CN108166092A - A kind of preparation method of polyacrylonitrile-graphene oxide composite fibre - Google Patents
A kind of preparation method of polyacrylonitrile-graphene oxide composite fibre Download PDFInfo
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- CN108166092A CN108166092A CN201711489154.1A CN201711489154A CN108166092A CN 108166092 A CN108166092 A CN 108166092A CN 201711489154 A CN201711489154 A CN 201711489154A CN 108166092 A CN108166092 A CN 108166092A
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- Prior art keywords
- graphene oxide
- composite fibre
- polyacrylonitrile
- solvent
- acrylonitrile
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Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
- C08F220/46—Acrylonitrile with carboxylic acids, sulfonic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
Abstract
The present invention relates to a kind of preparation methods of polyacrylonitrile oxidation graphene composite fibre, by adding spherical graphene oxide, improve dispersion effect of the graphene oxide in arcylic acid system, the polyacrylonitrile oxidation graphene composite fibre of preparation has excellent mechanical property and higher yields and stability.In addition, multistage hot-stretch is carried out by the polyacrylonitrile oxidation graphene fiber to preparation, graphene oxide can be reduced into RGO, the mechanical property and electric conductivity of composite fibre are further promoted, the polyacrylonitrile oxidation graphene composite fibre finally prepared has excellent electricity and mechanical property.
Description
Technical field
The present invention relates to a kind of preparation methods of polyacrylonitrile-graphene oxide composite fibre
Technical background
Since 20 middle of century polyacrylonitrile fibres come out, polyacrylonitrile fibre is as a kind of heavy in textile industry
Raw material is wanted, in China, modified acrylic fibre or virgin pp nitrile fiber are referred to as " acrylic fibers ".Acrylic fibers have excellent warming
Property, resilience and flexibility, and its appearance has natural aesthetic feeling, referred to as synthetic wool.At the same time, polyacrylonitrile
Fiber also has against weather, light resistance, the stronger itrile group of polarized, therefore has stronger dyeability, in textile industry
The application in field is also increasingly broader.With the development of the times, it is increasingly vigorous for the demand of multifunction acrylic fibers, herein by
Spherical graphene oxide and acrylonitrile, acrylic acid, itaconic acid monomer in situ polymerization, it is multiple to be prepared for polyacrylonitrile-graphene oxide
Condensating fiber, the composite fibre have excellent antistatic property, uvioresistant performance, sterilization and far infrared performance.
Shi Qiquan etc. prepares spinning solution by the way that graphene oxide is dispersed in polyacrylonitrile solution, then passes through Wet-spinning
Silk is prepared for polyacrylonitrile-graphene oxide composite fibre, and this method directly prepares spinning using graphene oxide and PAN blendings
Liquid, it is difficult to solve scattering problem of the sheet graphene oxide in polyacrylonitrile solution.In addition, some researchs are it is also proposed that utilize
Graphene oxide is copolymerized with acrylonitrile, acrylic acid, itaconic acid, but in the copolymerization system of slant acidity, sheet graphene oxide
Be also easy to produce fold, sheet lamination is reunited together, and graphene oxide is caused to be unevenly distributed in polymerization process, preparation it is compound
Stability of fiber is poor, and yields is low, while performance parameter distribution is wide.
Spherical graphene oxide is dispersed in copolymerization system by the present invention by stirring at low speed, due to spherical graphene oxide
To be spherical, therefore can't reunite during being dispersed in copolymerization system such as the easy lamination of sheet graphene oxide together, it is spherical
After graphene oxide is uniformly dispersed in copolymerization system, with the progress of reaction, stir speed (S.S.), spherical graphite oxide are stepped up
Alkene can gradually unfold to hemispherical or sheet, carry out copolyreaction with monomer, become a part for composite fibre main chain.Using this
It is more excellent that composite fibre prepared by method compares traditional composite fibre performance, and properties have good stability, performance ginseng
Number is distributed narrower, yields higher.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of high intensity, rate of good quality rate, excellent antistatic capability polypropylene
The preparation method of nitrile composite fibre.
