H_6P_2W_(18)O_(62)/SiO_2的制备、表征及其对四氢呋喃的催化合成  

Preparation,characterization of H_6P_2W_(18)O_(62)/SiO_2 and catalyzing synthesis of tetrahydrofuran

作　　者：曹小华[1,2] 任杰[1] 柳闽生[3] 徐常龙[2] 

机构地区：[1]浙江工业大学化学工程与材料学院,浙江杭州310014 [2]九江学院化学与环境工程学院,江西九江332005 [3]南京晓庄学院生物化工与环境工程学院,江苏南京211171

出　　处：《江苏大学学报（自然科学版）》2013年第3期340-344,共5页Journal of Jiangsu University：Natural Science Edition

基　　金：国家自然科学基金资助项目(21161009);江西省自然科学基金资助项目(20114BAB213002,20122BAB213001);江西省教育厅科技项目(GJJ11613)

摘　　要：通过溶胶-凝胶法制备了SiO2负载Dawson型磷钨酸H6P2W18O62/SiO2催化剂.表征结果表明:负载后磷钨酸仍保持Dawson结构,负载量为30%;磷钨酸比较均匀地分散在SiO2载体上.以催化1,4-丁二醇脱水制备四氢呋喃作为探针反应,考察催化剂的酸催化性能.正交试验和单因次试验结果表明:催化剂对1,4-丁二醇环化脱水合成四氢呋喃反应具有良好的催化性能;最佳反应条件为催化剂用量占1,4-丁二醇质量的6.6%,反应温度为185～190℃,反应时间为40 min,四氢呋喃平均收率为91.70%;催化剂重复使用5次后,催化活性基本保持不变,四氢呋喃收率仍可达90.90%.Phosphotungstic acids with Dawson structure（ H6P2W18O62） supported on SiO2 were prepared by sol-gel method. The Dawson structure of phosphotungstic acids after loading on SiO2 and 30%H6P2W18O62 loading quantity are confirmed, and H6P2W18O62/ can be well dispersed on the SiO2 support. The catalytic performance of H6P2W18O62 was investigated by the catalytic synthesis of tetrahydrofu- ran from 1,4-butanediol. The results of orthogonal experiments and simple factor experiments show that H6P2W18O62//SiO2 exhibits good catalytic performance for catalytic synthesis of tetrahydro-furan fiom 1 ,4- butanediol. Under the optimal conditions with H6P2W18O62/ of 6.6% relative to the dosage of 1,4-butane- diol, reaction temperature of 185 - 190 ~C and reaction time of 40 rain, the isolated yield of tetrahydrofu- ran can reach 91.70%. The catalyst can be reused for five times with no evident decline of catalytic per- formance, and the isolated yield of tetrahydro-furan is still above 90.90%.

关 键 词：H6P2W18O62 SIO2 DAWSON结构 1 4-丁二醇 环化脱水 四氢呋喃 

分 类 号：TQ426.6[化学工程]