Dawson结构磷钨酸铝催化剂的制备、表征及其催化合成己二酸

利用复分解法制备出Dawson结构磷钨酸铝AlH₃P₂W₁₈O₆₂·nH₂O催化剂,以30% H₂O₂为氧源,催化氧化环己酮合成了己二酸.采用FT-IR、SEM、XRD、EDS对催化剂进行表征.用正交实验法优化反应工艺条件,考察了反应时间、催化剂用量、反应温度和催化剂重复套用次数等因素对己二酸收率的影响.确定较优工艺条件为:w(催化剂)= 7.6%(基于环己酮质量),n(环己酮):n(30%H₂O₂)=100:450,反应时间6.0h,反应温度105℃.通过3次平行实验,己二酸平均收率为91.4%.催化剂重复使用5次,己二酸收率仍可达72.3%.

Preparation,characterization of AlH3P2W18O62·nH2O and its catalytic performance in synthesis of adipic acid

Dawson-type aluminum phosphotungstate(AlH₃P₂W₁₈O₆₂·nH₂O)was prepared by the double decomposition method,and characterized by FT-IR,SEM,XRD and EDS. The catalyst was used to catalyze synthesis of adipic acid from oxidation of cyclohexanone by 30% hydrogen peroxide. Orthogonal experiments were used to optimize reaction conditions. The optimum reaction conditions were:mass ratio of catalyst to cyclohexanon 7.6%,molar ratio of cyclohexanone to 30 percent hydrogen peroxide 100:450,reaction time 6.0h,reaction temperature 105℃,and isolated yield of adipic acid could reach 91.4%. The filtrate containing the catalyst could be concentrated by rotary evaporation and be reused five times by easy separation of the product after reaction,and isolated yield of adipic acid was still above 72.3%.