Polyimide synthetic method

A technology of polyimide and synthesis method, which is applied in the field of polyimide synthesis, can solve the problems of poor transparency of polyimide, and achieve the effect of improving transparency and high transparency

Active Publication Date: 2016-03-02
HUBEI DINGLONG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem of poor transparency of polyimide in the prior art, the embodiment of the present invention provides a synthesis method of polyimide

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0034] Introduce nitrogen into a 250mL three-neck flask equipped with a mechanical stirring device, first add 2.9112g (0.0091mol) 2,2'-bis(trifluoromethyl)diaminobiphenyl and 0.2422g (0.0009mol) 1,1' - Mixed diamines of bis(4-aminophenyl)cyclohexane, followed by 62.56 g of ionic liquid 1,3-bis(2-methoxy-2-oxoethyl)imidazole tetrafluoroborate, 1 , The structural formula of 3-bis(2-methoxy-2-oxyethyl)imidazolium tetrafluoroborate is:

[0035]

[0036] Turn on the mechanical stirring and heat to make it dissolve. At this time, the temperature of the mixed solution in the three-neck flask is not higher than 50°C. After the mixed diamine is completely dissolved, add 3.1021g (0.01mol) 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride into the three-necked flask, stir for 10min, squeeze the nitrogen bag to make the three-necked flask Remove as much air as possible. The mixture in the three-necked flask was slowly heated up to 180° C., stirred at a constant temperature of 180°...

Embodiment 2

[0041] Argon was passed into a 250mL three-neck flask equipped with a mechanical stirring device, and 1.6012g (0.005mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 1.3319g (0.005mol) of 1,1 The mixed diamine of '-bis(4-aminophenyl) cyclohexane, then add 14.75g ionic liquid 1,3-bis(2-methoxy-2-oxoethyl) imidazole tetrafluoroborate, And turn on the mechanical stirring, heat to make it dissolve, and the temperature of the mixed solution in the three-necked flask is not higher than 50°C at this time. After the mixed diamine is completely dissolved, add 4.4424g (0.01mol) 4,4'-hexafluoroisopropyl phthalic anhydride to the three-necked flask, and after stirring for 10min, squeeze the argon bag to make the air in the three-necked flask Eliminate as much as possible. The mixed solution in the three-neck flask was slowly heated up to 150° C., stirred at a constant temperature of 150° C. for 10 h, and then cooled down to room temperature naturally to obtain a pale yellow polyimide ...

Embodiment 3

[0045] Nitrogen was passed into a 250mL three-neck flask equipped with a mechanical stirring device, and 2.6579g (0.0083mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 0.4528g (0.0017mol) of 1,1' - Mixed diamines of bis(4-aminophenyl)cyclohexane, and then add 17.21g of ionic liquid chloride 1,3-bis(2-methoxy-2-oxyethyl)imidazole chloride, chloride 1, The structural formula of 3-bis(2-methoxyl-2-oxyethyl)imidazole is:

[0046]

[0047] Turn on the mechanical stirring and heat to make it dissolve. At this time, the temperature of the mixed solution in the three-neck flask is not higher than 50°C. After the mixed diamine is completely dissolved, add 1.5511g (0.005mol) of 3,3',4,4'-diphenyl ether tetracarboxylic dianhydride and 2.2212g (0.005mol) of 4,4'-hexafluoroiso Propyl phthalic anhydride, after stirring for 10 minutes, squeeze the nitrogen bag to remove the air in the system as much as possible. The mixed solution in the three-necked flask was slowly heated up to 2...

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Abstract

The invention discloses a polyimide synthetic method and belongs to the field of high polymer materials. The method comprises the steps of causing dianhydride and diamine to undergo polymerization reaction in ionic liquid; mixing polyimide prepolymer solution with methanol or deionized water, obtaining sediments, filtering and drying the sediments to obtain polyimide prepolymer powder; dissolving the polyimide prepolymer powder in polar solution, and obtaining polyimide prepolymer glue solution; smearing the polyimide prepolymer glue solution to a flat plate to undergo curing, performing cooling to room temperature to perform stripping, and obtaining film-shaped polyimide. Through the ionic liquid, the generated polyimide prepolymer can undergo complete imidization reaction at a low temperature, and prepared polyimide is colorless and very high in transparency.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a synthesis method of polyimide. Background technique [0002] Polyimide is a high-performance polymer material with excellent chemical stability, thermal stability and high mechanical strength, and has been widely used in aerospace, microelectronics and chemical industries. [0003] The existing conventional method of synthesizing polyimide is to form soluble polyimide by dianhydride and diamine in aprotic strong polar solvent at high temperature, wherein, aprotic strong polar solvent can be N, N-Dimethylformamide, N,N-Dimethylacetamide or N-methylpyrrolidone. [0004] In the process of realizing the present invention, the inventor finds that there are at least the following problems in the prior art: [0005] The color of the polyimide synthesized by the above method is generally light yellow or brownish yellow, which makes the polyimide poor in transparency, thereby limiting...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/18
Inventor 尤庆亮刘继延陈妤红张玲于洁阮敏胡思泉付华刘学清谭时友曹元成徐亨陈灵瑄
Owner HUBEI DINGLONG CO LTD
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