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Clapboard adsorption device and method for removing boron impurities in chlorosilane system

An adsorption device, chlorosilane technology, applied in halosilanes, halogenated silicon compounds, fractionation and other directions, to achieve the effect of reducing energy consumption, simplifying process flow, reducing energy consumption and equipment costs

Active Publication Date: 2013-02-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problem of how to effectively remove boron impurities currently faced by the domestic polysilicon industry, the present invention proposes a process and a device for removing boron impurity compounds in chlorosilanes with a partition adsorption rectification device, with the purpose of obtaining polysilicon with relatively high purity. Reduce energy consumption and equipment investment while producing chlorohydrogen silicon products

Method used

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  • Clapboard adsorption device and method for removing boron impurities in chlorosilane system

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] The chlorosilane system contains 95.0% trichlorosilane, 2.0% silicon tetrachloride, 2.0% dichlorodihydrosilane and 1.0% boron trichloride. The throughput of raw material is 378.8kg / hr, which translates to a molar flow rate of 2.8Kmol / hr. The tower adsorption section adopts ion exchange resin adsorbent with high adsorption capacity. The main tower adopts metal mesh corrugated packing.

[0023] The pressure at the top of the tower is 300Kpa, the temperature at the top of the tower is 49.2°C, the thermal condition of the feed is 30.0°C, and the bubble point feed is fed. The heat load is 0.0120M*kcal / hr, the reboiler heat load is 0.0154M*kcal / hr, the number of theoretical plates in the public rectification section is 19, the number of theoretical plates in the public stripping section is 9, the number of theoretical plates in the tower adsorption section is 10, and the side line The number of theoretical plates in the production section is 20, and the reflux ratio is 35. ...

example 2

[0026] Contain 98% trichlorosilane in the chlorosilane system, 0.8% silicon tetrachloride, 0.7% dichlorodihydrosilane, 0.5% boron trichloride, the processing capacity of raw material is 379.1kg / hr, is converted into The molar flow rate is 2.8 Kmol / hr. The tower adsorption section adopts zeolite molecular sieve adsorbent.

[0027] The pressure at the top of the tower is 400Kpa, the temperature at the top of the tower is 70.8°C, and the thermal condition of the feed is 30.0°C. The heat load of the reboiler is 0.0153M*kcal / hr, and the heat load of the reboiler is 0.0199M*kcal / hr. The number of theoretical plates in the section is 20, and the reflux ratio is 45.

[0028] The yield of trichlorosilane is 72.1%, the purity of trichlorosilane is 99.1%, the content of B is 0.11%, and the removal efficiency of B is 84.0%. And use two towers to remove light and heavy to simulate when reaching trichlorosilane purity 99.1% and when the removal efficiency of B is 84.0%, trichlorosilane y...

example 3

[0030] The chlorosilane system contains 95.0% trichlorosilane, 2.0% silicon tetrachloride, 2.0% dichlorodihydrosilane and 1.0% boron trichloride. The throughput of raw material is 378.8kg / hr, which translates to a molar flow rate of 2.8Kmol / hr. The tower adsorption section uses silica gel as the adsorbent.

[0031] The pressure at the top of the tower is 500Kpa, the temperature at the top of the tower is 65.3°C, and the thermal condition of the feed is 30.0°C. The heat load of the reboiler is 0.0143M*kcal / hr, and the heat load of the reboiler is 0.0197M*kcal / hr. The number of theoretical plates in the section is 20, and the reflux ratio is 45.

[0032] The yield of trichlorosilane is 73.0%, the purity of trichlorosilane is 97.6%, the B content is 0.25%, and the removal efficiency of B is 82.0%. And when using two towers to remove light and heavy to simulate, when reaching the removal efficiency of trichlorosilane purity 97.6% and B is 82.0%, the yield of trichlorosilane is ...

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Abstract

The invention relates to a clapboard adsorption device and method for removing boron impurities in a chlorosilane system. The device is divided into four areas by a clapboard which has the same height as a tower type adsorption section and is placed in the middle of the tower: a public rectifying section (1), a tower type adsorption section (2), a side withdrawing section (3) and a public stripping section (4), wherein an adsorbent is filled in the tower type adsorption section (2). A chlorosilane material (5) containing impurities of boron compounds is fed at the middle part of the tower type adsorption section, light components (6) are obtained from the tower top, the purified product trichlorosilane (7) is obtained from the side withdrawing section, heavy components (8) are obtained from the tower bottom, and the operation pressure of the tower is 300-500 Kpa. Through the process, the removal rate of the boron impurities is 80%, and the energy consumption is reduced by 60-80%. Compared with the former boron removal process, the flow is greatly simplified, and the energy consumption and equipment expenses are remarkably reduced. Based on effective removal of boron, the key components are separated, the separated components enter corresponding units of polycrystalline silicon production respectively, and the production cost is reduced.

Description

technical field [0001] The invention relates to a partition adsorption method and device, which removes boron-containing impurity compounds in a chlorosilane system and improves the removal efficiency. And the separation of key components is realized while removing impurity boron, and trichlorosilane with higher purity is obtained. The process simplifies the process flow of boron removal by chlorosilane, and reduces energy consumption and equipment cost. Background technique [0002] The development of the semiconductor and solar cell industries has made the production of raw material polysilicon a hot industry. At the same time, the requirements for the purity of polysilicon are getting higher and higher. How to effectively remove impurities in polysilicon has become a difficult problem for my country's polysilicon industry. In particular, there are many types of boron-containing compounds, complex components, and the boiling point of the chlorosilane system is very close...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/32B01D53/04C01B33/107
Inventor 黄国强石秋玲王红星华超王国峰姚帅鹏
Owner TIANJIN UNIV