Issue
Korean Chemical Engineering Research,
Vol.51, No.3, 407-410, 2013
실리콘의 염소화반응에 의한 사염화규소 제조
Preparation of Silicon Tetrachloride by Chlorination of Silicon
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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