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作 者:刘玲[1] 赵月昌[1] 程文萍[1] 王有菲[1] 杨建国[1]
机构地区:[1]华东师范大学上海市绿色化学与化工过程绿色化重点实验室,上海200062
出 处:《石油化工》2008年第4期368-372,共5页Petrochemical Technology
基 金:国家科技支撑计划项目(2006BAE03B06);上海市科委国际科技合作项目(06SR07101);上海市重点学科建设项目(B409)
摘 要:以异丁醛和2,2,4-三甲基-1,3-戊二醇(TMPD)为原料合成青叶噁烷,考察了不同铜盐催化剂的催化性能。实验结果表明,对甲苯磺酸铜的催化性能最佳。以对甲苯磺酸铜为催化剂制备青叶噁烷,并进一步考察溶剂种类、催化剂用量、醛与醇摩尔比、反应时间和催化剂重复使用次数等因素对合成青叶噁烷反应的影响。合成青叶噁烷适宜的条件为:n(异丁醛):n(TMPD)=3:1,催化剂0.34mmol,甲苯10mL,反应时间1.5h,反应温度110℃。在此条件下,TMPD的转化率达到94.4%,青叶噁烷的选择性为99.8%。对甲苯磺酸铜催化剂重复使用5次后,TMPD的转化率为90.1%,青叶噁烷的选择性为99.2%。用对甲苯磺酸铜催化TMPD与其他醛(酮)的缩合反应,也取得较好的催化效果。Green oxane was synthesized from isobutyraldehyde and 2,2,4-trimethyl-1,3- pentanediol (TMPD) catalyzed by different copper salts. Copper p-toluene sulfonate was chosen as most effective catalyst for the reaction. Effects of different solvents, catalyst dosage, mole ratio of aldehyde to diol and reaction time on conversion of TMPD and selectivity to green oxane were investigated. Optimum reaction conditions are: n(isobutyraldehyde) : n(TMPD) 3 : 1, catalyst 0.34 mmol, toluene 10 mL, reaction time 1.5 h and reaction temperature 110 ℃. Under the conditions, conversion of TMPD and selectivity to green oxane is 94.4% and 99.8%, respectively. Copper p-toluene sulfonate catalyst can be reused. After 5 recycles, conversion of TMPD is 90. 1% and selectivity to green oxane keeps at 99.2%. Moreover, copper p-toluene sulfonate is a very efficient catalyst in other acetalization and ketalization processes.
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