摘要
制备了Dawson结构磷钨酸(H6P2W18O62.13H2O)催化剂,并通过UV-Vis及电化学方法分别对其结构和电化学性能进行了表征;以微波辐射促进30%(w)H2O2氧化环己酮制备己二酸为探针反应,考察了该催化剂的性能。通过正交实验和单因次实验探讨了反应条件对催化反应的影响,最适宜的反应条件为:n(环己酮):n(H2O2):n(草酸):n(催化剂)=100:500:3.0:0.25、反应温度100℃、微波辐射功率400 W、反应时间3.5 h,在该反应条件下,己二酸收率达91.78%。当催化剂重复使用5次后,收率仍可达62.50%。相比常规加热,微波辐射加热具有操作简便、反应时间短、收率高和环境友好等优点。
Phosphotungstic acid（H6P2W18O62·13H2O） with Dawson structure was prepared and characterized by means of UV-Vis and electrochemical methods. The synthesis of adipic acid from cyclohexanone（C6HmO） and 30%（w） H2O2 under microwave irradiation was carried out as a probe to study the catalytic activity of the phosphotungstic acid. The effects of the reaction conditions on the catalytic reaction were investigated by orthogonal experiments. The results show that under the optimal conditions of n（C6H100） ：n（H2O2） ： n（H2C204·2H20） ： n（H6P2W18062·13H20） 100 ： 500 ： 3.0 ： 0.25, the reaction temperature 100℃, the microwave power 400 W and the reaction time 3.5 h, the yield of adipic acid could reach 91.78%. The catalyst could be reused for 5 times and the yield of adipic acid was still above 62.50%. Compared with conventional heating methods, microwave irradiation in the synthesis possessed the advantages of simpler operation, shorter reaction time, higher yield and environmental friendliness.
出处
《石油化工》
CAS
CSCD
北大核心
2012年第6期694-698,共5页
Petrochemical Technology
基金
国家自然科学基金项目(21161009)
江西省自然科学基金项目(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)
关键词
微波辐射
己二酸
草酸
环己酮
过氧化氢
磷钨酸催化剂
microwave irradiation
adipic acid
oxalic acid
cyclohexanone
hydrogenperoxide
phosphotungstic acid catalyst
