Catalyst for transforming silicon tetrachloride into trichlorosilane through hydrodechlorination and preparation method of catalyst

A technology for dechlorinating and converting trichlorosilane and silicon tetrachloride, which is applied in the direction of metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, silicon halide compounds, etc., and can solve the problem of difficult bulk storage and transportation , strong corrosiveness and toxicity, low conversion rate, etc., to achieve the effect of low raw material cost, uniform particle size distribution, and improved catalytic efficiency

Inactive Publication Date: 2014-04-30
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silicon tetrachloride is a liquid under normal pressure, with a low boiling point, easy to vaporize and deliquescent, highly corrosive and toxic, and difficult to store and transport in batches
Although several catalyst schemes suitable for cold hydrogenation have been proposed at home and abroad, these catalysts themselves or the catalytic process still have many shortcomings such as low conversion rate, high cost, and difficult recovery. Therefore, the present invention provides A catalyst suitable for the cold hydrogenation and hydrogenation conversion of silicon tetrachloride to prepare trichlorosilane, and a preparation process for the catalyst is proposed

Method used

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Examples

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preparation example Construction

[0022] The preparation method of the catalyst that converts silicon tetrachloride hydrodechlorination into trichlorosilane comprises the following steps:

[0023] (1) Preparation of nickel ammonium complex ion solution: at room temperature, add soluble nickel salt to the ammonia solution, then add water to the solution, adjust the pH to 8-12, and control the Ni 2+ The final concentration in the solution is 0.1~0.5mol·l -1 , the stable [Ni(NH 3 ) 6 ] 2+ Complex ion solution;

[0024] (2) Preparation of copper ammonium ion solution: at room temperature, add soluble copper salt to the ammonia solution, then add water to the solution, adjust the pH to 8-12, and control the Cu 2+ The final concentration in the solution is 0.1~0.5mol·l -1 , the stable [Cu(NH 3 ) 4 ] 2+ Complex ion solution;

[0025] (3) Preparation of palladium ammonium ion solution: at room temperature, add soluble palladium salt to the ammonia solution, then add water to the solution, adjust the pH to 8-1...

Embodiment 1

[0041] Step 1: Take 7.5ml of ammonia water with a mass content of 15% and add it to a beaker, add 1.8g of nickel acetate, add water to 100ml, stir well until it is completely dissolved, and make Ni 2+ The concentration reaches 0.1mol·l -1 , the pH value of the solution is 10, clear and transparent, forming a stable [Ni(NH 3 ) 6 ] 2+ Complex ion solution;

[0042] Step 2: Take 5ml of ammonia water with a mass content of 15% and add it to a beaker, add 1.6g of copper sulfate, add water to 100ml, and stir until it is completely dissolved, so that Cu 2+ The concentration reaches 0.1mol·l -1 , the pH value of the solution is 9.5, clear and transparent, forming a stable [Cu(NH 3 ) 4 ] 2+ Complex ion solution;

[0043] Step 3: Take 0.5ml of ammonia water with a mass content of 15% and add it to a beaker, add 0.09g of palladium chloride, add water to 50ml, and stir until it is completely dissolved, so that the Pd 2+ The concentration reaches 0.01mol·l -1 , the pH value of th...

Embodiment 2

[0048] Step 1: Take 37.5ml of ammonia water with a mass content of 15% and add it to a beaker, add 9.2g of nickel nitrate, add water to 100ml, stir well until it is completely dissolved, and make Ni 2+ The concentration reaches 0.5mol·l ～1 , the pH value of the solution is 12, clear and transparent, forming a stable [Ni(NH 3 ) 6 ] 2+ Complex ion solution;

[0049] Step 2: Take 25ml of ammonia water with a mass content of 15% and add it to a beaker, add 6.8g of copper chloride, add water to 100ml, and stir until it is completely dissolved, so that Cu 2+ The concentration reaches 0.5mol·l -1 , the pH value of the solution is 12, clear and transparent, forming a stable [Cu(NH 3 ) 4 ] 2+ Complex ion solution;

[0050] Step 3: Take 1.3ml of ammonia water with a mass content of 15% and add it to a beaker, add 0.45g of palladium chloride, add water to 50ml, and stir until it is completely dissolved, so that the Pd 2+ The concentration reaches 0.05mol·l -1 , the pH value of ...

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Abstract

The invention discloses a catalyst for transforming silicon tetrachloride into trichlorosilane through hydrodechlorination and a preparation method of the catalyst. Nickel, copper and palladium are taken as major active ingredients of the hydrodechlorination catalyst, nickel particles, copper particles and palladium particles are slowly adsorbed, reduced and deposited in surface and pore of activated carbon layer by layer through step-by-step controlled reduction and in-situ deposition, and the three metallic particles are uniformly distributed and mutually cooperated, so as to effectively improve a catalytic efficiency of transforming silicon tetrachloride into trichlorosilane through hydrodechlorination. The catalyst preparation method disclosed by the invention has the characteristics of simple process, moderate condition and relatively low investment; the prepared catalyst has certain magnetism, which is favorable for magnetic separation and recovery after using the catalyst. According to the catalyst, mass percentage of loading three metals on an activated carbon load is 15-30%, and specific surface area is 300-700m<2> / g.

Description

technical field [0001] The invention mainly relates to polysilicon production technology, in particular to a catalyst for converting silicon tetrachloride into trichlorosilane by hydrodechlorination and a preparation method thereof, belonging to the technical field of industrial catalysis. Background technique [0002] At present, most of the production processes adopted by my country's polysilicon enterprises are the improved Siemens method, that is, mixed chlorosilanes (silicon tetrachloride, trichlorosilane, etc.) , to separate trichlorosilane, and then reduce trichlorosilane with high-purity hydrogen at high temperature, and the silicon vapor in the product is subjected to chemical vapor deposition to obtain high-purity polysilicon rods. A large number of by-products are produced during the reaction process of this process, that is, more than 10 tons of silicon tetrachloride and 1 to 5 tons of hydrogen chloride will be associated with every 1 ton of polysilicon produced. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/107B01J23/89
Inventor 张军白孝康米刚杜西刚宋帮才牛睿祺
Owner HENAN UNIV OF SCI & TECH
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