利用复分解法制备出Dawson型磷钨酸钕NdH3P2W(18)O(62)·nH2O,并通过FTIR、UV-Vis、SEM、XRD、EDS、CV对催化剂进行表征。以H2O2为催化剂,30%H2O2为氧源,催化氧化环己酮合成了己二酸。考察了催化剂用量、H2O2用量、反应时间及催化剂重复套用次数等因素对己二酸收率的影响。结果表明,在优化反应条件下:即w(催化剂)=6.4%(基于环己酮质量),n(环己酮)∶n(30%H2O2)=100∶450,105℃反应5.0 h,己二酸收率为91.1%。催化剂套用5次,己二酸收率仍可达67.5%。
Neodymium salts of Dawson- type tunstophosphoric acids( NdH3P2W(18)O(62)·nH2O) were prepared by the double decomposition reaction. FTIR,UV- Vis,SEM,XRD,EDS and CV were used to characterize the catalysts. The catalysts were used to catalyze the synthesis of adipic acid from cyclohexanone oxidized by 30% hydrogen peroxide. The effects of various factors such as catalyst and hydrogen peroxide dosage,reaction time and reusability of the catalyst were investigated.The results indicated that under the optimal reaction conditions,i. e.,w( NdH3P2W(18)O(62)·nH2O) = 6. 4%( based on the mass of cyclohexanone),n( cyclohexanone) ∶ n(30% H2O2) = 100∶ 450,reaction time of 5. 0 h and reaction temperature of105 ℃,average yield of adipic acid reached 91. 1%. The yield of adipic acid was still above 67. 5% as the catalyst system was reused 5 times.