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Preparation method for dimethoxymethylphenylsilane

A technology of methylphenyldimethoxysilane and methyltrimethylmethoxysilane, which is applied in the field of preparation of methylphenyldimethoxysilane, can solve problems such as environmental pollution, and achieve easy separation and purification, simple process and excellent reaction conditions mild effect

Active Publication Date: 2015-05-13
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to: provide a mild reaction condition, simple process, suitable for large-scale industrial production, to solve the separation of impurities and the use of a large amount of solvents when the existing sodium condensation method is used to synthesize methylphenyldimethoxysilane Preparation method of methylphenyldimethoxysilane facing environmental pollution problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a dry 1000ml four-neck flask equipped with a reflux condenser, a mechanical stirrer, and an oil bath temperature control, add 350g of methyltrimethyl oligomer, add 34.5g of metal sodium wire under stirring, and heat up to 98°C to dissolve the metal sodium wire Beat into sodium sand.

[0020] Within 5 hours, a mixture of 102.5 g of methyl trimethyl and 84.5 g of chlorobenzene was added dropwise into the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled at 125° C. After the dropwise addition, the aging reaction was continued for 3 h.

[0021] After cooling to 63°C, slowly add 2.4g of anhydrous methanol within 0.2h to neutralize unreacted metallic sodium, and then continue to react at 63°C for 2h after the dropwise addition.

[0022] When cooled to 25°C, 41g of methyltrichlorosilane was added dropwise to the reaction system within 0.5h to neutralize the sodium alkoxide generated by the reaction. After the dropwise ...

Embodiment 2

[0025] In a dry 1000ml four-necked flask equipped with a reflux condenser, a mechanical stirrer and an oil bath temperature control, add 350g of methyl trimethyl oligomer, add 34.5g of metal sodium wire under stirring, and heat up to 102°C to dissolve the metal sodium wire Beat into sodium sand.

[0026] Within 3 hours, a mixture of 102.5 g of methyl trimethyl and 84.5 g of chlorobenzene was added dropwise into the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled at 120° C. After the dropwise addition, the reaction was continued for 15 h.

[0027] After cooling to 62°C, add 2.4g of anhydrous methanol slowly within 0.5h to neutralize the unreacted metal sodium, and then continue the reaction at 62°C for 3h after the dropwise addition is completed.

[0028] When cooled to 25°C, 41g of methyltrichlorosilane was added dropwise to the reaction system within 0.3h to neutralize the sodium alkoxide generated by the reaction. ...

Embodiment 3

[0031] In a dry 1000ml four-necked flask equipped with a reflux condenser, a mechanical stirrer and an oil bath temperature control, add 350g of methyl trimethyl oligomer, add 34.5g of metal sodium wire under stirring, and heat up to 100°C to dissolve the metal sodium wire Beat into sodium sand.

[0032] Within 4 hours, a mixture of 102.5 g of methyl trimethyl and 92.5 g of chlorobenzene was added dropwise to the reaction system through a constant pressure dropping funnel, and the reaction temperature was controlled at 120° C. After the dropwise addition, the reaction was continued for 8 h.

[0033] After cooling to 61°C, slowly add 2.4g of anhydrous methanol within 0.2h to neutralize unreacted metal sodium, and then continue to react at 61°C for 4h after the dropwise addition.

[0034] When cooled to 25°C, 41g of methyltrichlorosilane was added dropwise to the reaction system within 0.2h to neutralize the sodium alkoxide generated by the reaction. After the dropwise addit...

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PUM

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Abstract

The invention relates to a preparation method for dimethoxymethylphenylsilane and belongs to the field of silicon chemistry. The method is used for preparing dimethoxymethylphenylsilane through a sodium reductive coupling process by taking a methyltrimethoxysilane oligomer as a solvent and taking methyltrimethoxysilane, sodium and chlorobenzene as raw materials. Problems of impurity separation and environmental pollution caused by use of a large amount of solvents in an existing process for synthesizing dimethoxymethylphenylsilane by utilizing the sodium reductive coupling process are solved; the preparation method for dimethoxymethylphenylsilane does not use the solvent such as methylbenzene and is mild in reaction condition, simple in process and very suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to a preparation method of methylphenyldimethoxysilane, which belongs to the field of organic silicon chemistry. Background technique [0002] Methylphenyldimethoxysilane is an important synthetic monomer. It is relatively active and can be used to synthesize organosilicon intermediates, silicone oil, silicone rubber and other polymer compounds because of its high molar refractive index. , can be used to increase the refractive index of organic silicon materials, and plays an important role in the fields of LED packaging, optical waveguide devices, optical interconnect devices, and optical lenses. [0003] The sodium condensation method is a classic method for constructing organosilicon compounds at present, that is, the use of sodium condensation method can introduce functional groups with high refractive index such as phenyl into the organosilicon molecules, and improve the refractive index of organosilicon compounds and their d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 刘宇甘俊黄怡萍刘明锋王灿陈圣云甘书官
Owner JINGZHOU JIANGHAN FINE CHEM