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Polyamic acid composition and preparation method and application thereof

A technology for polyamic acid and composition, which is applied to polyamic acid composition, preparation and application fields, can solve the problems of unstable viscosity control, difficult polymer molecular chain growth, etc., and achieves the effect of good technical effect

Active Publication Date: 2017-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is that the viscosity control of the polyamic acid solution is unstable in the previous preparation process and the further growth of the polymer molecular chain is difficult in the subsequent imidization process. A polyamic acid solution with controllable viscosity is provided. A method for preparing an amic acid composition, the preparation method is as a comonomer component by preparing a composition generated from tetracarboxylic acid and diamine, and controlling the viscosity of the polymer by adjusting the content of the tetracarboxylic acid component Purpose

Method used

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  • Polyamic acid composition and preparation method and application thereof
  • Polyamic acid composition and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Add 10.814g (0.1mol) of p-phenylenediamine and 243ml N,N-dimethylacetamide in the four-necked flask (water content 380ppmw), stir at room temperature and 2 Under protection, after completely dissolving, cool in an ice-water bath to 0°C, add 0.3303g (0.001mol) 3,3′,4,4′-biphenyltetraic acid, stir within the temperature range of 0°C, and the stirring speed is 200 rpm , after completely dissolving, maintain the reaction for 1 hour to obtain a reddish-brown solution, then add 28.8336g (0.098mol) 3,3',4,4'-biphenyltetraic acid dianhydride powder to the solution obtained above, Stir for 3 hours to obtain a light brown low-viscosity solution, then add 0.2942g (0.001mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the above solution, and continue stirring for 1 hour to obtain a light brown As a yellow transparent viscous solution, the desired polyamic acid composition solution with a solid content of 14.8% was obtained. After testing, the kinematic viscosity is 138Pa·s a...

Embodiment 2

[0057] Add 10.814g (0.1mol) of p-phenylenediamine and 170ml N,N-dimethylacetamide in the four-necked flask (water content 380ppmw), stir at room temperature and 2 Under protection, after completely dissolving, cool in an ice-water bath to 0°C, add 0.6605g (0.002mol) of 3,3′,4,4′-biphenyltetraacid, stir within a temperature range of 40°C, and the stirring speed is 250 rpm , after completely dissolving, maintain the reaction for 1 hour to obtain a reddish-brown solution, then add 26.4798g (0.090mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the solution obtained above, Stir for 3 hours to obtain a light brown low-viscosity solution, then add 2.3538g (0.008mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the above solution, and continue stirring for 2 hours to obtain a red Yellow viscous solution, the desired polyamic acid composition solution with a solid content of 20.0% was obtained. After testing, the kinematic viscosity is 62Pa·S at 25°C, and the intrinsic vis...

Embodiment 3

[0059] 10.814g (0.1mol) of p-phenylenediamine and 346ml N-methylpyrrolidone (water content 800ppmw) were added in the four-necked flask, stirred at room temperature and heated under N 2 Under protection, after completely dissolving, cool in an ice-water bath to 0°C, add 1.3210g (0.004mol) 3,3′,4,4′-biphenyltetraic acid, stir within a temperature range of 30°C, and the stirring speed is 250 rpm After completely dissolving, the reaction was maintained for 1 hour to obtain a reddish-brown solution, and then 26.4798g (0.090mol) of 3,3',4,4'-biphenyltetraacid dianhydride powder was added to the solution obtained above, Stir for 3 hours to obtain a light brown low-viscosity solution, then add 1.7653g (0.006mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the above solution, and continue stirring for 2 hours to obtain a black viscous solution to obtain the desired polyamic acid composition solution with a solid content of 10.0%. After testing, the kinematic viscosity is 36Pa·S...

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Abstract

The invention relates to a polyamic acid composition and a preparation method and application thereof, and mainly solves the problems that a polyamic acid solution is not stable in viscosity control in the preparation process and polymer molecule chains are difficult to further grow in a subsequent imidization process in the prior art. The preparation method of the polyamic acid composition comprises the following steps: a) a tetracid and diamine composition solution is prepared by evenly stirring a tetracarboxylic acid and a diamine in an organic solvent at low temperature of-10 to 40 DEG C; b) the main part of a tetracarboxylic dianhydride is added into the tetracid and diamine composition solution for stirring for reaction at the low temperature of-10 to 40 DEG C to obtain a low viscosity polyamic acid composition solution; and c) the rest part of the tetracarboxylic dianhydride is added into the low viscosity polyamic acid composition solution to obtain the polyamic acid composition. The polyamic acid composition well solves the problems that the polyamic acid solution is not stable in viscosity control in the preparation process and the polymer molecule chains are difficult to further grow in the subsequent imidization process, and can be used in industrial production of a polyimide material.

Description

technical field [0001] The invention relates to a polyamic acid composition with controllable viscosity, a preparation method and application thereof. Background technique [0002] Polyimide is a kind of polymer with excellent comprehensive performance, which has excellent heat resistance, low temperature resistance, self-lubrication, radiation resistance and flame retardancy, as well as excellent mechanical properties and dielectric properties . Therefore, it is widely used in high-temperature radiation-resistant materials for spacecraft, satellites, space vehicles, etc.; advanced structural composite materials, electrical insulation materials, high-temperature-resistant adhesives, high-temperature-resistant sealing materials, etc. in aerospace, automotive, electromechanical, etc.; In the field of microelectronics, it can be used as the base material of FPC or PCB, the interlayer insulation material of IC, the passivation coating of very large scale integrated circuit and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10D01F6/78
Inventor 孙旭阳陈雪黄森彪崔晶周文乐
Owner CHINA PETROLEUM & CHEM CORP
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