磷钨钒杂多酸的制备、表征及催化合成四氢呋喃  

Preparation and catalytic application of tungstovanadophosphoric heteropolyacid with Keggin structure for the synthesis of tetrahydrofuran

作　　者：严平[1] 徐常龙[1] 谢宝华[1,2] 陶春元[1,2] 占昌朝[1,2] 

机构地区：[1]九江学院化学与环境工程学院,江西九江332005 [2]江西省鄱阳湖生态经济研究中心,江西九江332005

出　　处：《化学试剂》2012年第11期1009-1012,共4页Chemical Reagents

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);江西省教育厅科技资助项目(GJJ10626;GJJ11613);九江学院质量工程项目(10XSCXXSY48;10XSCXXSY52;11XSCXXSY4)

摘　　要：通过水热法制备了系列Keggin结构磷钨钒杂多酸催化剂,并通过FT-IR、UV-Vis对催化剂结构进行表征。以1,4-丁二醇脱水合成四氢呋喃为探针反应,考察催化剂催化性能。通过正交实验确定了反应的优化条件:钒原子取代个数为3,催化剂质量分数为3.93%(相对1,4-丁二醇质量),反应温度180～190℃,反应时间50 min,四氢呋喃平均收率达85.4%。催化剂重复使用3次,收率仍可达82.3%。本工艺具有绿色、安全、操作简单等优点。Series of tungstovanadophosphoric heteropolyacid with Keggin structure were prepared by hydrothermal synthe- sis and characterized by FT-IR, UV-Vis. The results indicated that the heteropolyacids had Keggin structure. The catalytic performance in synthesis of tetrahydrofuran from 1,4-butane- diol was investigated. The main effects of the reaction were optimized with orthogonal experiments. The results showed that under the optimal condition,i, e. the vanadium atom num- ber was three,the mass ratio of the catalyst to total reactant was 3.93% ,the reaction temperature was 180- 190 ℃ ,the reaction time was 50 rain, the yield of tetrahydrofuran could reach 85.4%. The catalyst could be reused for 3 times and the yield was still above 82. 3%. This method provided a green, safe and operation simple process to produce tetra- hydrofuran.

关 键 词：磷钨钒杂多酸 KEGGIN结构 1 4-丁二醇 四氢呋喃 

分 类 号：TQ426.6[化学工程]