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Polyimide and preparation process thereof

A technology of polyimide and mixture, which is applied in the field of chemical polymer material preparation, can solve the problems of time-consuming and energy consumption, and achieve the effects of improving production efficiency, considerable economic value, and shortening the dropping time

Inactive Publication Date: 2014-05-14
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Then stop the reaction, pour the mixture into water, acetone, methanol, etc. to wash off the solvent. The disadvantage is that the reaction time is more than 7 hours, which is time-consuming and energy-consuming.

Method used

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  • Polyimide and preparation process thereof
  • Polyimide and preparation process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 80.5 g of benzophenone tetracarboxylic dianhydride (BTDI) to 250 ml of N,N'-dimethylformamide (DMF), add 0.075 g of NaOH, and dissolve in 0.2 ml of water. Mechanical stirring, nitrogen protection, heating at 80 °C to dissolve, after dissolution, add two diisocyanates at one time - a mixture of 4,4`-diphenylmethane diisocyanate (MDI) and toluene diisocyanate (TDI) (The molar ratio of TDI to MDI was 4:1) 37.88 g, reacted for 1 hour, and the temperature was controlled at 80°C. Next, 9.47 g of the diisocyanate mixture was added dropwise to the reaction system for 1 hour, and the temperature was controlled at 80°C. The reaction was carried out for 1 hour after the completion of the dropwise addition. The mixture was poured into acetone to wash off the solvent. The reduced viscosity test result is about 0.8 (NMP is the solvent, C=0.005g / ml).

Embodiment 2

[0033] 161g of benzophenone tetraacid dianhydride (BTDI) was added to 500ml of N,N'-dimethylacetamide (DMAc), 0.15g of NaOH was added, and dissolved in 0.4ml of water. Mechanical stirring, nitrogen protection, heating at 120 ° C to dissolve, after dissolution, two diisocyanates - 4,4`-diphenylmethane diisocyanate (MDI) and toluene diisocyanate (TDI) mixture ( The molar ratio of TDI to MDI was 4:1) 66.29 g, the reaction was performed for 45 minutes, and the temperature was controlled at 120 °C. 28.41 g of the diisocyanate mixture was added dropwise to the reaction system, the dropwise addition time was 1 hour, and the temperature was controlled at 120°C. The reaction was carried out for 2 hours after the completion of the dropwise addition. After the reaction was stopped, the mixture was poured into acetone to wash off the solvent. The reduced viscosity test result is about 0.8 (NMP is the solvent, C=0.005g / ml).

Embodiment 3

[0035] 322g of benzophenone tetraacid dianhydride (BTDI) was added to 500ml of N,N'-dimethylacetamide (DMAc), 0.3g of NaOH was added, and dissolved in 0.8ml of water. Mechanical stirring, nitrogen protection, heating at 60 °C to dissolve, after dissolution, two diisocyanates - 4,4`-diphenylmethane diisocyanate (MDI) and toluene diisocyanate (TDI) mixture ( The molar ratio of TDI to MDI was 4:1) 151.52 g, the reaction was performed for 1 hour, and the temperature was controlled at 60 °C. 37.88 g of the diisocyanate mixture was added dropwise to the reaction system, the dropwise addition time was 1 hour, and the temperature was controlled at 60°C. The reaction was carried out for 1.5 hours after the completion of the dropwise addition. After the reaction was stopped, the mixture was poured into acetone to wash off the solvent. The reduced viscosity test result is about 0.8 (NMP is the solvent, C=0.005g / ml).

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Abstract

The invention relates to a polyimide containing a structure represented by the following formula and a preparation process thereof. The preparation process includes using a rapid two-step polymerization process, subjecting di-anhydride and a mixture of two kinds of diisocyanate to co-condensation and polymerization to obtain the polyimide. A solvent containing low toxicity is used as a reaction medium in the process of reaction so that fewer by-products are produced, separation purification is absent, and the reaction process is simple. The post-treatment of the final products is very easy, and the purity of the products is high. The polyimide has wide application fields and can be used in the fields of filter screens for high-temperature filtering, protective clothing, heat insulation materials and aerospace, and also in various high-temperature extreme environments. The formula is shown in the desctiption.

Description

technical field [0001] The invention relates to the technical field of chemical polymer material preparation, in particular to a high-performance polyimide and a preparation method thereof. Background technique [0002] A polyimide prepared by the reaction of aromatic anhydrides and aromatic isocyanates has excellent thermal stability and non-melting properties, and its glass transition surface temperature is 315°C. Moreover, the fiber carbonization temperature of this material is 370°C. At the same time, due to the existence of the aromatic ring structure, this polyimide material has high fire resistance and is not easy to burn. The oxygen index is 38. Generally, it can be used at 260°C. This polyimide is resistant to various organic agents, such as alcohols, ethers, and halogenated hydrocarbons. However, strong polar and protic solvents can dissolve it. Such as N,N'-dimethylformamide (DMF), N,N'-dimethylacetamide (DMAc), N-methylpyrrolidone (NMP), concentrated sulfuri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10
Inventor 白静史子兴印杰
Owner SHANGHAI JIAOTONG UNIV
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