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Dawson型磷钨钼杂多酸的制备及其对H2O2氧化环己酮制己二酸的催化

曹小华1,2,任杰1*,柳闽生3*,徐常龙2,严平2   

  1. (1.浙江工业大学化工与材料学院 杭州 310014；2.九江学院化学与环境工程学院 九江 332005；
    3.南京晓庄学院生物化工与环境工程学院 南京 211171)
  • 收稿日期:2011-09-13 修回日期:2011-11-23 出版日期:2012-08-10 发布日期:2012-08-10
  • 通讯作者: 任杰，教授; Tel:0571-88320208; Fax:0571-88320238; E-mail:Renjie.R@263.net; 研究方向：石油化工
  • 基金资助:
    国家自然科学基金(21161009)江西省自然科学基金(20114BAB213002,2009GQH0053)江西省教育厅科技(GJJ10626，GJJ11613)资助项目

Preparation of Tungstomolybdophosphate Acid with Dawson Structure and Its Catalytic Activity for the Synthesis of Adipic Acid via Hydrogen Peroxide Oxidaton of Cyclohexanone

CAO Xiaohua1,2, REN Jie1*, LIU Minsheng3*, XU Changlong2, YAN Ping2   

  1. (1.College of Chemical Engineering and Materials Science，
    Zhejiang University of Technology，Hangzhou 310014，China；
    2.College of Chemistry and Chemical Engineering,Jiujiang University,Jiujiang 332005,China；
    3.College of Bio-Chemical and Environmental Engineering,Xiaozhuang University,Nanjing 211171,China)
  • Received:2011-09-13 Revised:2011-11-23 Published:2012-08-10 Online:2012-08-10
  • Contact: xu changlong

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摘要： 采用水热法制备了新型H6P2W9Mo9O62·24H2O催化剂，并用UV-Vis、FT-IR和TG-DTA等测试技术对催化剂进行了表征。 以微波促进30%过氧化氢氧化环己酮制备己二酸合成反应为探针，考察了催化剂的催化性能。 通过正交实验探讨了几种因素对反应的影响，确定了优化工艺条件为:n(环己酮)∶n(过氧化氢)∶n(草酸)∶n(催化剂)=100∶400∶1.25∶0.25，反应温度100 ℃，微波辐射功率400 W，反应时间3.5 h，己二酸产品的收率达87.33%，纯度可达99.7%。 反应结束后，将反应后含催化剂的溶液浓缩至一定浓度，催化产率降低，重复使用5次收率降低为45.89%。

关键词: H6P2W9Mo9O62·, 24H2O, 水热合成, 微波, 己二酸, 环己酮

Abstract: Tungstomolybdophosphate acid with Dawson structure was prepared by hydrothermal synthesis and characterized by means of FT-IR, UV-Vis and TG-DTA. The synthesis of adipic acid from the reaction of cyclohexanone with 30% hydrogen peroxide under microwave irradiation was used as a probe to study the catalytic activity of tungstomolybdophosphate acid. The main effects of the reaction were optimized with orthogonal experiments. The results show that under the optimal conditions, i.e. the molar ratio of C6H10O∶H2O2∶H2C2O4∶H6P2W9Mo9O62·24H2O=100∶400∶1.25∶0.25, 100 ℃ for the reaction temperature, 400 W for the microwave power, and 3.5 h for the irradiation time, the isolated yield of adipic acid can reach 87.33% with a purity of 99.7%. The filtration containing the catalyst can be concentrated by the rotary evaporation and be reused five times by facile separation of the product after reaction, with an isolated yield of above 45.89% for adipic acid.

Key words: H6P2W9Mo9O62·, 24H2O, hydrothermal synthesis, microwave irradiation, adipic acid, cyclohexanone

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