화학공학소재연구정보센터
Journal of the Korean Industrial and Engineering Chemistry, Vol.9, No.3, 394-398, June, 1998
실험계획법에 의한 메틸염화실란 합성의 최적공정조건
Optimum Process Condition by Experimental Design Method for the Synthesis of Methylchlorosilanes(MCS)
초록
실리콘의 모노머로 사용되고 있는 MCS의 합성 최적조건에 관한 연구를 수행하였다. 4원촉매계(CuCl/ZnCl2/Sn/Cd)와 원료규소로부터 접촉물질을 제조한 후, 염화메틸과 반응시켜 MCS를 합성할 때 실험계획법에 따라 실험하고 해석하여 하나의 공정조건을 확립하였다. 접촉물질 50g, 교반속도 60rpm, 상압에서 최적반응온도와 MeCl 유량은 각각 300-305℃와 70-80cm3/min이었다. 또한 연속적으로 실험을 수행하여 최적공정조건을 확인하였으며, MeCl의 전환율 67%와 규소소모율 92%에서 평균반응속도는 170(g-MCS/hr.kg-Si), 평균선택도는 0.05이었으며, 연속식 실험결과로부터 총괄반응속도식의 파라미터와 최적압력을 구하였다.
An optimum synthetic condition was studied for the MCS used as a silicone monomer. The contact mixture was made from the four component catalyst system(CuCl/ZnCl2/Sn/Cd) and silicon particles. The contact mass was used for a series of experiments with methyl chloride, which were designed and done to explore the optimum condition for MCS synthesis by an experimental design method. The optimum temperature and MeCl flow rate, which were obtained using 50g contact mass at 60rpm and 1 atm, were in the range of 300-305℃ and of 70-80ccm. Also a continuous run was performed to confirm the conditions. The results showed that the average reaction rate and selectivity were 170(g-MCS/hr.kg-Si) and 0.05 respectively at 67% conversion of MeCl and 92% silicon utilization rate. Also the parameters of overall reaction rate equation and a total pressure were estimated on the basis of the results of the continuous run.
  1. Voorhoeve RJH, Vlugter JC, J. Catal., 3, 414 (1964) 
  2. Voorhoeve RJH, Vlugter JC, J. Catal., 4, 43 (1965) 
  3. Silicones S, SRI Report No. 160, Process Economics Program (1983)
  4. Voorhoeve RJH, Vlugter JC, J. Catal., 4, 123 (1965) 
  5. Joklik J, Kraus M, Bazant V, Col. Czech. Chem. Commun., 26, 427 (1961)
  6. Voorhoeve RJH, Vlugter JC, J. Catal., 4, 220 (1965) 
  7. Ward WJ, Ritzer A, Carroll KM, Llock JW, J. Catal., 100, 240 (1986) 
  8. Cho CK, Han KD, J. Korean Ind. Eng. Chem., 8(5), 804 (1997)
  9. Montegomery DC, Design and Analysis of Experiments, John Wiley and Sons (1991)
  10. Banholzer WF, Lewis N, Ward W, J. Catal., 101, 405 (1986) 
  11. Kim JP, Rethwisch DG, J. Catal., 134, 168 (1992)