应用化学 ›› 2011, Vol. 28 ›› Issue (08): 907-912.DOI: 10.3724/SP.J.1095.2011.00563

• 研究论文 • 上一篇    下一篇

稀土固体超强酸的制备及其对硬脂肪酸酯化反应的催化

饶蔚兰,潘志权*,向守信   

  1. (武汉工程大学,绿色化工过程省部共建教育部重点实验室 武汉 430073)
  • 收稿日期:2010-07-30 修回日期:2010-12-20 出版日期:2011-08-10 发布日期:2011-08-10
  • 通讯作者: 潘志权,教授; Tel:027-87194980; Fax:027-87194465; E-mail:zhiqpan@163.com; 研究方向:配位化学
  • 基金资助:
    湖北省高等学校优秀中青年科技创新团队(T200802),湖北省自然科学基金重大项目(2008CDA031)

Preparation of Rare Earth Solid Superacid and Catalysis on the Esterification Reactions of Stearic Acid

RAO Weilan, PAN Zhiquan*, XIANG Shouxin   

  1. (Key Laboratory for Green Chemical Process of Ministry of Education,
    Wuhan Institute of Technology,Wuhan 430073)
  • Received:2010-07-30 Revised:2010-12-20 Published:2011-08-10 Online:2011-08-10

摘要:

采用溶胶-凝胶法以钛酸四丁酯为原料,经水解缩聚再缩聚,并用浸渍法添加稀土Ce和La,一定温度焙烧后制得稀土掺杂纳米二氧化钛固体超强酸。 红外光谱表明,该固体超强酸中SO2-4以桥式双配位与金属氧化物结合,XRD证明固体超强酸为锐钛矿型,SEM图像证明超强酸颗粒为球形。 将该超强酸用于硬脂酸与正丁醇的酯化反应,显示出很高的催化活性。 经0.12 mol/L Ce4+的硫酸(1.0 mol/L)溶液、0.07 mol/L La3+的硫酸(1.25 mol/L)溶液浸渍10~14 h后,500~550 ℃温度下焙烧3 h的超强酸,催化硬脂肪酸正丁酯反应的酯化率分别达到97.8%和96.7%。

关键词: 溶胶-凝胶法, 锐钛型, 纳米二氧化钛, 稀土固体超强酸, 硬脂肪酸,酯化反应, 催化

Abstract:

Nanometer hybrid rare earth solid superacid was prepared by sol-gel method. Tetrabutyl titanate was hydrolyzed and condensation polymerized, then doped with rare earth elements of Ce and La, respectively, by immersion process, and activated under certain temperatures to give a nanometer hybrid rare earth solid superacid catalyst. The structure and morphology of samples were characterized by FT-IR, SEM, and XRD. The results show that the SO2-4 is bonded to the metal oxide by bridged bidentate coordination mode. XRD shows the crystal form is anatase, and SEM reveals the catalyst is globular shape. It also proves that the rare earth solid superacid catalysts exhibit high catalytic activity for the esterification of stearic acid. The precursor soaked in the solution c(Ce4+)=0.12 mol/L, c(H2SO4)=1.0 mol/L and the solution c(La3+)=0.07 mol/L, c(H2SO4)=1.25 mol/L for 10~14 h, then calcinated at 500~550 ℃ for 3 h to obtain the solid superacid catalysts. Under the optimum conditions, the yields of esterification can reach 97.8% and 96.7%, respectively, by using these catalysts.

Key words: sol-gel method, anatase, nanometer titanium dioxide, rare earth solid superacid, stearic acid, esterification reaction, catalysis

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