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Preparation method of flame-retardant polyimide

A technology of flame-retardant polyimide and polyamic acid, which is applied in the field of preparation of flame-retardant polyimide, can solve the problems of insufficient flame retardancy and limited application of polyimide films, and achieve excellent transparency and mechanical properties The effect of performance, simple reaction steps, and excellent compatibility

Pending Publication Date: 2022-04-05
WUXI CHUANGCAI OPTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical problem to be solved by the present invention is: the flame retardancy of polyimide film in its application field is insufficient, which limits its application

Method used

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  • Preparation method of flame-retardant polyimide
  • Preparation method of flame-retardant polyimide
  • Preparation method of flame-retardant polyimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A preparation method of flame retardant polyimide, comprising the following steps:

[0035] (1) First prepare polyamic acid solution

[0036] At room temperature, disperse 4,4-diaminodiphenyl ether and modified flame retardant in an organic solvent, then slowly add pyromellitic dianhydride, the dianhydride monomer, diamine monomer and modified flame retardant The molar ratio of the fuel is 0.9:1:0.05, and the stirring reaction is carried out for 12 hours to obtain the amic acid solution;

[0037] Its infrared data is as follows: 2900-3400cm -1 :-NH 2 , -OH exists; 914cm -1 : Primary amine-N-H exists; 3064cm -1 : benzene ring-C-H exists; 2920cm -1 : C-H exists in P-CH-; 1593cm -1 、1544cm -1 : benzene ring exists; 1302cm -1 : P=O exists; 1190cm -1 :P-O-Exist.

[0038] (2) Imination

[0039] Stir and disperse the obtained amic acid solution evenly, and then cast it on a glass substrate to form a film. Under the protection of an inert gas, raise the temperature t...

Embodiment 2

[0053] A preparation method of flame retardant polyimide, comprising the following steps:

[0054] (1) First prepare polyamic acid solution

[0055] At room temperature, the molar ratio of 4,4-diaminobenzophenone and 4,4-diaminodiphenyl ether is 7 / 3, the modified flame retardant is dispersed in an organic solvent, and then slowly added 3,3', 4,4'-biphenyltetracarboxylic dianhydride and dimethyl ketone tetracarboxylic dianhydride are composed of a molar ratio of 8 / 2, and the mol ratio of the dianhydride monomer, diamine monomer and modified flame retardant is 1.05: 1:0.09, stirred and reacted for 10h to obtain the amic acid solution;

[0056] Its infrared data is as follows: 2900-3400cm -1 :-NH 2 , -OH exists; 914cm -1 : Primary amine-N-H exists; 3064cm -1 : benzene ring-C-H exists; 2920cm -1 : C-H exists in P-CH-; 1593cm -1 、1544cm -1 : benzene ring exists; 1302cm -1 : P=O exists; 1190cm -1 :P-O-Exist.

[0057] (2) Imination

[0058] Stir and disperse the obtained ...

Embodiment 3

[0072] A preparation method of flame retardant polyimide, comprising the following steps:

[0073] (1) First prepare polyamic acid solution

[0074] At room temperature, disperse 4,4'-diaminobenzene and 4,4'-diaminobiphenyl in a molar ratio of 4 / 6 and a modified flame retardant in an organic solvent, then slowly add monoether tetraacid dianhydride Composed of bis[4-(3,4-dicarboxyphenoxy)phenyl]propane dianhydride in a molar ratio of 3 / 7, the molar ratio of the dianhydride monomer, diamine monomer and modified flame retardant 0.9:1:0.1, stirred and reacted for 4h to obtain the amic acid solution;

[0075] Its infrared data is as follows: 2900-3400cm -1 :-NH 2 , -OH exists; 914cm -1 : Primary amine-N-H exists; 3064cm -1 : benzene ring-C-H exists; 2920cm -1 : C-H exists in P-CH-; 1593cm -1 、1544cm -1 : benzene ring exists; 1302cm -1 : P=O exists; 1190cm -1 :P-O-Exist.

[0076] (2) Imination

[0077] Stir and disperse the obtained amic acid solution evenly, and then ca...

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Abstract

The invention relates to the technical field of functional materials, in particular to a preparation method of flame-retardant polyimide. The flame retardance of the polyimide film needs to be further improved. Based on the problems, the invention provides the preparation method of the flame-retardant polyimide, and a self-made flame-retardant modifier is added in the preparation process of a polyimide film, so that the flame retardance of the polyimide can be effectively improved, and the mechanical property, the thermal property and the optical property of the polyimide can be further improved.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a preparation method of flame-retardant polyimide. Background technique [0002] With the rapid development of industries such as aerospace, national defense, and electronics, polyimide (PI) materials have attracted widespread attention due to their excellent mechanical properties, high temperature resistance, chemical corrosion resistance, and good flame retardancy. PI is a class of organic polymer materials containing imide ring repeating units in the main chain, with rich structures. PI materials with excellent performance can be obtained through molecular structure design and regulation. PI can be made into fibers, foam plastics, composite materials, separation membranes, etc., and is used in photoresist, electro-optical materials, microelectronic devices, medical equipment and other products. Studies have shown that the introduction of heterocyclic units into t...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 周浪郁胜振
Owner WUXI CHUANGCAI OPTICAL MATERIALS