The present invention uses following technical scheme：A kind of preparation method of polyacrylonitrile-graphene oxide composite fibre, including
Following steps：
(1) acrylonitrile, acrylic acid, itaconic acid are scattered according to mass ratio 92-98,1.24-7.49,0.51-0.76 molten
In agent；
(2) spherical graphene oxide powder is added in solvent, stir speed (S.S.) is controlled in 50-100rpm, and stirring 2h is extremely
Spherical graphene oxide is uniformly dispersed, and obtains graphene oxide dispersion；
(3) graphene oxide dispersion that step 2 is configured is added in the mixed solution that step 1 is configured, in 50-
Be dispersed with stirring under 100rpm stir speed (S.S.)s, wherein the quality of spherical graphene oxide powder for acrylonitrile, acrylic acid,
The 0.1%~1% of itaconic acid gross mass.
(4) initiator is added in solvent, obtains initiator solution；Wherein the quality of initiator is acrylonitrile, propylene
The 0.2-0.8% of acid, itaconic acid gross mass.It is then added in the mixed solution of step 3 configuration, stir speed (S.S.) is controlled in 300-
400rpm obtains the mixed solution that solid content is 20~30%.
(5) mixed solution that step 4 obtains is transferred in reaction kettle, 60 DEG C are reacted 10-24 hours, while are passed through nitrogen
Make protective gas.
(6) after reaction, obtained dope discharging will be polymerize, is washed and filtered by deionized water, then 100
To remove the complete monomer of unreacted and remaining solvent, PAN powder is obtained after dry for boiling under the conditions of DEG C, filtering.
(7) PAN powder is dissolved in solvent, polyacrylonitrile-graphene oxide fiber is prepared using wet spinning technology.
(8) wet spun composite fibre is stretched by washing, multistage water-bath, and first order control is at 60-70 DEG C, stretching ratio
It it is 6.5 times, the second level is controlled at 70-80 DEG C, and stretching ratio is 6.2 times, and the third level is controlled at 80-90 DEG C, and stretching ratio is 4.7
Times, the fourth stage is controlled at 90-100 DEG C, and stretching ratio is 4.5 times；After completing water-bath stretching, high steam stretching, drying are carried out
After obtain polyacrylonitrile-graphene oxide composite fibre.
Further, according to claim 1 step (1), it is characterised in that the solvent can be DMSO, DMF,
DMAc, high concentration NaSCN solution etc..
The beneficial effects of the present invention are：Spherical graphene oxide is evenly dispersed in blending monomer, it will not be such as piece
Shape graphene oxide lamination is reunited together, and sheet graphene oxide is also easy to produce fold in acid condition, is more easy to reunite
Together, spherical graphene oxide overcomes these technological deficiencies, with the progress of reaction, by adjusting rotating speed, spherical oxidation stone
Black alkene expansion, is copolymerized with acrylonitrile, acrylic acid, itaconic acid, polyacryl-nitrile spinning fluid is made, and is then prepared by wet spinning poly-
Acrylonitrile-
Graphene oxide composite fibre.
Description of the drawings
Fig. 1 is the tensile strength curve figure of product obtained by embodiment 2；
Fig. 2 is the antistatic property figure of product obtained by embodiment 2.
Specific embodiment
Embodiment one
(1) acrylonitrile 920g, acrylic acid 74g, itaconic acid 5.1g are weighed respectively is scattered in 2500g in solvent；
(2) spherical graphene oxide powder is added in solvent, stir speed (S.S.) is controlled in 50-100rpm, and stirring 2h is extremely
Spherical graphene oxide is uniformly dispersed, and obtains the graphene oxide dispersion of a concentration of 20mg/ml；
(3) graphene oxide dispersion that step 2 is configured is added in the mixed solution that step 1 is configured, in 50-
Be dispersed with stirring under 100rpm stir speed (S.S.)s, wherein the quality of spherical graphene oxide powder for acrylonitrile, acrylic acid,
The 0.2% of itaconic acid gross mass.
(4) 2g initiators are weighed to be added in solvent, obtain initiator solution.It is then added to the mixing of step 3 configuration
In solution, stir speed (S.S.) controls the mixed solution in 300-400rpm, obtaining that solid content is 20%.
(5) mixed solution that step 4 obtains is transferred in reaction kettle, 60 DEG C are reacted 24 hours, while are passed through nitrogen work
Protective gas.
(6) after reaction, obtained dope discharging will be polymerize, is washed and filtered by deionized water, then 100
To remove the complete monomer of unreacted and remaining solvent, PAN powder is obtained after dry for boiling under the conditions of DEG C, filtering.
(7) PAN powder is dissolved in solvent, polyacrylonitrile-graphene oxide fiber is prepared using wet spinning technology.
