Method for deep removal of chlorine in tetraethyl orthosilicate

A tetraethyl orthosilicate, deep technology, applied in the direction of silicon organic compounds, can solve the problem of high chlorine content in tetraethyl orthosilicate, and achieve the effect of low cost, strong operability and simple process

Active Publication Date: 2019-11-26
SUZHOU JINHONG GAS CO LTD
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Problems solved by technology

[0005] In view of this, the application provides a method for deeply removing chlorine in tetraethyl orthosilicate. The method for purifying the crude product of t

Method used

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  • Method for deep removal of chlorine in tetraethyl orthosilicate

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Embodiment 1

[0046] Orthoethyl silicate crude product (chlorine 461ppb, water 125ppm) enters reaction kettle R01 from TEOS raw material tank V01 through feed delivery pump P01, and sodium ethylate solution (17% ethanol solution of sodium ethylate) enters from sodium ethylate solution tank V02 The material delivery pump P02 enters the reactor R01; the mass ratio of sodium ethoxide to TEOS crude product is 0.05%; in the reactor, first react at 45°C for 0.5 hours, and gradually raise the temperature to 120°C after the first step of reaction, and continue to react for 2 hours; The pressure in the reactor was maintained at 0.15 MPa, and 6N nitrogen was used to protect and control the pressure.

[0047] After the reaction, the material is discharged through the reactor discharge pump P03, and the reacted material is filtered through the filter F01 with a pore size of 0.5 μm to remove the formed particles such as sodium chloride, and the liquid phase enters the intermediate tank V03. The material...

Embodiment 2

[0050] Orthoethyl silicate crude product (chlorine 384ppb, water 118ppm) enters reactor R01 from TEOS raw material tank V01 through feed delivery pump P01, and sodium ethylate solution (18% ethanol solution of sodium ethylate) enters from sodium ethylate solution tank V02. The material delivery pump P02 enters the reactor R01; the mass ratio of sodium ethoxide to crude TEOS is 0.08%; in the reactor, first react at 50°C for 0.5 hours, and gradually raise the temperature to 110°C after the first step of reaction, and continue to react for 2 hours; The pressure in the reactor was maintained at 0.1 MPa, and 6N nitrogen was used to protect and control the pressure.

[0051] After the reaction, the material is discharged through the reactor discharge pump P03, and the reacted material is filtered through the filter F01 with a pore size of 0.5 μm to remove the formed particles such as sodium chloride, and the liquid phase enters the intermediate tank V03. The material in the intermed...

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Abstract

The invention provides a method for deep removal of chlorine in tetraethyl orthosilicate. The method includes the steps of: mixing a tetraethyl orthosilicate crude product with a sodium ethoxide-ethanol solution, firstly carrying out reaction under the condition of a temperature not exceeding 60DEG C, then performing heating to 80DEG C-140DEG C for further reaction to obtain a reacted material; filtering the reacted material to obtain a liquid phase, and rectifying the liquid phase to remove light component and heavy component so as to obtain a tetraethyl orthosilicate product. The method provided by the inventioneffectively solves the problem of too high chlorine content in tetraethyl orthosilicate, can achieve deep removal of both free chlorine ions and organochlorine, and reduce the chlorine content in tetraethyl orthosilicate to 50ppb or below; and at the same time of chlorine removal, trace water in tetraethyl orthosilicate can be removed, the water content can reach 5ppm or below, thus being beneficial to subsequent application. The method provided by the invention has the characteristics of simple and stable process, low cost and strong operability.

Description

technical field [0001] The invention belongs to the technical field of ethyl orthosilicate purification, in particular to a method for deeply removing chlorine in ethyl orthosilicate. Background technique [0002] Orthoethyl silicate (TEOS) is a colorless liquid, mainly used as heat-resistant coatings, chemical-resistant coatings, silane coupling agents, organic synthesis intermediates, and chemical vapor deposition (CVD) SiO in the semiconductor field. 2 Thin film precursors, etc. The melting point of ethyl orthosilicate is -77°C, the boiling point is 165.5°C, slightly soluble in water, soluble in ethanol and ether. The synthesis method of ethyl orthosilicate basically includes two kinds of silicon tetrachloride method and silicon powder method. The reaction between silicon powder and ethanol in a chlorine-containing catalytic system is used to obtain ethyl orthosilicate and by-product hydrogen. These two process systems contain chlorine-containing compounds, so that the...

Claims

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Application Information

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IPC IPC(8): C07F7/04
Inventor 金向华栗鹏伟齐相前钱钦孙猛王新喜
Owner SUZHOU JINHONG GAS CO LTD
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