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Catalyst for producing ethyl orthosilicate by silicon powder method and preparation method thereof

A technology of tetraethyl orthosilicate and catalyst, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve problems such as difficult recovery and regeneration, speed up the reaction speed of silicon and ethanol, and achieve stable properties , solve the effect of easy loss and high catalytic efficiency

Inactive Publication Date: 2012-06-13
KUNMING METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention improves the existing homogeneous catalyzed silicon powder method, and proposes a novel catalyst for producing tetraethyl orthosilicate by the silicon powder method and its preparation method, which overcomes the problem that the catalyst used in the silicon powder method is difficult to recycle and regenerate problem, can greatly accelerate the reaction rate of silicon and ethanol, and can be recycled as a catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 2.5g of cuprous oxide, 2.5g of copper oxide and 4.0g of copper powder and mix evenly; prepare 100g of titanium isopropoxide alcohol solution with a concentration of 5%; add the prepared catalyst active material into the alcohol solution of titanium isopropoxide After stirring for 2 hours, add a small amount of distilled water dropwise, continue stirring for 8 hours and then filter to obtain a filter residue, dry the filter residue at 80°C, and roast at 450°C for 9 hours without air to obtain a catalyst.

[0021] The evaluation experiment of the catalyst was carried out in a high-pressure reactor, and the mass ratio of the catalyst, silicon powder and ethanol was 1:10:80. Weigh silicon powder, ethanol and catalyzer, join in the autoclave, after closing the autoclave, open the inlet valve and the exhaust valve and start to charge nitrogen; close the exhaust valve after 5 minutes, and then charge nitrogen, when the pressure After reaching 1.5MPa, close the intake val...

Embodiment 2

[0023] Weigh 3.0g of cuprous oxide, 3.0g of cupric oxide and 3.0g of copper powder and mix evenly; configure 100g of aluminum isopropoxide alcohol solution with a concentration of 15%; add the prepared catalyst active material into the alcohol solution of aluminum isopropoxide After stirring for 2 hours, add a small amount of distilled water dropwise, continue stirring for 12 hours and then filter to obtain a filter residue, dry the filter residue at 100°C, and roast at 550°C for 12 hours without air to obtain a catalyst.

[0024] The evaluation experiment of the catalyst was carried out in a high-pressure reactor, and the mass ratio of the catalyst, silicon powder and ethanol was 1:10:80. Weigh silicon powder, ethanol and catalyzer, join in the autoclave, after closing the autoclave, open the inlet valve and the exhaust valve and start to charge nitrogen; close the exhaust valve after 5 minutes, and then charge nitrogen, when the pressure After reaching 1.5MPa, close the inta...

Embodiment 3

[0026] Weigh 4.0g of cuprous oxide, 3.0g of cupric oxide and 3.0g of copper powder and mix evenly; configure 100g of tetraethyl orthosilicate alcohol solution with a concentration of 20%; add the prepared catalyst active material into the alcohol of tetraethyl orthosilicate In the solution, after stirring for 2 hours, add a small amount of distilled water dropwise, continue to stir for 16 hours, then filter to obtain the filter residue, dry the filter residue at 120°C, and roast at 420°C for 16 hours without air to obtain the catalyst.

[0027] The evaluation experiment of the catalyst was carried out in a high-pressure reactor, and the mass ratio of the catalyst, silicon powder and ethanol was 1:10:80. Weigh silicon powder, ethanol and catalyzer, join in the autoclave, after closing the autoclave, open the inlet valve and the exhaust valve and start to charge nitrogen; close the exhaust valve after 5 minutes, and then charge nitrogen, when the pressure After reaching 1.5MPa, ...

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Abstract

The invention relates to a catalyst for producing ethyl orthosilicate by a silicon powder method and a preparation method thereof. The catalyst comprises the following components in percentage by weight: 20%-50% of cuprous oxide, 10%-40% of copper oxide, 10%-40% of copper powder and 10%-30% of catalyst carrier. The preparation method comprises the following steps of: uniformly mixing the active components such as cuprous oxide, copper oxide and copper powder according to the composition of the catalyst; preparing a 30-40% alcohol or aqueous solution of the catalyst carrier; and adding the mixed active components in the alcohol solution of the catalyst carrier, stirring for 1-2 hours, then dripping a small amount of distilled water, continuously stirring for 1-24 hours, and then filtering,thus obtaining filter residue; and drying the filter residue at the temperature of 70-120 DEG C, and roasting for 8-24 hours with air isolation at the temperature of 400-700 DEG C, thus obtaining thecatalyst. The catalyst has the characteristics of high activity and stability, long service life and capability of being utilized repeatedly for multiple times.

Description

technical field [0001] The invention proposes a novel catalyst used in the production of ethyl orthosilicate by a silicon powder method and a preparation method thereof. Background technique [0002] Ethyl orthosilicate is an important chemical product, mainly used in the synthesis of organic silicon intermediates, crosslinking agents for room temperature vulcanized silicone rubber, chemical-resistant coatings, heat-resistant coatings, and fire-resistant adhesives and precision casting etc. Phosphor powder can be produced from very fine silicon oxide powder produced after complete hydrolysis of tetraethyl orthosilicate. There are many ways to prepare tetraethyl orthosilicate, but so far there are only two routes for real industrialization, namely silicon tetrachloride method and silicon powder method. Most manufacturers in my country use the silicon tetrachloride method, that is, the reaction of ethanol and silicon tetrachloride to prepare ethyl silicate. The process is c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J37/04C07F7/04
Inventor 翟忠标李永佳包崇军陈加希和晓才李怀仁杨大锦刘俊场徐庆鑫陈家辉
Owner KUNMING METALLURGY INST
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