摘要
采用分沉淀-共浸渍法制备了新型稀土固体超强酸SO42-/ZrO2-SnO2-Nd2O3,利用IR、TG-DTA、XRD测试技术表征了催化剂的物化性质,并用于催化乙酸酐和松油醇合成乙酸松油酯,显示了良好的反应活性和重复使用性。对反应条件进行优化的结果表明,n(松油醇)∶n(乙酸酐)=1∶1.5,反应温度50℃,反应时间5 h,催化剂用量占松油醇质量分数的2%,在此反应条件下松油醇的转化率为93%左右,产物中乙酸松油酯的含量为88%。催化剂失活主要原因是由于有机物在表面吸附,通过无水乙醇洗涤,干燥,即可再生。
Rare earth solid superacid catalyst SO4^2-/ZrO2-SnO2-Nd2O3 is prepared by precipitation-co-impregnation method. The obtained catalyst if characterized by IR, TG-DTA and XRD, and used to the synthesis of terpinyl acetate. The results show that catalyst SO4^2-/ZrO2-SnO2-Nd2O3 has an excellent reactivity and reusability. Factors influencing the esterification are investigated, and the optimum reaction conditions have been found ： the molar ratio between terpineol and acetic anhydride is 1. 0： 1.5, the reaction temperature is 50℃ and the reaction time is 5 h, the amount of catalyst is 2% of the mass of terpineol. Under the optimum conditions, the conversion of terpineol is about 93%, the content of terpinyl acetate in the product is 88%. The main reason of the catalyst deactivation is that the active sites are covered by organic materials coming from reacting solution. The catalyst can be regenerated by alcohol washing and drying at 110 ℃ for 12 h.
出处
《应用化学》
CAS
CSCD
北大核心
2009年第5期576-581,共6页
Chinese Journal of Applied Chemistry
基金
广东省自然科学基金资助项目(7010338)
广东省科技厅资助项目(2005B40703004)
广东林产化工星火技术产业带项目(2006B23003)
