning obtains blending type or core-skin type after making blend solution, because cellulosic hygroscopicity and and polyacrylonitrile between the half-phase capacitive, multi-cellular structure can appear in the gained fiber, gives the fiber moisture permeability.But no matter be that polyacrylonitrile is carried out surface graft protein or co-blended spinning is made composite fibre, because grafting limited amount and the restriction of blend ratio make that the hygroscopic raising of acrylic fibers is limited, modified effect is not obvious.
In addition, also there is the method for monomer by adding hydrophilic radical in the polymerization formula or latent crosslinker to prepare the report of similar hydrophily polyacrylonitrile fibre, but because the change of copolymerization process is to polymerization production control and polymerizate Effect on Performance, and the follow-up basic hydrolysis processing of spinning the long period indispensable on the journey, make these class methods not have the condition of online production moisture absorption polyacrylonitrile fibre.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of hydrophilic polypropylene nitrile stoste, the present invention is directed to the above-mentioned state of the art, from satisfying the requirement of taking of polyacrylonitrile fibre, provide a kind of preparation method of hydrophilic polypropylene nitrile stoste.
The objective of the invention is under the prerequisite that does not change polymerization technique, a kind of preparation method of hydrophilic polypropylene nitrile stoste is provided.Be specially and adopt polyacrylonitrile basic hydrolysis solution and the conventional polyacrylonitrile stoste that obtains of producing to carry out a certain proportion of blend, thereby obtain hydrophilic polypropylene nitrile stoste.
The preparation method of a kind of hydrophilic polypropylene nitrile stoste 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;
Acrylonitrile copolymer is 1:0.5～1:2.0 with the ratio of the quality of alkaline metal salt, and hydrolysising reacting temperature is 80～110 ℃, and hydrolysis time is 1～10 hour;
Cyano group in the acrylonitrile copolymer has greater activity, and cyano group reacts under the effect of alkalinous metal saline solution, can hydrolysis generate hydrophilic radicals such as amide groups, carboxyl.
(2) precipitating
In order to improve the concentration of polyacrylonitrile hydrolyzed thing in hydrolyzate, with 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 polyacrylonitrile hydrolyzed thing;
(3) preparation hydrolyzed polyacrylonitrile stoste
For the ease of adding, further realize and the even blend of conventional stoste, need polyacrylonitrile hydrolyzed thing is mixed with solution.Described polyacrylonitrile hydrolyzed thing is deployed into hydrolyzed polyacrylonitrile stoste with spin solvent, and the adjusting solid content is 10～40wt%;
(4) preparation hydrophilic polypropylene nitrile stoste
Polyacrylonitrile is through the molecular weight and molecular weight after the hydrolysis, water-solublely improves greatly, can't satisfy the wet spinning requirement, and hydrolyzed polyacrylonitrile stoste and conventional polyacrylonitrile stoste can be obtained stable and uniform, satisfy the stoste of spinning fibre requirement with the certain proportion blend.
With described hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃～80 ℃, the polyacrylonitrile stoste 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, hydrophilic polypropylene nitrile stoste contains the hydrolysising original liquid of a large amount of hydrophilic radicals owing to the blend molecular structure, thereby has the suction moisture pick-up properties.
As optimized technical scheme:
The preparation method of aforesaid a kind of hydrophilic polypropylene nitrile stoste, 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 aforesaid a kind of hydrophilic polypropylene nitrile stoste, 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 aforesaid a kind of hydrophilic polypropylene nitrile stoste, described acrylonitrile copolymer is the copolymer of acrylonitrile monemer and other second comonomer and/or the 3rd comonomer; Described other second comonomer is a kind of in acrylate monomer, methacrylate monomers or the vinyl acetate, and the 3rd comonomer is a kind of in methylpropene sodium sulfonate, Sodium styrene sulfonate, sodium vinyl sulfonate or the 2-acrylamido-2-methyl propane sulfonic acid.
The preparation method of aforesaid a kind of hydrophilic polypropylene nitrile stoste, 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 aforesaid a kind of hydrophilic polypropylene nitrile stoste, 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 aforesaid a kind of hydrophilic polypropylene nitrile stoste, 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 aforesaid a kind of hydrophilic polypropylene nitrile stoste, described solvent is absolute ethyl alcohol, acetone or methyl alcohol.
In a kind of hydrophilic polypropylene nitrile stoste that the present invention makes, the acrylonitrile copolymer main chain is the C-C singly-bound, contains carboxyl, amide groups and a large amount of cyano group in the big molecule of acrylonitrile copolymer simultaneously.Described hydrophilic polypropylene nitrile stoste is by conventional polyacrylonitrile stoste, the 5～40wt% hydrolyzed polyacrylonitrile stoste of 60～95wt%, and when adopting inorganic solvent, wherein polyacrylonitrile is 10～24.4wt%, and solvent is 38～45wt%, and water is 30.6～52wt%; When adopting organic solvent, wherein polyacrylonitrile is 20～30wt%, and solvent is 70～80wt%.
