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Reactive distillation purifying method and device for removing carbon-containing impurities in chlorosilane

A technology of reactive distillation and reactive distillation tower, which is applied in the field of reactive distillation purification and equipment for removing carbon-containing impurities in chlorosilane, can solve the problems that methyldichlorosilane cannot be removed, and has not been raised, so as to achieve thorough removal, Less equipment investment, high purity effect

Inactive Publication Date: 2020-04-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent is a method for preparing silane, the process is also to convert methyldichlorosilane into methyltrichlorosilane, so it has certain reference
[0005] Cao Lingling and others analyzed the source, separation and purification, transformation and distribution of carbon elements in each production process of polysilicon in the influencing factors and control measures of carbon mass fraction in polysilicon products, and controlled the production of chlorosilane by optimizing the purification process parameters and other measures. The content of methyldichlorosilane in the polycrystalline silicon can control the carbon mass fraction in the product polysilicon, but this method only reduces the content of carbon-containing impurities as much as possible through the optimization of process conditions, and cannot completely remove methyldichlorosilane
[0006] The method described above does not propose a perfect process and device for removing carbon-containing impurities in chlorosilane. The present invention proposes a method for preparing chlorosilane by reactive distillation. In this method, catalytic reaction and rectification are combined. The reaction and rectification are carried out simultaneously and promote each other. On the one hand, rectification enriches the reactants to improve the reaction efficiency. On the other hand, combining the two parts into one part can save investment costs.

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  • Reactive distillation purifying method and device for removing carbon-containing impurities in chlorosilane

Examples

Experimental program
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Effect test

example 1

[0035] The chlorosilane raw material enters the reactive distillation column from the top to the middle of the second and third fillers in the rectification section, and dichloromethane enters the reactive distillation column from the middle of the rectification section and the reaction section, and the rectification section is filled with three Sectional wire mesh corrugated packing, 5m per section; 6m of wire mesh corrugated packing is filled in the stripping section; 1m of wire mesh corrugated packing and 1m of structural catalyst are alternately filled in the reaction section of the tower from bottom to top, a total of 4 sections of 8m, and the catalyst is 1 % nickel-supported alumina catalyst, the temperature at the top of the tower is controlled between 30°C and 35°C, and the cooling medium of the condenser is 10°C circulating water. The operating pressure of the reactive distillation tower is controlled at 70Kpa, the temperature of the tower tank is about 80°C, the tempe...

example 2

[0037] The chlorosilane raw material enters the reactive distillation column from the top to the bottom of the middle of the second and third fillers in the rectification section, and chloroform enters the reactive distillation column from the middle of the rectification section and the reaction section, and the rectification section is filled with three Sectional orifice corrugated packing, 5m per section; 6m of orifice corrugated packing is filled in the stripping section, 1m of wire mesh corrugated packing and 1m of structural catalyst are alternately filled in the reaction section of the tower from bottom to top, a total of 5 sections of 10m, and the catalyst is 1 % iron-loaded molecular sieve catalyst, the temperature at the top of the tower is controlled between 30°C and 35°C, and the cooling medium of the condenser is 10°C circulating water. The operating pressure of the reactive distillation tower is controlled at 150Kpa, the temperature of the tower bottom is about 90°...

example 3

[0039] The chlorosilane raw material enters the reactive distillation tower from the middle of the second and third fillers from top to bottom in the rectification section, and silicon tetrachloride enters the reactive distillation tower from the middle of the rectification section and the reaction section, and the filling in the rectification section Three sections of grid packing, 4m in each section; 6m of wire mesh corrugated packing in the stripping section; 1m of wire mesh corrugated packing and 1m of structural catalyst alternately filled in the reaction section of the tower from bottom to top, a total of 4 sections of 8m, the catalyst is 1 % copper-loaded artificial zeolite catalyst, the temperature at the top of the tower is controlled between 45°C and 50°C, and the cooling medium of the condenser is circulating water at 10°C. The operating pressure of the reactive distillation tower is controlled at 200Kpa, the temperature of the tower bottom is about 100°C, the temper...

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Abstract

The intention provides a reactive distillation purifying method and device for removing carbon-containing impurities in chlorosilane, and belongs to the technical field of polycrystalline silicon production, wherein the reactive distillation tower device comprises a distillation section, a reaction section and a stripping section, the distillation section is filled with three sections of packing,the stripping section is filled with the packing, and the packing in the distillation section and the stripping section is structured packing; wherein a structural catalyst is arranged in the reactionsection, the stripping section is provided with a chlorine donor substance circulating device, a chlorosilane crude material is fed from the middle lower part of the distillation section, a chlorinedonor substance is fed from the upper part of the reaction section, and carbon-containing impurity methyl dichlorosilane in the chlorosilane crude material in the reaction section reacts with the chlorine donor under the action of the catalyst to generate high-boiling-point substance methyl trichlorosilane; the methyl trichlorosilane is finally extracted from the bottom of the tower, and high-purity chlorosilane is extracted from the side line of the middle upper part of the distillation section. The method solves the problem that the carbon-containing impurities in the chlorosilane are difficult to remove thoroughly under the existing process conditions, is simple to operate and low in investment cost, and the purity of the product chlorosilane can reach 99.999%.

Description

technical field [0001] The invention relates to a reactive distillation purification method and device for removing carbon-containing impurities in chlorosilane, a raw material for polysilicon production. Aiming at the trichlorosilane product in the conventional chlorosilane distillation process, the reactive distillation method is used to remove carbon-containing impurities, thereby obtaining High-purity chlorosilane. Background technique [0002] Polysilicon is one of the best materials for photoelectric conversion, and it is also the main material required by the electronics industry. Its demand increases rapidly with the development of photovoltaic industry and electronic information industry. It has a significant impact on the mechanical properties, especially the carbon-containing impurities, which have a significant impact on the photoelectric conversion efficiency of silicon materials or the electrical properties of electronic components. Trace amounts of carbon in ...

Claims

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Application Information

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IPC IPC(8): C01B33/107C07F7/12
CPCC01B33/10778C07F7/123Y02P20/10
Inventor 黄国强张明鑫
Owner TIANJIN UNIV
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