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采用沉淀法制备了磷酸铜、焦磷酸铜和三聚磷酸铜催化剂,并采用X射线衍射仪对催化剂进行了表征。以环己烷氧化为探针反应,过氧化氢为氧化剂,考察了催化剂、溶剂、氧化剂、反应温度以及反应时间对氧化效果的影响。结果表明,非均相焦磷酸铜催化剂的催化活性最高,在乙腈用量10 mL,环己烷用量8 mmol,焦磷酸铜用量0.03 g,w(H2O2)=30%的双氧水用量3.0 mL,反应温度65℃的条件下,反应10 h后,环己烷的转化率为54.1%,环己醇和环己酮(简称醇酮,以下同)的收率分别为21.3%和32.8%。
Copper phosphate, copper pyrophosphate and copper tripolyphosphate catalysts were prepared by precipitation method. The catalysts were characterized by X-ray diffraction. Oxidation was carried out by cyclohexane oxidation and hydrogen peroxide as oxidant. The effects of catalyst, solvent, oxidant, reaction temperature and reaction time on the oxidation were investigated. The results showed that the catalytic activity of heterogeneous copper pyrophosphate catalyst was the highest. Under the conditions of 10 mL of acetonitrile, 8 mmol of cyclohexane, 0.03 g of copper pyrophosphate and 3.0 mL of H2O2 = 30%, the reaction temperature Under the condition of 65 ℃, the conversion of cyclohexane was 54.1% after 10 h reaction, the yields of cyclohexanol and cyclohexanone were 21.3% and 32.8%, respectively.