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Preparation method of polyimide

A polyimide and polymerization reaction technology, applied in the field of polyimide preparation, can solve the problems of high cost, solvent toxicity, unfavorable polyimide production, etc., to shorten production cycle, reduce production cost, and save production cost effect

Active Publication Date: 2012-07-25
CHANGCHUN HIPOLYKING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, when adopting above-mentioned method to prepare polyimide powder, all need through complicated aftertreatment, just can obtain the higher polyimide powder of purity as washing etc. repeatedly; When the polyimide obtained can be dissolved in When in a solvent, it is necessary to go through steps such as solvent removal and crushing to obtain polyimide powder. Not only the steps are cumbersome and the cost is high, but some solvents are more toxic, which is not conducive to the production of polyimide.
High Perf.Polym., 1999, 11: 205; High Perf.Polym., 2003, 15: 269; High Perf.Polym., 2006, 18: 31. etc. also disclose the use of water as a medium for polyimide Synthesis, but this method needs to be carried out under pressure, and the obtained polyimide molecular weight is low

Method used

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preparation example Construction

[0020] The invention provides a kind of preparation method of polyimide, comprises the following steps:

[0021] a) The acid anhydride of diamine and organic acid undergoes a dehydration polymerization reaction in a non-polar solvent to obtain a mixture, and the non-polar solvent is one of aromatic hydrocarbons, aliphatic hydrocarbons, halogenated aromatic hydrocarbons or halogenated aliphatic hydrocarbons or multiple, the anhydride of the organic acid is one or more of dianhydride and monoanhydride;

[0022] b) filtering and drying the mixture obtained in step a) to obtain polyimide.

[0023] In the present invention, the anhydride of diamine and organic acid can be directly dehydrated and polymerized in a non-polar solvent to obtain a polyimide, and the polyimide is insoluble in a non-polar solvent, and the reaction mixture obtained after the reaction is directly filtered , without washing, fine polyimide powder can be obtained after drying, not only does not need complicat...

Embodiment 1

[0040] Measure 300mL of xylene in a reactor with a water separator and agitator, start stirring, pour 43.8 grams of triphenyl ether tetracarboxylic acid into the reactor, heat to 144°C and reflux with water; when there is no When the water comes out, cool down to normal temperature and analyze the effect of anhydride formation; when the anhydride formation is greater than 98%, add 20.00 grams of 4,4'-diaminodiphenyl ether, continue to stir and heat to 144 ° C with water; When the water comes out, lower the temperature to normal temperature, filter the obtained reaction mixture, vacuum-dry the filter cake at 200°C-240°C for 1 hour, discharge and sieve to obtain bisether anhydride polyimide powder. The rate is above 95%.

[0041] The bisether anhydride polyimide powder was dissolved in m-cresol, and its logarithmic viscosity was measured to be 1.21 dL / g.

Embodiment 2

[0043] Measure 300mL of xylene in a reactor with a water separator and agitator, start stirring, pour 43.8 grams of triphenyl ether tetracarboxylic acid into the reactor, heat to 144°C and reflux with water; when there is no When the water comes out, cool down to normal temperature and analyze the effect of anhydride formation; when the anhydride formation is greater than 98%, add 4.17 grams of carbon fiber and 20.00 grams of 4,4'-diaminodiphenyl ether, continue to stir and heat to 144 ° C with water; When there is no water coming out of the water tank, cool down to normal temperature, filter the obtained reaction mixture, and vacuum-dry the filter cake at 240°C to 290°C, discharge and sieve to obtain bisether anhydride polyimide powder. Its yield is above 95%.

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Abstract

The invention provides a preparation method of polyimide, comprising the following steps: a) carrying out a dehydration polymerization reaction on a diamine and an anhydride of an organic acid in a non-polar solvent to obtain a mixture, wherein the non-polar solvent is one or more of arene, aliphatic hydrocarbon, halogenated arene or halogenated aliphatic hydrocarbon, and the anhydride of the organic acid is one or more of dianhydride and single anhydride; and b) filtering the mixture obtained in step a) and drying to obtain the polyimide. According to the invention, the dehydration polymerization reaction between the diamine and the anhydride of the organic acid can be conducted directly in the non-polar solvent to obtain the polyimide which cannot be dissolved in the non-polar solvent; therefore, the polyimide powder with fine particles can be obtained by directly filtering and drying the reaction mixture without washing and grinding, and the production period is shortened and the production cost is reduced, and the large-scale production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of polyimide, in particular to a preparation method of polyimide. Background technique [0002] Polyimide is one of the organic polymer materials with the best comprehensive performance. It has the advantages of high temperature resistance up to 400°C, long-term use range of -200°C to 300°C, and high insulation performance. It is used in aerospace, aviation, microelectronics, nano , liquid crystal, separation membrane, laser and other fields have been widely used. [0003] The prior art generally uses dianhydrides and diamines as raw materials to synthesize polyimides. At first, diamines and dianhydrides are dissolved in an aprotic polar solvent, such as N, N-dimethylacetamide, N, N-dimethyl Low-temperature polycondensation reaction in formamide and N-methylpyrrolidone to obtain soluble polyamic acid. After forming a film or spinning the polyamic acid solution, heat it to about 300°C to dehydrate and form a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
CPCC08G73/10C08G73/1014C08G73/1032C08G73/1046C08G73/105C08G73/1053C08G73/1067C08G73/1071C08L79/08
Inventor 张鑫钟吉彬丁孟贤吕晓义
Owner CHANGCHUN HIPOLYKING
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