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作 者:李贵贤[1] 滕志君[1] 余华[1] 宋维维[1] 樊洁[1] 尚立慧[1]
机构地区:[1]兰州理工大学石油化工学院,甘肃兰州730050
出 处:《精细化工》2009年第11期1098-1101,1110,共5页Fine Chemicals
基 金:甘肃省教育厅科研基金项目(2005GJ0281)~~
摘 要: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%。Synthesized Dawson P-Mo-V Cobalt Heteropolyacid Salts were characterized by FTIR,XRD and 31PNMR.Cyclohexane was oxidated to cyclohexanol and cyclohexanone under the conditions with cyclohexane as the raw material,H2O2 as the oxidant and the cobalt substitute for dawson P-Mo-V cobalt heteropolyacid salts as catalysts.The reaction conditions such as the type of catalyst,the amount of catalyst and H2O2,reaction time and temperature were investigated.Experimental results show that Co2H5P2Mo15V3O62 has the highest activity of catalysts,The conversion of cyclohexane was 88.37% and the total yield of cyclohexanol and cyclohexanone was 16.56% under the conditions of the amount of Co2H5P2Mo15V3O62catalyst 0.20 mmol,H2O2 with w(H2O2)=50% amounting to 0.2 mol,reaction time 10 h,the temperature 75 ℃.
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