Beneficial effect:
The preparation method of a kind of hydrophilic polypropylene nitrile stoste provided by the present invention, on the basis of original polymerization technique, can prepare hydrophilic polypropylene nitrile stoste more simply, have advantages such as method is simple, the stoste homogeneity is good, less demanding to equipment, cost is lower.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The acrylonitrile compolymer body of being made up of acrylonitrile, methyl acrylate and methylpropene sodium sulfonate is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained absolute ethyl alcohol precipitating, filter the back with nitre acid for adjusting pH value to 4, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 13wt% with sodium thiocyanate water solution.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 5wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 2
The acrylonitrile compolymer body of being made up of acrylonitrile and methyl methacrylate is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained absolute ethyl alcohol precipitating, filter the back with first acid for adjusting pH value to 5, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 12wt% with dimethyl sulfoxide (DMSO).With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 15wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 3
The acrylonitrile compolymer body of being made up of acrylonitrile and ethyl acrylate is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained acetone precipitating, filter the back with salt acid for adjusting pH value to 5, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 15wt% with solder(ing)acid.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 10wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 4
Receiving the acrylonitrile compolymer body of forming by acrylonitrile, ethyl acrylate and vinyl sulfonic acid is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained acetone precipitating, filter the back with sulphur acid for adjusting pH value to 6, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 15wt% with dimethylacetylamide.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 5wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 5
The acrylonitrile compolymer body of being made up of acrylonitrile, butyl acrylate and Sodium styrene sulfonate is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, filter the back with second acid for adjusting pH value to 6, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 13wt% with sodium thiocyanate water solution.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 20wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 6
The acrylonitrile compolymer body of being made up of acrylonitrile, butyl acrylate and 2-acrylamido-2-methyl propane sulfonic acid is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, filter the back and regulate pH value to 7 with ethanedioic acid, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 40wt% with dimethyl formamide.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 25wt% of described hydrophilic polypropylene nitrile stoste.
Embodiment 7
The acrylonitrile compolymer body of being made up of acrylonitrile, vinyl acetate and methylpropene sodium sulfonate is hydrolyzed in the 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 with the hydrolyzate of hydrolysis process gained methyl alcohol precipitating, filter the back with salt acid for adjusting pH value to 7, then resulting polyacrylonitrile hydrolyzed thing is deployed into the hydrolyzed polyacrylonitrile stoste that solid content is 20wt% with dimethyl formamide.With this hydrolyzed polyacrylonitrile stoste temperature adjustment to 80 ℃, fully mix with conventional polyacrylonitrile stoste of producing, obtain hydrophilic polypropylene nitrile stoste, wherein hydrolyzed polyacrylonitrile stoste accounts for the 40wt% of described hydrophilic polypropylene nitrile stoste.
Claims (8)
1. the preparation method of a hydrophilic polypropylene nitrile stoste is characterized in that comprising the steps:
(1) acrylonitrile copolymer hydrolysis;
With the aqueous solution of alkaline metal salt to the polymer processing that is hydrolyzed;
Acrylonitrile copolymer is 1:0.5～1:2.0 with the ratio of the quality of alkaline metal salt, and hydrolysising reacting temperature is 80～110 ℃, and hydrolysis time is 1～10 hour;
(2) precipitating;
With the hydrolyzate solvent precipitation of described hydrolysis process gained, filter the back and add acid for adjusting pH value to 4～7, the polyacrylonitrile hydrolyzed thing that obtains;
(3) preparation hydrolyzed polyacrylonitrile stoste;
Described polyacrylonitrile hydrolyzed thing is deployed into hydrolyzed polyacrylonitrile stoste with spin solvent, and the adjusting solid content is 10～40wt%;
(4) preparation hydrophilic polypropylene nitrile stoste;
With described hydrolyzed polyacrylonitrile stoste temperature adjustment to 70 ℃～80 ℃, the polyacrylonitrile stoste 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.
2. the preparation method of a kind of hydrophilic polypropylene nitrile stoste according to claim 1 is characterized in that, 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%.
3. the preparation method of a kind of hydrophilic polypropylene nitrile stoste according to claim 2 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 stoste according to claim 1 is characterized in that, described acrylonitrile copolymer is the copolymer of acrylonitrile monemer and other second comonomer and/or the 3rd comonomer; Described other second comonomer is a kind of in acrylate monomer, methacrylate monomers or the vinyl acetate, and the 3rd comonomer is a kind of in methylpropene sodium sulfonate, Sodium styrene sulfonate, sodium vinyl sulfonate or the 2-acrylamido-2-methyl propane sulfonic acid.
5. the preparation method of a kind of hydrophilic polypropylene nitrile stoste 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 stoste 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 stoste 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 stoste according to claim 1 is characterized in that, described solvent is absolute ethyl alcohol, acetone or methyl alcohol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220256A (en) * | 2014-06-06 | 2016-01-06 | 中国石油化工股份有限公司 | Be applicable to spinning solution and the preparation method of dry acrylic spinning |
| CN105273125A (en) * | 2014-06-06 | 2016-01-27 | 中国石油化工股份有限公司 | Polyacrylonitrile dry powder suitable for dry acrylic fiber spinning, and preparation method thereof |
| CN108085766A (en) * | 2017-12-13 | 2018-05-29 | 华南理工大学 | A kind of cellulose nanometer fibril enhancing acrylic fiber and preparation method and application |
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| 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 |
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2013
- 2013-04-27 CN CN2013101526630A patent/CN103205822A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220256A (en) * | 2014-06-06 | 2016-01-06 | 中国石油化工股份有限公司 | Be applicable to spinning solution and the preparation method of dry acrylic spinning |
| CN105273125A (en) * | 2014-06-06 | 2016-01-27 | 中国石油化工股份有限公司 | Polyacrylonitrile dry powder suitable for dry acrylic fiber spinning, and preparation method thereof |
| CN108085766A (en) * | 2017-12-13 | 2018-05-29 | 华南理工大学 | A kind of cellulose nanometer fibril enhancing acrylic fiber and preparation method and application |
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Application publication date: 20130717 |