發(fā)布時間：2018-03-05 05:30

  本文選題：間歇萃取精餾　切入點：萃取劑　出處：《天津大學》2015年碩士論文　論文類型：學位論文

【摘要】：仲丁醇和醋酸仲丁酯均為重要的化工原料。在醋酸仲丁酯與醇類進行酯交換反應(yīng)的過程中,形成仲丁醇和醋酸仲丁酯的混合物。常壓下,該混合物在仲丁醇質(zhì)量含量高于85%時形成二元“擬共沸物”。用普通精餾操作很難實現(xiàn)二者的分離,萃取精餾是分離此混合物的有效途徑。目前,關(guān)于萃取精餾分離仲丁醇-醋酸仲丁酯二元物系的報道很少,文獻中缺乏仲丁醇、醋酸仲丁酯和萃取劑所組成的體系的汽液平衡數(shù)據(jù),導致該過程的模擬、設(shè)計和工業(yè)化存在很大的盲目性,所以,研究該體系的汽液平衡數(shù)據(jù)及各種因素對該分離過程的影響,具有重要的理論和現(xiàn)實意義。本文通過查閱文獻并結(jié)合實際經(jīng)驗,初步確定了三種單一萃取劑:N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAC)和二甲基亞砜(DMSO)和一種混合溶劑DMF+DMSO。通過實驗測定了仲丁醇-醋酸仲丁酯-單一萃取劑(DMF、DMAC和DMSO)及仲丁醇-醋酸仲丁酯-混合萃取劑(DMF+DMSO)組成的萃取精餾體系的二元、三元和四元汽液平衡數(shù)據(jù),并采用NRTL、Wilson和UNIQUAC熱力學模型對二元汽液平衡數(shù)據(jù)進行回歸,得到了模型的二元交互作用參數(shù),利用這些參數(shù)預測的二元、三元和四元物系汽液平衡數(shù)據(jù)的計算結(jié)果與實驗值吻合較好。同時,汽液平衡測定結(jié)果表明,DMF+DMSO混合溶劑做萃取劑的分離效果優(yōu)于單一溶劑。本文采用DMF+DMSO混合溶劑作萃取劑,進行了間歇萃取精餾分離仲丁醇-醋酸仲丁酯的實驗,實驗結(jié)果表明:以DMF+DMSO混合溶劑作萃取劑分離仲丁醇-醋酸仲丁酯混合物是可行的。采用PROII 7.1流程模擬軟件對該實驗過程進行了模擬,模擬結(jié)果與實驗結(jié)果吻合較好。利用PROII 7.1流程模擬軟件考察了多種因素對該間歇萃取精餾過程的影響,得到了適宜的操作條件,在該條件下醋酸仲丁酯的收率為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.
【學位授予單位】：天津大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TQ028.31

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