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作 者:温朋鹏[1] 孙永强[1] 史修启[1] 张勇[1]
机构地区:[1]中国日用化学工业研究院,山西太原030001
出 处:《日用化学工业》2012年第6期424-427,456,共5页China Surfactant Detergent & Cosmetics
基 金:科技部国际科技合作资助项目(2011DFA40640);山西省国际科技合作资助项目(2011081018)
摘 要:以硬脂酸和三乙醇胺为原料合成硬脂酸三乙醇胺酯,采用经典柱层析的方法对酯化反应的混合产物进行硬脂酸三乙醇胺三酯(三酯胺)的分离,并对混合产物和混合产物分离得到的第一馏分进行IR和1HNMR表征。在单因素实验的基础上,通过正交试验优化反应条件,考察了反应温度、物料摩尔比、催化剂用量等因素对三酯胺在反应混合产物中含量的影响,得到较佳反应条件,即反应温度200℃,n(硬脂酸)∶n(三乙醇胺)=3.3∶1.0,催化剂用量为0.1%。在此优化条件下,酯化反应产物中三酯胺质量分数可达97.06%。Stearic acid triethanolamine ester was prepared by reaction of stearic acid and triethanolamine. The method of classical column chromatography was employed for the separation of the product stearic acid triethanolamine tri - ester from the reaction product mixture. Structure of the reaction product mixture as well as the first fraction separated from the reaction product mixture was characterized by IR and 1HNMR. On the basis of single factor experiments, the reaction conditions were optimized by orthogonal experiments. The effects of reaction temperature, molar ratio of the starting materials and the dosage of catalyst on the content of stearic acid triethanolamine tri - ester in the reaction product mixture were studied. The optimal reaction conditions were identified as : reaction temperature 200℃ ; mole ratio of stearic acid to triethanolamine 3.3 : 1.0 ; and dosage of catalyst 0. 1%. Under the optimal conditions, the content of stearic acid triethanolamine tri - ester in the reaction product mixture achieves 97.06%.
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