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作 者:黄润均[1] 周家添 谢威[3] 陈东莲[1] 韦冬萍[2] 袁爱群[2] 梁慧[2]
机构地区:[1]桂林理工大学南宁分校,南宁530001 [2]广西民族大学化学化工学院,南宁530006 [3]广西工业职业技术学院,南宁530004
出 处:《应用化学》2016年第6期649-654,共6页Chinese Journal of Applied Chemistry
基 金:2015广西科技开发项目(14125002-6);2014年南宁市科技开发项目(20145201);2013广西教育厅项目(2013YB105;200103YB041);2014广西工业职业技术学院项目~~
摘 要:采用硝酸改性活性炭后负载三聚磷二氢铝用于催化合成苯甲醛乙二醇缩醛,通过单因素实验考察醇醛摩尔比、催化剂用量及反应时间等因素对产品收率的影响,并采用正交实验获取较佳工艺条件。结果表明,该催化反应中,当反应温度为110℃时,各因素对收率的影响顺序为:醇醛比>反应时间>带水剂加入量>催化剂用量。优化反应条件为:苯甲醛0.2 mol,醇醛摩尔比2.5,反应时间75 min,催化剂加入量4%(占反应物总质量),带水剂加入量25 m L,苯甲醛乙二醇缩醛收率86.5%,催化剂经5次重复使用后收率仍大于86.0%。Benzaldehyde glycol acetal was synthesized by aluminum dihydrogen tripolyphosphate supported on nitric acid modified activated carbon. The effect of the molar ratio of alcohol to aldehyde,catalyst amount and reaction time on the yield were studied by single-factor experiments. Orthogonal design was used to obtain the optimized conditions for the synthesis of benzaldehyde glycol acetal. The results show that the three main influencing factors are in the order as follows: the molar ratio of alcohol to aldehyde the reaction time the quantity of water carrying agent the quantity of catalyst. The optimal technical conditions are: temperature110 ℃,benzaldehyde 0. 2 mol,the molar ratio of alcohol to aldehyde is 2. 5,reaction time 75 min,the quantity of catalyst 4%,water-carrying agent of cyclohexane 25 m L. Under these conditions,the yield of benzaldehyde glycol acetal is above 86. 5%. The catalyst can be recycled for multiple uses and the acetal yield is 86. 0% after five cycles.
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