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Preparation method of liquid crystalline polyimide solution

The technology of polyimide and solution is applied in the field of preparation of polyimide liquid crystal solution, which can solve the problems of large environmental impact of phenolic solvents, and achieve the effects of overcoming large environmental impact, simple process and good application prospect.

Inactive Publication Date: 2012-07-25
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of polyimide liquid crystal solution, which has simple process and low cost, and overcomes the problem that phenolic solvents have a great impact on the environment

Method used

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  • Preparation method of liquid crystalline polyimide solution
  • Preparation method of liquid crystalline polyimide solution
  • Preparation method of liquid crystalline polyimide solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 60 g of P to a 100 ml flask 2 o 5 Content is 80% polyphosphoric acid, add 15 grams of P 2 o 5 Stirred at 150°C for 2 hours under the protection of nitrogen, a clear P 2 o 5 Content is the polyphosphoric acid solution of 84%, cool down to 120 ℃, set aside.

[0023] Add weighed 3.60 gram of 6-amino-2-(p-aminophenyl) benzimidazole (BIA) and 4.73 gram of biphenyltetra-acid dianhydride BPDA into the flask, adopt stepwise heating, and stir to make it at 120 ℃ for 3 hours, 150 ℃ for 4 hours, and then reacted at 220 ℃ for 1 hour to obtain a liquid crystal polyimide solution. The yield is 93%, and the intrinsic viscosity is 1.86 (concentrated sulfuric acid is used as a solvent, measured at 25° C.).

Embodiment 2

[0025] Add 60 g of P to a 100 ml flask 2 o 5 Content is 80% polyphosphoric acid, add 15 grams of P 2 o 5 Stirred at 150°C for 2 hours under the protection of nitrogen, a clear P 2 o 5 Content is the polyphosphoric acid solution of 84%, cool down to 120 ℃, set aside.

[0026] Add 3.42 grams of 6-amino-2-(p-aminophenyl)benzimidazole (BIA) and 4.92 grams of BTDA into the flask, raise the temperature in stages, and stir to polymerize at 150°C for 5 hours, then at 160°C Polymerize for 5 hours, and then react at 180° C. for 2 hours to obtain a liquid crystal polyimide solution. The yield is 92%, and the intrinsic viscosity is 1.50 (concentrated sulfuric acid is used as a solvent, measured at 25° C.).

Embodiment 3

[0028] Add 60 g of P to a 100 ml flask 2 o 5 Content is 80% polyphosphoric acid, add 6 grams of P 2 o 5 Stirred at 120°C for 2 hours under the protection of nitrogen, a clear P 2 o 5 Content is the polyphosphoric acid solution of 82%, cool down to 100 ℃, set aside.

[0029] Add 3.50 grams of 6-amino-2-(p-aminophenyl)benzimidazole (BIA) and 4.84 grams of ODPA into the flask, and heat up in stages, stirring to polymerize at 140°C for 4 hours, and then 170°C Polymerize for 4 hours, and then react at 210° C. for 2 hours to obtain a liquid crystal polyimide solution. The yield is 95%, and the intrinsic viscosity is 2.91 (concentrated sulfuric acid is used as a solvent, measured at 25° C.).

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Abstract

The invention relates to a preparation method of a liquid crystalline polyimide solution. The preparation method comprises the following steps of: mixing P2O5 and polyphosphoric acid under the protection of nitrogen gas at 100-150 DEG C, stirring to obtain a polyphosphoric acid solution of P2O5, and cooling the polyphosphoric acid solution to 100-120 DEG C; and (2) adding a diamine monomer containing heterocyclic rings and a dianhydride monomer into the polyphosphoric acid solution to obtain a reactant with the solid content of 5-20wt%, raising the temperature to 120-220 DEG C under the protection of nitrogen gas and reacting for 4-6h to obtain the liquid crystalline polyimide solution. The liquid crystalline polyimide solution is prepared on the basis of realizing the solubility of polyimide, which lays the technological basis for further preparing high-performance polyimide fiber or film; and the preparation method is simple in process, low in cost, capable of solving the problem that a phenol solvent has great influence to the environment and favorable in application prospect.

Description

technical field [0001] The invention belongs to the field of polyimide preparation, in particular to a preparation method of polyimide liquid crystal solution. Background technique [0002] Polyimide has excellent electrical and mechanical properties, high thermal and chemical stability, good dimensional stability and other excellent properties, and is widely used in aerospace, electronics and other fields. The conjugated system, ladder and semi-ladder structures formed by the aromatic and heterocyclic structures in the polyimide molecule make the molecular chain have high rigidity, so that the polyimide has a high glass transition temperature and thermal conductivity. It has high stability and good chemical inertness, but at the same time it is insoluble and infusible, which affects its processing performance. Therefore, seeking a solvent that can dissolve polyimide is one of the key technologies for preparing high-performance polyimide fibers. [0003] At present, the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C09K19/38
Inventor 张清华夏清明刘俊鹏董杰许千陈大俊
Owner DONGHUA UNIV
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