利用室温沉淀法制备出 Dawson 结构磷钨酸铯,考察了其在催化微波促进30％H2 O2氧化环己酮合成己二酸反应中的催化性能,并通过 FT-IR、SEM、XRD、EDS、ICP-AES对催化剂进行表征.探讨了铯离子取代个数、催化剂用量、微波功率、反应温度、反应时间、H2 O2用量等对己二酸收率的影响.结果表明,最优的反应条件为 Cs 离子取代个数为3,w(催化剂)＝7．6％(基于环己酮质量),n(环己酮)∶n(30％H2 O2)＝100∶375,反应时间4．0 h,微波功率300 W,反应温度100℃.在此条件下己二酸收率可达90．4％.催化剂重复使用5次,己二酸收率为73．1％.
Cesium salts of Dawson-type tungstophosphoric acids were prepared by the precipitation method,and characterized by FT-IR,SEM,XRD,EDS and ICP-AES.The catalysts were used in the synthesis of adipic acid. The results showed that under the best reaction conditions,i.e.,the number of cesium in cesium salt replaced was 3,the mass ratio of the catalyst to cyclohexanone was 7.6%,molar ratio of cyclohexanone to 30 percent hydrogen peroxide of 100∶375,reaction time of 4.0 h,microwave power of 300 W,reaction temperature of 100 ℃,the yield of adipic acid could reach 90.4%.The filtration containing the catalyst could be concentrated by the rotary evaporation and be reused five times by easily separation of the product after reaction,the isolated yield of adipic acid was still above 7 3 .1%.
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