Chemical Industry and Engineering Progree ›› 2016, Vol. 35 ›› Issue (01): 145-149.DOI: 10.16085/j.issn.1000-6613.2016.01.019

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Preparation,characterization of Cu2H2P2W18O62·nH2O/diatomite and its catalytic performance on the synthesis of tetrahydrofuran

CAO Xiaohua1,2   

  1. 1 Jiangxi Provincial Engineering Research Center of Ecological Chemical Industry, Jiujiang 332005, Jiangxi, China;
    2 College of Chemical and Environmental Engineering, Jiujiang University, Jiujiang 332005, Jiangxi, China
  • Received:2013-08-05 Revised:2013-10-28 Online:2016-01-05 Published:2016-01-05

Cu2H2P2W18O62·nH2O/硅藻土催化剂的制备、表征及其催化绿色合成四氢呋喃

曹小华1,2   

  1. 1 江西省生态化工工程技术研究中心, 江西 九江 332005;
    2 九江学院化学与环境工程学院, 江西 九江 332005
  • 通讯作者: 曹小华(1978-),男,博士,副教授,从事多酸化学与石油化工研究。E-mail::caojimmy@126.com。
  • 作者简介:曹小华(1978-),男,博士,副教授,从事多酸化学与石油化工研究。E-mail::caojimmy@126.com。
  • 基金资助:
    国家自然科学基金(21161009)、江西省自然科学基金(20132BAB203004,20122BAB213001)、江西省教育厅科技项目(GJJ13723)及九江学院科技项目(2013KJ005)。

Abstract: Diatomite supported dawson structure copper phosphotungstate (40%Cu2H2P2W18O62·nH2O/diatomite) was prepared by liquid impregnation and was characterized with fourier transforming infrared spectrum (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-Ray spectroscopy(EDS). Then it was used to catalyze the cyclodehydration of 1, 4-butanediol to prepare tetrahyfrofuran (THF). The effects of catalyst dosage, reaction temperature, reaction time and catalyst reusability were investigated. The results showed that Cu2H2P2W18O62·nH2O were spherical and distributed evenly on the surface of the diatomite supports which were holemesh-shaped. Copper phosphotungstate kept in the dawson structure before or after supported on the diatomite carrier. Under the optimal reaction conditions, i.e. the mass ratio of catalyst to 1, 4-butanediol 2.3%, reaction temperature 185℃ and reaction time 35min, the yield of THF reached 94.8%. Even used for six times, the catalyst made the yield of THF reach 86.5%. Cu2H2P2W18O62·nH2O/diatomite catalyst showed good activity, stability and simple process to prepare, providing a new route for the synthesis of THF.

Key words: copper phosphotungstate, diatomite, catalyst support, catalysis, tetrahydrofuran

摘要: 利用液相浸渍法制备出新型硅藻土负载Dawson结构磷钨酸铜催化剂(40%Cu2H2P2W18O62·nH2O/硅藻土),并对其进行FTIR、XRD、SEM及EDS表征。以40%Cu2H2P2W18O62·nH2O/硅藻土为催化剂,催化1,4-丁二醇合成四氢呋喃,考察了各相关因素对四氢呋喃收率的影响。结果表明:磷钨酸铜呈球状,比较均匀地负载在圆筛型的硅藻土载体上,且负载前后均保持Dawson结构。在优化反应条件下即:w(催化剂)=2.3%(相对1,4-丁二醇质量),温度为185℃,时间为35min,四氢呋喃收率为94.8%。催化剂重复使用6次,四氢呋喃收率仍可保持在86.5%。催化剂具有良好的活性及稳定性,工艺简单,为四氢呋喃的绿色合成提供了新的途径。

关键词: 磷钨酸铜, 硅藻土, 催化剂载体, 催化, 四氢呋喃

CLC Number: 

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