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50min,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.