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Synthesis method of silane coupling agent Si69 and synthesis method of intermediate of silane coupling agent Si69

A technology of silane coupling agent and synthesis method, which is applied in the synthesis of silane coupling agent Si69 and its intermediate, and in the field of synthesis of silane coupling agent Si69 intermediate, which can solve the difficulty of post-processing, high production cost, and reaction time. Long-term problems, to achieve the effect of simple post-processing, low cost, and simple recycling

Pending Publication Date: 2020-12-08
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this synthesis method, the synthesis of intermediate γ2 uses ethanol as the alcoholysis substrate, the reaction time is longer, and hydrogen chloride will be produced as a by-product. Generally, an organic solvent with insoluble hydrogen chloride is used to heat and reflux, or nitrogen gas is passed during the synthesis reaction. Vacuum and the addition of basic compounds as hydrogen chloride absorbents are used to remove hydrogen chloride to promote the positive reaction, but these operations have the disadvantages of cumbersome operation, high production cost, and difficult post-processing.

Method used

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  • Synthesis method of silane coupling agent Si69 and synthesis method of intermediate of silane coupling agent Si69
  • Synthesis method of silane coupling agent Si69 and synthesis method of intermediate of silane coupling agent Si69

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Experimental program
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Effect test

Embodiment 1

[0027] Add 86.52g of γ1 (γ-chloropropyltrichlorosilane, the same below) into a 500mL flask, then add 93.78g of ether and 11.13g of zinc chloride, slowly raise the temperature to 60°C, and react for 3 hours under stirring. The formed ethyl chloride was collected by a condensing device, and zinc chloride was removed by suction filtration after the reaction to obtain 96.27 g of intermediate γ2 (γ-chloropropyltriethoxysilane, the same below). Based on γ1, the yield was 97.9%.

Embodiment 2

[0029] Add 83.57g of γ1 into a 500mL flask, then add 87.66g of ether and 8.06g of zinc chloride, slowly raise the temperature to a system temperature of 30°C, and react for 4 hours under stirring. Afterwards, zinc chloride was removed by suction filtration to obtain 90.14 g of intermediate γ2. Based on γ1, the yield was 94.9%.

Embodiment 3

[0031] Add 90.24g of γ1 into a 500mL flask, then add 100.97g of ether and 14.75g of zinc chloride, slowly raise the temperature to a system temperature of 70°C, and react for 4 hours under stirring. Afterwards, zinc chloride was removed by suction filtration to obtain 98.46 g of intermediate γ2. Based on γ1, the yield was 96.0%.

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Abstract

The invention discloses a synthesis method of a silane coupling agent Si69 and a synthesis method of an intermediate of the silane coupling agent Si69. When the intermediate is synthesized, diethyl ether is used as an alcoholysis substrate to attack gamma-chloropropyl trichlorosilane, and in order to improve the reaction efficiency, zinc chloride is used as a catalyst to promote the forward proceeding of the reaction. Compared with a common synthesis process, the methods of the invention have the advantages that the byproduct chloroethane is low in boiling point, escapes directly in a gas formin a reaction system, and is collected through condensation, so the reaction can be carried out forwards; and the chloroethane has a certain economic value, the intermediate does not need to be subjected to alkali washing, and aftertreatment is simple, green and environment-friendly.

Description

technical field [0001] The invention relates to a synthesis method of a silane coupling agent Si69 intermediate, in particular to a synthesis method of a silane coupling agent Si69 and its intermediate with short reaction time, simple post-treatment process, high economic benefits, and environmental protection, belonging to Organosilicon synthesis technology field. Background technique [0002] As a molecular bridge connecting inorganic materials and organic materials, silane coupling agents are widely used in various fields such as automobiles, aviation, medical treatment, construction, and electronics. For example, in the field of automobile tires, silica can be used as a reinforcing agent and filler for rubber, but due to the large difference in physical and chemical properties between the two, the dispersion of silica in rubber is poor, and the introduction of silane coupling agents is very difficult. It solves the problem of poor dispersion of silica and significantly ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/188C07F7/1892Y02P20/584
Inventor 马松王庆振吴彩英冉升亮潘琳琳苏冉
Owner SHANDONG YANGGU HUATAI CHEM