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Method for preparing dimethyl phenyl ethoxy silane

A technology of dimethylphenylethoxysilane and dimethyldiethoxysilane is applied in the field of preparation of dimethylphenylethoxysilane and can solve environmental pollution, dimethylphenylethoxysilane The problems of low yield of silane and other problems have been overcome, and the effects of overcoming environmental pollution, high content of dimethylphenylethoxysilane, and overcoming the problem of solvent recovery and utilization have been achieved.

Inactive Publication Date: 2014-03-05
佛山市华联有机硅有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of dimethylphenylethoxysilane, aiming at solving the problem of the low yield of dimethylphenylethoxysilane prepared by the existing sodium condensation method, and the use of solvents such as toluene in the preparation process environmental pollution problems

Method used

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  • Method for preparing dimethyl phenyl ethoxy silane
  • Method for preparing dimethyl phenyl ethoxy silane
  • Method for preparing dimethyl phenyl ethoxy silane

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preparation example Construction

[0025] The reaction process of the preparation method of this dimethylphenylethoxysilane is as follows: 1) Add dimethyldiethoxysilane and metal sodium into the reaction kettle, heat up under stirring, and melt the metal sodium in dimethyl dimethoxysilane Form sodium sand in ethoxysilane; 2) Add chlorobenzene dropwise for reaction; 3) Add ethanol dropwise to neutralize excess metallic sodium; 4) Add methylchlorosilane dropwise to neutralize the generated sodium alkoxide; 5) Dilute the reaction mixture Suction filtration under reduced pressure to recover the filtrate; 6) Distill the filtrate under normal pressure and reduced pressure to obtain the target product dimethylphenylethoxysilane. The reaction equation of the above reaction process is shown in formula (1):

[0026] (1)

[0027] The preparation method of this dimethylphenylethoxysilane directly uses dimethyldiethoxysilane, one of the reaction raw materials, as a solvent and a reaction raw material, and disperses met...

Embodiment 1

[0052] Step A00: In a dry 250mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance thermometer, add 87g of dimethyldiethoxysilane, and add 18g of freshly cut sodium flakes under stirring, Raise the temperature to 102°C, beat the sodium flakes into sodium sand;

[0053] Step B00: Add 44g of chlorobenzene dropwise through a constant pressure dropping funnel within 4h, control the reaction temperature between 108~110°C, and continue to react for 2h after the dropwise addition;

[0054] Step C00: After cooling to 25°C, slowly add 1.5g of absolute ethanol to neutralize excess metal sodium within 0.5h, and then maintain at 25°C for 1h after the dropwise addition;

[0055] Step D00: Then, 23.4 mL of dimethyldichlorosilane was added dropwise to the mixture within 1 h to neutralize the generated sodium alkoxide. After the dropwise addition was completed, the reaction was continued at 25° C. for 3 h;

[0056] Step E00: Then the react...

Embodiment 2

[0058] Step A00: In a dry 1000mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistor, add 450g of dimethyldiethoxysilane, and add 58.2g of freshly cut sodium flakes under stirring, Raise the temperature to 105°C, beat the sodium flakes into sodium sand;

[0059] Step B00: Add 142g of chlorobenzene dropwise through a constant pressure dropping funnel within 2h, control the reaction temperature between 102~105°C, and continue to react for 4h after the dropwise addition;

[0060] Step C00: After cooling to 30°C, slowly add 5.1g of absolute ethanol to neutralize excess metal sodium within 1.0h, and then maintain at 30°C for 1.5h after the dropwise addition;

[0061] Step D00: Then, 76 mL of dimethyldichlorosilane was added dropwise to the mixture within 2 hours to neutralize the generated sodium alkoxide; after the dropwise addition, the reaction was continued at 30° C. for 4 hours;

[0062] Step E00: Then, the reaction mixture ...

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Abstract

The invention discloses a method for preparing dimethyl phenyl ethoxy silane. The process comprises the following steps: 1) adding diethoxydimethylsilane and metal sodium into a reaction kettle, and heating while stirring so as to melt the metal sodium in the diethoxydimethylsilane to form sodium sand; 2) dropwise adding chlorobenzene and reacting; 3) dropwise adding ethanol to neutralize the excessive metal sodium; 4) dropwise adding methyl chlorosilane to neutralize the generated sodium alkoxide; 5) carrying out reduced-pressure suction filtering on a reaction mixture and recycling filtrate; and 6) distilling the filtrate at normal pressure and reduced pressure to obtain the target product dimethyl phenyl ethoxy silane. According to the method disclosed by the invention, no additional solvent is needed in the process of a sodium condensation method, the reaction raw material diethoxydimethylsilane is directly used as the solvent to prepare the sodium sand, the reaction conditions are mild, the process is simple, the conversion rate of the raw material chlorobenzene is high, the content of the target product dimethyl phenyl ethoxy silane is high, the product selectivity is good, and the utilization rate of reaction equipment is high.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation method of dimethylphenylethoxysilane. Background technique [0002] The sodium shrinkage method refers to the introduction of functional groups with high refractive index such as phenyl into silicone molecules to increase the refractive index of organic silicon compounds and their derived polymers, improve the optical properties of silicone products, and increase the refractive index of silicone materials. The sodium condensation method is also used in the preparation of dimethylphenylethoxysilane. [0003] The yield of dimethylphenylethoxysilane produced each time through the existing sodium shrinkage process is relatively low. To obtain a large amount of dimethylphenylethoxysilane must be achieved through multiple productions However, multiple productions will inevitably increase production costs and waste manpower and material resources; and most of the existing...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 曹健肖燕平许锋
Owner 佛山市华联有机硅有限公司
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