Method for preparing polyimide coating adhesive with high adhesive force

A technology of adhesion polyimide and coating glue, applied in the direction of adhesives, etc., can solve the problems of high imidization temperature, only give the adhesion, instructions, etc., achieve low end group content, cost reduction, excellent Effects of hydrolysis resistance and thermal stability

Active Publication Date: 2015-09-30
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Patent [CN 104277458 A] discloses a polyimide with high adhesion and low linear expansion coefficient synthesized by diamine containing rigid structure and cyano group in proportion to other diamine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0038] Example 1

[0039] (1) Dissolve 4.005g (0.02mol) 4,4'-diaminodiphenyl ether in 43mL N-methylpyrrolidone under the protection of nitrogen at 15~20℃, and reduce the reaction system to 0~5℃ after dissolving completely , Add 6.825g (0.022mol) 4,4'-oxydiphthalic dianhydride, add 0.188mL (0.0008mol) 3-aminopropyltriethoxysilane after 1 hour of reaction, and form low Polymer polyamic acid solution;

[0040] (2) Under the protection of nitrogen at 15-20℃, dissolve 16.019g (0.08mol) 4,4'-diaminodiphenyl ether in 173mL N-methylpyrrolidone, and after dissolving completely, reduce the reaction system to 0-5℃ , Add 27.299g (0.088mol) 4,4'-oxydiphthalic dianhydride, react for 10 hours to form a polymer polyamic acid solution;

[0041] (3) Under the protection of nitrogen at 0~5℃, add the solution obtained in step (1) to the solution obtained in step (2) and mix to continue the reaction. After 2.5 hours, add 0.936mL (0.004mol) 3-aminopropyltriethoxy Base silane, the polyimide coating glue...

Example Embodiment

[0044] Example 2

[0045] (1) Under the protection of nitrogen at 20~25℃, dissolve 2.002g (0.01mol) 4,4'-diaminodiphenyl ether in 18mL N-methylpyrrolidone. After dissolving completely, reduce the reaction system to 0~5℃ , Add 2.482g (0.008mol) 4,4'-oxydiphthalic dianhydride and 0.436g (0.002mol) pyromellitic dianhydride, add 0.089mL (0.00038mol) 3-aminopropyl after reacting for 0.5 hours Triethoxysilane, reacted for 0.5 hours to form a polyamic acid oligomer solution;

[0046] (2) Under the protection of nitrogen at 20~25℃, dissolve 9.011g (0.045mol) 4,4'-diaminodiphenyl ether in 88mL N-methylpyrrolidone. After dissolving completely, reduce the reaction system to 0~5℃ , Add 11.168g (0.036mol) 4,4'-oxydiphthalic dianhydride and 1.963g (0.009mol) pyromellitic dianhydride, react for 9 hours to form a polymer polyamic acid solution;

[0047] (3) Under the protection of nitrogen at 0~5℃, add the solution obtained in step (1) to the solution obtained in step (2) and mix to continue the r...

Example Embodiment

[0050] Example 3

[0051] (1) Under the protection of nitrogen at 35~40℃, combine 0.801g (0.004mol) 4,4'-diaminodiphenyl ether and 0.276mL (0.001mol) 1,3-bis(aminopropyl)tetramethyldiphenyl ether Siloxane was dissolved in 12mL N,N-dimethylformamide, and the reaction system was reduced to 0~5℃ after complete dissolution, and 1.7725g (0.0055mol) 3,3',4,4'-benzophenone was added Tetraacid dianhydride, add 0.04mL (0.00017mol) 3-aminopropyltriethoxysilane after 0.3 hours of reaction, and form oligomer polyamic acid solution after 1 hour of reaction;

[0052] (2) Under the protection of nitrogen at 35~40℃, combine 4.005g (0.02mol) 4,4'-diaminodiphenyl ether and 1.381mL (0.005mol) 1,3-bis(aminopropyl)tetramethyldiphenyl ether Siloxane was dissolved in 57mL N,N-dimethylformamide, and after the complete dissolution, the reaction system was reduced to 0~5℃, and 8.862g (0.028mol) 3,3',4,4'-benzophenone was added Tetraacid dianhydride, which forms a polymer polyamic acid solution after 8 hou...

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Abstract

The invention discloses a method for preparing a polyimide coating adhesive with high adhesive force by jointly blending two polyamide acid solutions of different relative molecular mass. The method comprises the steps that firstly, after aromatic organic diamine and aromatic organic dianhydride are reacted, termination is performed by adopting 3-aminopropyltriethoxysilane to form polyamide acid of low molecular mass; secondly, the aromatic organic diamine and aromatic organic dianhydride monomers are additionally used to react and synthesize polyamide acid of high molecular mass; thirdly, after the polyamide acid of low molecular mass and the polyamide acid of high molecular mass are mixed and reacted, termination is performed by adding the 3-aminopropyltriethoxysilane, and then the polyimide coating adhesive with low polymers and high polymers in an appropriate proportion is obtained. Imidization catalysts are added in the coating adhesive, and then high-performance polyimide thin-film materials can be obtained through heat treatment at 150-200 DEG C. According to the method for preparing the polyimide coating adhesive with the high adhesive force, the prepared polyimide coating adhesive has the high adhesive force, the adhesive force level of the polyimide coating adhesive with the surfaces of aluminum, copper, glass, ceramic and the like can reach 0 level, the polyimide coating adhesive does not fall off completely when the polyimide coating adhesive is boiled in 80 DEG C water for 3000 hours, and the polyimide coating adhesive can be used in fields such as microelectronic packaging.

Description

Technical field [0001] The invention relates to a method for preparing a high-adhesion polyimide coating glue by blending two polyamic acid solutions with different relative molecular masses, and belongs to the field of polymer material preparation. Background technique [0002] Polyimide refers to a type of polymer containing imide ring (-CO-NH-CO-) in the main chain. Because of its outstanding comprehensive performance, it is widely used in aerospace, electronic appliances, automotive and chemical industries. application. Polyimide coating glue is the precursor of thermoplastic polyimide. After imidization, a polyimide film material with excellent properties can be obtained, and it has excellent adhesion to glass, metal surfaces, semiconductor devices, etc. , Can be used as the passivation layer of the chip, the interlayer insulating film of the multilayer metal interconnection circuit, glass paint, etc. [0003] The methods currently reported to improve the adhesion of polyimi...

Claims

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Application Information

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IPC IPC(8): C08G73/10C09J179/08
Inventor 徐勇张晶晶
Owner NANJING UNIV OF SCI & TECH
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