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Citation: CAO Xiaohua, REN Jie, LIU Minsheng, XU Changlong, YAN Ping. Preparation of Tungstomolybdophosphate Acid with Dawson Structure and Its Catalytic Activity for the Synthesis of Adipic Acid via Hydrogen Peroxide Oxidaton of Cyclohexanone[J]. Chinese Journal of Applied Chemistry, ;2012, 29(8): 915-920. doi: 10.3724/SP.J.1095.2012.00408 shu

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

CAO Xiaohua ^a,b ,
REN Jie ^a,, ,
LIU Minsheng ^c,, ,
XU Changlong ^b ,
YAN Ping ^b

1.
a College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China;
2.
b College of Chemistry and Chemical Engineering, Jiujiang University, Jiujiang 332005, China;
3.
c College of Bio-Chemical and Environmental Engineering, Xiaozhuang University, Nanjing 211171, China

Corresponding author: REN Jie, LIU Minsheng,
Received Date: 13 September 2011
Available Online: 23 November 2011
Fund Project: 国家自然科学基金(21161009) (21161009)江西省自然科学基金(20114BAB213002,2009GQH0053) (20114BAB213002,2009GQH0053)江西省教育厅科技(GJJ10626,GJJ11613)资助项目 (GJJ10626,GJJ11613)

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.
- H₆P₂W₉Mo₉O₆₂·24H₂O,
- hydrothermal synthesis,
- microwave irradiation,
- adipic acid,
- cyclohexanone
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