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Method for preparing ultra-high heat resistant polyimide polymer

A polyimide, heat-resistant technology, applied in the chemical field, can solve the problems of the final polymer's solubility degradation, hindering material processing and recycling, etc.

Active Publication Date: 2015-09-30
GENERAL ENG RES INST CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the disadvantage of this method is that it reduces the solubility of the final polymer, which further hinders the processing and recycling of materials (Chem.Mater.1998,10,734)
In addition, this method has only a certain effect on improving the thermal stability of polyimide materials.

Method used

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  • Method for preparing ultra-high heat resistant polyimide polymer
  • Method for preparing ultra-high heat resistant polyimide polymer
  • Method for preparing ultra-high heat resistant polyimide polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Synthesis of 1,7-bis-aniline-m-carborane

[0029] Weigh 1.0 g of 1,7-bis-phenyl-m-carborane, dissolve it in 50 mL of dichloromethane, and place the reaction system in an ice bath to cool. Then slowly add a mixture of 5mL nitric acid and 25mL concentrated sulfuric acid. The resulting mixture was stirred and reacted at room temperature for 15 hours. After the reaction was completed, the acid layer was discarded, and the organic phase was washed with saturated sodium carbonate solution and then with deionized water. The organic phase after layering is dried with anhydrous magnesium sulfate, and magnesium sulfate is filtered off after drying, and a light yellow solid is obtained after vacuum distillation, and the synthetic route diagram is as follows: figure 1 shown.

[0030] The obtained pre-yellow solid was dissolved in 50 mL of ethanol, heated to reflux, and then 0.68 g of reduced iron powder and 4 mL of concentrated hydrochloric acid were added. After completion, th...

Embodiment 2

[0035] Synthesis of 1,7-bis-(3-methyl-4-nitrophenyl)-m-carborane

[0036] Weigh 0.8g of 1,7-bis-phenyl-m-carborane, dissolve it in 50mL of dichloromethane, and place the reaction system in an ice bath to cool. Then slowly add a mixture of 5mL nitric acid and 25mL concentrated sulfuric acid. The resulting mixture was stirred and reacted at room temperature for 15 hours. After the reaction was completed, the acid layer was discarded, and the organic phase was washed with saturated sodium carbonate solution and then with deionized water. The stratified organic phase was dried with anhydrous magnesium sulfate, and the magnesium sulfate was filtered off after drying, and a light yellow solid was obtained after vacuum distillation. The resulting pale yellow solid is crystallized from a mixed solution of ethyl acetate and petroleum ether to obtain the product, and the synthetic route diagram is as follows: figure 2 shown.

[0037] 1 H NMR (400MHz, DMSO) δ8.09 (d, J = 2.1Hz, 4H)...

Embodiment 3

[0045] Synthesis of 1,7-bis-[4-(3-nitrophenyl)-benzyl]-m-carborane

[0046] Weigh 0.5 g of 1,7-bis-(3-iodobenzyl)-m-carborane and 0.79 g of cesium fluoride and dissolve it in 50 mL of dry DME, and bubble the resulting suspension with argon for 20 minutes to remove solids. system air. Then add 0.10g Pd(PPh 3 ) 4 , the reaction mixture was stirred at 80° C. for 16 h under nitrogen atmosphere. The collected supernatant was evaporated and dried under reduced pressure to obtain a yellow oily product. The obtained oil was dissolved in ethyl acetate and separated by column chromatography. The eluent was ethyl acetate / petroleum ether (1 / 4) mixed solution.

[0047] 1 H NMR (400MHz, DMSO) δ8.38 (t, J = 2.0Hz, 2H), 8.19 (ddd, J = 8.2, 2.2, 0.7Hz, 2H), 8.11 (dd, J = 4.7, 3.7Hz, 2H) , 7.74(d, J=1.8Hz, 2H), 7.71(d, J=1.6Hz, 4H), 7.24(d, J=8.2Hz, 4H), 2.31-1.30(br s, 10H). 13 C NMR(101MHz,DMSO)δ148.83,141.61,137.85,137.21,133.51,131.10,130.90,127.28,122.59,121.35,77.06,41.62.IR(KBr):2...

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Abstract

The invention discloses a method for preparing ultra-high heat resistant polyimide polymer. The method includes the following steps: dissolving aromatic-diamine containing carborane component and traditional aromatic dianhydride or aromatic dianhydride containing the carborane component and traditional aromatic-diamine into DMF or DMAc, carrying out ring opening polymerization to obtain polyamic acid; adding proper amounts of acetic oxide and pyridine into the obtained polyamic acid solution, stirring at room temperature for appropriate time, adding a proper amount of methyl alcohol to precipitate solid, and drying the solid to obtain polyimide containing the carborane component. According to the method provided by the invention, the 5% weight loss temperature of the prepared polyimide in nitrogen is greater than 600 DEG C, and that in the air is greater than 1000 DEG C, which are higher than those of the currently developed polyimide materials.

Description

technical field [0001] The invention relates to the chemical field, in particular to a preparation method of polyimide polymer with ultrahigh heat resistance. Background technique [0002] Due to its excellent high and low temperature resistance and mechanical properties, polyimide, as a commonly used polymer material in the aerospace field, plays an irreplaceable and important role. The weight loss temperature of traditional fully aromatic polyimide in nitrogen is greater than 400°C. If a rigid monomer with a conjugated structure is used in the preparation of polyimide, the intramolecular and intermolecular forces of the final polymer can be increased, and finally the thermal stability of polyimide can be further improved (Prog. Polym. Sci. 2012, 37, 907). But the disadvantage of this method is that it reduces the solubility of the final polymer, which further hinders the processing and recycling of materials (Chem. Mater. 1998, 10, 734). In addition, this method has onl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10
Inventor 邢涛张凯吴菊英黄渝鸿
Owner GENERAL ENG RES INST CHINA ACAD OF ENG PHYSICS
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