SiO2负载Ti(SO4)2-Zr(SO4)2复合固体酸催化剂的制备及催化性能

石油炼制与化工 ›› 2013, Vol. 44 ›› Issue (8): 23-28.

SiO2负载Ti(SO4)2-Zr(SO4)2复合固体酸催化剂的制备及催化性能

刘养春,钟宏,王帅,黄志强

中南大学化学化工学院

收稿日期:2012-11-12 修回日期:2013-01-15 出版日期:2013-08-12 发布日期:2013-07-25
通讯作者: 钟宏 E-mail:zhongh@mail.csu.edu.cn
基金资助:
国家高技术研究发展计划（863）项目

PREPARATION AND CATALYTIC PERFORMANCE OF Ti (SO4)2-Zr (SO4)2/SiO2 SOLID ACID CATALYST

Received:2012-11-12 Revised:2013-01-15 Online:2013-08-12 Published:2013-07-25

摘要/Abstract

摘要： 以Ti(SO4)2和Zr(SO4)2为活性组分，以SiO2为载体，通过浸渍法制备复合固体酸催化剂Ti(SO4)2-Zr(SO4)2/SiO2。采用TG、酸量分析、FT-IR、XRD等方法对催化剂进行表征，考察焙烧温度、活性组分负载量对催化剂性能的影响。结果表明，催化剂制备的适宜条件为：焙烧温度300 ℃、焙烧时间3 h、活性组分负载量50%。将制备的催化剂用于油酸甲酯的合成反应，在催化剂用量20 g/mol、醇酸摩尔比4、反应时间5 h、反应温度85 ℃的条件下，酯化率达到95.6%。催化剂的重复使用性能考察结果表明，在不经处理的条件下连续使用5次后，酯化率下降到80%以下。对失活催化剂的红外光谱分析结果表明，积炭是催化剂失活的主要原因，可通过焙烧、补充活性组分恢复其催化性能。

Abstract: Silica-supported titanic sulfate and zirconium sulfate solid acid catalyst (Ti(SO4)2-Zr(SO4)2/SiO2) was prepared by impregnation method. The supported catalyst was characterized by TG, acidimetric analysis, FT-IR and XRD. The effects of calcination and loading amount on the catalyst activity were investigated. The results indicate that the catalyst prepared has a esterification rate of 95.6% at the conditions of m(catalyst)2.0g/0.1mol oleic acid, ratio of methanol to oleic acid 4, reaction temperature 85℃ and reaction time 5h. It is found after the catalyst was continuously used for 5 times, the esterification rate drops to below 80% because of coking，proved by infrared analysis of deactivated catalyst, but the activity of the catalyst can successfully recovered after activation by roasting and/or supplementing certain amount of active components needed.

刘养春钟宏王帅黄志强. SiO2负载Ti(SO4)2-Zr(SO4)2复合固体酸催化剂的制备及催化性能[J]. 石油炼制与化工, 2013, 44(8): 23-28.