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Method for synthesis of high-temperature-resistant carborane-containing polyimide resin

A technology of polyimide resin and synthesis method, which is applied in the field of resin synthesis, can solve problems such as inability to meet application requirements, and achieve the effects of improving oxidation stability, excellent heat resistance and oxidation stability

Active Publication Date: 2017-12-12
CAPITAL AEROSPACE MACHINERY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] With the development of modern industrial technology, traditional metal materials can no longer meet the application requirements of special types of aviation and aerospace, with high specific strength and specific stiffness, strong designability, good fatigue resistance, corrosion resistance and special electromagnetic properties A class of advanced resin-based composite materials with high-performance fibers as reinforcements came into being

Method used

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  • Method for synthesis of high-temperature-resistant carborane-containing polyimide resin
  • Method for synthesis of high-temperature-resistant carborane-containing polyimide resin
  • Method for synthesis of high-temperature-resistant carborane-containing polyimide resin

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preparation example Construction

[0047] A kind of synthetic method of high temperature resistant carborane-containing polyimide resin of the present invention comprises the following steps:

[0048] Chemical formula:

[0049]

[0050] Among them, compound 1 is 4-ethynyltoluene, compound 2 is 4-carborane toluene, compound 3 is 2,6-dinitro-4-carborane toluene, compound 4 is 2,6-diamino-4 - carborane toluene.

[0051] (1) Synthesis of compound 2 from compound 1

[0052] In the three-necked flask a, add compound 1 of Ag and B of Bg in sequence 10 h 12 (CH 3 EN) 2 and C g toluene, compounds 1 and B 10 h 12(CH 3 EN) 2 It can be completely dissolved in toluene, where A:B=1:1.5~1:3, A:C=1:17~1:20, then react at 100~120°C for 20~24 hours, then stop heating to end the reaction.

[0053] Next, the toluene was distilled off under reduced pressure at 60-90°C, and then methanol was added for recrystallization, finally M g white crystal compound 2 was obtained, wherein A:M=1:1~1:1.5.

[0054] (2) Synthesis of ...

Embodiment 1

[0065] In a 250mL three-necked flask, add 5.2g of 4-ethynyltoluene, 14.8g of B 10 h 12 (CH 3 EN) 2 And 100g toluene, after reacting at 110°C for 20h, the reaction was terminated. Toluene was distilled off under reduced pressure at 70° C., and methanol was added for recrystallization to obtain 5.6 g of compound 2 as white crystals.

[0066] Put 5.6g of compound 2 in a 100mL three-neck flask, add 10g of dichloromethane, and stir evenly. Next, 2 g of fuming nitric acid and 20 g of concentrated sulfuric acid were added dropwise at a rate of 1 drop / second in an ice-water bath. After the dropwise addition, the reaction was continued for 3 h at room temperature and the reaction was terminated to obtain a mixture. The mixture was poured into ice water and separated with a separatory funnel to obtain a water phase solution and an oil phase solution, wherein the water phase solution was extracted with dichloromethane and combined with the oil phase solution, and then the solution wa...

Embodiment 2

[0071] In a 500mL three-necked flask, add 11g of 4-ethynyltoluene, 20g of B 10 h 12 (CH 3 EN) 2 And 200g toluene, after reacting at 110°C for 24h, the reaction was terminated. Toluene was distilled off under reduced pressure at 80°C, and methanol was added for recrystallization to obtain 12 g of compound 2 as white crystals.

[0072] Take 12g of compound 2 and place it in a 200mL three-necked flask, then add 20g of dichloromethane, and mechanically stir evenly. Next, 3 g of fuming nitric acid and 25 g of concentrated sulfuric acid were added dropwise at a rate of 2 drops / second in an ice-water bath. After the dropwise addition, the reaction was continued for 5 h at room temperature and the reaction was terminated to obtain a mixture. The mixture was poured into ice water and separated with a separatory funnel to obtain a water phase solution and an oil phase solution, wherein the water phase solution was extracted with dichloromethane and combined with the oil phase soluti...

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Abstract

The invention relates to the technical field of resin synthesis and particularly discloses a method for synthesis of a high-temperature-resistant carborane-containing polyimide resin. The method comprises a first step of using 4-ethynyltoluene to synthesize 4-carborane methylbenzene; a second step of causing 4-carborane methylbenzene to synthesize 2,6-binitro-4-carborane methylbenzene; a third step of causing 2,6-binitro-4-carborane methylbenzene to synthesize 2,6-diamido-4-carborane methylbenzene; and a fourth step of causing 2,6-diamido-4-carborane methylbenzene to synthesize the modified polyimide resin. The phenylacetylene end-capped thermosetting polyimide resin is used as a matrix, and monomeric diamine is molecularly designed to synthesize the m-phenylenediamine containing a carborane boron cage structure, and then m-phenylenediamine undergoes polymerization reaction with anhydride and an end-capped reagent, finally the modified polyimide resin is obtained, the maximum service temperature of a polymer of the modified polyimide resin can reach 600 DEG C, and the polymer has excellent oxidation stability.

Description

technical field [0001] The invention belongs to the technical field of resin synthesis, and in particular relates to a synthesis method of a high-temperature-resistant carborane-containing polyimide resin. Background technique [0002] With the development of modern industrial technology, traditional metal materials can no longer meet the application requirements of special types of aviation and aerospace, with high specific strength and specific stiffness, strong designability, good fatigue resistance, corrosion resistance and special electromagnetic properties A class of advanced resin-based composites with high-performance fibers as reinforcements emerged as the times require. The use of advanced resin-based composite materials instead of metal materials such as aluminum alloys can significantly reduce the structural weight. Compared with traditional structural materials such as steel and aluminum alloy, the density of resin-based composite materials is about 1 / 5 of that...

Claims

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Application Information

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IPC IPC(8): C08G73/10
CPCC08G73/1014C08G73/1067
Inventor 邱银冯晨丁鹏飞陈济轮黑艳颖苏会丽
Owner CAPITAL AEROSPACE MACHINERY
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