(8) wet spun composite fibre is stretched by washing, multistage water-bath, and first order control is at 60-70 DEG C, stretching ratio
It it is 6.5 times, the second level is controlled at 70-80 DEG C, and stretching ratio is 6.2 times, and the third level is controlled at 80-90 DEG C, and stretching ratio is 4.7
Times, the fourth stage is controlled at 90-100 DEG C, and stretching ratio is 4.5 times；After completing water-bath stretching, high steam stretching (saturation is carried out
Water vapour pressure is 0.5MPa, and draft ratio is 2.5 times), it is dry after obtain polyacrylonitrile-graphene oxide composite fibre.
Comparative example 1
(1) acrylonitrile 920g, acrylic acid 74g, itaconic acid 5.1g are weighed respectively is scattered in 2500g in solvent；
(2) mixing that existing a concentration of 20mg/ml graphene oxide solutions (sheet dispersion) are added to step 1 configuration is molten
It in liquid, is dispersed with stirring under 50-100rpm stir speed (S.S.)s, wherein the quality of graphene oxide is acrylonitrile, acrylic acid, itaconic acid
The 0.2% of gross mass.
(3) 2g initiators are weighed to be added in solvent, obtain initiator solution.It is then added to the mixing of step 3 configuration
In solution, stir speed (S.S.) controls the mixed solution in 300-400rpm, obtaining that solid content is 20%.
(4) mixed solution that step 4 obtains is transferred in reaction kettle, 60 DEG C are reacted 24 hours, while are passed through nitrogen work
Protective gas.
(5) after reaction, obtained dope discharging will be polymerize, is washed and filtered by deionized water, then 100
To remove the complete monomer of unreacted and remaining solvent, PAN powder is obtained after dry for boiling under the conditions of DEG C, filtering.
(6) PAN powder is dissolved in solvent, polyacrylonitrile-graphene oxide fiber is prepared using wet spinning technology.
(7) wet spun composite fibre is stretched by washing, multistage water-bath, and first order control is at 60-70 DEG C, stretching ratio
It it is 6.5 times, the second level is controlled at 70-80 DEG C, and stretching ratio is 6.2 times, and the third level is controlled at 80-90 DEG C, and stretching ratio is 4.7
Times, the fourth stage is controlled at 90-100 DEG C, and stretching ratio is 4.5 times；After completing water-bath stretching, high steam stretching (saturation is carried out
Water vapour pressure is 0.5MPa, and draft ratio is 2.5 times), it is dry after obtain polyacrylonitrile-graphene oxide composite fibre.
Extension test, polyacrylonitrile-spherical oxidation stone are carried out to three kinds of fibers of preparation using isodromicing elongation's type tensilometer
Black alkene fracture strength is 5.24CN/dtex-5.46CN/dtex, and polyacrylonitrile-sheet graphene oxide intensity is 4.25CN/
Dtex-5.17CN/dtex, the fracture strength of virgin pp nitrile fiber is 4.41CN/dtex-4.68CN/dtex.In addition polypropylene
The sheet resistance of nitrile-spherical graphene oxide composite fibre be 10^10 Ω, polyacrylonitrile-sheet graphene oxide composite fibre
Sheet resistance for 10^11 Ω, the sheet resistance of virgin pp nitrile fiber is 10^13 Ω.
Embodiment two
(1) acrylonitrile 980g, acrylic acid 12.4g, itaconic acid 7.6g are weighed respectively is scattered in 2500g in solvent；
(2) spherical graphene oxide powder is added in solvent, stir speed (S.S.) is controlled in 50-100rpm, and stirring 2h is extremely
Spherical graphene oxide is uniformly dispersed, and obtains the graphene oxide dispersion of a concentration of 20mg/ml；
(3) graphene oxide dispersion that step 2 is configured is added in the mixed solution that step 1 is configured, in 50-
It is dispersed with stirring under 100rpm stir speed (S.S.)s, wherein the quality of spherical graphene oxide powder is acrylonitrile, acrylic acid, itaconic acid are total
0.1%, 0.5%, 0.75%, the 1% of quality, one of which does not add left blank sample.
(4) 2g initiators are weighed to be added in solvent, obtain initiator solution.It is then added to the mixing of step 3 configuration
In solution, stir speed (S.S.) controls the mixed solution in 300-400rpm, obtaining that solid content is 20%.
(5) mixed solution that step 4 obtains is transferred in reaction kettle, 60 DEG C are reacted 10 hours, while are passed through nitrogen work
Protective gas.
