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Chinese Journal of Organic Chemistry >

2013 , Vol. 33 >Issue 05: 1035 - 1041

DOI: https://doi.org/10.6023/cjoc201210040

Articles

Dehydration of 1,4-Butanediol to Tetrahydrofuran Catalyzed by H6P2W18O62/Diatomite

  • Cao Xiaohua ,
  • Ren Jie ,
  • Liu Minsheng ,
  • Zhan Changchao ,
  • Xie Baohua
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  • a College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014;
    b College of Chemical and Environmental Engineering, Jiujiang University, Jiujiang 332005;
    c School of Biochemical and Environmental Engineering, Nanjing Xiaozhuang University, Nanjing 211171

Received date: 2012-12-21

  Revised date: 2013-01-06

  Online published: 2013-01-11

Supported by

Project supported by the National Natural Science Foundation of China (No. 21161009), the Natural Science Foundation of Jiangxi Province (Nos. 20114BAB213002, 20122BAB213001), the Science and Technology Foundation of Educational Commission of Jiangxi Province (Nos. GJJ10626, GJJ11613).

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Abstract

Diatomite supported Dawson-type phosphotungstic acid catalysts with diferent loadings were prepared by the incipient impregnation method and characterized by FT-IR, UV-Vis, XRD, SEM, EDS, TG and Py-IR. Their catalytic behaviors were investigated via the cyclodehydration of 1,4-butanediol to synthesize tetrahydrofuran. The reaction conditions for tetrahydrofuran synthesis were optimized, and the stability of H6P2W18O62/Diatomite in the cyclodehydration reaction was investigated. The catalysts showed both Brönsted and Lewis acidity, and the catalyst with 40% H6P2W18O62 loading had the highest total acidity and catalytic activity because of the monolayer coverage of the active species. 97.1% yield of tetrahydrofuran could be obtained under the reaction conditions of 180 ℃ for 45 min, catalyst amount 3.2% of 1,4-butanediol. These catalysts could be recycled and still exhibited catalytic activity with a yield of 62.9% after five cycle reactions. It was found by means of UV-Vis, TG-DTA and Py-IR that the catalyst deactivation was due to the dissolution of H6P2W18O62 and decrease of the acid sites, which was caused by coking on catalyst surface. Compared with using sulfuric acid as catalyst, the present procedure is a green productive technology characterized by process simplification, higher yield and no corrosion for facilities. Moreover, the H6P2W18O62/Diatomite can be used for many times.

Key words： diatomite; phosphotungstic acid; dawson-type; tetrahydrofuran; catalytic behavior

Cite this article

Cao Xiaohua , Ren Jie , Liu Minsheng , Zhan Changchao , Xie Baohua . Dehydration of 1,4-Butanediol to Tetrahydrofuran Catalyzed by H6P2W18O62/Diatomite[J]. Chinese Journal of Organic Chemistry, 2013 , 33(05) : 1035 -1041 . DOI: 10.6023/cjoc201210040

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