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A kind of polyamic acid precipitation fiber and polyimide precipitation fiber and preparation method thereof

A technology of precipitating fibers and polyamic acid, which is applied in the chemical characteristics of fibers, textiles and papermaking, one-component synthetic polymer rayon, etc., which can solve the mechanical properties and insulation properties that limit the large-scale production of polyimide paper products. and other problems, to achieve the effect of improving mechanical strength and insulation performance, low dielectric loss, and high wave transmission performance

Active Publication Date: 2019-11-08
JIANGSU XIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although my country has made great progress in the research and production of polyimide fiber in recent years, the research and development of polyimide fiber pulp is still in its infancy, which severely limits the large-scale production of polyimide paper products. Production and improvement of mechanical properties and insulation properties

Method used

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  • A kind of polyamic acid precipitation fiber and polyimide precipitation fiber and preparation method thereof
  • A kind of polyamic acid precipitation fiber and polyimide precipitation fiber and preparation method thereof
  • A kind of polyamic acid precipitation fiber and polyimide precipitation fiber and preparation method thereof

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preparation example Construction

[0014] On the one hand, the invention provides a kind of preparation method of polyamic acid fibrid, the method comprises:

[0015] (1) react amine monomer and acid anhydride monomer in polar solvent to generate polyamic acid product;

[0016] (2) Dilute the product obtained in step (1) until the polyamic acid concentration is 1-14% by weight and the viscosity is less than 500cp, and then inject the diluted solution into the precipitant under stirring conditions;

[0017] Wherein, the precipitating agent is at least one of water, ethanol, methanol, acetone and toluene.

[0018] According to the method of the present invention, in step (1), the amine monomers are various amines in the art, such as diamines and / or triamines, preferably diamines, more preferably At least one of hexafluorodiamine, biphenylenediamine, 3,4-diaminodiphenyl ether, 4,4'-diamino-4"-hydroxytriphenylmethane, which can significantly improve the obtained polyamide The specific surface area of ​​acid preci...

Embodiment 1

[0041] This example is used to illustrate the polyamic acid fibrids and polyimide fibrids of the present invention and their preparation methods.

[0042] (1) Dissolve 3,4-diaminodiphenyl ether in a mixed solvent of N,N-dimethylacetamide and xylene with a volume ratio of 6:1, and then add acid anhydride monomers (acid anhydride monomers The composition is: 2,3,3',4'-biphenyl tetra-acid dianhydride, 3,3',4,4'-benzophenone tetra-acid dianhydride and 3,3',4,4'-biphenyl tetra-acid dianhydride Phenyl ether tetra-acid dianhydride, the weight ratio is 1:1:5), the molar ratio of 3,4-diaminodiphenyl ether and acid anhydride monomer is controlled to be 1:0.95, and the solid content in every liter of mixed solvent is 200g , stirring and reacting at 10°C for 2h to generate polyamic acid product;

[0043] (2) Add the above-mentioned mixed solvent to the polyamic acid product obtained in step (1) until the content of polyamic acid is 5% by weight, and the solution viscosity is 200cp, and t...

Embodiment 2

[0046] This example is used to illustrate the polyamic acid fibrids and polyimide fibrids of the present invention and their preparation methods.

[0047] (1) Hexafluorodiamine is dissolved in N, N-dimethylacetamide and xylene in a mixed solvent with a volume ratio of 7:1, and then an acid anhydride monomer is added (the composition of the acid anhydride monomer is: 2 , 3,3',4'-biphenyl tetraacid dianhydride, 3,3',4,4'-benzophenone tetraacid dianhydride and 3,3',4,4'-diphenyl ether tetraacid di Anhydride, the weight ratio is 1:2:2), the molar ratio of hexafluorodiamine and acid anhydride monomer is controlled to be 1:1, and the solid content in each liter of mixed solvent is 240g, and the reaction is stirred at 25°C for 1h to form poly Amic acid products;

[0048] (2) Add the above-mentioned mixed solvent to the polyamic acid product obtained in step (1) until the content of polyamic acid is 7% by weight, and the solution viscosity is 250cp, and then inject it at 50°C and 800...

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Abstract

The invention relates to the field of fiber pulp materials high in specific surface area, and discloses a preparation method of polyamide acid fibrid. The method includes the steps of firstly, making amine monomers and anhydride monomers react in polar solvent to generate a polyamide acid product; secondly, diluting the product obtained in the first step till polyamide acid has the concentration of 1-14% by weight and the viscosity smaller than 500 cp, injecting a diluted solution into a precipitator under the stirring conditions, wherein the precipitator is at least one of water, ethyl alcohol, methyl alcohol, acetone and methylbenzene. The invention further discloses the polyamide acid fibrid prepared through the method, polyimide fibrid and the preparation method of the polyamide acid fibrid. The prepared polyamide acid fibrid and the polyimide fibrid have large specific surface areas, and polyamide acid paper prepared with the prepared polyamide acid fibrid and the polyimide fibrid as the raw materials is excellent in high temperature resistance, mechanical property and insulating performance.

Description

technical field [0001] The present invention relates to the field of high specific surface area fiber pulp materials, in particular to a preparation method of polyamic acid fibrids, polyamic acid fibrids prepared by the method, and preparation of polyimide fibrids The method and the polyimide fibrids prepared by the method. Background technique [0002] With its unique aromatic heterocyclic rigid structure, polyimide material has excellent high temperature resistance, mechanical properties, insulation properties, corrosion resistance, radiation resistance and other performance characteristics. Films, fibers, and composite materials produced using it as raw materials have been widely used in various fields such as electronics, machinery manufacturing, and aerospace. The polyimide paper prepared with polyimide fiber as raw material well retains the performance characteristics of polyimide material, and has a very broad application in high-performance motors, dry-type transfor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78D01F6/74
CPCD01F6/74D01F6/78
Inventor 俞建刚
Owner JIANGSU XIANNUO NEW MATERIAL TECH
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