硫酸氢钾催化合成柠檬酸三丁酯—孙钢锋.docVIP

硫酸氢钾催化合成柠檬酸三丁酯 摘要 增塑剂是应用于高分子材料行业的一类重要添加剂。目前，主要应用的是邻苯二甲酸酯类增塑剂，近年来，研究表明领苯二甲酸酯增塑剂可能致癌，其应用受到限制，开发新型、无毒、高效增塑剂势在必行。柠檬酸三丁酯（简称TBC）作为增塑剂具有相容性好、增塑效率高、无毒、挥发性低、耐光、耐水、耐寒等优良特点。由于这些显著的优点，所以柠檬酸三丁酯已被美国食品与药物管理局批准用于食品包装材料、医疗制品及儿童玩具等领域，可替代具有致癌作用领本二甲酸酯类增塑剂。 传统的柠檬酸三丁酯的合成工艺以浓硫酸、对甲苯磺酸等强酸性催化剂，这些工艺存在副反应多、后处理工艺复杂、设备腐蚀严重以及废酸污染环境等弊端。近期文献报道合成柠檬酸三丁酯催化剂有氯化铁、四氯化锡、氨基磺酸、固体杂多酸、固体超强酸等，这些催化剂都有较好的催化效果，但无机路易斯酸易潮解而失效，固体超强酸则存在制备成本高，本课题对硫酸氢钾做催化剂合成柠檬酸三丁酯的工艺过程进行探讨。发现硫酸氢钾是一种良好的合成TBC的催化剂，除克服了强酸性催化剂的不足外，还具有价格便宜、易得、可重复使用等优点。研究的主要方法是，通过改变醇酸体积比、回流时间和催化剂用量，得出当柠檬酸、正丁醇和硫酸氢钾的量比为1.25：11:1，在150C°温度下，回流2.5h，酯化率达98.47%。 关键词：柠檬酸三丁酯 硫酸氢钾 催化合成 Catalytic Synthesis of potassium hydrogen sulfate tributes citrate Abstract Plasticizers are used in polymer industry, an important class of additives. Currently, the main application is phthalate plasticizers, in recent years, studies have shown that lead phthalate plasticizers may cause cancer， its application is limited, the development of new, non-toxic, high potential in the plasticizer the pipeline. Tributes citrate (referred to as TBC) as a plasticizer with good compatibility plasticized, high efficiency, non-toxic, low volatility, light, water, cold and other excellent features. Because of these significant advantages, so tributes citrate has been approved by the U.S. Food and Drug Administration for food packaging materials, medical products and childrens toys and other fields can replace the role of leading the carcinogenic diethyl ester plasticizer. The traditional synthesis of n-butyl citrate with concentrated sulfuric acid, 4-methylbenzene-sulfonic acid and other strong acid catalysts, there are side effects of these processes and more complex post-processing technology, equipment corrosion, and waste acid pollution of the environment and other serious defects. Recently reported in the literature synthesis catalyst tributes citrate ferric chloride, stannic chloride, amino acid, solid heterophony acid, solid super acid, these catalysts have better catalytic effec