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制备了稀土杂多酸盐磷钨酸镧LaPW12O40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使用性等因素对己二酸收率的影响。使用该催化剂无须在反应体系中使用有机溶剂和相转移剂,有益于降低成本和简化分离工艺。实验结果表明,合成己二酸适宜的反应条件为:环己酮100 mmol,30%双氧水55 mL,催化剂用量为环己酮摩尔数的0.264%,回流反应5 h,己二酸收率为68.0%。磷钨酸镧用量少且重复利用7次仍具有良好的催化活性。
The rare earth heteropoly acid salt lanthanum phosphotungstate LaPW12O40 was prepared as catalyst, and 30% H2O2 as oxygen source. Cyclohexanone was oxidized to synthesize adipic acid. The effect of catalyst dosage, H2O2 dosage, reaction time and catalyst reusability on the yield of adipic acid was investigated. The use of this catalyst does not require the use of organic solvents and phase transfer agents in the reaction system, which helps to reduce costs and simplify the separation process. The experimental results show that the suitable reaction conditions for the synthesis of adipic acid are as follows: 100 mmol of cyclohexanone and 55 mL of 30% hydrogen peroxide; the amount of catalyst is 0.264 mol of cyclohexanone; the yield of adipic acid is 68.0 %. Lanthanum phosphotungstate with less dosage and reuse 7 times still has good catalytic activity.