间歇萃取精馏分离仲丁醇—醋酸仲丁酯的研究

发布时间：2018-03-05 05:30

本文选题：间歇萃取精馏　切入点：萃取剂　出处：《天津大学》2015年硕士论文　论文类型：学位论文

【摘要】：仲丁醇和醋酸仲丁酯均为重要的化工原料。在醋酸仲丁酯与醇类进行酯交换反应的过程中,形成仲丁醇和醋酸仲丁酯的混合物。常压下,该混合物在仲丁醇质量含量高于85%时形成二元“拟共沸物”。用普通精馏操作很难实现二者的分离,萃取精馏是分离此混合物的有效途径。目前,关于萃取精馏分离仲丁醇-醋酸仲丁酯二元物系的报道很少,文献中缺乏仲丁醇、醋酸仲丁酯和萃取剂所组成的体系的汽液平衡数据,导致该过程的模拟、设计和工业化存在很大的盲目性,所以,研究该体系的汽液平衡数据及各种因素对该分离过程的影响,具有重要的理论和现实意义。本文通过查阅文献并结合实际经验,初步确定了三种单一萃取剂:N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)和二甲基亚砜(DMSO)和一种混合溶剂DMF+DMSO。通过实验测定了仲丁醇-醋酸仲丁酯-单一萃取剂(DMF、DMAC和DMSO)及仲丁醇-醋酸仲丁酯-混合萃取剂(DMF+DMSO)组成的萃取精馏体系的二元、三元和四元汽液平衡数据,并采用NRTL、Wilson和UNIQUAC热力学模型对二元汽液平衡数据进行回归,得到了模型的二元交互作用参数,利用这些参数预测的二元、三元和四元物系汽液平衡数据的计算结果与实验值吻合较好。同时,汽液平衡测定结果表明,DMF+DMSO混合溶剂做萃取剂的分离效果优于单一溶剂。本文采用DMF+DMSO混合溶剂作萃取剂,进行了间歇萃取精馏分离仲丁醇-醋酸仲丁酯的实验,实验结果表明:以DMF+DMSO混合溶剂作萃取剂分离仲丁醇-醋酸仲丁酯混合物是可行的。采用PROII 7.1流程模拟软件对该实验过程进行了模拟,模拟结果与实验结果吻合较好。利用PROII 7.1流程模拟软件考察了多种因素对该间歇萃取精馏过程的影响,得到了适宜的操作条件,在该条件下醋酸仲丁酯的收率为85.66%。
[Abstract]:Secondary butyl alcohol and secondary butyl acetate are important chemical raw materials. In the process of transesterification between secondary butyl acetate and alcohols, a mixture of secondary butyl alcohol and secondary butyl acetate is formed. When the mass content of secondary butanol is higher than 85, the mixture forms a binary "azeotropic compound". It is difficult to separate the mixture by ordinary distillation operation, and extractive distillation is an effective way to separate the mixture. There are few reports on the separation of the binary system of sec-butanol-butyl acetate by extractive distillation, and the lack of vapor-liquid equilibrium data of the system composed of sec-butanol, sec-butyl acetate and extractant in the literature, which leads to the simulation of the process. There is great blindness in design and industrialization. Therefore, it is of great theoretical and practical significance to study the vapor liquid equilibrium data of the system and the influence of various factors on the separation process. Three kinds of single extractants, 1: N- (N-dimethyl-formamide) and dimethyl sulfoxide (DMAC-) and a mixed solvent, DMF DMSOrespectively, were preliminarily determined. The DMAC, DMSOand DMSO) were determined by experiments, and the DMAC and DMSOs were determined as well as the dimethyl sulfoxide and dimethyl sulfoxide (DMAC) and dimethyl sulfoxide (DMAC) and dimethyl sulfoxide (DMSO), respectively. Binary extraction Distillation system composed of Butyl Alcohol-secbutyl Acetate and mixed extractant DMF DMSO, The ternary and quaternion vapor-liquid equilibrium data were obtained, and the binary interaction parameters were obtained by using NRTL Wilson and UNIQUAC thermodynamic models. The calculated results of vapor-liquid equilibrium data of ternary and quaternion systems are in good agreement with the experimental data. At the same time, the results of vapor-liquid equilibrium measurement show that the separation efficiency of DMSO mixed solvent is better than that of single solvent. In this paper, DMF DMSO mixed solvent is used as extractant. The separation of sec-butanol-sec-butyl acetate by batch extractive distillation was studied. The experimental results show that it is feasible to separate the mixture of sec-butanol and sec-butyl acetate with DMF DMSO mixed solvent as extractant, and the experimental process is simulated by PROII 7.1 process simulation software. The simulation results were in good agreement with the experimental results. The effects of various factors on the batch extractive distillation process were investigated by using PROII 7.1 process simulation software. The optimum operating conditions were obtained. The yield of sec-butyl acetate was 85.66 under this condition.
【学位授予单位】：天津大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ028.31

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