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Catalyst used in preparation of silane by disproportionation, preparation method for catalyst and method for preparing SiH4 by disproportionating SiH2C12

A catalyst and silane technology are applied in the field of disproportionating halosilane to prepare catalysts with higher hydrogen-containing halosilanes and silanes, catalyst preparation, and disproportionating SiH2Cl2 to prepare SiH4 fields, which can solve the problems of limiting primary conversion efficiency, low service temperature, etc., Achieve the effect of being beneficial to large-scale production and application, improving yield, and high silane conversion rate

Inactive Publication Date: 2011-03-23
BYD CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

[0010] The present invention overcomes the disadvantages of the prior art that the large-scale disproportionation of halosilanes to prepare higher hydrogen-containing halosilanes and silane catalysts has a low use temperature, which limits the primary conversion efficiency of the preparation reaction.

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  • Catalyst used in preparation of silane by disproportionation, preparation method for catalyst and method for preparing SiH4 by disproportionating SiH2C12
  • Catalyst used in preparation of silane by disproportionation, preparation method for catalyst and method for preparing SiH4 by disproportionating SiH2C12
  • Catalyst used in preparation of silane by disproportionation, preparation method for catalyst and method for preparing SiH4 by disproportionating SiH2C12

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preparation example Construction

[0023] The present invention also provides a preparation method for the above-mentioned catalyst, the steps comprising: (1) contacting the salt solution of metal M with an acidic cation exchange resin, ion exchange reaction and M diffusion adsorption take place; (2) washing and drying the product obtained in step (1) , and then activated by heating with hydrogen to prepare the catalyst, the preparation method is simple and easy to realize.

[0024]Wherein, M in the salt solution of M can be selected from one or more of Ru, Rh, Fe, Co, Ni, Pd, Cd, Cu, Zn, Ag, Pt, Au, etc., and the specific salt solution can be M Sulfate, chlorate, nitrate, acetate and other salt solutions; the acidic cation exchange resin has a styrene or acrylic acid backbone, and the exchangeable group is connected to the backbone, and the exchangeable group can be selected from -SO 3 H, -COOH, -OH, -NHR, -NR 2 , -NH 2 Wait. The specific acidic cation exchange resin can be various strongly acidic and weakl...

Embodiment 1

[0032] 1) Catalyst preparation: mix 500ml of cobalt chloride solution of 1mol / L with 200g of D001 acidic cation exchange resin (pore diameter is 10-15nm, porosity is 0.09-0.21ml / g, particle diameter is 0.31-1.25mm, specific surface is 20-36m 2 / g) mixed evenly, ultrasonically dispersed at 60°C for 20h, then washed with high-purity water until neutral, dried in vacuum at 100°C for 48h, and then heated to 120°C for hydrogen activation for 4h to obtain a Co / D001 resin catalyst. After the prepared catalyst was ground into powder, the content of Co element in it was tested by EDS elemental analyzer to be 11.8% by weight (based on the dry weight of the acidic cation exchange resin).

[0033] 2) Disproportionation of SiH 2 Cl 2 Preparation of SiH 4 : Load the catalyst prepared above on the catalytic bed of the sealed reactor A2, the filling height is 500mm, open the valve K1, purge the whole preparation system 5 times with high-purity nitrogen, remove the air in the system, open t...

Embodiment 2

[0035] Adopt the same method as embodiment 1 to prepare Rh / D001 catalyst and disproportionated SiH 2 Cl 2 Preparation of SiH 4 . The difference is that the metal salt solution used is RhCl 3 .

[0036] Using the same method to measure the dry weight of the acidic cation exchange resin as a benchmark, the weight percentage of M is 14.6%. The primary conversion efficiency of silane was measured to be 15.8%, and the primary conversion efficiency of the catalyst after 200 hours of reaction was 15.0%.

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Abstract

The invention provides a catalyst used in preparation of silane by disproportionation, a preparation method for the catalyst and a process for preparing SiH4 by disproportionating SiH2C12. The catalyst is used for preparing higher hydrogen-containing halogeno silane and silane by disproportionating halogeno silane. The catalyst is M / acid cation exchange resin, wherein M may be one or more of Ru, Rh, Fe, Co, Ni, Pd, Cd, Cu, Zn, Ag, Pt and Au. The catalyst has higher activity and high-temperature resistance during preparation of silane, and particularly has the maximum service temperature up to 150 DEG C in large-scale production, thereby improving disproportionation temperature and contributing to improving primary conversion efficiency of the reaction. A carrier has no adsorbability to a silane product, thereby contributing to catalyst stability and yield improvement. In addition, the preparation method is simple, easy, and highly stable.

Description

【Technical field】 [0001] The invention relates to a catalyst for preparing silane by disproportionation, a preparation method of the catalyst and disproportionation of SiH 2 Cl 2 Preparation of SiH 4 The process method, more specifically relate to a kind of disproportionation halosilane to prepare the catalyst of higher hydrogen-containing halosilane and silane, the preparation method of this kind of catalyst and disproportionation SiH 2 Cl 2 Preparation of SiH 4 process method. 【Background technique】 [0002] Silane is the basic raw material of a series of silicon compounds such as monocrystalline silicon, polycrystalline silicon, amorphous silicon, metal silicide, silicon nitride, silicon carbide, silicon oxide and other key materials required for semiconductors, and has been widely used and mass-produced. [0003] The prior art generally uses cheap and easily available higher-level halogenated silanes such as silicon tetrachloride as raw materials to prepare relative...

Claims

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Application Information

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IPC IPC(8): B01J23/75B01J23/46B01J37/00C01B33/04
Inventor 丁显波周勇姜占锋张松林
Owner BYD CO LTD
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