Process for purifying trichlorosilane and silicon tetrachloride

A technology for purifying trichlorosilane and silicon tetrachloride, applied in halogenated silicon compounds, halogenated silanes, fractional distillation, etc., can solve the problems of insufficient quality, poor product yield, large amounts of frozen water, etc., and achieve stable production control and personnel. The effect of labor intensity reduction, application and benefit improvement

Inactive Publication Date: 2009-09-02
山东齐泉硅业有限公司
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Problems solved by technology

In addition, Chinese patent CN1693192A proposes a purification method and device for separating trichlorosilane in a single tower, but its product contains relatively high content of light components such as boron and phosphorus. Although it can meet the requirements of solar cell grade polysilicon, its quality is still low. It is not enough, and the separation efficiency is low, and the energy consumption is high; Chinese patent CN1010455362A has proposed the technology of double-tower separation of trichlorosilane, but there is the problem of unstable product quality index, and the whole process needs a large amount of chilled water and high energy consumption. Big
[0004] In the production of trichlorosilane, as a side reaction, a certain amount of silicon tetrachloride will inevitably be produced. According to the current production process, there are many other by-products in addition to silicon tetrachloride, so the product four The purity of silicon chloride can only reach 95.0%. Generally, the purity of the trichlorosilane product obtained by this method is acceptable, but the purity of silicon tetrachloride is poor, so it cannot be used in a deeper way.
Silicon tetrachloride of this quality can only be used in lower-grade product applications, and the product yield is poor

Method used

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  • Process for purifying trichlorosilane and silicon tetrachloride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Such as figure 1 As shown, the trichlorosilane liquid raw material enters the middle part of the 1# rectification tower with a pressure of 0.35MPa from the synthetic liquid storage tank with a pressure of 0.50MPa under the action of the pressure difference. 110°C, maintain the set pressure and temperature in the tower; the refrigerant of the condenser is ordinary circulating water, the gas phase at the top of the 1# rectification tower is extracted and refluxed after being condensed by the condenser, and the rest of the high-purity trichlorosilane is stored in Trichlorosilane storage tank; the bottom of the tower is connected to the reboiler, and the temperature in the adjustment tower is maintained by heating part of the liquid phase in the rectification tower; the liquid phase of the 1# rectification tower is produced to contain a small amount of trichlorohydrogen Silicon tetrachloride solution of silicon, the solution enters the middle part of the 2# rectification to...

Embodiment 2

[0024] The trichlorosilane liquid raw material enters the middle part of the 1# rectification tower with a pressure of 0.40MPa from the synthetic liquid storage tank with a pressure of 0.55MPa under the action of pressure difference. The temperature at the top of the tower is 80-85°C and the temperature at the bottom of the tower is 120-130°C Maintain the set pressure and temperature in the tower; the refrigerant in the condenser is ordinary circulating water, the gas phase at the top of the 1# rectification tower is extracted and condensed by the condenser, and part of it is refluxed, and the rest of the high-purity trichlorosilane is stored in trichlorohydrogen Silicon storage tank; the bottom of the tower is connected with the reboiler, and the temperature in the adjustment tower is maintained by heating part of the liquid phase in the rectification tower; the liquid phase of the 1# rectification tower is produced as tetrachloride containing a small amount of trichlorosilane ...

Embodiment 3

[0026]The trichlorosilane liquid raw material enters the middle part of the 1# rectification tower with a pressure of 0.30MPa from the synthetic liquid storage tank with a pressure of 0.60MPa under the action of pressure difference. The temperature at the top of the tower is 60-62°C, and the temperature at the bottom of the tower is 90-105°C Maintain the set pressure and temperature in the tower; the refrigerant in the condenser is ordinary circulating water, the gas phase at the top of the 1# rectification tower is extracted and condensed by the condenser, and part of it is refluxed, and the rest of the high-purity trichlorosilane is stored in trichlorohydrogen Silicon storage tank; the bottom of the tower is connected with the reboiler, and the temperature in the adjustment tower is maintained by heating part of the liquid phase in the rectification tower; the liquid phase of the 1# rectification tower is produced as tetrachloride containing a small amount of trichlorosilane ...

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Abstract

The invention discloses a process for purifying trichlorosilane and silicon tetrachloride. The process purifies the trichlorosilane and the silicon tetrachloride by means of three-tower continuous rectification and comprises: setting two towers as three-tower continuation; by adjusting process conditions, extracting high-purity trichlorosilane at the top of a rectifying tower 1 by gas phase, while extracting a silicon tetrachloride solution containing a small amount of the trichlorosilane by liquid phase, and feeding the solution into a rectifying tower 2; completing gas phase extraction of residual trichlorosilane and a small amount of the silicon tetrachloride at the top of the rectifying tower 2, and returning the extracts to a synthetic fluid intermediate tank after condensation; and feeding the silicon tetrachloride and high-boiling saline obtained through liquid phase extraction in the rectifying tower 2 into a rectifying tower 3; and carrying out purification on the silicon tetrachloride and the high-boiling saline by the rectifying tower 3 to obtain the high-purity silicon tetrachloride at the top of the tower. The process increases the product yield, the quality, the application and benefits, and realizes stable production control and greatly reduces labor intensity.

Description

technical field [0001] The invention relates to a process for purifying trichlorosilane and silicon tetrachloride, in particular to a process for purifying trichlorosilane and silicon tetrachloride by three-tower continuous distillation, which belongs to the field of silicon chemical industry. Background technique [0002] Trichlorosilane and silicon tetrachloride products are mainly used as raw materials for the production of organic silicon and polysilicon. Among them, trichlorosilane is a basic raw material for the production of organic silicon and polysilicon, while silicon tetrachloride is mainly used for the production of organic silicon coupling agent, white carbon black and other products. At present, trichlorosilane is produced by reacting silicon powder and hydrogen chloride in a fluidized bed, and then the synthetic liquid after the reaction enters the rectification tower and is continuously purified through two rectification towers. [0003] Chinese patent CN200...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/107B01D3/14
Inventor 乌洪涛齐峰全孙东兰文忠
Owner 山东齐泉硅业有限公司
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