Synthesizing method of polyimide

A polyimide and synthesis method technology, applied in the field of polymer material synthesis, can solve the problems of high recycling cost, organic solvent volatility and harm to the environment and operators, and achieve easy recycling, easy recycling, and recycling high rate effect

Active Publication Date: 2011-10-19
BEIJING RADIATION APPL RES CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the solvent used in the two-step method is less toxic, the volatility of organic solvents causes great harm to the environment and operators, and the cost of recycling is relatively high

Method used

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  • Synthesizing method of polyimide
  • Synthesizing method of polyimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, the preparation of polyimide

[0020] Add 52.002 g of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid into a dry four-necked flask equipped with a mechanical stirrer, a thermometer, and a nitrogen gas inlet and outlet tube, raise the temperature to 60 ° C, and protect it with nitrogen gas. Under mechanical stirring, add 9.157g (25mmol) of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (Bis-AP-AF), stir until completely dissolved and then add 8.177g (25.375mmol ) of 3,3',4,4'-benzophenonetetraacid dianhydride (BTDA), wherein, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and 3,3', The molar ratio of 4,4'-benzophenone tetraacid dianhydride is 1:1.015; 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and 3,3',4,4'- The total mass of benzophenone tetraacid dianhydride accounts for 25% of the mass percentage of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid. After the dissolution is complete, the temperature is raised to 200 ° C ...

Embodiment 2

[0021] Embodiment 2, the preparation of polyimide

[0022] The method of this embodiment is the same as that of Example 1, except that the ionic liquid is changed to 1-butyl-3-methylimidazolium hexafluorophosphate; a yellow solid powder is finally obtained, and its infrared absorption spectrum is as follows: figure 2 shown by figure 2 (imino and carbonyl characteristic absorption peaks) it can be seen that the corresponding polyimide target product is obtained by polymerization, and Mn is 0.817 × 10 4 , The yield of this product is 94%.

Embodiment 3

[0023] Embodiment 3, the preparation of polyimide

[0024] The method of this embodiment is the same as that of Example 1, except that the temperature of the polymerization reaction is changed to 180° C., the time of the polymerization reaction is changed to 6 hours, and finally a yellow solid powder is obtained, and its infrared absorption spectrum is the same as that of figure 1 Similar; 95% yield of this product.

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Abstract

The invention discloses a synthesizing method of polyimide. The method comprises the following step that: an aromatic diamine compound and an aromatic dianhydride compound are subject to a polymerization reaction in an ionic liquid, such that polyimide is obtained. The ionic liquid can be any one of 1-ethyl-3-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium acetate, 1-ethyl-3-methylimidazolium dicyanamide, 1-butyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, and 1-butyl-3-methylimidazolium trifluoromethanesulfonate. The operation of the method is simple, the product made with the method is easy to purify and has high dissolvability (the product can be dissolved in regular solvents of N, N-dimethylacetamide, or tetrahydrofuran). The method has advantages of high yield, stable performance, good application prospect, and is suitable for industrialized production. Withthe method, polyimide films or fibers can be produced.

Description

technical field [0001] The invention relates to a synthesis method of polyimide, which belongs to the technical field of polymer material synthesis. Background technique [0002] In the field of polymer material technology, polyimide material is a high-performance polymer material with imide ring structure characteristics, which has excellent chemical stability, thermal stability and mechanical properties, and is more and more popular among people. It is widely used in industries such as aerospace, electrical engineering, microelectronics and chemical industry. There are two traditional methods for synthesizing polyimide: one-step synthesis method and two-step synthesis method. Higher temperature (about 200°C) and catalyst action to obtain polyimide in the next step of ring formation and direct polymerization; the disadvantage of this method is that the solvent used in the synthesis process is toxic and carcinogenic, which does not meet the development requirements of curre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 郑艳红王连才曾心苗鲍矛李淑凤
Owner BEIJING RADIATION APPL RES CENT
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