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High temperature resistant phenyl polysiloxane, compound and preparation method of high temperature resistant phenyl polysiloxane

A technology of phenyl polysiloxane and compound, which is applied in its compound and preparation, in the field of high temperature resistant phenyl polysiloxane, which can solve the problems of low bonding strength, low toughness, poor sealing, etc., and reach the curing temperature Low, good adhesion, high toughness effect

Active Publication Date: 2015-07-15
上海庸捷新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing organic high-temperature-resistant composite materials have shortcomings such as low bond strength, high thermal decomposition rate, low toughness, and poor sealing performance under high temperature conditions above 600 ° C, which cannot meet the new requirements of technological development

Method used

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  • High temperature resistant phenyl polysiloxane, compound and preparation method of high temperature resistant phenyl polysiloxane
  • High temperature resistant phenyl polysiloxane, compound and preparation method of high temperature resistant phenyl polysiloxane
  • High temperature resistant phenyl polysiloxane, compound and preparation method of high temperature resistant phenyl polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Preparation of hydrolyzate

[0043] According to the configuration plan, weigh 41.6g of monomethyltrichlorosilane, 27.7g of methylethoxydichlorosilane, 8g of dimethylvinylchlorosilane, 12.6g of monophenyltrichlorosilane, and 9.8g of diphenyldichlorosilane g into a clean container for later use.

[0044] b. Weigh 320g of the hydrolyzing agent into the reaction vessel according to the configuration plan, keep the temperature at 25~30°C, add the above mixed monomers dropwise under stirring, and carry out the hydrolysis reaction. 4h dropwise addition is completed, stand still for 30min, separate the lower layer of acidic water, with 2% NaHCO 3 Neutralize until the pH of the system is 7.0, wash once with water until the system is neutral.

[0045] 2. Rearrangement and condensation reactions

[0046] Distill under reduced pressure, remove the solvent, cool down to room temperature, add 0.15g of catalyst I, raise the temperature to T=125~130°C, react for 2h, continue to ...

Embodiment 2

[0053] 1. Preparation of complexes

[0054] formula

[0055] Component A

[0056]

[0057] Component B

[0058] γ-Aminopropyltriethoxysilane 0.2 parts

[0059] γ-Mercaptopropyltriethoxysilane 0.6 parts

[0060] 0.2 parts of tin acetate

[0061] 2. Operation steps

[0062] a. Put the filler in an oven and bake at 130~140°C for 12 hours.

[0063] b. Sieve the filler through a 100-mesh sieve, weigh the filler and silane coupling agent according to the configuration ratio, mix them evenly in a mixer, put them in an oven, and bake at 90°C for 1 hour.

[0064] c. Weigh the high-temperature-resistant phenyl polysiloxane and the treated filler according to the configuration ratio, put them in a mixer, and mix them evenly.

[0065] d. Raise the temperature to 145~150°C, and remove the low boilers in vacuum.

[0066] c. Cool to room temperature, and refine it three times in a rubber mixer to obtain a high temperature resistant phenyl polysiloxane compound.

[0067] The technic...

Embodiment 3

[0071] 1. Preparation of hydrolyzate

[0072] a. According to the configuration plan, weigh 86.2g of monomethyltrichlorosilane, 51.3g of methylethoxydichlorosilane, 13.2g of dimethylvinylchlorosilane, 26.4g of monophenyltrichlorosilane, diphenyldichlorosilane Add 20 g of chlorosilane into a clean container for later use.

[0073] b. Weigh 788.4 g of the hydrolyzing agent into the reaction vessel according to the configuration plan, keep the temperature at 30° C., add the above-mentioned mixed monomers dropwise while stirring, and carry out the hydrolysis reaction. After 3 hours of dropwise addition, let it stand for 25 minutes, separate the acidic water in the lower layer, neutralize the pH value = 7.0 with 2% NaHCO3, and wash once with water until the system is neutral.

[0074] 2. Rearrangement and condensation reactions

[0075] Distill under reduced pressure, remove the solvent, cool down to room temperature, add 0.37g of catalyst I, raise the temperature to T=120~125°C,...

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Abstract

The invention relates to phenyl polysiloxane, a compound and a preparation method of phenyl polysiloxane, in particular to high temperature resistant phenyl polysiloxane, a compound and a preparation method of high temperature resistant phenyl polysiloxane. The preparation method comprises the steps of mixing a chlorosilane monomer containing phenyl, and one or more out of alkylchlorosilane, alkoxyl chlorosilane, unsaturated alkyl chlorosilane and cyclosiloxane accounting for 70-88% of the total mass, and obtaining phenyl polysiloxane by hydrolysis, condensation, rearrangement, cracking, cyclization and copolymerization, wherein the chlorosilane monomer accounts for 2-22% of the total mass. A mixture mixed by phenyl polysiloxane prepared by the method with filling, a curing agent and an accelerator has the advantages of low curing temperature, as well as good binding property, high toughness and the like under a high temperature condition. Phenyl polysiloxane and the compound of phenyl polysiloxane can be used for bonding, sealing and coating protection of high-temperature-resistant and high-durability spare parts, and special sealing and protection positions with transparency requirements.

Description

[technical field] [0001] The invention relates to phenyl polysiloxane, a compound and a preparation method thereof, in particular to a high-temperature resistant phenyl polysiloxane, a compound and a preparation method thereof. [Background technique] [0002] With the development of modern science and technology, aviation, aerospace, electronics, automobiles, equipment manufacturing and other technical fields have higher and higher requirements for the heat resistance of adhesives, sealing and protective coatings, such as the leading edge of the space shuttle wing, the aerodynamics of the spacecraft, etc. Heating parts, high-speed missile body structure, aircraft engines, aircraft brake discs, thermal protection of chemical equipment and gas welding parts of shipbuilding, etc. In the foreseeable future, the demand for special high-temperature-resistant materials in the national defense security and civilian fields will grow rapidly. [0003] Existing organic high-temperatur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08L83/04C08K3/22C08K3/36C08K5/544C08K5/5435C08K5/5425C08K5/548
Inventor 刘旭军王西民黄新武章基凯
Owner 上海庸捷新材料科技有限公司