年产800吨无毒增塑剂酰柠檬酸三丁酯的工艺设计.docVIP

北京化工大学北方学院 化学与材料工程学院 班级：高材1105 学号：110120138 姓名：王佳伟 指导老师：孟令强老师 诚信申明 本人申明： 我所呈交的毕业论文是本人在老师指导下进行的研究工作及取得的研究成果。据我查证，除了文中特别加以标注和致谢的地方外，论文中不包含其他人已经发表或撰写过的研究成果，也不包含为获得其他教育机构的学位或证书而使用过的材料。我承诺，论文中的所有内容均真实、可信。 本人签名 日期 年产800吨无毒增塑剂乙酰柠檬酸三丁酯的工艺设计 王佳伟 高分子材料与工程 1105班 学号110120138 指导老师 孟令强老师 摘 要 目前常用的邻苯二甲酸酯类增塑剂可能诱发致癌，国内外都在寻找能够替代的无毒增塑剂．柠檬酸酯类增塑剂是安全的替代增塑剂之一，今以柠檬酸三丁酯和己酸酐为原料，研究了硫酸氢钠、大孔强酸性阳离子交换树脂催化合成乙酰柠檬酸三丁酯的过程．考察了原料摩尔配比、催化剂用量、反应时间、反应温度对乙酰柠檬酸三丁酯收率的影响。在适宜条件下，两种催化剂催化台成乙酰柠檬酸三丁酯的收率可分别达到99 5％和99 8％。精制后，乙酰柠檬酸三丁酯的含量经气相色谱分析大于99％。催化剂重复使用情况的考察表明：硫酸氢钠有较好的重复使用性：使用后经无水乙醇洗涤并干燥过的大孔强酸性阳离子交换树脂也具有很好的重复使用性。 关键词：柠檬酸三丁酯 乙酰柠檬酸三丁酯 合成 Abstract Studies have shown that dioctyl-phthalate which is the most commonly used plasticizer is toxic and it might induce cancer.Because of its significant security and outstanding plasticity,tributly citrate(TBC)and acetyl tri-n-butyl citrate(ATBC)were considered to be phthalate non-toxic substitutes.This paper studies the process of synthesizing TBC and ATBC by using citric acid,n-butyl alcohol and acetylating agent.And the pilot plant for this process has been designed. This paper took as the catalyst of esterification．The effects ofreaction conditions on the yield of TBC,such as the amount of catMyst used,catalyst feeding way,molar ratio of n-butyl acohol to citric acid,heating temperature and reaction time,were investigated and the optimal conditions were obtained.Under the optimized conditions with molar ratio of 46.3％catalyst feeded in saturated solution,heated at 150℃with the reaction time of 150 min,the yield of TBC could reach 98.0％.Moreover,the results of neutralization washing in different alkali concentrations had been obtained,and the proper alkali concentration was 6％(in mass concentration). The reaction results of using acetyl chloride or acetic anbydride as acetylating agent were compared,and acetic anbydridewas chosen as the acetylating agent in this paper.ATBC Was synthesized by using ac