(6) after reaction, obtained dope discharging will be polymerize, is washed and filtered by deionized water, then 100
To remove the complete monomer of unreacted and remaining solvent, PAN powder is obtained after dry for boiling under the conditions of DEG C, filtering.
(7) PAN powder is dissolved in solvent, polyacrylonitrile-graphene oxide fiber is prepared using wet spinning technology.
(8) wet spun composite fibre is stretched by washing, multistage water-bath, and first order control is at 60-70 DEG C, stretching ratio
It it is 6.5 times, the second level is controlled at 70-80 DEG C, and stretching ratio is 6.2 times, and the third level is controlled at 80-90 DEG C, and stretching ratio is 4.7
Times, the fourth stage is controlled at 90-100 DEG C, and stretching ratio is 4.5 times；After completing water-bath stretching, high steam stretching (saturation is carried out
Water vapour pressure is 0.5MPa, and draft ratio is 2.5 times), it is dry after obtain polyacrylonitrile-graphene oxide composite fibre.
It is compound to the spherical graphene oxide content of difference of preparation using isodromicing elongation's type tensilometer and surface resistivity meter
Fiber carries out extension test, and tensile strength and antistatic property are as illustrated in fig. 1 and 2.
Claims (3)
1. the preparation method of a kind of polyacrylonitrile-graphene oxide composite fibre, which is characterized in that include the following steps：
(1) acrylonitrile, acrylic acid, itaconic acid are scattered according to mass ratio 92-98,1.24-7.49,0.51-0.76 in solvent；
(2) spherical graphene oxide powder is added in solvent, stir speed (S.S.) control is in 50-100rpm, and stirring 2h is to spherical
Graphene oxide is uniformly dispersed, and obtains graphene oxide dispersion；
(3) graphene oxide dispersion that step 2 is configured is added in the mixed solution that step 1 is configured, is stirred in 50-100rpm
It mixes and is dispersed with stirring under rate, wherein the quality of spherical graphene oxide powder is acrylonitrile, acrylic acid, itaconic acid gross mass
0.1%~1%.
(4) initiator is added in solvent, obtains initiator solution；Wherein the quality of initiator is acrylonitrile, acrylic acid, clothing
The 0.2-0.8% of health acid gross mass.It is then added in the mixed solution of step 3 configuration, stir speed (S.S.) is controlled in 300-
400rpm obtains the mixed solution that solid content is 20~30%.
(5) mixed solution that step 4 obtains is transferred in reaction kettle, 60 DEG C are reacted 10-24 hours, while are passed through nitrogen and go bail for
Protect gas.
(6) after reaction, obtained dope discharging will be polymerize, is washed and filtered by deionized water, then in 100 DEG C of items
To remove the complete monomer of unreacted and remaining solvent, PAN powder is obtained after dry for boiling under part, filtering.
(7) PAN powder is dissolved in solvent, polyacrylonitrile-graphene oxide fiber is prepared using wet spinning technology.
(8) wet spun composite fibre is stretched by washing, multistage water-bath, and first order control is in 60-70 DEG C, stretching ratio
6.5 times, the second level is controlled at 70-80 DEG C, and stretching ratio is 6.2 times, and the third level is controlled at 80-90 DEG C, and stretching ratio is 4.7
Times, the fourth stage is controlled at 90-100 DEG C, and stretching ratio is 4.5 times；After completing water-bath stretching, high steam stretching, drying are carried out
After obtain polyacrylonitrile-graphene oxide composite fibre.
2. according to the method described in claim 1, it is characterized in that, the solvent can be DMSO, DMF, DMAc, high concentration
NaSCN solution etc..
3. according to the method described in claim 1, it is characterized in that, the quality of spherical graphene oxide powder is acrylonitrile, third
The 0.5% of olefin(e) acid, itaconic acid gross mass.
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| CN201711489154.1A CN108166092A (en) | 2017-12-30 | 2017-12-30 | A kind of preparation method of polyacrylonitrile-graphene oxide composite fibre |
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| CN201711489154.1A CN108166092A (en) | 2017-12-30 | 2017-12-30 | A kind of preparation method of polyacrylonitrile-graphene oxide composite fibre |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112127000A (en) * | 2020-09-04 | 2020-12-25 | 河北艾科瑞纤维有限公司 | Far infrared acrylic fiber and preparation method thereof |
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