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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (23): 2471-2476. 上一篇    下一篇

研究论文

萃取法脱除介孔磷酸镍模板剂的研究

王业红, 谭涓, 刘靖, 陈颖, 李旭影   

  1. (大连理工大学精细化工重点实验室 大连 116012)
  • 投稿日期:2010-03-22 修回日期:2010-06-03 发布日期:2010-08-09
  • 通讯作者: 王业红 E-mail:wyh20707278@yahoo.cn
  • 基金资助:

    新型介孔磷酸镍的合成、结构和选择氧化机理研究

Removal of Template from Mesostructured Nickel Phosphates by Solvent Extraction

WANG Ye-Hong, TAN Juan, LIU Jing, CHEN Ying, LI Xu-Ying   

  1. (State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012)
  • Received:2010-03-22 Revised:2010-06-03 Published:2010-08-09
  • Supported by:

    Synthesis,structure and oxidation mechanism of novel mesoporous nickel phosphates

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1487

被引次数

15

采用溶胶-凝胶法, 以十六烷基三甲基溴化铵(CTAB)为模板剂合成了介孔磷酸镍NiPO-1和NiPO-2, 并采用溶剂萃取法进行了模板剂的脱除. 采用XRD, IR, CHN元素分析以及N2吸附等手段研究了不同萃取剂体系、温度、萃取剂浓度及萃取次数对介孔磷酸镍(NiPOs)骨架结构和模板剂脱除率的影响. 结果表明: 在0.1 mol/L CH3COONa/EtOH为萃取剂, 78 ℃下交换4次, 每次1 h 条件下, NiPO-1和NiPO-2中模板剂的去除率均超过97%. 萃取后介孔材料保持了较好的完整性和有序度. 萃取后样品的衍射峰强度增大, 主衍射峰d100值亦增大主要是由于萃取过程中, 在较高的温度下NiPOs的纳米管簇结构在萃取剂中有溶胀作用|氮气吸附表明萃取后NiPO-1和NiPO-2的比表面可分别达309.5 m2•g－1和263.9 m2•g－1.

关键词: 介孔材料, 磷酸镍, 脱除模板剂, 萃取, CTAB

The mesostructured nickel phosphates, NiPO-1 and NiPO-2, were synthesized with cetyltrimethylammonium bromide (CTAB) as a template via sol-gel method. The template was removed by solvent extraction in order to make their mesopores accessible. The influence of extractant, temperature, concentration and repetitions on the mesostructure and the removal efficiency were studied and optimized by XRD, FT-IR, CHN element analysis and N2 adsorption techniques. The removal of the template in NiPO-1 and NiPO-2 exceeded 97% by using 0.1 mol/L CH3COONa/EtOH as an extractant under 78 ℃ for 1 h and repeated for 4 times. The integrity and the ordering of the mesostructure were maintained. In the XRD patterns of the extracted samples, the diffraction intensity of (100) increased significantly, while the d100 space also increased owing to the swelling behavior of the nanotubes in the extractant under elevating temperature. The results of N2 adsorption showed that the surface areas of the extracted NiPO-1 and NiPO-2 reached 309.5 m2•g－1 and 263.9 m2•g－1 respectively.

Key words: mesoporous material, nickel phosphate, template removal, extraction, CTAB