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Synthetic method of semi-aromatic polyimide and application thereof

A polyimide and semi-aromatic technology, which is applied in the field of synthesis of semi-aromatic polyimide, can solve the problems of difficult removal of catalysts and the influence of polyimide electrical properties, so as to improve electrical insulation performance and produce three wastes little effect

Active Publication Date: 2017-08-22
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this invention patent uses a noble metal catalyst or a transition metal salt catalyst. After the reaction, the catalyst is difficult to remove. The catalyst remaining in the polyimide material will cause the polyimide material to degrade to varying degrees at high temperatures, and the metal The presence of ions has a significant effect on the electrical properties of polyimide

Method used

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  • Synthetic method of semi-aromatic polyimide and application thereof
  • Synthetic method of semi-aromatic polyimide and application thereof
  • Synthetic method of semi-aromatic polyimide and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] like figure 1 Shown, the synthetic method of the semiaromatic polyimide of the present embodiment, comprises the steps:

[0033] (1) Add 10.33g (0.033mol) of 4,4'-oxydiphthalic anhydride into a 250mL single-necked flask equipped with a magnetic stirrer and a reflux condenser, then add 103.33g of anhydrous methanol, and heat with an oil bath To 75°C, reflux at this temperature for 5 hours to obtain dimethyl 4,4'-oxydiphthalate;

[0034] (2) Cool the reaction solution in step (1) to 60°C, keep the stirring rate at 80r / min, and slowly add 3.91g (0.0336mol) of 1,6-hexamethylenediamine dropwise to the reaction solution, and continue Insulated for 30 minutes to obtain the hexamethylene diammonium salt of dimethyl 4,4'-oxydiphthalate;

[0035] (3) The hexamethylene diammonium salt of dimethyl 4,4'-oxydiphthalate obtained in step (2) is spray-dried, and the process conditions of spray-drying are: the inlet air temperature is 80°C, and the outlet air temperature is 80°C. The ...

Embodiment 2

[0048] Such as figure 1 Shown, the synthetic method of the semiaromatic polyimide of the present embodiment, comprises the steps:

[0049] (1) Add 7.19g (0.033mol) of pyromellitic dianhydride into a 250mL single-necked flask equipped with a magnetic stirrer and a reflux condenser, then add 103.33g of anhydrous methanol, and heat it to 75°C with an oil bath. Reflux reaction at high temperature for 5h to obtain dimethyl pyromellitic acid;

[0050] (2) Cool down the reaction solution in step (1) to 60°C, keep the stirring rate at 70r / min, and slowly add 3.91g (0.0336mol) of 1,6-hexamethylenediamine dropwise to the above reaction solution. Continue to insulate for 30min to obtain the hexamethylene diammonium salt of dimethyl pyromellitic acid;

[0051] (3) The hexamethylene diammonium salt methanol solution of dimethyl pyromellitate obtained in step (2) is spray-dried, and the process conditions of spray-drying are: the inlet air temperature is 80°C, the outlet air temperature i...

Embodiment 3

[0056] Such as figure 1 Shown, the synthetic method of the semiaromatic polyimide of the present embodiment, comprises the steps:

[0057] (1) Add 9.71g (0.033mol) of biphenyltetracarboxylic dianhydride into a 250mL single-necked flask equipped with a magnetic stirrer and a reflux condenser, then add 103.33g of anhydrous methanol, and heat it to 75°C with an oil bath. Reflux reaction at high temperature for 5h to obtain dimethyl biphenyl tetracarboxylate;

[0058] (2) Cool down the reaction solution in step (1) to 60°C, keep the stirring rate at 80r / min, and slowly add 3.91g (0.0336mol) of 1,6-hexamethylenediamine dropwise to the above reaction solution. Continue to insulate for 30min to obtain the hexamethylene diammonium salt of dimethyl biphenyl tetracarboxylate;

[0059] (3) The hexamethylene diammonium salt methanol solution of dimethyl biphenyl tetracarboxylate obtained in step (2) is spray-dried. The medium volume is 1800ml / h, the maximum feed volume is 200ml / h, and ...

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Abstract

The invention relates to a synthetic method of semi-aromatic polyimide. The synthetic method comprises the following steps: (1) performing an esterification reaction on a dianhydride monomer and alcohol to obtain aromatic quadribasic binary ester; (2) performing a reaction on a diamine monomer and the aromatic quadribasic binary ester to obtain amine carboxylate of binary ester; (3) spraying and drying the amine carboxylate of binary ester to obtain a white powdery solid; (4) adding the white powdery solid into water to fully react in a high pressure reaction kettle to prepare a product a; (5) performing centrifugal separation on the product a and then washing the solid product by an eluant; and (6) drying the washed solid product in a nitrogen atmosphere to obtain the semi-aromatic polyimide. The prepared polyimide is used for modifying a nylon material, the electric insulating performance and the bending strength of the modified nylon material can be obviously improved, and the hygroscopic property can be reduced.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a method for synthesizing semi-aromatic polyimide and its application. Background technique [0002] Because of its excellent high temperature resistance, low temperature resistance, solvent resistance, radiation resistance, outstanding mechanical strength and dielectric properties, polyimide is widely used in many high-tech fields such as aviation, aerospace, automobiles, electronics, electrical appliances, etc. . Usually, polyimide needs to be synthesized by low-temperature solution polycondensation using strong polar solvents such as N-methylpyrrolidone, N,N-dimethylformamide, and N,N-dimethylacetamide. The use of the above-mentioned high-boiling-point organic solvents, due to the strong hydrogen bond between the solvent and the polyimide material, it is difficult to remove the residual high-boiling-point organic solvents in the product, and the separation and recovery of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08L77/02C08L79/08
CPCC08G73/1007C08G73/1053C08G73/1082C08L77/02C08L79/08
Inventor 王进高敬民王文志彭博胡天辉姜其斌李鸿岩
Owner ZHUZHOU TIMES NEW MATERIALS TECH
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