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Polyamide acid composition and preparation method and application thereof

A technology of polyamic acid and composition, which is applied to polyamic acid composition and the fields of preparation and application thereof, can solve the problems of unstable viscosity control, difficulty in increasing polymer molecular chain, etc., and achieve 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 solution, 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 the goal of

Method used

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  • Polyamide acid composition and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] 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 29.1278g (0.099mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the solution obtained above, Stirring was continued for 5 hours to obtain a light yellow transparent viscous solution, and a desired polyamic acid composition solution with a solid content of 14.8%. After testing, the kinematic viscosity is 146Pa·s at 25°C, and the intrinsic viscosity is 1.58dL / g at 25°C.

Embodiment 2

[0053] 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 0.6606g (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 28.8336g (0.098mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the solution obtained above, Stirring was continued for 5 hours to obtain a red-yellow solution, and the desired polyamic acid composition solution with a solid content of 20.0% was obtained. After testing, the kinematic viscosity is 68Pa·S at 25°C, and the intrinsic viscosity is 0.95dL / g at 25°C.

Embodiment 3

[0055] 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 1.321g (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, maintain the reaction for 1 hour to obtain a reddish-brown solution, then add 28.2451g (0.096mol) 3,3',4,4'-biphenyltetraacid dianhydride powder to the solution obtained above, Stirring was continued for 6 hours to obtain a black solution, and the desired polyamic acid composition solution with a solid content of 10.0% was obtained. After testing, the kinematic viscosity is 38Pa·S at 25°C, and the intrinsic viscosity is 0.62dL / g at 25°C.

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Abstract

The invention relates to a polyamide acid composition with the viscosity capable of being controlled and a preparation method and application thereof. The problems that in the prior art, controlling of the viscosity is unstable in the preparation process of a polyamic acid solution, and further lengthening of a polymer molecular chain is difficult in the subsequent imidization process are solved. The preparation method for the polyamide acid composition comprises the following steps that (a) tetracarboxylic acid and diamine are stirred in an organic solvent at the low temperature of minus 10-40 DEG C and evenly mixed, and thus a composition solution of tetracid and the diamine is obtained; and (b) tetracarboxylic acid dianhydride is added into the composition solution of the tetracid and the diamine and stirred for reaction at the low temperature of minus 10-40 DEG C. The problems are solved through the technical scheme for obtaining the polyamide acid composition, controlling of the viscosity of the polyamic acid solution and further lengthening of the polymer molecular chain in the subsequent imidization process are achieved, and the polyamide acid composition with the viscosity capable of being controlled and the preparation method can be applied to industrial production of polyimide materials.

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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IPC IPC(8): C08G73/10C08L79/08
Inventor 崔晶黄森彪周文乐陈雪孙旭阳
Owner CHINA PETROLEUM & CHEM CORP
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