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Received March 8, 2013
Accepted March 31, 2013
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실리콘의 염소화반응에 의한 사염화규소 제조
Preparation of Silicon Tetrachloride by Chlorination of Silicon
Kyun Young Park†
Mi Sun Lee
Min Cheol Kim
Chan Hee Lee
Hoey Kyung Park
Tae Won Kang
Hae Seong Jeong1
Kyoung Ah Han1
Weon Hoe Huh1
Ji Cheol You1
공주대학교 화학공학부, 330-717 충남 천안시 부대동 275 1실리스, 331-822 충남 천안시 서북구 입장면 35-3
Department Chemical Engineering, Kongju National University, 275 Budae-dong, Cheonan, Chungnam 330-717, Korea 1Korea Institute of Industrial Technology PP2-303, Silice Co., Ltd., 35-3, Ipjang-myeon, Seobuk-gu, Cheonan, Chungnam 331-822, Korea
Korean Chemical Engineering Research, June 2013, 51(3), 407-410(4), 10.9713/kcer.2013.51.3.407 Epub 3 June 2013
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Abstract
직경 25 mm의 파이렉스 튜브 내에서 실리콘의 유동층 염소화 반응이 수행되었다. 반응기에 공급되는 질소 유량 0.8~1.0 L/min, 염소 유량 0.2 L/min, 반응온도 450 ℃, SiCl4 응축기의 냉매온도는 -5 ℃로 설정하였다. 반응기에 도입되는 가스 내 염소의 몰분율이 증가하면 SiCl4의 수율이 증가하였다. 반응가스 중 염소의 몰분율 0.2의 조건에서 SiCl4의 수율은 28% 이었다. 염소의 몰분율 증가는 반응열 상승에 의해 반응온도 상승을 가져옴으로써 안전을 고려하여 염소의 몰분율을 0.2 이상으로 올리지 못했다. 실리콘의 유동층 염소화 반응에 의한 사염화실리콘의 제조 가능성이 입증되었으며, 향후 보다 가혹한 조건에서의 실용화 연구를 위한 기초로 활용될 수 있을 것으로 기대된다.
The chlorination of a metallurgical-grade silicon was carried out in a fluidized bed reactor, 25 mm in diameter. The flow rate of the chlorine admitted into the reactor was 0.2 L/min and that of the carrier nitrogen was 0.8~1.0 L/min. The reactor temperature was maintained at 450 ℃ and the temperature of the coolant at the SiCl4 condenser was at -5 ℃. The SiCl4 yield increased with increasing the mole fraction of chlorine in the feed gas, exhibiting 28% at the mole fraction of 0.2. Further increase of the chlorine mole fraction was not attempted in a worry that the reactor might be failed due to the high exothermicity of the reaction. The production of SiCl4 from silicon by fluidized bed chlorination was demonstrated on a laboratory scale, which is a stepping stone for future studies under more severe conditions toward industrial application.
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References
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Park HK, Park KY, Mater. Res. Bull., 43(11), 2833 (2008)
Silenko PM, Shlapak AN, Bykov AI, Danilenko NI, Klochkov LA, Ragulya AV, Theor.Exp. Chem., 43(2), 85 (2007)
Falcone JS, “Silicon Compounds,” in Kirk-Othmer Encyclopedia of Chemical Technology, 3rd Ed. by Grayson M., John Wiley & Sons, Inc. (1982)
Seo ESM, Brocchi EA, Carvalho RJ, Soares EP, Andreoli M, J.Mater. Process. Technol., 141, 370 (2003)
HSC Chemistry 5.1, Chemical Reaction and Equilibrium Software with Extensive Thermochemical Database, Outo Kumpu (2002)
Grace JR, “Fluidized-Bed Hydrodynamics,” in Handbook of Multiphase Systems by Hetsroni G., Washington, Hemisphere Publishing Corporation (1982)
Crookston RB, Canjar LN, J. Chem. Eng.Data., 8(4), 544 (1963)
Kim HY, Korean Chem. Eng. Res., 46(1), 37 (2008)
Jain MP, Sathiyamoorthy D, Govardhana Rao V, Indian Chem. Eng., 51, 272 (2010)