石油炼制与化工 ›› 2016, Vol. 47 ›› Issue (11): 8-13.

• 催化剂 • 上一篇    下一篇

Fe3O4微球的可控制备及在合成气制低碳烯烃中的应用

刘达1,吴彤1,张征湃1,石变芳1,2   

  1. 1 华东理工大学化学工程联合国家重点实验室
    2 华东理工大学化工学院985大型仪器公共测试中心
  • 收稿日期:2016-04-13 修回日期:2016-06-11 出版日期:2016-11-12 发布日期:2016-10-27
  • 通讯作者: 石变芳 E-mail:shibf@ecust.edu.cn
  • 作者简介:2016-04-30
  • 基金资助:
    国家自然科学基金项目;中央高校基本科研业务费探索基金项目

CONTRLLABLE PREPARATION OF Fe3O4 MICROSPHERES AND THEIR APPLICATION IN LOWER OLEFINS SYNTHESIS FROM SYNGAS

    

  1.  
  • Received:2016-04-13 Revised:2016-06-11 Online:2016-11-12 Published:2016-10-27
  • Supported by:
     

摘要: 采用氯化铁为铁前躯体,通过改变溶剂热反应时间、有机醇和羧酸盐的种类等参数,可控制备了不同结构的Fe3O4微球。采用高分辨场发射扫描电镜(SEM)和X射线衍射仪(XRD)表征了微球的初级晶粒尺寸(初级粒径)和次级团簇粒径(次级粒径),利用BET法通过N2吸附-脱附测定了微球比表面积,采用H2-TPR表征了不同粒径微球在H2气氛下的还原性能,并选择不同粒径的催化剂进行合成气制备低碳烯烃的性能研究。结果表明:通过调变Fe3O4微球的制备参数,微球的初级粒径在5.6~25.1 nm范围内可调,次级粒径在149~503 nm范围内可控;随着初级粒径的减小,Fe3O4微球的比表面积增大,有利于催化剂的还原;Fe3O4微球初级粒径的减小有利于烯烃选择性的提高、CO2选择性的降低,次级粒径的减小有利于CO转化率的提高。

关键词: Fe3O4, 微球, 溶剂热反应, 低碳烯烃, 合成气

Abstract: A series of Fe3O4 microspheres with controllable structures was prepared from ferric chloride by solvothermal reaction method with different preparation parameters (solvothermal reaction times, types of alcohols and carboxylate) and characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and H2-TPR, separately to investigate the size of primary grains and secondary particles, their surface areas as well as reducibilities. The results indicate that by adjusting the preparation parameters, the size of primary grain can be controlled in the range of 5.6-25.1 nm, while the particle size of microspheres is in the range of 149-503 nm. With the decrease of grain size, the surface area of Fe3O4 microspheres increases and the reducibility is improved. It is found based on the test results of syngas to olefins that the decrease of the grain size increases the selectivity of lower olefins and decreases the CO2 selectivity. While the decrease of the microscopes particle sizes is favorable to improve CO conversion.

Key words: Fe3O4, microspheres, solvothermal reaction, lower olefins, syngas

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