催化学报 ›› 2008, Vol. 29 ›› Issue (7): 629-632.

• 研究论文 • 上一篇    下一篇

1-丁基-3-甲基咪唑磷钨酸盐的制备及其对酯化反应的催化性能

施介华1,2,潘高1   

  1. 1 浙江工业大学药学院, 浙江杭州 310032; 2 浙江工业大学绿色合成技术国家重点实验室培育基地, 浙江杭州 310032
  • 收稿日期:2008-07-25 出版日期:2008-07-25 发布日期:2012-06-07

Preparation of 1-Butyl-3-methylimidazolium Dodecatungstophosphate and Its Catalytic Performance for Esterification of Ethanol and Acetic Acid

SHI Jiehua1,2*, PAN Gao1   

  1. 1 College of Pharmaceutical Sciences, Zhejiang University of Technology, Hangzhou 310032, Zhejiang, China; 2 State Key Laboratory Breeding Base of Green Chemistry Synthesis Technology, Zhejiang University of Technology, Hangzhou 310032, Zhejiang, China
  • Received:2008-07-25 Online:2008-07-25 Published:2012-06-07

摘要: 以溴化1-丁基-3-甲基咪唑盐([bmim]Br)和磷钨酸(H3PW12O40)为原料制备了1-丁基-3-甲基咪唑磷钨酸盐([bmim]3PW12O40)催化剂,并用傅里叶变换红外光谱、热重分析-差示扫描量热法、正丁胺电位滴定及元素分析等技术对催化剂进行了表征,考察了催化剂对乙醇与乙酸酯化合成乙酸乙酯反应的催化活性. 结果表明, [bmim]3PW12O40中有3个结晶水,并保持有H3PW12O40的Keggin结构和酸强度, [bmim]3PW12O40的酸量明显少于H3PW12O40的酸量. 在乙醇与乙酸酯化合成乙酸乙酯反应中, [bmim]3PW12O40催化剂具有较高的催化活性和较好的重复使用性能.

关键词: 溴化1-丁基-3-甲基咪唑盐, 磷钨酸, 杂多酸, 1-丁基-3-甲基咪唑磷钨酸盐, 乙醇, 乙酸, 酯化反应, 乙酸乙酯

Abstract: A 1-butyl-3-methylimidazolium dodecatungstophosphate ([bmim]3PW12O40) catalyst with high resistance to water was prepared from 1-butyl-3-methylimidazolium bromide ([bmim]Br) and dodecatungsto-phosphoricacid (H3PW12O40). The catalyst was characterized by means of Fourier transform infrared spectroscopy, thermogravimetry-differential scanning calorimetry, n-BuNH2 potentiometric titration, and elemental analysis. Its catalytic activity for esterification of ethanol and acetic acid to ethyl acetate was measured. The results showed that there were three crystal-water molecules in the [bmim]3PW12O40catalyst, and it preserved the primary Keggin structure and acid strength of H3PW12O40. The acid amount of the [bmim]3PW12O40catalyst was less than that of H3PW12O40. The [bmim]3PW12O40catalyst exhibited higher catalytic activity and reusability in the esterification of ethanol and acetic acid to ethyl acetate.

Key words: 1-butyl-3-methylimidazolium bromide, dodecatungstophosphoric acid, heteropolyacid, 1-butyl-3-methylimidazolium dodecatungstophosphate, ethanol, acetic acid, esterification, ethyl acetate