硫酸铵改性粉煤灰催化合成环己酮乙二醇缩酮.pdf

学兔兔 化 工 进 展 2009年第28卷第3期 CHEMICAL INDUSTRY AND ENGINEERING PROGRESS ·499· 硫酸铵改性粉煤灰催化合成环己 -．醇缩酮 刘贤响，杨 柱，袁治冶，尹笃林，王季惠 (资源精细化与先进材料湖南省高校重点实验室，湖南师范大学精细催化合成研究所，湖南 长沙 410081) 摘 要：以粉煤灰(FA)为原料制备了一种新型的固体酸催化剂，用X射线衍射、热分析和红外光谱等手段表征 了催化剂的物化性能。研究了催化剂在环己酮与乙二醇的缩合反应中的催化性能，系统考察了带水剂种类、带水 剂用量、酮醇量比、催化剂用量、反应时间等因素对缩酮产率的影响。通过正交实验得出了最佳反应条件：n(环 己酮)： (乙二醇)=1：1．4、催化剂用量为环己酮质量的2％、带水剂环己烷用量10．0 mL、反应时间2 h，缩酮产 率可达99．6％。该催化剂活性较高，可重复使用。 关键词：粉煤灰；硫酸铵；固体酸；环己酮乙二醇缩酮 中图分类号：TQ 244．2 文献标识码：A 文章编号：1000—6613(2009)03—0499—05 Synthesis of cyclohexanone glycol ketal with fly ash catalyst modified by ammonium sulfate L／UXianxiang，YANGZhu，YUANZhiye，YINDulin，WANGJihui (The Key Lab of Resources Fine—Processing and Advanced Materials of Hunan Province，Institute of Fine Catalysis and Synthesis，Hunan Normal University，Changsha 410081，Hunan，China) Abstract：Cyclohexanone gbrcol ketal was synthesis from cyclohexanone and ethylene glycol in the presence of a late—model catalyst．which was prepared with fly ash as raw materia1．T|le catalysts were characterized by means of XRD．TG and FTIR．Various reaction parameters．such as the molar ratio of cyclohexanone to ethylene glycol，amount of catalyst，reaction time，water—carrying reagent and other factors influencing the synthesis were discussed and the optimum conditions was established．The results showed that molar ratio of cyclohexanone to ethylene glvcol was 1：1．4，the am ount of catalyst was 2％ cyclohexanone，amount of cyclohexane was 10 mL，the reaction time 2 h．the yield of cvclOhexanOne ethylene k