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机构地区:[1]北京化工大学教育部超重力工程研究中心,北京100029
出 处:《高校化学工程学报》2015年第4期897-902,共6页Journal of Chemical Engineering of Chinese Universities
基 金:国家自然科学基金重大项目(20990221)
摘 要:用三种聚苯乙烯磺酸树脂在Sn Cl4无水乙醇溶液中进行改性制备酯化催化剂,考察了改性时间、Sn Cl4用量、洗涤方式、产物等因素对催化合成乙酸正丁酯性能的影响。结果表明,用D001-CC树脂在Sn Cl4用量为10.71%(V),改性时间6 h的条件下所制得的改性树脂具有较优的催化效果,120℃下催化乙酸和正丁醇反应70分钟,乙酸的转化率可以达到98.56%。利用FT-IR、XRF、XRD等手段对改性树脂进行了表征。结果表明,Sn Cl4和树脂发生了络合反应形成了新的酸性中心;改性树脂与水发生部分水解,但在连续分水的条件下,可以保持稳定高效的催化效果,能重复使用10次以上。Three sulfonated polystyrene resins were modified in ethanol solutions of tin tetrachloride to prepare catalysts for esterification of acetic acid with n-butyl alcohol. Effects of modification time, SnCI4 dosage, washing method and water separation on catalytic activity were studied. The optimal conditions found for resin modification are: D001-CC as the raw resin, tin tetrachloride concentration 10.71% (v) and modification time 6 h. Acetic acid conversion of 98.56% can be achieved after 70 minutes under 120℃. FT-IR, XRF and XRD techniques were used to characterize the prepared catalysts, and the results show that SnCI4 reacts with -SO3H groups of the resin to form new Lewis acid centers. The catalyst activity decreases due to hydrolysis with water produced in esterification. However, under continuous water separation conditions, the catalytic activity is stable and can be reused for at least 10 times.
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