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Process for preparing biphenyl polyimide

A polyimide and biphenyl type technology, which is applied in the field of preparation of biphenyl type polyimide, can solve the problems of low yield, difficulty in separation and purification, and high production cost of biphenyl type polyimide, and achieves a reduction in The effect of production costs

Inactive Publication Date: 2003-02-12
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the many synthesis steps of biphenyl dianhydride, the catalyst is expensive, or the yield is low, or the reaction conditions are harsh, or the separation and purification are difficult, the production cost of biphenyl polyimide is too high, so that the scope of application is limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 5mmol of nickel bromide, 20mmol of triphenylphosphine and 50mmol of zinc powder into the reaction flask, fill with nitrogen to remove oxygen, add 25ml of DMAc, and stir the reaction at 120°C. After the system turns reddish brown, add 115ml of DMAc and 50mmol of 4 , 4′-bis(4-chloroimide) diphenyl ether, reacted for 2h, then poured the reactant into 1000ml of ethanol, added 60ml of concentrated hydrochloric acid, stirred for 10min, filtered to obtain the product, refluxed with 500ml of ethanol for 2h, Filtrate and dry at 100°C to obtain 22.2g of product with a yield of 97%. Mix cresol as a solvent and measure the inherent viscosity at 30°C to be 0.2dl / g.

Embodiment 2

[0020] Add 5mmol of nickel bromide, 80mmol of triphenylsulfone and 200mmol of zinc powder into the reaction flask, fill with nitrogen to remove oxygen, add 30ml of DMAc, and stir the reaction at 90°C. After the system turns reddish brown, add 115ml of DMAc and 50mmol of 4 , 4'-bis(3-chloroimide) diphenyl ether, reacted for 5h, then poured the reactant into 1000ml ethanol, added 90ml concentrated hydrochloric acid, stirred for 20min, filtered to obtain the product, refluxed with 30ml ethanol for 2h, Filtrate and dry at 100°C to obtain 22.0g of product with a yield of 96%. Mix cresol as a solvent and measure the inherent viscosity at 30°C to be 0.25dl / g.

Embodiment 3

[0022] Add 5mmol of nickel bromide, 60mmol of triphenylsulfone and 400mmol of zinc powder into the reaction flask, fill with nitrogen to remove oxygen, add 40ml of DMAc, and stir the reaction at 90°C. After the system turns reddish brown, add 620ml of DMAc and 62.5mmol of 4,4`-bis(4-chloroimide)diphenoxy-4``,4```-diphenyl ether, react for 3h, then pour the reactant into 1500ml ethanol, add 100ml concentrated hydrochloric acid , stirred for 10 minutes, filtered to obtain the product, refluxed with 500ml of ethanol for 2h, filtered, and dried at 100°C to obtain 39.3g of the product, with a yield of 98%, mixed with cresol as a solvent, and the inherent viscosity at 30°C was 0.21dl / g .

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Abstract

A process for preparing biphenyl polyimide includes such steps as dissolving bichlorodiphthalimide monomer, triphenylphosphino nickel as catalyst and zinc powder as reducer in non-proton solvent, reaction at 60-120 deg.C to generate Ni mating substance, oxydizing addition reaction on bichlorodiphthalimide to generate intermediate, and dereducing reaction to generate its condensate and zinc chloride while reducing Ni to react on chloroimide to generate polyimide. Its advantages are simple process and low cost.

Description

Technical field: [0001] The invention belongs to the preparation method of biphenyl type polyimide. Background technique: [0002] As a polymer material, biphenyl polyimide has attracted much attention due to its unique properties and wide application prospects. U.S. Patent [Itatani, US Pat., 4 568 715 (1986); Itatani, US Pat., 4 247 443 (1981); Sasaki, US Pat., 4 290 936 (1981); Sasaki, US Pat., 4 473 523 (1984); Kaneda, T., J.Appl.Polym.Sci; 32, 3151 (1986) etc.] the disclosed traditional biphenyl type polyimide preparation method is to be obtained by the reaction of biphenyl dianhydride and diamine imide. Due to the many synthesis steps of biphenyl dianhydride, the catalyst is expensive, or the yield is low, or the reaction conditions are harsh, or the separation and purification are difficult, the production cost of biphenyl polyimide is too high, so that the scope of application is limited. . Invention content: [0003] The purpose of this invention is to provide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 张所波高昌录丁孟贤高连勋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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