Method for improving polyimide slurry production efficiency

A technology of polyimide slurry and production efficiency, applied in the production of bulk chemicals, etc., can solve the problems of affecting performance, difficult storage and recycling, and extremely high environmental requirements, and achieves improved activity and selectivity. Period, the effect of increasing the movement rate

Inactive Publication Date: 2018-09-14
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned ionic liquid as a medium greatly shortens the reaction time, but it also has the following defects: 1. The reaction conditions need to be heated to above 150°C, and the energy cost after scale-up production is high; 2. The price of ionic liquid is extremely high, and the price per 100g is 200 -500 yuan, while the price of ordinary organic solvents is only 1-2 yuan per 100g. The high cost of ionic liquids is difficult to use in large quantities; 3. Ionic liquids have extremely high requirements on the environment, and they strongly absorb moisture in the air. Ionic liquids will react with water, and the performance of some non-reactive ionic liquids will be greatly reduced due to water absorption, so it is difficult to store and recycle. Once mixed with impurities, its performance will be easily affected
[0005] The above shortcomings limit the application of ionic liquids as solvents in polyimide slurries. Therefore, it is necessary to develop a method for improving the production efficiency of polyimide slurries that undergoes polymerization at room temperature, has short reaction times, and is economical.

Method used

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  • Method for improving polyimide slurry production efficiency

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Under nitrogen protection, 0.713g ionic liquid (0.475g 1-hexyl-3-methylimidazolium tetrafluoroborate and 0.238g 1-butyl-3-methyl imidazole hexafluorophosphate) to form 72g mixed solvent, at room temperature, mix 1.394g (0.0052mol) 1,1-bis(4-aminophenyl) cyclohexane BAPC and 16.645g (0.052mol) TFMB Dissolve the diamine in a strictly dry mixed solvent, stir mechanically until it is completely dissolved, add 17.366g (0.0560mol) ODPA to it, continue stirring for 1h, then add 0.595g (0.0024mol) 4-PEPA, stir and age for 12h to obtain Polyamic acid solution with capping agent.

[0024] Add 8.235g (0.056mol) of phthalimide to the polyamic acid solution, stir at room temperature for 4h, and obtain a polyimide prepolymer solution after the reaction is completed, and precipitate the polyimide prepolymer solution into methanol, filtered, washed, and dried at 60°C to obtain solid polyimide prepolymer, which is dissolved in NMP to obtain polyimide prepolymer glue, with a solid conte...

Embodiment 2

[0027]Under the protection of nitrogen, 0.716g ionic liquid (0.409g 1-hexyl-3-methylimidazolium tetrafluoroborate and 0.307g 1-butyl-3-methyl imidazole hexafluorophosphate) to form 144g mixed solvent, at room temperature, 7.937g (0.0296mol) 1,1-bis(4-aminophenyl) cyclohexane BAPC and 9.477g (0.0296mol) TFMB Dissolve in 20g of strictly dry mixed solvent, under nitrogen protection, mechanically stir until completely dissolved, add 17.99g (0.058mol) ODPA to it, continue stirring for 1h, then add 0.595g (0.0024mol) 4-PEPA, stir and age After 12 hours, a polyamic acid solution with an end-capping agent was obtained.

[0028] 12.796g (0.087mol) of phthalimide was added to the polyamic acid solution, stirred at room temperature for 3.5h, the reaction was completed to obtain a polyimide prepolymer solution, and the polyimide prepolymer solution was Precipitate into methanol, filter, wash, and dry at 60°C to obtain polyimide prepolymer solid, dissolve in DMF to obtain polyimide prepol...

Embodiment 3

[0031] Under nitrogen protection, add 0.252g ionic liquid (0.126g 1-hexyl-3-methylimidazolium tetrafluoroborate and 0.126g 1-butyl -3-Methylimidazole hexafluorophosphate mixed) to form 252g mixed solvent, 2.572g (0.0096mol) 1,1-bis(4-aminophenyl) cyclohexane BAPC and 15.355g (0.048 mol) of TFMB was dissolved in a strictly dry mixed solvent, mechanically stirred until it was completely dissolved, and then 17.478g (0.0564mol) ODPA was added to it, and after stirring for 1 hour, 0.595g (0.0024mol) 4-PEPA was added to it, and aged with stirring After 12 hours, a polyamic acid solution with an end-capping agent was obtained.

[0032] 16.576g (0.1128mol) of phthalimide was added to the polyamic acid solution, stirred at room temperature for 2h, and the polyimide prepolymer solution was obtained after the reaction, and the polyimide prepolymer solution was Precipitate into methanol, filter, wash, and dry at 60°C to obtain polyimide prepolymer solid, dissolve in DMF to obtain polyimi...

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Abstract

The invention discloses a method for improving polyimide slurry production efficiency. The method is characterized by including the steps: adding ionic liquid into a polar solvent under protection ofnitrogen or argon to form mixed solvent; sequentially and completely dissolving a diamine monomer, a dianhydride monomer and an end capping agent in the mixed solvent; adding a catalyst to react mixture for 2-4 hours at normal temperature to obtain polyimide prepolymer slurry. The ionic liquid accounts for 0.05-1% of the weight of the polar solvent. According to the method, mixture of the polar solvent and the ionic liquid serves as a reaction medium, the ionic liquid has a catalytic function of accelerating reaction, so that a reaction process is shortened, reaction conditions are mild, the problem of cost caused by a lot of ionic liquid is improved, and economy is greatly improved.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for improving the production efficiency of polyimide slurry. Background technique [0002] Polyimide has excellent mechanical properties, heat resistance, low temperature resistance, flame retardancy, solvent resistance and electrical properties. It can be used as a structural composite material and is widely used in aerospace, aviation, precision machinery, microelectronic devices and Transparent conductive film, TFT substrate and flexible printed circuit substrate, etc. [0003] The Chinese invention patent with the publication number CN 104558608 B discloses a preparation method of polyimide and its transparent film, using organic solvents N-methylpyrrolidone NMP, dimethyl sulfoxide DMSO, Amide DMAc or N,N-dimethylformamide DMF is used as the reaction medium to carry out the polymerization reaction of diamine and dianhydride. The invention can prepare polyamic acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/1032Y02P20/54
Inventor 尤庆亮刘继延肖标邹立勇刘学清
Owner JIANGHAN UNIVERSITY
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