Preparation method of graphene/polyacrylonitrile spinning solution

A technology of polyacrylonitrile spinning and graphene, applied in the direction of conductive/antistatic filament manufacturing, rayon manufacturing, one-component synthetic polymer rayon, etc.

Active Publication Date: 2020-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There are many ways to prepare graphene (including graphene oxide and reduced graphene oxide) / polyacrylonitrile, mainly by copolymerizing graphene oxide or reduced graphene oxide with acrylonitrile monomer, or blending with polyacrylonitrile, but these reports focus on However, the dispersion and stability of graphene in polyacrylonitrile spinning solution are seldom reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The polymerization adopts a two-step aqueous phase suspension polymerization process, with acrylonitrile (AN) as the first monomer, methyl acrylate (MA) as the second monomer, and sodium methacrylate (A1) as the third monomer. Sodium chlorate (A2) and sodium metabisulfite (A3) are initiators, β-hydroxyethanethiol (A4) is a molecular weight regulator, and pure water is a reaction medium. After polymerization, termination, single removal, and water washing, the polymer sludge is prepared. The slurry is stored in storage tanks.

[0030] The ratio of the feed quality of AN and MA is 91.4:8.6; The ratio of each material feed flow is: the mass concentration of the first monomer and the second monomer is 34%, the A1 / M mass ratio is 0.23%, A2 / The mass ratio of M is 0.50%, the molar ratio of A3 / A2 is 1.5, the mass ratio of A4 / M is 0.22%, and the quality of pure water accounts for 65% of the total mass of the solution; the volume of the polymerization tank is 8.3m 3 , the react...

Embodiment 2

[0038] The polymerization adopts a two-step aqueous phase suspension polymerization process, with acrylonitrile (AN) as the first monomer, vinyl acetate (VAC) as the second monomer, and sodium methacrylate (A1) as the third monomer. Sodium chlorate (A2) and sodium metabisulfite (A3) are initiators, β-hydroxyethanethiol (A4) is a molecular weight regulator, and pure water is a reaction medium. After polymerization, termination, single removal, and water washing, the polymer sludge is prepared. The slurry is stored in storage tanks.

[0039] The feed mass ratio of AN and VAC is 89.5:10.5. The ratio of each material feed flow rate is: the mass concentration of monomer (AN and MA) is 34%, the A1 / M mass ratio is 0.23%, the A2 / M mass ratio is 0.50%, the A3 / A2 molar ratio is 1.5, and the A4 The mass ratio of / M is 0.22%, and the quality of pure water accounts for 65% of the total mass of the solution; the volume of the polymerization tank is 8.3m 3 , the reaction time was 53min, th...

Embodiment 3

[0043] The polymerization adopts a two-step aqueous phase suspension polymerization process, with acrylonitrile (AN) as the first monomer, methyl acrylate (MA) as the second monomer, and sodium methacrylate (A1) as the third monomer. Sodium chlorate (A2) and sodium metabisulfite (A3) are initiators, β-hydroxyethanethiol (A4) is a molecular weight regulator, and pure water is a reaction medium. After polymerization, termination, single removal, and water washing, the polymer sludge is prepared. The slurry is stored in storage tanks.

[0044] The feed mass ratio of AN and MA was 90:10. The ratio of each material feed flow is: the mass concentration of monomer (AN and MA) is 30%, and A1 / M mass ratio is 0.2%, and A2 / M mass ratio is 0.40%, and A3 / A2 mol ratio is=1, The mass ratio of A4 / M is 0.2%, and the pure water mass accounts for 69% of the total mass of the solution; the volume of the polymerization tank is 8.3m 3 , the reaction time is 52min, the reaction temperature is 55°C...

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PUM

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Abstract

The invention discloses a preparation method of a graphene / polyacrylonitrile spinning solution suitable for industrial production. According to the method, a conventional two-step process, including aqueous suspension polymerization and polyacrylonitrile resin dissolution in an inorganic solvent, is adopted, special equipment is not added, polyacrylonitrile filter cake dilution water in an original spinning process is switched into a stably dispersed graphene aqueous solution, graphene is uniformly dispersed in polyacrylonitrile slurry, then the slurry is mixed with NaSCN, and the graphene / polyacrylonitrile spinning solution is obtained through stirring and high shearing. The spinning solution prepared by the adoption of the method has good spinnability, and the graphene can be dispersed uniformly and stably in the spinning solution for 48 hours or above. Compared with pure polyacrylonitrile fibers, the specific resistance of graphene / polyacrylonitrile fibers prepared by the adoption of the spinning solution is increased by 3-5 orders of magnitudes, and strength is improved by 20% or above.

Description

technical field [0001] The invention relates to the technical field of textile chemicals, in particular to a method for preparing a graphene / polyacrylonitrile spinning dope that is stably dispersed at the industrial production site. Background technique [0002] Acrylic fiber has good light resistance, weather resistance, moth resistance, radiation resistance, anti-microbial degradation and good dyeability, etc. Its fabric is an ideal wool-like and cashmere-like fabric. However, conventional acrylic fiber is an insulating material, and it is easy to generate static electricity during post-processing, which makes it difficult to bundle. The finished product has strong static electricity, is easy to stain and absorb dust, and has low wearing comfort. These greatly limit the application of acrylic fiber. Therefore, antistatic acrylic fiber came into being. [0003] The volume specific resistance of antistatic acrylic is generally lower than 10 9 Ohm.cm, can be used as fluff-f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/54D01F1/09D01F1/10C08F220/44C08F218/08C08F228/02C08F220/14C08F2/38C08F2/18
CPCD01F6/54D01F1/09D01F1/103C08F220/44C08F2/38C08F2/18C08F218/08C08F228/02C08F220/14
Inventor 伍三华黄翔宇韩风辛美音邓文彬宋铮顾丹凤毕建东薛丽姚坚顾枫吴赟
Owner CHINA PETROLEUM & CHEM CORP
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