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过程工程学报 ›› 2016, Vol. 16 ›› Issue (5): 767-773.DOI: 10.12034/j.issn.1009-606X.216160

• 过程与工艺 • 上一篇    下一篇

Experimental Study on Hydrogenation of SiCl4 to SiHCl3 in a Stirred Bed React

李庆远,李佩龙,王铁峰   

  1. 清华大学化工系绿色反应工程与工艺北京市重点实验室
  • 收稿日期:2016-03-18 修回日期:2016-05-05 出版日期:2016-10-20 发布日期:2016-10-14
  • 通讯作者: 王铁峰 wangtf@tsinghua.edu.cn

Experimental Study on Hydrogenation of SiCl4 to SiHCl3 in a Stirred Bed Reactor

LI Qing-yuan ,LI Pei-long ,WANG Tie-feng   

  1. Beijing Key Laboratory of Green Chemical Reaction Engineering and Technology, Department of Chemical Engineering, Tsinghua University
  • Received:2016-03-18 Revised:2016-05-05 Online:2016-10-20 Published:2016-10-14
  • Contact: WANG Tie-feng wangtf@tsinghua.edu.cn

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摘要： The hydrogenation of SiCl4 to SiHCl3 was studied in a stirred bed reactor with CuCl catalyst. The properties of the CuCl catalysts and silicon particles before and after the reaction were characterized by SEM, XRD and XPS. The XRD showed that the active component of Cu3Si was formed during the reaction, and the EDX proved the molar ratio of Cu and Si on the region of apertures. The valent of Cu was discussed by XPS before and after the hydrogen reaction. Then the effects of the reaction temperature, pressure, molar ratio of H2 to SiCl4, weight hourly space velocity (WHSV), and catalyst loading were studied. The results showed that the conversion rate of SiCl4 was about 38% at WHSV of 190 Nm3/(t?h), temperature of 540℃, pressure of 1.8 MPa, catalyst loading of 0.9%(?), and molar ratio of H2 to SiCl4 1.7:1. Based on the experemental results, a reaction mechanism was proposed, which involved the continuous consumption of silicon (many apertures was showed on SEM image) and formation of new Cu3Si active component during the hydrogenation reaction.

关键词: silicon tetrachloride, trichlorosilane, hydrogenation, stirred bed reactor

Abstract: The hydrogenation of SiCl4 to SiHCl3 was studied in a stirred bed reactor with CuCl catalyst. The properties of the CuCl catalysts and silicon particles before and after the reaction were characterized by SEM, XRD and XPS. The XRD showed that the active component of Cu3Si was formed during the reaction, and the EDX proved the molar ratio of Cu and Si on the region of apertures. The valent of Cu was discussed by XPS before and after the hydrogen reaction. Then the effects of the reaction temperature, pressure, molar ratio of H2 to SiCl4, weight hourly space velocity (WHSV), and catalyst loading were studied. The results showed that the conversion rate of SiCl4 was about 38% at WHSV of 190 Nm3/(t?h), temperature of 540℃, pressure of 1.8 MPa, catalyst loading of 0.9%(?), and molar ratio of H2 to SiCl4 1.7:1. Based on the experemental results, a reaction mechanism was proposed, which involved the continuous consumption of silicon (many apertures was showed on SEM image) and formation of new Cu3Si active component during the hydrogenation reaction.

Key words: silicon tetrachloride, trichlorosilane, hydrogenation, stirred bed reactor