应用化学 ›› 2010, Vol. 27 ›› Issue (04): 428-431.DOI: 10.3724/SP.J.1095.2010.90272

• 研究论文 • 上一篇    下一篇

溶胶-凝胶法制备负载磷钼杂多酸铵催化苯硝化反应

龚树文1*,王向宇2,李考真1,崔庆新1,邓秀娟1   

  1. (1.聊城大学化学化工学院 聊城 252059;2.郑州大学化学系 郑州)
  • 收稿日期:2009-04-14 修回日期:2009-06-30 出版日期:2010-04-10 发布日期:2010-04-10
  • 通讯作者: 龚树文,男,副教授; E-mail:gongshw@lcu.edu.cn; 研究方向:工业催化
  • 基金资助:
    国家自然科学基金(20771053)山东省教育厅科研基金(J09LB58)资助项目

Nitration of benzene catalyzed by supported ammonium molybdophosphat catalyst

GONG Shu-Wen1*, WANG Xiang-Yu2, LI Kao-Zhen1, CUI Qing-Xin1, DENG Xiu-Juan1   

  1. (1.College of Chemistry and Chemical Engineering,Liaocheng University,Liaocheng 252059;
    2.Department of Chemistry,Zhengzhou University,Zhengzhou)
  • Received:2009-04-14 Revised:2009-06-30 Published:2010-04-10 Online:2010-04-10

摘要:

以正硅酸乙酯为硅源,利用溶胶-凝胶法制备负载磷钼杂多酸铵催化剂(AMPA/SiO2),采用X射线衍射和红外光谱测试技术对催化剂进行了表征,并初步评价了催化剂苯硝化反应催化性能。结果表明,溶胶-凝胶法制备的AMPA/SiO2保持了磷钼酸铵(AMPA)杂多酸盐的Keggin结构。AMPA以及AMPA/SiO2催化剂均表现出较强的苯硝化反应催化活性和100 %的一硝基苯选择性,苯最高转化率为96 %。反应后负载催化剂活性组分有所损失,但催化剂整体物相和结构没有发生明显变化。

关键词: 溶胶-凝胶, 磷钼酸铵, 负载催化剂, 苯, 硝化

Abstract:

A series of supported ammonium molybdophosphat catalysts(AMPA/SiO2) with different loading was prepared from tetraethyl orthosilicate, ammonium molybdate and ammonium dihydrogen phosphate by sol-gel method. The samples were characterized by X-ray diffraction(XRD) and IR spectrometry. The catalytic activities of these catalysts were evaluated for the liquid phase nitration of benzene in 65% nitric acid without solvent at 70 ℃. Results indicate that supported catalyst still maintained the Keggin structure of ammonium molybdophosphate catalyst and exhibited high nitration reaction catalytic activity and high selectivity of mononitrobenzene. Among these catalysts, the catalyst with 10% loading showed maximum activity(96%), with 100% selectivity towards mononitrobenzene. The reusability of the catalysts was also studied, and it was found that there was no obvious change for catalyst phase and structure after being reused four times, although the active component had somewhat been lost in the reaction process.

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