Method for preparing high-temperature resisting organic adhesive by utilizing liquid silicon carbide precursor

A technology of silicon carbide and high temperature resistance, applied in the direction of adhesives, etc., can solve the problems of polysiloxane molecular structure change, lower use temperature, low bonding strength, etc., and achieve low surface energy, reliable source, and good bonding performance Effect

Inactive Publication Date: 2012-06-20
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inherent low bonding strength and high curing temperature of silicone resin limit its application range.
In addition, in a high-temperature oxidizing atmosphere, silicone resins are prone to degradation reactions, which cause changes in the molecular structure of polysiloxane and reduce its use temperature.

Method used

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  • Method for preparing high-temperature resisting organic adhesive by utilizing liquid silicon carbide precursor
  • Method for preparing high-temperature resisting organic adhesive by utilizing liquid silicon carbide precursor
  • Method for preparing high-temperature resisting organic adhesive by utilizing liquid silicon carbide precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] To a 250ml three-necked flask equipped with condensation reflux and mechanical stirring, add 20g of liquid polymethylsilane (self-made), 20ml of toluene, and 5g of tetramethyltetravinylcyclotetrasiloxane, heated to 180°C for reaction for 5h, and then cooled to 150 ℃, under reduced pressure distillation for 0.5h to remove the solvent and small molecules to obtain a light yellow viscous liquid, the entire reaction process is under nitrogen protection.

[0022] see figure 1 and figure 2 : by IR, 1 H-NMR analysis showed that the polymer contained Si-H, Si-OH, Si-CH 3 , Si-O-Si, CH=CH 2 chemical bonds. The polymer has excellent high temperature resistance, N 2 The weight loss at 1200 ℃ in the atmosphere is only 18.8%, and the weight loss at 1200 ℃ in the air atmosphere is only 8.6%.

Embodiment 2

[0024] Add 20g liquid polycarbosilane, 20ml tetrahydrofuran, 20g tetramethyltetraenyl cyclotetrasiloxane to the 250ml three-necked flask equipped with condensation reflux and mechanical stirring, add 1.7ppm of platinum-containing catalyst, heat to 100 ° C with mechanical stirring After 1.5h, the temperature was lowered to 80°C, and the solution was distilled under reduced pressure for 0.25h to remove the solvent and small molecules, and a pale yellow viscous liquid was obtained. The whole reaction process was under nitrogen protection. The resulting polymer N 2 The weight loss at 1200 ℃ in the atmosphere is 20.4%, and the weight loss at 1200 ℃ in the air atmosphere is 14.5%.

Embodiment 3

[0026] Into a 250ml three-necked flask equipped with condensation reflux and mechanical stirring, add 20g of liquid polysilane, 10g of tetramethyltetravinylcyclotetrasiloxane, add 2.1ppm of chloroplatinic acid, heat to 150°C and mechanically stir for 1.5h, then The temperature was lowered to 80° C., and distilled under reduced pressure for 0.25 h to remove small molecules to obtain a white viscous liquid. The whole reaction process was under nitrogen protection. The resulting polymer N 2 The weight loss at 1200 ℃ in the atmosphere is 21.5%, and the weight loss at 1200 ℃ in the air atmosphere is 17.6%.

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PUM

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Abstract

The invention relates to a method for preparing a high-temperature resisting organic adhesive by utilizing a liquid silicon carbide precursor. The method comprises the following steps: taking the liquid silicon carbide precursor (liquid polysilane, polymethylsilane and liquid polycarbosilane) and low-molecule siloxane containing an ethylene group as original raw materials, taking methylbenzene or tetrahydrofuran as a solvent and taking chloroplatinic acid as a catalyst; after mixing at a certain ratio, increasing the temperature to 20-300 DEG C; keeping the temperature for a period of time; cooling the temperature to a certain temperature and then performing pressure-reducing distillation; and cooling to the room temperature, thereby obtaining the high-temperature resisting organic adhesive, namely, the poly-carbon siloxane. The raw materials are simply and easily obtained; the resource is reliable; the reaction process is simple; the obtained products have excellent high-temperature resistance; the adhesive contains a plenty of active Si-H, Si-OH, Si-Si and CH-CH2 groups, so that the adhesive can be easily cross-linked and cured; the surface energy is lower; the adhesive can be easily paved and wetted on the surface of objects, such as ceramics, metal, and the like; the adhering property is better; and the adhesive has wide application prospect in adhering SiC ceramic materials, oxide ceramics, carbon materials and titanium alloy materials.

Description

technical field [0001] The invention relates to a method for preparing high temperature resistant organic adhesive polycarbosiloxane from liquid silicon carbide precursor. Background technique [0002] At present, the main high temperature resistant organic adhesives are epoxy resin, phenolic resin, polyimide, silicone resin, polybenzimidazole, polyphenylquinoxaline, etc. The main chain of epoxy resin and phenolic resin is C-C structure, the bond energy is low, easy to be oxidized, and the operating temperature in air atmosphere is generally not more than 500 ℃; polyimide has high rigidity, poor toughness of cured product, high melting point, and high curing temperature. High (260-320℃); polybenzimidazole and polyphenylquinoxaline raw materials have high cost, complex synthesis process, harsh use conditions (high curing temperature, high pressure, long time), and cannot enter the production field. The silicone resin has the characteristics of both inorganic and organic mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/00C09J183/00C04B37/00
Inventor 王军王小宙王浩谢征芳
Owner NAT UNIV OF DEFENSE TECH
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