Environment-friendly stable polyamide acid solution and preparation method thereof

A polyamic acid and stability technology, applied in the field of polyamic acid solution and its preparation, can solve the problems of poor batch stability, difficult preparation of polyamic acid aqueous solution, wide molecular weight distribution, etc., and achieve increased quality stability and improved production. Membrane efficiency, the effect of increasing the solid content

Active Publication Date: 2016-04-06
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention solves the problems of large-scale preparation of existing polyamic acid aqueous solution, wide molecular weight distribution, and poor batch stability, and provides an environment-friendly stable polyamic acid solution and a preparation method thereof

Method used

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  • Environment-friendly stable polyamide acid solution and preparation method thereof
  • Environment-friendly stable polyamide acid solution and preparation method thereof
  • Environment-friendly stable polyamide acid solution and preparation method thereof

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Experimental program
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specific Embodiment approach 1

[0048] Embodiment 1: An environment-friendly stable polyamic acid solution of this embodiment, an environment-friendly stable polyamic acid solution is made of tertiary amine, aromatic primary amine, aromatic dianhydride, aromatic diamine and water; The molar ratio of the aromatic diamine to the tertiary amine is 1:(0.05~2); the molar ratio of the aromatic diamine to the primary aromatic amine is 1:(0.01~1); the aromatic diamine and The molar ratio of the aromatic dianhydride is 1:(0.97~1.03); the mass ratio of the total mass of the aromatic dianhydride and aromatic diamine to water is 1:(2~10); the aromatic diamine is 4 ,4'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether, 4,4'-diaminodiphenylmethane, bis(3-aminophenoxy)benzophenone, p-phenylenediamine , m-phenylenediamine or 2-(3-aminophenyl)-5-aminobenzoxazole;

[0049] When the aromatic dianhydride is 3,3,4',4'-diphenyl ether tetracarboxylic dianhydride, 3,3,4',4'-disulfone tetracarboxylic dianhydride or 3,3, 4',4'-benz...

specific Embodiment approach 2

[0064] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the tertiary amine is triethylamine, trialkyl tertiary amine, octadecyl dimethyl tertiary amine and dodecyl dimethyl One or a mixture of several tertiary amines. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0065] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the aromatic primary amine is 4-fluoroaniline, 3-aminopyridine, 3-acetylaniline and 2-nitroaniline one or a mixture of several of them. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a polyamide acid solution and a preparation method thereof, in particular to an environment-friendly stable polyamide acid solution and a preparation method thereof. The environment-friendly stable polyamide acid solution and the preparation method thereof aim at solving the problems of difficultly of large-scale preparation of a polyamide acid aqueous solution, wide molecular weight distribution and poor batch stability in the prior art. The environment-friendly stable polyamide acid solution is prepared from tertiary amine, aromatic primary amine, aromatic dianhydride, aromatic diamine and water, wherein repetitive units of polyamide acid in the polyamide acid aqueous solution are shown in the specification. The preparation method includes the steps that tertiary amine, aromatic primary amine, aromatic dianhydride, aromatic diamine and water are taken, and weighed tertiary amine is divided into tertiary amine A and tertiary amine B; water and aromatic primary amine are added into a three-necked bottle under certain conditions for a reaction; weighed tertiary amine A and weighed aromatic diamine are added into the three-necked bottle for a reaction, reaction liquid is heated, then weighed aromatic dianhydride is added into the three-necked bottle and stirred for a reaction, then the reaction liquid is cooled, weighed tertiary amine B is added and stirred for a reaction, and the reaction liquid is cooled and subjected to standing.

Description

technical field [0001] The invention relates to a polyamic acid solution and a preparation method thereof. Background technique [0002] Polyimide is an aromatic heterocyclic polymer containing imide rings in repeating structural units. It is the highest heat-resistant polymer material used in the industrial field so far. With its excellent comprehensive performance, it can be used in films, resins, Fibers and separation membranes are widely used in aerospace, electronics and electrical fields. Traditional polyimides are usually made of aromatic tetracarboxylic anhydride and aromatic diamine in aprotic polar solvents, such as N,N-dimethylacetamide, N,N-dimethylformamide, N -Methylpyrrolidone, etc., by first forming polyamic acid, and then imidizing and dehydrating to form polyimide. Aprotic polar solvents can form polyamic acid with high molecular weight and narrow molecular weight distribution at room temperature because the equilibrium constant of this acylation reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18
CPCC08G73/1028C08G73/1067C08G73/1071C08J5/18C08J2375/10
Inventor 刘长威曲春艳王德志肖万宝张杨宿凯李洪峰杨海东冯浩王海民
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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