化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2015年
8期
3029-3035
,共7页
饶辉%张峰%仲兆祥%邢卫红%金万勤
饒輝%張峰%仲兆祥%邢衛紅%金萬勤
요휘%장봉%중조상%형위홍%금만근
氯化亚铜%膜%二甲基二氯硅烷%催化剂%固定床
氯化亞銅%膜%二甲基二氯硅烷%催化劑%固定床
록화아동%막%이갑기이록규완%최화제%고정상
cuprous chloride%membranes%dimethyldichlorosilane%catalyst%fixed-bed
将沉淀反应器与陶瓷膜耦合构成一体式膜反应器,用于制备单分散高活性球形 CuCl 颗粒。考察陶瓷膜孔径、操作条件和沉淀反应条件对 CuCl 颗粒形貌和粒径分布的影响,评价氯化亚铜的催化性能。结果表明,陶瓷膜的孔径对 CuCl 平均粒径影响显著,但对颗粒形貌影响不大;稳定剂对催化剂形貌影响显著,聚乙烯吡咯烷酮K-30(PVP)的加入使CuCl颗粒由三角形变为球形,使得颗粒粒径更加均一。在铜离子浓度为0.1 mol·L?1,PVP浓度为1μg·ml?1和进料速率为40 ml·min?1的条件下,采用平均孔径为0.05μm的陶瓷膜分散Na2SO3溶液,可以制备出平均粒径为5.1μm的单分散球形CuCl颗粒;该颗粒用于直接法制备有机硅单体的反应中,二甲基二氯硅烷的选择性和硅粉的转化率分别为94%和38%,优于商业化氯化亚铜的催化性能。通过比较不同制备条件下氯化亚铜颗粒的催化性能,发现相比于三角形颗粒,形貌规整的球形氯化亚铜对M2的选择性更高。
將沉澱反應器與陶瓷膜耦閤構成一體式膜反應器,用于製備單分散高活性毬形 CuCl 顆粒。攷察陶瓷膜孔徑、操作條件和沉澱反應條件對 CuCl 顆粒形貌和粒徑分佈的影響,評價氯化亞銅的催化性能。結果錶明,陶瓷膜的孔徑對 CuCl 平均粒徑影響顯著,但對顆粒形貌影響不大;穩定劑對催化劑形貌影響顯著,聚乙烯吡咯烷酮K-30(PVP)的加入使CuCl顆粒由三角形變為毬形,使得顆粒粒徑更加均一。在銅離子濃度為0.1 mol·L?1,PVP濃度為1μg·ml?1和進料速率為40 ml·min?1的條件下,採用平均孔徑為0.05μm的陶瓷膜分散Na2SO3溶液,可以製備齣平均粒徑為5.1μm的單分散毬形CuCl顆粒;該顆粒用于直接法製備有機硅單體的反應中,二甲基二氯硅烷的選擇性和硅粉的轉化率分彆為94%和38%,優于商業化氯化亞銅的催化性能。通過比較不同製備條件下氯化亞銅顆粒的催化性能,髮現相比于三角形顆粒,形貌規整的毬形氯化亞銅對M2的選擇性更高。
장침정반응기여도자막우합구성일체식막반응기,용우제비단분산고활성구형 CuCl 과립。고찰도자막공경、조작조건화침정반응조건대 CuCl 과립형모화립경분포적영향,평개록화아동적최화성능。결과표명,도자막적공경대 CuCl 평균립경영향현저,단대과립형모영향불대;은정제대최화제형모영향현저,취을희필각완동K-30(PVP)적가입사CuCl과립유삼각형변위구형,사득과립립경경가균일。재동리자농도위0.1 mol·L?1,PVP농도위1μg·ml?1화진료속솔위40 ml·min?1적조건하,채용평균공경위0.05μm적도자막분산Na2SO3용액,가이제비출평균립경위5.1μm적단분산구형CuCl과립;해과립용우직접법제비유궤규단체적반응중,이갑기이록규완적선택성화규분적전화솔분별위94%화38%,우우상업화록화아동적최화성능。통과비교불동제비조건하록화아동과립적최화성능,발현상비우삼각형과립,형모규정적구형록화아동대M2적선택성경고。
A direct sediment reactor was coupled with a ceramic membrane for the preparation of high-activity CuCl particles with spherical structure. The effects of the membrane pore size, types of stabilizer, concentration of Cu2+ as well as the dispersed phase flow rate on the size and uniformity of the particles were investigated. The catalytic properties of these CuCl particles were exploredvia Rochow reaction. The results showed that the average particle size of CuCl decreased with the decrease of membrane pore size. The morphology of the particles changed from triangular structure to spherical when adding polyvinylpyrrolidine(PVP) to the continuous and dispersion phase. The uniform spherical CuCl particles, with the average size of 5.1μm, were obtained under the conditions that the dispersed phase flow rate of Na2SO3 with a ceramic membrane of 0.05μm pore size was 40 ml·min?1, the concentration of Cu2+ was 0.1 mol·L?1 and the concentration of PVP was 1μg·ml?1. The catalytic performance of the uniform spherical CuCl particles, with the dimethyldichlorosilane selectivity of 94% and the Si conversion of 38%, is much better than those of the commercial CuCl particles. Regular spherical particles have a higher selectivity of M2 compared to the triangular particles.