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A kind of method for preparing high adhesion polyimide coating glue

A technology of adhesion polyimide and coating glue, which is applied in the direction of adhesives, etc., can solve the problems of high imidization temperature, description, and only give adhesion, etc., and achieve low end group content, cost reduction, and synthesis The effect of simple process

Active Publication Date: 2017-05-17
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 diamines and acid anhydride monomers, but its The imidization temperature is higher, and only the adhesion between the polyimide coating glue and the copper plate is given, and other substrates are not described

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039](1) Under nitrogen protection at 15-20°C, dissolve 4.005g (0.02mol) 4,4'-diaminodiphenyl ether in 43mL N-methylpyrrolidone, and lower the reaction system to 0-5°C after complete dissolution , add 6.825g (0.022mol) 4,4'-oxydiphthalic dianhydride, add 0.188mL (0.0008mol) 3-aminopropyltriethoxysilane after 1 hour of reaction, form low Polymer polyamic acid solution;

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

[0041] (3) Under the protection of nitrogen at 0-5°C, 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) of 3-aminopropyltriethoxy base silane, after 1.5 hours of reaction, pol...

Embodiment 2

[0045] (1) Under nitrogen protection at 20-25°C, dissolve 2.002g (0.01mol) 4,4'-diaminodiphenyl ether in 18mL N-methylpyrrolidone, and lower the reaction system to 0-5°C after complete dissolution , add 2.482g (0.008mol) 4,4'-oxydiphthalic dianhydride and 0.436g (0.002mol) pyromellitic dianhydride, add 0.089mL (0.00038mol) 3-aminopropane after reacting for 0.5 hours Base triethoxysilane, after reacting for 0.5 hours, polyamic acid oligomer solution was formed;

[0046] (2) Under the protection of nitrogen at 20-25°C, dissolve 9.011g (0.045mol) of 4,4'-diaminodiphenyl ether in 88mL of N-methylpyrrolidone, and lower the reaction system to 0-5°C after complete dissolution , add 11.168g (0.036mol) 4,4'-oxydiphthalic dianhydride and 1.963g (0.009mol) pyromellitic dianhydride, react for 9 hours to form a high polymer polyamic acid solution;

[0047] (3) Under the protection of nitrogen at 0-5°C, add the solution obtained in step (1) to the solution obtained in step (2) and mix to c...

Embodiment 3

[0051] (1) Under the protection of nitrogen at 35-40°C, mix 0.801g (0.004mol) 4,4'-diaminodiphenyl ether and 0.276mL (0.001mol) 1,3-di(aminopropyl)tetramethyldiphenyl ether Dissolve siloxane in 12mL N,N-dimethylformamide, after complete dissolution, lower the reaction system to 0-5°C, add 1.7725g (0.0055mol) 3,3',4,4'-benzophenone Tetraacid dianhydride, add 0.04mL (0.00017mol) 3-aminopropyltriethoxysilane after reacting for 0.3 hours, form oligomer polyamic acid solution after reacting for 1 hour;

[0052] (2) Under nitrogen protection at 35-40°C, mix 4.005g (0.02mol) 4,4'-diaminodiphenyl ether and 1.381mL (0.005mol) 1,3-di(aminopropyl)tetramethyldiphenyl ether Dissolve siloxane in 57mL N,N-dimethylformamide, after complete dissolution, lower the reaction system to 0-5°C, add 8.862g (0.028mol) 3,3',4,4'-benzophenone Tetraacid dianhydride, form high polymer polyamic acid solution after reacting for 8 hours;

[0053] (3) Under the protection of nitrogen at 0-5°C, add the solut...

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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 polyimide coating glue with high adhesion by blending two kinds of polyamic acid solutions with different relative molecular masses, and belongs to the field of polymer material preparation. Background technique [0002] Polyimide refers to a class of polymers containing imide rings (-CO-NH-CO-) in the main chain. Because of its outstanding comprehensive performance, it is widely used in aerospace, electronic appliances, automobiles and chemical industries. application. Polyimide coating adhesive is the precursor of thermoplastic polyimide. After imidization, a polyimide film material with excellent performance can be obtained, which has excellent bonding performance to glass, metal surfaces, semiconductor devices, etc. , can be used as the passivation layer of the chip, the interlayer insulating layer film of the multilayer metal interconnection circuit, glass coating, etc. [0003] The methods current...

Claims

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Application Information

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