石油炼制与化工 ›› 2013, Vol. 44 ›› Issue (7): 53-58.

• 催化剂 • 上一篇    下一篇

盐酸预处理对精对苯二甲酸精制用Pd/c催化剂微观结构的影响

肖发新1,2,3,任永鹏2,李岩松1,徐新阳3   

  1. 1. 沈阳有色金属研究院
      2. 河南科技大学材料科学与工程学院
      3. 东北大学资源与土木工程学院
  • 收稿日期:2012-12-19 修回日期:2013-02-22 出版日期:2013-07-12 发布日期:2013-06-27
  • 通讯作者: 肖发新 E-mail:hkdxfx@163.com
  • 基金资助:

    河南省教育厅自然科学研究基金;河南科技大学青年科学基金;国家自然科学基金

INFLUENCE OF HCl PRETREATMENT ON MICROSTRUCTURE OF Pd/C PTA REFINING CATALYST

  • Received:2012-12-19 Revised:2013-02-22 Online:2013-07-12 Published:2013-06-27

摘要: 采用不同浓度的盐酸对椰壳活性炭预处理,然后以浸渍法制备精对苯二甲酸(PTA)精制用Pd/C催化剂。通过SEM,EDS,TEM,XRD及氮气吸附脱附测试等手段,研究盐酸预处理对Pd/C催化剂微观结构的影响,并探讨盐酸浓度与催化剂活性的关系。结果表明,活性炭载体经盐酸预处理后所得Pd/C催化剂的活性随盐酸浓度的增加呈先增大后减小的趋势,在盐酸浓度为0.6 mol/L时达到最佳。SEM和吸附脱附结果均表明,盐酸预处理使Pd/C催化剂平均孔径有所增大,后者中孔孔体积有所增加。能谱测试结果表明,盐酸预处理后,催化剂Pd含量变化不大,但由于盐酸对孔结构造成的改变,使得表面下的活性炭基体曝露出来,出现O及微量杂质Si、Cl元素。盐酸预处理对Pd/C催化剂物相的影响尚未发现。由于盐酸预处理增加孔径及中孔孔体积,从而增大有效负载面积,促进Pd在载体上的分散,从而提高了催化剂的活性。

Abstract: A commercial coconut activated carbon was firstly pretreated by HCl with different concentrations. Then the Pd/C catalyst used for purification of terephthalic acid was prepared using immersion method based on the pretreated carbon. By means of SEM, EDS, TEM, XRD and BET techniques, the impact of HCl pretreatment on microstructure and activity of the catalysts was investigated, and the relationship between HCl concentration and catalyst activity was explored. Test results show that the catalytic activity first increases and then decreases with the increase of HCl concentration and the maximum activity was obtained at the HCl concentration of 0.6mol/L. SEM and adsorption-desorption tests show that the pretreatment of HCl can increase the average pore diameter and the mesopore volume of activated carbon. The EDS result indicates that the content of Pd maintains nearly constant, while some O element and trace impurity of Si and Cl appear on the carbon surface after HCl pretreatment. The changes of the surface morphology of HCl pretreated active carbon are not found. Owing to the increase of pore diameter and mesopore volume, the effective surface area of carbon for loading Pd component is increased, which is beneficial to the dispersity of Pd, and to the catalytic activity of Pd/C catalyst.