负载型HMCM-22/PW分子筛催化合成十二烷基磷酸酯  

Synthesis of Dodecyl Phosphate Catalyzed with Supported PW/MCM-22 Molecular Sieve

作　　者：刘燕军[1,2,3] 郭明明 邵建楠 LIU Yanjun;GUO Mingming;SHAO Jiannan(College of Chemistry and Chemical Engineering,Tianjin Polytechnic University,Tianjin 300387, China;Tianjin Engineering Research Center of Textile Fiber Interface Treatment Technology, Tianjin 300270, China;Tianjin Polytechnic University for the Textile Auxiliaries Co, Ltd,Tianjin 300270, China)

机构地区：[1]天津工业大学化学与化工学院,天津300387 [2]天津工业大学精细化工研究所,天津300387 [3]天津工业大学纺织助剂有限公司,天津300270

出　　处：《中国塑料》2019年第4期66-71,共6页China Plastics

基　　金：中石化项目(217010-3)

摘　　要：用磷钨酸(PW)以浸渍法改性HMCM-22分子筛,并用X射线衍射、扫描电子显微镜、红外光谱对催化剂进行表征。结果表明,改性后的HMCM-22分子筛原有的结构和特征未发生变化;在应用于十二醇与五氧化磷(P_2O_5)摩尔比为2∶1的合成单十二烷基酯化反应中,产物中单酯的选择性有了显著的提高,说明PW与HMCM-22分子筛的活性中心发生了协同作用促进了酯化反应的进行,同时也表明该催化剂有优良的催化性能;在催化剂用量为总反应物的1.5%,加水的量为6.5%,PW的负载量为4%,反应温度为90℃,反应时间为4 h的条件下单酯的选择性达90%。The HMCM-22 molecular sieve was modified with phosphotungstic acid(PW) by an impregnation method, and the resulting composite catalysts were characterized by XRD, SEM, FT-IR.The results indicated that there was no change in the original structure and characteristics of the modified HMCM-22 molecular sieve. The productivity of monododecyl ester was improved significantly for the synthesis of mono-alkyl phosphate(MPA) through esterification of dodecanol and phosphorus pentoxide at a molar ration of 2/1,indicating that the esterification was promoted synergistically by the active center of composite catalysts, thus resulting in excellent catalytic performance. For the composite catalyst loaded with 4 wt % PW, a high productivity of 90 %was achieved when the amount of water was 9 g,the amount of composites catalysts in total reactants was 1.5 wt %, the reaction temperature was set at 90 ℃, and the reaction time was set as 4 h. This suggests that the PW/HMCM-22 composite molecular sieve has an excellent catalytic effect.

关 键 词：磷钨酸 HMCM-22分子筛 单十二烷基磷酸酯 浸渍法 

分 类 号：TQ314.24[化学工程—高聚物工业]