从阻聚剂生产废液中回收N,N-二甲基乙酰胺研究

发布时间：2018-01-21 00:57

本文关键词： N N-二甲基乙酰胺精馏热力学提纯 ProⅡ　出处：《华东理工大学》2017年硕士论文　论文类型：学位论文

【摘要】：N,N-二甲基乙酰胺(简称DMAC)作为一种具有高沸点、强极性的质子化有机溶剂,对于多种有机物都有极强的溶剂性能,同时因其具有稳定性好、挥发性低、不易水解和腐蚀性低等特点,广泛应用于树脂、橡胶、石油化工及其他有机合成等领域。随着国内腈纶、氨纶行业的需求增长和化工行业的发展,DMAC将会拥有更为广阔的发展和应用前景。论文探讨了从阻聚剂生产废液中回收N,N-二甲基乙酰胺的方法。针对废液中的酸性组分,首先研究了中和法处理废液的方法,使用碱液与废液中的酸性组分进行反应,考察了直接中和后分离的可行性。结果表明,直接中和分离法操作复杂,分离困难,不具备可行性。之后,研究了采用反应法处理废液,在废液中通入二甲胺,使二甲胺与废液中的酸性组分进行反应,一方面使废液中的酸性组分浓度降低,另一方面使废液中的DMAC浓度提高。使用Benson基团贡献法估算DMAC等组分的热力学参数,并对二甲胺与乙酸和乙酸酐反应进行热力学分析,研究了反应的可行性和最优进行条件。在热力学研究的基础上,通过二甲胺与废液中的乙酸和乙酸酐的反应,考察了催化剂种类、催化剂用量、二甲胺与酸性组分摩尔配比、反应温度和反应时间等因素对提高废液中DMAC浓度的影响。在最优条件组下进行反应,可以有效提升废液中DMAC含量,废液中DMAC的含量由原废液的57.07%提高到83.77%,酸性组分含量由26.44%降低到1.54%,大大降低了后续精馏分离的难度。论文还使用ProII模拟软件对反应终液的精馏分离流程进行模拟分析。在一定分离条件下通过简捷法获取塔参数,并使用严格法检验相关塔参数。分析理论塔板数、进料板位置、最小回流比、再沸器热负荷和冷凝器热负荷等参数对分离结果的影响,并对塔参数进行优化。最终分离得到合格的DMAC产品,为工厂的可持续处理流程奠定了实验室基础。该工艺流程可以同时处理废液中的乙酸和乙酸酐等双重酸性组分,且流程简单、反应成本低,同时使用软件模拟可以获得高纯度的DMAC产品。通过分析和模拟,获取了工艺流程的优化参数,降低了废液对环境的污染,节省了资源,并为企业创造了一定的经济效益。
[Abstract]:As a kind of proton organic solvent with high boiling point and strong polarity, N- N- dimethyl acetamide (DMAC) has very strong solvent properties for many kinds of organic matter, at the same time, it has good stability. It is widely used in many fields such as resin, rubber, petrochemical and other organic synthesis. With the increasing demand of domestic acrylic and spandex industry and the development of chemical industry. DMAC will have a wider prospect of development and application. This paper discusses the method of recovering N- N- dimethyl acetamide from the waste liquor of polymerization inhibitor production, aiming at the acid component in the waste liquid. Firstly, the neutralization method was studied, and the feasibility of direct neutralization separation was investigated by reaction of alkali solution with acid component. The results showed that the direct neutralization separation method was complicated. The separation is difficult and not feasible. After that, the reaction method is used to treat the waste liquid, and the dimethylamine is added into the waste liquid to make the dimethylamine react with the acid component in the waste liquid. On the one hand, the concentration of acid component in waste liquid is decreased, on the other hand, the concentration of DMAC in waste liquid is increased. The thermodynamic parameters of DMAC and other components are estimated by Benson group contribution method. The thermodynamic analysis of the reaction of dimethylamine with acetic acid and acetic anhydride was carried out, and the feasibility and optimum conditions of the reaction were studied. On the basis of thermodynamic study, the reaction of dimethylamine with acetic acid and acetic anhydride in waste liquid was carried out. The effects of catalyst type, amount of catalyst, molar ratio of dimethylamine to acid component, reaction temperature and reaction time on the concentration of DMAC in waste liquor were investigated. The content of DMAC in waste liquid increased from 57.07% to 83.77, and the content of acid component decreased from 26.44% to 1.54%. The difficulty of subsequent distillation separation is greatly reduced. ProII simulation software is also used to simulate and analyze the distillation separation process of the final reaction liquid. Under certain separation conditions, the column parameters are obtained by the simplified method. The influence of theoretical tray number, feed plate position, minimum reflux ratio, reboiler heat load and condenser thermal load on the separation results was analyzed. The parameters of the tower were optimized. Finally, the qualified DMAC product was obtained. This process can simultaneously treat the acid components such as acetic acid and acetic anhydride in the waste liquor, and the process is simple, and the reaction cost is low. At the same time, high purity DMAC products can be obtained by software simulation. Through analysis and simulation, the optimization parameters of process flow are obtained, which can reduce the pollution of waste liquid to the environment and save resources. And for the enterprise to create certain economic benefits.
【学位授予单位】：华东理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X78;TQ413.26

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