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磷钨钼杂多酸催化清洁氧化环己酮合成己二酸

Clear Oxidation of Cyclohexanone to Adipic Acid Catalyzed by Tungstomolybdophosphate acid

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【作者】 严平徐常龙曹小华占昌朝雷艳虹

【Author】 Yan Ping 1 ,Xu Changlong 2* ,Cao Xiaohua 1 ,Zhan Changchao 1 , Lei Yanhong 1 1 College of Chemistry and Environmental Engineering, 2 College of life of science, Jiujiang University, Jiujiang Jiangxi 332000,China

【机构】 九江学院化环学院九江学院生命科学学院

【摘要】 <正>采用水热法制备了新型磷钨钼杂多酸催化剂,并对其进行FT-IR、TG-DTA表征,用它催化30%H2O2氧化环己酮制备己二酸。通过正交实验确定了优化工艺条件,并探讨了反应机理。结果表明,当n(环己酮):n(过氧化氢):n(草酸):n(催化剂)=100:350:1.00:0.15,反应温度100℃,反应时间4h,进行三次平行实验,己二酸产品的收率可达70.5%,纯度可达99.6%。反应结束后,将含有催化剂的液体相浓缩至一定浓度,催化剂重复使用至第5次,收率为50.1%。

【Abstract】 Tungstomolybdophosphate acid was prepared by hydrothermal synthesis and characted by means of FT-IR, TG-DTA. The synthesis of adipic acid with cyclohexanone and 30 percent hydrogen peroxide was carried out as a probe reaction to study the catalytic activity. The main effects of the reaction were optimized with orthogonal experiments, the mechanism was proposed. The results showed that under the optimal condition, i.e. the mole ratio of C6H10O:H2O2:H2C2O4:H6P2W9Mn9O62·nH2O=100:350: 1.00:0.15, the reaction temperature was 100℃, irradiation time 4 h, the isolated yield of adipic acid could reach 70.5% and its purity was 99.6%. The filtration containing the catalyst could be concentrated by the rotary evaporation and be reused five times by easily separation of the product after reaction, the isolated yield of adipic acid was still above 50.1%.

【关键词】 磷钨钼杂多酸环己酮己二酸
【基金】 国家自然科学基金(21161009);江西省自然科学基金(20132BAB203004;20122BAB213001);江西省教育厅科技资助项目(GJJ10626;GJJ11613)
  • 【会议录名称】 中国化学会第五届全国多酸化学学术研讨会论文摘要集
  • 【会议名称】中国化学会第五届全国多酸化学学术研讨会
  • 【会议时间】2013-07-15
  • 【会议地点】中国黑龙江哈尔滨
  • 【分类号】O623.613
  • 【主办单位】中国化学会、国家自然科学基金委员会
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