超重力场共沉淀法制备Cu/ZrO2催化剂的研究
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O643.3

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湖南省科技厅资助项目(2009FJ3043)


Study on preparation of Cu/ZrO2 catalyst by high gravity co-precipitation method
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    摘要:

    以硝酸铜、氧氯化锆为原料,以w(NaOH)=20%溶液为沉淀剂,采用超重力场共沉淀法,制备出用于二乙醇胺脱氢制亚氨基二乙酸的Cu/ZrO2催化剂。通过正交实验获得了较优的催化剂制备条件:超重力场反应器转速为800r/min、沉淀终点pH=12、陈化时间为5h、原料锆铜原子比为2:1和锆盐初始浓度为0.2mol/L。优化条件下制得的催化剂前驱体,经500℃焙烧5h、220~240℃下还原5h得到Cu/ZrO2催化剂。将催化剂用于二乙醇胺催化脱氢性能研究,亚氨基二乙酸钠的收率达97.50%,选择性达98.05%。将该催化剂重复使用5次,平均收率为95.02%,单程失活率为1%~2%,具有较稳定的催化活性和较长的使用寿命。且在实验室小试条件下该催化剂的催化性能优于传统共沉淀方法制备的Cu/ZrO2催化剂。

    Abstract:

    By the help of high gravity co-precipitation, with copper nitrate and zirconium oxychloride solution, using 20% sodium hydroxide as the precipitant, the Cu/ZrO2 catalyst was prepared, which was used for synthesis of iminodiacetic acid from diethanolamine via dehydrogenation. The optimal conditions were obtained by orthogonal experiments: high gravity reactor speed of 800r/min, precipitation end-point pH of 12, aging time of 5h, zirconium/copper atomic ratio of 2:1 and initial concentration of zirconium salt of 0.2mol/L. Under these optimal conditions, the catalyst precursor was roasted 5h at 500℃ and reduced 5h at 220~240℃ to obtain Cu/ZrO2 catalys. The catalyst using for the dehydrogenation effect of diethanolamine was investigated, the reaction yield of iminodiacetic acid sodium was 97.50%, selectivity can reach 98.05%. Via using repeatedly 5 times, the average reaction yield was 95.05%, and the one-way deactivation yield was 1%~2%. The results can be included that it has a relatively stable catalytic activity and long catalytic life. Compared with traditional co-precipitation method, the catalytic performance of the catalyst was better under laboratory test conditions.

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罗爱文,段正康.超重力场共沉淀法制备Cu/ZrO2催化剂的研究[J].精细化工,2011,28(1):

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  • 收稿日期:2010-08-20
  • 最后修改日期:2010-10-22
  • 录用日期:2010-10-26
  • 在线发布日期: 2010-12-13
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