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合成了Dawson型磷钼钒钴杂多酸盐,用傅立叶变换红外光谱、X射线衍射和31P核磁共振等方法表征了磷钼钒钴的结构。以环己烷为原料、H2O2为氧化剂、磷钼钒钴杂多酸盐为催化剂催化氧化制备了环己醇和环己酮,考察了催化剂的钒含量和反应条件(催化剂用量、H2O2用量、反应时间、反应温度)对环己烷氧化反应的影响。实验结果表明,钒含量适中的Co2H5P2Mo15V3O62催化剂活性最高。在Co2H5P2Mo15V3O62用量0.20 mmol、w(H2O2)=50%的双氧水用量13.6 g(0.2 mol)、反应时间10 h、反应温度75℃、叔丁醇用量30 mL的优化反应条件下,环己烷的转化率为88.37%,环己醇和环己酮的总收率可达16.56%。
Dawson phosphomolybdovanadobalt heteropolyacid salt was synthesized. The structure of cobalt, molybdenum, vanadium and cobalt was characterized by Fourier transform infrared spectroscopy, X-ray diffraction and 31P nuclear magnetic resonance. Cyclohexanol and cyclohexanone were prepared by using cyclohexane as raw material, H2O2 as oxidant and phosphomolybdovanadoboron heteropolyacid as catalyst for catalytic oxidation. The vanadium content and reaction conditions (catalyst dosage, H2O2 dosage, reaction time , Reaction temperature) on the oxidation of cyclohexane. The experimental results show that Co2H5P2Mo15V3O62 catalyst with moderate vanadium content has the highest activity. Under the optimal reaction conditions of the dosage of Co2H5P2Mo15V3O62 0.20 mmol, w (H2O2) = 50%, the amount of hydrogen peroxide 13.6 g (0.2 mol), the reaction time 10 h, the reaction temperature 75 ℃ and the amount of tert-butyl alcohol 30 mL, the conversion of cyclohexane The rate of 88.37%, the total yield of cyclohexanol and cyclohexanone up to 16.56%.