以活性炭负载钛酸四丁酯为催化剂,正丁醚为带水剂,采用直接酯化法合成二乙二醇二苯甲酸酯(DEDB); 运用低温氮气吸附脱附(BET)与电子顺磁共振波谱(ESR)分析对催化剂进行表征,采用IR和1H-NMR进行反应产物的表征; 探讨原料比、带水剂用量、反应温度等因素对酯化率的影响。确定了活性炭固载钛酸四丁酯催化二乙二醇(DEG)和苯甲酸(BA)酯化的适宜工艺条件为:原料量比n(DEG):n(BA)=1:2,带水剂占苯甲酸质量分数为20%,催化剂占苯甲酸质量分数为1.5%,反应温度200 ℃,反应时间6 h。催化剂可循环使用3次,具有较好的稳定性。
Abstract
Diethylene glycol dibenzoate(DEDB)was synthesized by catalyzing with n-butyl titanate supported on activated carbon and using n-butyl ether as the water carrier. These catalysts were characterized by BET and ESR.Effects of the ratio of substrates, amount of water carrier, and reaction temperature on esterification were examined,and the suitable esterification conditions was determined as follows:n(DEG)/n(BA)=0.5, 20%(wt)of water carrier and 1.5%(wt)of catalyst based on BA, 200 ℃ of reaction temperature and 6 h of reaction time. Meanwhile, the catalyst could be reused for 3 times, and showed good stability. The structure of product was characterized by IR and 1H-NMR.
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基金
收稿日期:2014-03-28 修回日期:2014-09-20
第一作者:陈燕青,硕士生。*通信作者:朱新宝,教授。E-mail: zhuxinbao@njfu.com.cn。
引文格式:陈燕青,邹斌,董琳,等. 活性炭负载钛酸四丁酯催化合成二乙二醇二苯甲酸酯[J]. 南京林业大学学报:自然科学版,2015,39(2):121-126.
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