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Fluorine-containing phenyl hydrogen-containing siloxane monomer and preparation method thereof

A technology of fluorophenyldichlorosilane and fluorophenyldialkoxysilane, which is applied in the field of fluorine-containing phenyl hydrogen-containing siloxane monomer and its preparation, and can solve the problems of non-oil resistance and non-containing

Inactive Publication Date: 2013-04-03
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional hydrogen-containing silicone oil does not have oil-proof properties, and most traditional fluorosilicone oils do not contain active silicon-hydrogen bonds

Method used

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  • Fluorine-containing phenyl hydrogen-containing siloxane monomer and preparation method thereof
  • Fluorine-containing phenyl hydrogen-containing siloxane monomer and preparation method thereof
  • Fluorine-containing phenyl hydrogen-containing siloxane monomer and preparation method thereof

Examples

Experimental program
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Effect test

example 1

[0019] Example 1 Synthesis of 3,5-bis(trifluoromethyl)phenyldiethoxysilane

[0020]

[0021] Add 5.00 g of magnesium chips and ether into a four-necked flask equipped with a spherical condenser, a thermometer, and a constant pressure dropping funnel. in N 2 Under protection, stir, heat to 35°C, slowly add 58.60g of a mixture of 3,5-bis(trifluoromethyl)bromobenzene and ether dropwise, and keep the reaction temperature at about 35°C. After the dropwise addition, reflux and stir at 35°C for 4 hours to obtain 3,5-bis(trifluoromethyl)bromophenyl Grignard reagent.

[0022] Add 31.42g diethoxychlorosilane in the four-necked flask equipped with spherical condenser, stirrer, thermometer and constant pressure dropping funnel, 2 Under protection, slowly add the cooled 3,5-bis(trifluoromethyl)bromophenyl Grignard reagent according to the substance ratio of 1:1, continue the reaction for 1 hour after the addition, and raise the temperature to 60°C for 2 Hour. Suction filtration afte...

example 2

[0025] The synthesis of example 2 p-fluorophenyldiethoxysilane

[0026]

[0027] Add 5.00 g of magnesium chips and ether into a four-neck flask equipped with a spherical condenser, a thermometer, and a constant pressure dropping funnel. in N 2 Stir under protection, heat to 35°C, and slowly add 35.00g of a mixture of p-fluorobromobenzene and ether dropwise according to the ratio of the substance to 1:1, and keep the reaction temperature at about 35°C. Reflux and stir at 35°C for 4 hours to obtain p-fluorobromophenyl Grignard reagent.

[0028] Add 31.00g diethoxychlorosilane in a four-necked flask equipped with a spherical condenser, stirrer, thermometer and constant pressure dropping funnel, 2 Under protection, the cooled p-fluorobromophenyl Grignard reagent was slowly added, and the reaction was continued for one hour after the dropwise addition, and then the temperature was raised to 60° C. for 2 hours. Suction filtration after the reaction was completed, and the filtr...

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PUM

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Abstract

The invention discloses a fluorine-containing phenyl hydrogen-containing siloxane monomer and a preparation method thereof. The method comprises the following steps of: reacting dialkoxychlorosilane with a 3,5-bis(trifluoromethyl)phenyl Grignard reagent and a p-fluorophenyl Grignard reagent respectively to obtain 3,5-bis(trifluoromethyl)phenylsilane and p-fluorophenyl dialkoxy silane (wherein the alkoxy R=-OMe, -OEt, -OP(r-i) and the like); or reacting trichlorosilane with a 3,5-bis(trifluoromethyl)phenyl Grignard reagent and a p-fluorophenyl Grignard reagent respectively to obtain 3,5-bis(trifluoromethyl)phenyldichlorosilane and p-fluorophenyl dichlorosilane. A specific experimental process is provided by taking the synthesis from 3,5-bis(trifluoromethyl)phenyldiethyoxysilane and p-fluorophenyl diethyoxysilane for example, and the monomer is subjected to FT-IR and <1>H-NMR representation; and finally, high-temperature-resistant hydrophobic oil-proof characteristic polysiloxane capable of conducting a silicon-hydrogen addition reaction with an unsaturated bond is obtained.

Description

technical field [0001] The invention relates to two novel fluorine-containing phenyl hydrogen-containing organosilicon monomers and a preparation method thereof for preparing organosilicon products such as fluorine-containing phenyl hydrogen-containing polysiloxane. Background technique: [0002] Fluorine-containing phenyl hydrogen-containing silicone oil has excellent hydrophobic and oil-repellent properties because it contains active hydrogen and fluorine elements. It is often used as a surface treatment agent, surface protection agent and curing agent, etc., in the surface protection of airborne devices and aerospace There are a wide range of applications. Traditional hydrogen-containing silicone oils do not have oil-proof properties, and most traditional fluorosilicone oils do not contain active silicon-hydrogen bonds. Therefore, the present invention simultaneously introduces active silicon-hydrogen bonds and fluorine elements with oil-repelling properties into the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/12C08G77/24
Inventor 邹方鑫张爽陈功
Owner BEIHANG UNIV
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