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A kind of preparation method of liquid organosilicon polymer for high temperature resistant adhesive

A binder and silicone technology, applied in the direction of adhesives, etc., can solve the problems of lowering the use temperature, molecular structure change, low bonding strength, etc., and achieve the effect of reliable source, low surface energy, and good bonding performance

Active Publication Date: 2016-08-10
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 silicone polymers and reduce their use temperature.

Method used

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  • A kind of preparation method of liquid organosilicon polymer for high temperature resistant adhesive
  • A kind of preparation method of liquid organosilicon polymer for high temperature resistant adhesive
  • A kind of preparation method of liquid organosilicon polymer for high temperature resistant adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 46g (2mol) of sodium metal and toluene solvent into a three-necked flask equipped with condensing reflux device and mechanical stirring device, heating to 100℃ under the protection of inert atmosphere, and then adding 115g (1mol) methyldichlorosilane (CH 3 SiHCl 2 ), after the dripping is completed, keep it at 100°C for 6 hours, filter and distill off the organic solvent to obtain liquid polysilane;

[0026] Mix liquid polysilane with 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane at a mass ratio of 1:1, and under the protection of nitrogen, The temperature of the reaction system was raised to 180°C at a temperature rising rate of 3°C / min, mechanically stirred, and kept for 1 hour to obtain a liquid silicone polymer.

[0027] Reference figure 1 , figure 2 : By IR, 1 H-NMR analysis shows that the silicone polymer contains Si-H and Si-CH 3 , Si-O-Si, CH=CH 2 And other chemical bonds, the polymer has excellent high temperature resistance, N 2 At 1200℃, the weight ...

Embodiment 2

[0029] Add 69g (3mol) of sodium metal and toluene solvent into a three-necked flask equipped with condensing reflux device and mechanical stirring device, heat to 90°C under the protection of an inert atmosphere, and then add 115g (1mol) methyldichlorosilane (CH 3 SiHCl 2 ) And 70.5g (0.5mol) CH 3 (CH 2 =CH)SiCl 2 After the dripping is completed, keep it at 90°C for 8h, filter and distill off the organic solvent to obtain liquid polysilane;

[0030] Mix liquid polysilane with 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane at a mass ratio of 2:1, and under the protection of nitrogen, The temperature of the reaction system was raised to 120°C at a heating rate of 2°C / min, mechanically stirred, and kept for 4 hours to obtain a liquid silicone polymer.

[0031] Polymer N obtained in this example 2 The weight loss at 1200°C under the atmosphere is 17.4%, and the weight loss at 1200°C under the air atmosphere is 14.5%.

Embodiment 3

[0033] Add 69g (3mol) of sodium metal and toluene solvent to a three-necked flask equipped with condensing reflux device and mechanical stirring device, and heat to 90°C under the protection of an inert atmosphere, and then add 57.5g (0.5mol) methyldichlorosilane ( CH 3 SiHCl 2 ) And 70.5g (0.5mol) CH 3 (CH 2 =CH)SiCl 2 After the dropping, keep it at 90°C for 6h, filter and distill off the organic solvent to obtain liquid polysilane;

[0034] Mix liquid polysilane and tetramethyldivinyldisilazane in a mass ratio of 1:2. Under the protection of nitrogen, the temperature of the reaction system is raised to 180°C at a heating rate of 1°C / min, and mechanically stirred , After being kept for 4h, a liquid silicone polymer is obtained.

[0035] Polymer N obtained in this example 2 The weight loss at 1200℃ under the atmosphere is 22.4%, and the weight loss at 1200℃ under the air atmosphere is 25.5%.

[0036] Use the product obtained in Example 1 to bond the normal pressure sintered silicon ...

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Abstract

A method for preparing a liquid silicone polymer for a high-temperature-resistant adhesive, comprising the following steps: (1) adding metal sodium and an organic solvent to a three-necked flask equipped with a condensation reflux device and a mechanical stirring device, and under the protection of an inert atmosphere Heat to 60-120°C, then add chlorosilane dropwise. After the dropwise addition, keep warm at 60-120°C for 2-14 hours, filter and distill off the organic solvent to obtain liquid polysilane; Mix liquid polysilane with vinyl siloxane or vinyl silazane, under the protection of nitrogen, raise the temperature of the reaction system to 60-300°C at a heating rate of 0.5-10°C / min, mechanically stir, and keep warm for 1-300°C After 10 h, a liquid silicone polymer was obtained. The liquid organosilicon polymer prepared by the invention is used as a high-temperature-resistant adhesive and has wide application prospects in bonding SiC ceramics, oxide ceramics, carbon materials, and titanium alloy materials.

Description

technical field [0001] The invention relates to a preparation method of a liquid organic silicon polymer for a high-temperature-resistant adhesive. Background technique [0002] At present, the high-temperature-resistant adhesives used mainly include epoxy resins, phenolic resins, polyimides, silicone resins, polybenzimidazoles, polyphenylquinoxalines, and the like. The main chain of epoxy resin and phenolic resin is C-C structure, the bond energy is low, and it is easy to oxidize. The service temperature under air atmosphere generally does not exceed 500 °C; High (260-320°C); polybenzimidazole and polyphenylquinoxaline have high cost of raw materials, complex synthesis process, harsh use conditions (high curing temperature, high pressure, long time), and cannot enter the production field. Silicone resin has the characteristics of both inorganic materials and organic materials. It maintains the same physical and chemical properties in a wide temperature range (-60 ~ 1200 ° ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/42C08G77/62C09J183/10C09J183/16
Inventor 王小宙王军王浩简科
Owner NAT UNIV OF DEFENSE TECH
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