酯交换法制备乙酸正丁酯催化精馏的过程研究

发布时间：2017-12-28 12:15

本文关键词：酯交换法制备乙酸正丁酯催化精馏的过程研究　出处：《河北工业大学》2015年硕士论文　论文类型：学位论文

【摘要】：乙酸甲酯相比其它同系酯类,市场需求较小,而且它常作为工业副产大量出现。而乙酸正丁酯由于其优异的溶解性能,逐步成为甲苯、二甲苯等有毒有害溶剂的替代品,因此市场前景广阔。利用酯交换法将其转化为乙酸正丁酯,为乙酸甲酯提供了一种效益更高的利用方法。本文筛选出Si-3为最优催化剂后,在间歇搅拌釜式反应器中进行了酯交换制备乙酸正丁酯的实验研究。考察了转速、反应温度、催化剂用量、醇酯比等因素对反应过程的影响。将实验数据拟合后得到酯交换反应的动力学方程:r=6291exp(-53643/RT)(αMe OAcαBu OH-αMEOHαBu OAc/K)其中:K=exp(4.15-1.667/T)在动力学研究的基础上,使用化工模拟软件对酯交换催化精馏过程进行了模拟计算。考察了全塔理论级数、进料位置、醇酯比和回流比对催化精馏过程的影响。在自行搭建的催化精馏实验装置中,以乙酸甲酯和正丁醇为原料,采用酯交换法催化精馏制备乙酸正丁酯。催化精馏塔高1.7m,内装负载催化剂的不锈钢θ环填料层1.5m。实验结果显示:乙酸甲酯和正丁醇合适的进料位置为塔釜和距塔顶2/5处,正丁醇进料量为15m L/min,进料醇酯比1:1.2,回流比为1。此条件下正丁醇转化率可达90.17%,塔釜正丁酯含量为86.24%,均高于相关文献报道。同时塔顶中乙酸甲酯含量为22.11%,远离共沸组成点,后续分离过程简易。实验规律与计算机模拟结果吻合较好,为进一步研究提供基础数据。
[Abstract]:Compared with other homologous esters, methyl acetate has smaller market demand, and it often appears as a by-product of industrial by-products. Due to its excellent solubility, n-butyl acetate has gradually become a substitute for toxic and harmful solvents such as toluene and xylene, so the market has a broad prospect. It is converted into n-butyl acetate by transesterification, which provides a more efficient utilization method for methyl acetate. In this paper, the experimental study on the preparation of n-butyl acetate by transesterification in a batch reactor was carried out after screening Si-3 as the optimal catalyst. The influence of the speed, the reaction temperature, the amount of catalyst and the ratio of alcohol ester on the reaction process was investigated. The experimental data obtained after fitting the kinetic equation of the reaction of ester exchange: r=6291exp (-53643/RT) (alpha Me alpha Bu alpha MEOH alpha OH- OAc Bu OAc/K) where: K=exp (4.15-1.667/T) based on the kinetic study on the use of chemical simulation software of transesterification catalytic distillation process was simulated. The effects of the theoretical series of the whole tower, the position of feed, the ratio of alcohol and ester and the ratio of reflux to the catalytic distillation process were investigated. In the self constructed catalytic distillation unit, methyl acetate and n-butanol were used as raw materials, and n-butyl acetate was prepared by ester exchange catalytic distillation. Catalytic distillation tower 1.7m, built-in stainless steel ring packing layer 1.5m theta catalyst. The experimental results showed that the suitable location of methyl acetate and n-butanol was 2/5 at the top of the tower and from the top of the tower, the feed amount of n-butanol was 15m L/min, the feed alcohol ratio was 1:1.2, and the reflux ratio was 1. Under this condition, the conversion of n-butyl alcohol can reach 90.17%, and the content of n-butyl ester in the kettle is 86.24%, which is higher than the related literature. At the same time, the content of methyl acetate in the top of the tower is 22.11%, which is far away from the azeotropic composition point, and the subsequent separation process is simple. The experimental rules are in good agreement with the computer simulation results, and provide basic data for further research.
【学位授予单位】：河北工业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ225.24;TQ028.31

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