(CaO-MgO)@Fe3O4/C磁性固体碱催化甘油制备碳酸甘油酯
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Catalytic Performance of magnetic (CaO-MgO)@Fe3O4/C solid base catalyst for Glycerol carbonate production from Glycerol
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    摘要:

    通过共沉淀法制得磁性均相固体碱催化剂((CaO-MgO)@Fe3O4/C),磁核通过用活性炭N2气氛下还原得到。采用甘油制备碳酸甘油酯作为探针反应,考察了(CaO-MgO)@Fe3O4/C催化剂的催化性能碳酸甘油酯的收率高达98.80%,甘油的转换率达到95.20%。对磁性均相固体碱催化剂((CaO-MgO)@Fe3O4/C)进行了磁滞回线、X射线衍射(XRD)、透射电镜(TEM)、CO2-TPD及N2的吸附-脱附(BET)等表征。结果表明,CaO-MgO可以很好的包裹磁核Fe3O4/C,并且催化剂还具有较好的碱强度,催化剂显示出较好的磁性,磁化强度为23.8emu/g。进一步考察了不同的反应条件对碳酸甘油酯的影响。结果表明,最佳反应条件为反应温度为85oC,反应时间为1h,碳酸二甲酯和甘油的摩尔比为5:1,催化剂的用量为3%。催化剂在重复使用5次后,仍具有优良的性能,碳酸甘油酯的收率为94.45%。

    Abstract:

    Magnetic heterogeneous catalyst ((CaO-MgO)@Fe3O4/C) was prepared for co-precipitation methods and magnetic core Fe3O4/C was reduced by activated carbon under N2 atmosphere. The reaction of glycerol carboante prepared using glycerol as a probe reaction, it is investigated that the catalytic performance of (CaO-MgO)@Fe3O4/C catalyst. With (CaO-MgO)@Fe3O4/C catalyst, glycerol carbonate yield reached 98.80% and glycerol conversion reached 95.20%. The (CaO-MgO)@Fe3O4/C catalyst was characterized by magnetic hysteresis loop, X-ray diffraction (XRD), CO2-TPD and transmission electron microscopy (TEM) and BET. The results indicated that Fe3O4/C was well wrapped (CaO-MgO); the (CaO-MgO)@Fe3O4/C catalyst exhibited good magnetic properties with high saturation magnetization (23.8emu/g) and the (CaO-MgO)@Fe3O4/C catalyst had strong basicity. The different reaction conditions on the yield of glycerol carbonate were investigated. The optimal reaction conditions were as follows: the reaction temperature was 85 oC and the reaction time was 1h, the molar ratio of DMC/glycerol was 5:1 and the catalyst dosage was 5.0wt. %. The catalyst still had steadily catalytic performance after 5 cycles with a high glycerol carbonate yield of 94.45%.

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张萍波,柳利花,范明明,蒋平平.(CaO-MgO)@Fe3O4/C磁性固体碱催化甘油制备碳酸甘油酯[J].精细化工,2017,34(3):

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  • 收稿日期:2016-07-08
  • 最后修改日期:2016-11-21
  • 录用日期:2016-12-07
  • 在线发布日期: 2017-02-09
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