Preparation method of high-temperature-resistant polyimide resin

A technology of polyimide resin and high temperature resistance, which is applied in the field of preparation of high temperature resistant polyimide resin, can solve the problems of affecting molecular chain growth, limited molecular weight, large steric hindrance, etc. Application Potential, Effect of High Thermal Stability

Active Publication Date: 2022-07-26
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the above-mentioned synthetic methods, the preparation of fluorinated polyimide resins containing carborane structures is realized by polycondensation reaction of diamine monomers containing carborane structures and fluorine-containing dianhydrides. The steric hindrance of the structure in the polymer molecular chain is large, which will affect the growth of its molecular chain, so the molecular weight of this type of polyimide polymer is limited and the degree of polymerization is low

Method used

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  • Preparation method of high-temperature-resistant polyimide resin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] A preparation method of a high temperature resistant polyimide resin, the specific steps of the method are as follows:

[0029] (1) Under nitrogen protection, add 3.0983g (9.0mmol) of 1,2-bis(3-trifluoromethyl-4-aminophenyl)acetylene to a 250mL three-necked flask equipped with magnetic stirring and nitrogen guide , 90ml of DMAc, magnetically stirred until completely dissolved; then add 3.9982g (9.0mmol) of 4,4'-(hexafluoroisopropylidene) diphthalic anhydride, and then rinse the wall-mounted reaction with 30ml of DMAc The material powder was completely dissolved in the reaction solution, and the reaction was stirred at room temperature for 12 hours to obtain a viscous polyamic acid resin solution;

[0030] (2) adding toluene to the viscous polyamic acid solution prepared in step (1), warming up to 155°C and refluxing with water for 8 hours, sinking the reaction solution into deionized water to generate a precipitate; Filter, boil with boiling water, wash with ethanol, a...

Embodiment 2

[0035] A preparation method of a high temperature resistant polyimide resin, the specific steps of the method are as follows:

[0036] (1) Under nitrogen protection, add 1.5491g (4.5mmol) of 1,2-bis(3-trifluoromethyl-4-aminophenyl)acetylene to a 250mL three-necked flask equipped with magnetic stirring and nitrogen guide , 0.9372g (4.5mmol) of 1,2-bis(4-aminophenyl)acetylene and 90ml of NMP, stir magnetically until completely dissolved; then add 2.2869g (9.0mmol) of 1,4-difluoropyromellitic acid Dianhydride, rinse the wall-mounted reactant powder with 30ml of NMP, and stir and react at room temperature for 15 hours to obtain a viscous polyamic acid resin solution;

[0037] (2) adding toluene to the viscous polyamic acid solution prepared in step (1), warming up to 160° C. and refluxing with water for 4 hours, sinking the reaction solution into deionized water to form a precipitate; Filter, boil with boiling water, wash with ethanol, and dry in a vacuum drying oven at 70°C to o...

Embodiment 3

[0042] A preparation method of a high temperature resistant polyimide resin, the specific steps of the method are as follows:

[0043] (1) Under nitrogen protection, add 5.1638g (15mmol) of 1,2-bis(3-trifluoromethyl-4-aminobenzene)acetylene to a 500mL three-necked flask equipped with a magnetic stirring and a nitrogen leader, 2.0826g (10mmol) of 1,2-bis(4-aminophenyl)acetylene and 220ml of DMF, stir magnetically until completely dissolved; then add 8.8530g (25mmol) of 1,4-bis(trifluoromethyl)-2 , 3,5,6-benzenetetracarboxylic dianhydride, rinse the reactant powder hanging on the wall with 50ml of DMF, and stir the reaction at room temperature for 20 hours to obtain a viscous polyamic acid resin solution;

[0044] (2) adding toluene to the viscous polyamic acid solution prepared in step (1), warming up to 160° C. and refluxing with water for 6 hours, sinking the reaction solution into deionized water to form a precipitate; Filter, boil with boiling water, wash with ethanol, and...

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Abstract

The invention relates to a preparation method of high-temperature-resistant polyimide resin, and belongs to the technical field of high polymer materials. The method comprises the following steps: synthesizing a fluorinated polyimide polymer with a main chain containing alkynyl, and introducing a carborane structure into the main chain of the polymer by utilizing a macromolecular reaction to obtain the high-temperature-resistant polyimide resin. The method overcomes the defects that the molecular weight of the polyimide polymer is limited and the polymerization degree is low due to the fact that a carborane structure with large steric hindrance exists in reaction raw materials and influences increase of molecular chains of the reaction raw materials in the prior art, and the length and the molecular weight of the molecular chains can be designed according to actual application requirements; according to the high-temperature-resistant polyimide resin designed and synthesized by the method, fluorine atoms and a carborane structure with excellent thermal stability are introduced into a molecular main chain, so that the high-temperature-resistant polyimide resin has high thermal stability and thermal oxygen stability, low dielectric constant, refractive index, water absorption, cohesive energy and surface free energy, is hydrophobic and oleophobic, and has wider application potential.

Description

technical field [0001] The invention relates to a preparation method of a high temperature resistant polyimide resin, which belongs to the technical field of polymer materials. Background technique [0002] The polyimide polymer is mainly characterized by the imide ring structure in the main chain, and the aromatic heterocycle contained in the molecular structure and the conjugation effect between C-N-O make the polyimide have excellent properties. Therefore, polyimide resin has been known for its heat resistance and thermal oxidation resistance since its inception. It can be used for a long time in the temperature range of 200 ° C ~ 300 ° C, and has been widely used in aviation, aerospace, microelectronics, nano , liquid crystal, separation film and laser fields. At present, for special fields such as aerospace, polyimide materials with higher heat resistance are urgently needed to meet practical application needs. [0003] Since the discovery of carboranes, polymer chemi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12
CPCC08G73/126C08G73/123
Inventor 潘云星任爱民刘杰闫月明李栋梁
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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