对二甲氨基苯甲酸异辛酯的合成工艺.pdfVIP

学兔兔 化 工 进 展 2010年第29卷第11期 CHEMICAL IND1USTRY AND ENGINEERING PR,OGRESS ·2149· 对二甲氨基苯甲酸异辛酯的合成工艺 桂厚瑛，周秋名，胡新明，董留玉 (武汉理工大学理学院，湖北 武汉430070) 摘 要：对合成对二甲氨基苯甲酸异辛酯的原始工艺进行了改进，获得了收率高、成本低、毒性小、污染少的 合成工艺优化方法；可实现大规模工业生产。即以 M二甲基对氨基苯甲酸和异辛醇为原料，无需溶剂脱水， 用对甲苯磺酸作为酯化催化剂，采用高负压的方法除去反应过程中生成的水，从而使正反应能够最大限度地进 行，反应温度控制在 ll0～120℃。重点讨论了无溶剂参与的酯化反应条件：反应温度 11O～120℃，真空 度一0．095 MPa，反应时间6 h，对二甲氨基苯甲酸与异辛醇的摩尔比为1：3．5，以对二甲氨基苯甲酸计，产品收 率为90％。 关键词：对二甲氨基苯甲酸异辛酯；无溶剂脱水；酯化；合成 中图分类号：TQ 658 文献标志码：A 文章编号：1000—6613(2010)1l一2149—05 Synthesis of 2-ethylhexyl p-dimethylamiobenzoate GU／Houying，ZHOU Qiuming，HUXinming，DONG Liuyu (Institute of Science，Wuhan University ofTechnology，Wuhan 430070，Hubei，China) Abstract：2一Ethylhexyl P—dimethylamiobenzoate was synthesized with higher yield，lower cost and nontoxicity，which is easier realized for large．-scale industrial production．Dimethylamino benzoic acid and isooctanol were used as starting materials without any solvent by using P—toluenesulfonic acid as a esterification catalyst．The reaction proceeded as much as possible to remove the produced water under highly reduced pressure，and the reaction temperature was controlled in a range between 1 1 0~C and 1 20 ℃．The reaction conditions of the esterification without solvent should be emphasized that the temperature was between 1 10 and 1 20℃ at fl negative pressure of 0．095 MPa for 6h．The molar ratio of dimethyl—aminobenzoic acid with isooctanol was 1：3．5．2一Ethylhexyl P—dimethylamiobenzoate yield was higher than 90％based ondimethyl—aminobenzoic acid． Key