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Preparation method of high-purity ethyl silicate, and production system

A technology of ethyl orthosilicate and ethyl orthosilicate, which is applied in the field of preparation of high-purity ethyl orthosilicate, can solve the problems of restricting large-scale application, high risk of chlorine gas, leakage of equipment and pipelines, etc.

Active Publication Date: 2019-05-14
SUZHOU JINHONG GAS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because chlorine gas is extremely dangerous, and it is easy to corrode equipment and pipeline leakage, which restricts its large-scale application

Method used

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  • Preparation method of high-purity ethyl silicate, and production system
  • Preparation method of high-purity ethyl silicate, and production system
  • Preparation method of high-purity ethyl silicate, and production system

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preparation example Construction

[0044] The invention provides a method for preparing high-purity ethyl orthosilicate, comprising: S1) mixing high-purity silicon tetrachloride and high-purity ethanol for reactive distillation to obtain crude ethyl orthosilicate and crude hydrogen chloride; S2) After the crude orthosilicate is subjected to decolorization and adsorption treatment and alkaline adsorption treatment, it is subjected to lightening rectification to obtain light orthosilicate ethyl orthosilicate after lightening and rectification and the light components removed; S3) the obtained The orthosilicate ethyl ester after delightening rectification is treated with borophosphorus adsorption resin and metal ion adsorption resin, and then undergoes deheavy distillation to obtain high-purity ethyl orthosilicate.

[0045] Wherein, the present invention has no special limitation on the sources of all raw materials, which may be commercially available or self-made.

[0046] In the present invention, the high-purit...

Embodiment 1

[0115] The material (mainly ethanol, with a small amount of tetraethyl orthosilicate and trimethylchlorosilane azeotroped with silicon tetrachloride) obtained by purchasing industrial ethanol and delightening rectification tower T05 overhead condenser E10 is condensed Trimethylethoxysilane, methyltriethoxysilane and other impurities) enter the ethanol raw material storage tank V01, ethyl orthosilicate, trimethylethoxysilane, methyltriethoxysilane, etc. The water in the ethanol reacts to form silicon dioxide and ethanol, so as to remove the water in the ethanol raw material. The ethanol raw material storage tank V01 removes solid impurities such as silicon dioxide through the bag filter F01, and then removes solid impurities such as silicon dioxide from the ethanol through the ethanol feeding pump P01. The middle and upper part of the light distillation tower T01 is fed to the upper part of the tower, and the rectification is carried out at atmospheric pressure. The rectificatio...

Embodiment 2

[0127] The material (mainly ethanol, with a small amount of tetraethyl orthosilicate and trimethylchlorosilane azeotroped with silicon tetrachloride) obtained by purchasing industrial ethanol and delightening rectification tower T05 overhead condenser E10 is condensed Trimethylethoxysilane, methyltriethoxysilane and other impurities) enter the ethanol raw material storage tank V01, ethyl orthosilicate, trimethylethoxysilane, methyltriethoxysilane, etc. The water in the ethanol reacts to form silicon dioxide and ethanol, so as to remove the water in the ethanol raw material. The ethanol raw material storage tank V01 removes solid impurities such as silicon dioxide through the bag filter F01, and then removes solid impurities such as silicon dioxide from the ethanol through the ethanol feeding pump P01. The middle and upper part of the light distillation column T01 is fed to carry out rectification at atmospheric pressure, the rectification temperature is preferably 77°C to 79°C,...

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Abstract

The invention provides a preparation method of high-purity ethyl silicate. The preparation method comprises the following steps: S1), mixing high-purity silicon tetrachloride and high-purity ethanol to perform reaction rectification to obtain crude tetraethoxysilane and crude hydrogen chloride; S2) performing decoloring adsorption treatment on the crude tetraethoxysilane, and performing light-removal rectification treatment after performing alkaline adsorption treatment, thereby obtaining light-removed tetraethoxysilane and removed light components; S3) performing weight-removal rectificationtreatment on the light-removed tetraethoxysilane through the boron phosphorus adsorption resin and metal ion adsorptive resin treatment, thereby obtaining the high-purity tetraethoxysilane. Compared with the prior art, the high-purity silicon tetrachloride and high-purity ethanol as used as raw materials, the moisture content in the reaction system is less, side reactions, especially the polymerization of the tetraethoxysilane, are reduced, the production of the ethyl silicate polymer can be reduced, the pressure of the purification treatment is relieved, and the yield of the high-purity tetraethoxysilane is improved.

Description

technical field [0001] The invention belongs to the technical field of semiconductors, and in particular relates to a preparation method and a production system of high-purity ethyl orthosilicate. Background technique [0002] SiO 2 It is a natural oxide film, which has very important uses in semiconductor technology, such as masking impurities, gate oxide dielectric, surface passivation and protection, device isolation, and metal conductive interlayer insulating dielectric. Semiconductor process forms SiO 2 The methods of oxide layer mainly include thermal oxidation (for semiconductor materials that can form their own stable oxide layer), low pressure chemical vapor deposition (LPCVD), plasma enhanced chemical vapor deposition (PECVD) and atmospheric pressure chemical vapor deposition (APCVD), etc. , because of the large gas flow required by APCVD and the relatively large number of particles produced by the process, most semiconductor processes are rarely used at present....

Claims

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Application Information

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IPC IPC(8): C07F7/04C01B7/07C01B7/03
CPCY02P20/10
Inventor 金向华王新喜栗鹏伟刘晶齐相前师东升夏致远
Owner SUZHOU JINHONG GAS CO LTD
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