基于三单体废水浓缩料合成SIPE的研究  

SYNTHESIS OF SIPE BASED ON SIPM WASTEWATER CONCENTRATE

作　　者：汲彦君 刘明明 杨荣华 郭学阳 张秀玲 Ji Yanjun;Liu Mingming;Yang Ronghua;Guo Xueyang;Zhang Xiuling(College of Chemical and Pharmaceutical Engineering, Shandong First Medical University, Taian 271000, Shandong, China;Taian huagui pharmaceutical technology development co. LTD, Taian 271000, Shandong, China)

机构地区：[1]山东第一医科大学化学与制药工程学院,山东泰安271000 [2]泰安华贵医药科技开发有限公司,山东泰安271000

出　　处：《精细石油化工》2020年第3期60-64,共5页Speciality Petrochemicals

摘　　要：以三单体废水浓缩料为原料,与乙二醇(EG)通过酯交换和酯化反应合成间苯二甲酸乙二醇酯-5-磺酸钠(SIPE)。采用三组分催化剂(醋酸钙、醋酸锰和二丁基氧化锡)和防醚剂醋酸钠,分阶段控制温度、分两次加入催化剂、控制塔顶馏出物的方法,通过正交试验设计确定反应的最优化工艺条件:醋酸钙、二丁基氧化锡、醋酸钴、醋酸钠的用量(按EG质量计)分别为0.25%、0.12%、0.06%、0.04%,三单体废水浓缩料(干燥后)与EG质量比为1∶1.50,第一阶段反应温度170℃,第二阶段反应温度185℃,反应时间2.0 h。得到外观好、纯度高、杂质含量少的SIPE溶液,产品收率达77.45%,所合成的SIPE溶液放置1 a后含量、皂化值、酸值均达标,稳定性良好。Sodium ethylene glycol isophthalate-5-sulfonate(SIPE)was synthesized from wastewater concentrate of dimethyl isophthalate-5-sodium sulfonate(SIPM)process by transesterification and esterification with ethylene glycol(EG).Using three-component catalyst(calcium acetate,manganese acetate and dibutyl tin oxide)and sodium acetate as antiether agent,the optimum reaction conditions were determined by orthogonal test design:the dosage of calcium acetate,dibutyl tin oxide,cobalt acetate and sodium acetate(in terms of EG mass)were 0.25%,0.12%,0.06%and 0.04%respectively.The mass ratio of SIPM wastewater concentrate(after drying)to EG is 1∶1.50,the first stage reaction temperature is 170℃,the second stage reaction temperature is 185℃,and the reaction time is 2.0 h.The SIPE solution with good appearance,high purity and low impurity content was obtained,the yield of the product was 77.45%.The content,saponification value and acid value of the synthesized SIPE solution reached the standard one year later,and the stability was good.

关 键 词：三单体废水浓缩料 间苯二甲酸乙二醇酯-5-磺酸钠(SIPE) 酯化反应 酯交换反应 废料资源化利用 

分 类 号：TQ261.1[化学工程—有机化工]