微波辐射促进H_6P_2W_(18)O_(62)/SiO_2催化H_2O_2氧化环己酮合成己二酸  

H_2O_2 oxidation of cyclohexanone to adipic acid catalyzed by H_6P_2W_(18)O_(62)/SiO_2 under microwave irradiation

作　　者：曹小华[1] 严平[1] 刘新强[1] 徐常龙[1] 

机构地区：[1]九江学院化学化工学院,江西九江332005

出　　处：《合成纤维工业》2011年第6期11-13,共3页China Synthetic Fiber Industry

基　　金：国家自然科学基金(21161009);江西省自然科学基金(2009GQH0053);江西省教育厅科技资助项目(GJJ10626;GJJ11613);九江学院质量工程项目(09XSCXXSY25;09XSCXXSY62)

摘　　要：在微波辐射作用下,以自制的磷钨酸/二氧化硅为催化剂,在无有机溶剂、相转移催化剂的情况下,用w(H_2O_2)30%的H_2O_2氧化环己酮合成己二酸;通过正交实验和单因次实验探讨了各因素对反应的影响,确定了优化工艺条件。结果表明:最优化工艺为磷钨酸负载量30%,磷钨酸/二氧化硅用量1.20 g、草酸0.18 g,H_2O_2 32.0 mL,反应温度100℃,微波功率400 W,反应时间4.0 h,己二酸收率达73.24%;催化剂重复使用5次,己二酸收率仍可达50.42%。Adipic acid was synthesized by cyclohexanone oxidation with 30% w（ H2O2 ） catalyzed with self-made phosphotungstic acid/silicon dioxide in absence of organic solvent and phase transfer catalyst under microwave irradiation. The influential factors on the reaction were discussed by orthogonal and simple fact experiments. And the optimal process conditions were decided. The results showed that the yield of adipic acid reached 73.24% under the conditions as followed ： phosphotungstic acid loading 30%, 1.20 g phosphotungstic acid/silicon dioxide, 0.18 g oxalic acid, 32.0 mL H2O2 ,reaction temperature 100 ℃ ,microwave power 400 W, reaction time 4.0 h; and the adipic acid yield was still 50.42% while repeatedly using the catalyst 5 times.

关 键 词：负载型 磷钨酸 己二酸 环己酮 微波 辐射 

分 类 号：TQ225.146[化学工程—有机化工]