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Polyamide acid copolymer and polyimide film prepared from polyamide acid copolymer

The technology of polyamic acid copolymer and polyamic acid is applied in the field of preparation of high-performance polyimide, and can solve the problems of low solubility of dianhydride and diamine, difficulty in normal reaction, high viscosity of reaction system, and the like. Achieve excellent mechanical properties and thermal stability, good stirring performance, and improve the effect of alkali resistance

Inactive Publication Date: 2014-12-10
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But usually, the temperature is too low to make the solubility of the reaction system to dianhydride and diamine become smaller, and the viscosity of the reaction system is too high, which makes it difficult to carry out the reaction normally. Therefore, the reaction temperature of the common polyamic acid is only Can choose around 10-20℃

Method used

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  • Polyamide acid copolymer and polyimide film prepared from polyamide acid copolymer

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Experimental program
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Effect test

Embodiment 1

[0023] The reactor was filled with nitrogen, and then a total of 0.075mol of 2,2-bis[4-(4-amino-2-trifluoromethylphenoxy)benzene]hexafluoropropane and p-phenylenediamine monomer (molar ratio 1:1) was added to the reactor at one time, stirred at a constant temperature at 30°C, dissolved in N-methylpyrrolidone, and after the dissolution was complete, 1,1-bis[4-( 3,4-dicarboxyphenoxy)phenyl]cyclohexane dianhydride and 3,3'-phenylene sulfide-4,4',5,5'-biphenyltetracarboxylic dianhydride mixed monomer (total 0.076mol), the specific method is: lower the reaction temperature to 15°C, first add 0.025mol of the dianhydride mixture, then quickly lower the temperature to 5°C, then add once every hour, and add the remaining 0.051mol, then immediately move the reactor to an ultra-low temperature thermostat equipped with ethylene glycol and water cooling liquid, control the temperature at -5°C, and then react at constant temperature for 4 hours to obtain a viscous polyamic acid solution. T...

Embodiment 2

[0025]The reactor was filled with nitrogen, and then a total of 0.075 mol of 2,2-bis[4-(4-amino-2-trifluoromethylphenoxy)benzene]hexafluoropropane, p-phenylenediamine and m-phenylenediamine Mixed monomers (molar ratio 2:1:1) were added to the reactor at one time, stirred at a constant temperature at 30°C, dissolved in N,N-dimethylacetamide, and after the dissolution was complete, the molar ratio was 1 : 1,1-bis[4-(3,4-dicarboxyphenoxy)phenyl]cyclohexanedianhydride and pyromellitic dianhydride mixed monomer (0.079mol in total), the specific method is: Lower the reaction temperature to 15°C, first add 0.025mol of the dianhydride mixture, then quickly lower the temperature to 5°C, then add once every hour, add the remaining 0.054mol in three times, then immediately put the reactor Move it to an ultra-low temperature thermostat equipped with ethylene glycol and water cooling liquid, control the temperature at -10°C, and then react at a constant temperature for 8 hours to obtain a ...

Embodiment 3

[0027] The reactor was filled with nitrogen, and then a total of 0.063 mol of 2,2-bis[4-(4-amino-2-trifluoromethylphenoxy)benzene]hexafluoropropane and m-phenylenediamine mixed monomer (mol Ratio 1:1) was added to the reactor at one time, stirred at 30°C, dissolved in N,N-dimethylacetamide, after the dissolution was complete, 1,1- Bis[4-(3,4-dicarboxyphenoxy)phenyl]cyclohexane dianhydride and pyromellitic dianhydride mixed monomer (0.060mol in total), the specific method is: reduce the reaction temperature to 15°C , first add 0.020mol of the dianhydride mixture, then quickly lower the temperature to 5°C, then add once every hour, and add the remaining 0.040mol in three times, then immediately move the reactor to a place filled with ethylene glycol and In the ultra-low temperature constant temperature tank of water cooling liquid, the temperature is controlled at -15 ° C, and then the constant temperature reaction is carried out for 6 hours, and a viscous polyamic acid solution...

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Abstract

The invention discloses a polyamide acid copolymer and a polyimide film prepared from the polyamide acid copolymer. The polyamide acid copolymer is prepared by the following concrete experiment steps: firstly, dissolving diamine into an aprotic solvent at 30 DEG C, and then reducing the temperature to 15 DEG C; adding diamine for the first time, and quickly reducing the temperature to 5 DEG C; adding the diamine once every two hours, and adding the diamine in three times; after a dianhydride monomer is added, immediately transferring a reactor to an ultra-low constant temperature tank containing ethylene glycol and water cooling liquid, controlling the temperature between -5 DEG C and -20 DEG C, and reacting for a period of time, so as to obtain a viscous polyamide acid solution; and carrying out de-solvent and heat imidization on the synthetic polyamide acid, so as to obtain the polyimide film, wherein the obtained polyimide material has the advantages of excellent mechanical property, low hot-shrinkage rate, low water absorption rate, excellent alkaline resistance and the like.

Description

technical field [0001] The invention relates to the field of preparation of high-performance polyimide, in particular to its precursor polyamic acid copolymer and the prepared polyimide film. The polyimide film of the present invention can be applied to special occasions requiring high tensile strength, heat resistance and the like. technical background [0002] Polyimide (PI) is widely used in aviation, aerospace, machinery, electronics and other fields because of its outstanding mechanical and high temperature resistance properties. As a class of aromatic heterocyclic compounds containing imide rings on the main chain of the molecule, the number of diamine and dianhydride monomers used to synthesize polyimides has reached 200 to 300. Therefore, the development of different monomer combinations More than one thousand kinds of polyimides have been produced. In addition, there are various synthetic pathways, which can be independently selected according to specific applicat...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 徐勇刘飞龙张晶晶李林霜李宣曾皓
Owner NANJING UNIV OF SCI & TECH
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