催化学报 ›› 2006, Vol. 27 ›› Issue (11): 1028-1032.

• 研究论文 • 上一篇    下一篇

后处理法合成高热稳定性的中孔Ti-P-Al材料

刘子玉1,2,魏迎旭1,齐越1,刘中民1   

  1. 1 中国科学院大连化学物理研究所, 辽宁大连 116023; 2 中国科学院研究生院, 北京 100049
  • 收稿日期:2006-11-25 出版日期:2006-11-25 发布日期:2006-11-25

Synthesis of Mesoporous Ti-P-Al Material with High Thermal Stability by Post-Synthetic Treatment

LIU Ziyu1,2, WEI Yingxu1, QI Yue1, LIU Zhongmin1*   

  1. 1 Dalian Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116023, Liaoning, China; 2 Graduate University of The Chinese Academy of Sciences, Beijing 100049, China
  • Received:2006-11-25 Online:2006-11-25 Published:2006-11-25

摘要: 以阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)为模板剂,采用水热合成法制备了中孔氧化钛原粉,再采用磷酸和氯化铝溶液依次对中孔氧化钛原粉进行后处理,得到了具有高热稳定性的中孔Ti-P-Al材料. 通过粉末X射线衍射、透射电子显微镜和氮物理吸附等方法对样品进行了表征. 结果表明,反应凝胶组成对样品的中孔结构有较大的影响,当反应凝胶配比为Ti(SO4)2∶CTAB∶H2O=1∶0.54∶430, 温度为363 K, 处理时间为10~20 min时,所得的TiO2原粉具有较规整的中孔结构. 此样品经过0.25 mol/L的磷酸处理后有序性有较大程度的提高. 将磷酸处理过的样品进一步用氯化铝溶液处理,得到了中孔结构的Ti-P-Al材料,此材料经过873 K焙烧后仍具有典型的中孔特征,其比表面积为 382 m2/g, 孔径为3.13 nm.

关键词: 钛, 磷, 铝, 中孔材料, 后处理, 热稳定性

Abstract: Mesostructured TiO2 was prepared hydrothermally using cetyltrimethylammonium bromide (CTAB) as the structure directing agent, and the mesoporous Ti-P-Al material with high thermal stability was subsequently synthesized by a two-step post-synthetic treatment. The sample was characterized by powder X-ray diffraction, transmission electron microscopy, and N2 adsorption. It was found that the composition of the starting gel system greatly affected the mesostructure of TiO2 materials greatly. With the gel composition of Ti(SO4)2∶CTAB∶H2O=1∶0.54∶430 and after being treated at 363 K for 10-20 min, an ordered TiO2 mesostructure was obtained, which presented better long-range order after being treated with 0.25 mol/L phosphoric acid solution. Further treatment with AlCl3 solution resulted in a mesoporous Ti-P-Al material with high thermal stability, which had a high BET specific surface area of 382 m2/g and a pore size of 3.13 nm after calcination at 873 K.

Key words: titanium, phosphorus, aluminium, mesoporous material, post-synthetic treatment, thermal stability