化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2014年
7期
2776-2784
,共9页
武军伟%邢卫红%张峰%仲兆祥%金万勤%徐南平
武軍偉%邢衛紅%張峰%仲兆祥%金萬勤%徐南平
무군위%형위홍%장봉%중조상%금만근%서남평
陶瓷膜%流化床%二甲基二氯硅烷%反吹
陶瓷膜%流化床%二甲基二氯硅烷%反吹
도자막%류화상%이갑기이록규완%반취
ceramic membrane%fluidized bed reactor%dimethyldichlorosilane%back flush
提出将陶瓷膜与流化床反应器耦合构成一体式流化床膜反应器,用于直接法合成二甲基二氯硅烷。实验考察了催化剂浓度、脉冲反吹对反应效率和膜分离性能的影响,并对反应前后的触体及陶瓷膜进行了表征。结果表明,催化剂浓度小于4%(质量)时,二甲基二氯硅烷的选择性均可维持在85%以上,硅粉转化率随催化剂浓度的增大而增大;催化剂浓度在4%~8%时,二甲基二氯硅烷的选择性随催化剂浓度增加而略有下降,当催化剂浓度大于8%时,二甲基二氯硅烷选择性明显下降。触体失活后粒径减小,硅粉表面积碳随催化剂浓度的增加而升高。陶瓷膜表面形成内外两层滤饼,内层滤饼主要成分为铜,外层滤饼主要成分为碳;不同催化剂浓度下,陶瓷膜对粉尘的截留率均可达100%,反应过程中跨膜压差随时间变化较小,脉冲反吹可增加硅粉转化率。
提齣將陶瓷膜與流化床反應器耦閤構成一體式流化床膜反應器,用于直接法閤成二甲基二氯硅烷。實驗攷察瞭催化劑濃度、脈遲反吹對反應效率和膜分離性能的影響,併對反應前後的觸體及陶瓷膜進行瞭錶徵。結果錶明,催化劑濃度小于4%(質量)時,二甲基二氯硅烷的選擇性均可維持在85%以上,硅粉轉化率隨催化劑濃度的增大而增大;催化劑濃度在4%~8%時,二甲基二氯硅烷的選擇性隨催化劑濃度增加而略有下降,噹催化劑濃度大于8%時,二甲基二氯硅烷選擇性明顯下降。觸體失活後粒徑減小,硅粉錶麵積碳隨催化劑濃度的增加而升高。陶瓷膜錶麵形成內外兩層濾餅,內層濾餅主要成分為銅,外層濾餅主要成分為碳;不同催化劑濃度下,陶瓷膜對粉塵的截留率均可達100%,反應過程中跨膜壓差隨時間變化較小,脈遲反吹可增加硅粉轉化率。
제출장도자막여류화상반응기우합구성일체식류화상막반응기,용우직접법합성이갑기이록규완。실험고찰료최화제농도、맥충반취대반응효솔화막분리성능적영향,병대반응전후적촉체급도자막진행료표정。결과표명,최화제농도소우4%(질량)시,이갑기이록규완적선택성균가유지재85%이상,규분전화솔수최화제농도적증대이증대;최화제농도재4%~8%시,이갑기이록규완적선택성수최화제농도증가이략유하강,당최화제농도대우8%시,이갑기이록규완선택성명현하강。촉체실활후립경감소,규분표면적탄수최화제농도적증가이승고。도자막표면형성내외량층려병,내층려병주요성분위동,외층려병주요성분위탄;불동최화제농도하,도자막대분진적절류솔균가체100%,반응과정중과막압차수시간변화교소,맥충반취가증가규분전화솔。
A fluidized bed reactor was coupled with a ceramic membrane to construct a integrated fluidized bed membrane reactor for synthesis of dimethyldichlorosilane. The effects of catalyst concentration, back flush on reaction and membrane separation performance were studied. The ceramic membrane and the contact mass before and after reaction were characterized. Selectivity of dimethyldichlorosilane could be maintained above 85% and conversion ratio of silicon increased with increasing catalyst concentration, when catalyst concentration was less than 4%(mass). When catalyst concentration was in the range of 4%-8%, selectivity of dimethyldichlorosilane decreased slightly, but decreased obviously when catalyst concentration was above 8%. The particle size of the contact mass decreased after reaction. The carbon that deposited on the surface of silicon increased with increasing catalyst concentration. Two layers of filter cake formed on the membrane surface during the reaction process. The inner cake was copper, and the outer one was carbon. Under different catalyst concentrations, rejection of dust by the ceramic membrane could reach 100%. The change of trans-membrane pressure was little in the reactionprocess and back flush could increase silicon conversion.