盐效萃取分离部分互溶恒沸有机水溶液的研究
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摘要
本文通过理论分析与实验研究相结合的方式研究了盐效萃取分离部分互溶的环己酮-水和正丁醇-水体系,其中包括盐析剂的选择、加盐液-液相平衡实验和盐效萃取分离工艺实验,并通过对液-液相平衡数据的关联计算建立了适用上述体系的盐效应模型。
目前在工业上采用盐效萃取分离部分互溶的恒沸有机溶液体系具有重要的应用背景,相对于传统的共沸精馏或萃取精馏工艺,该方法能大幅度的降低能耗,符合低碳发展的趋势。所谓盐析效应是指将无机盐加入到互溶或部分互溶的恒沸有机物水溶液中时,由于无机盐与溶剂分子之间的相互作用,从而引起体系液-液相平衡的变化,即溶剂间分配系数的变化,从而实现混合体系的分离提纯。目前采用无机盐分离部分互溶的恒沸体系的相关研究报道较少,相平衡数据较为缺乏,给盐效萃取分离恒沸体系的研究和应用带来了许多的困难。本文主要研究了环己酮-水体系和正丁醇-水体系在加盐时的液-液相平衡,为其在工业中的应用提供了基础数据和理论依据,具有较高的理论价值和工业应用价值。具体完成了以下几个方面的工作:
1盐效萃取工艺中盐析剂的选择:通过理论计算、文献查阅及实验研究相结合的方式分别确定了适用于环己酮-水体系和正丁醇-水体系的盐析剂,并通过实验验证比较了几种选盐理论模型的优缺点,得出了其各自的适用范围,为盐效萃取工艺中盐析剂的选择提供了理论依据。
2环己酮-水-无机盐体系及正丁醇-水-无机盐体系液-液相平衡实验研究:系统的测定了环己酮-水-碳酸钾、环己酮-水-氟化钾、正丁醇-水-氟化钾、正丁醇-水-碳酸钾体系的液-液相平衡数据,为采用无机盐分离环己酮-水和正丁醇-水恒沸体系提供了基础数据。
3环己酮-水-无机盐及正丁醇-水-无机盐体系液-液相平衡数学模型的研究:分别采用Pitzer理论和NRTL、Wilson或UNIQUAC方程计算了环己酮-水-碳酸钾、环己酮-水-氟化钾、正丁醇-水-氟化钾、正丁醇-水-碳酸钾体系的液-液相平衡数据,为采用无机盐分离环己酮-水和正丁醇-水恒沸体系提供了计算依据。
4盐效萃取分离正丁醇-水体系工艺研究:根据液-液相平衡实验所得到的结果,采用碳酸钾水溶液萃取分离正丁醇-水体系,考察了碳酸钾水溶液的稳定性及溶液萃取比对萃取效果的影响,并确定了最佳萃取比。建立高浓度正丁醇废液资源化利用节能技术的工艺流程,为了对该流程与传统恒沸精馏流程的能耗情况进行比较,采用Aspen Plus流程模拟软件对新旧流程进行了模拟计算,结果发现盐效萃取工艺可大幅度的降低分离正丁醇-水体系的能耗。
The separation of partially miscible cyclohexanone - water and n-butanol - water systems based on salting-out principle is studied by the combined methods of theoretical analysis and experimental research, including the selection of inorganic salts, the liquid-liquid equilibrium(LLE) experiments and salting-out extraction process, and a theoretical model is established by the calculation of LLE data.
Currently, it has an important application background for the salting-out extraction of partially miscible of azeotropic organic/water system in industry. Compared to conventional azeotropic distillation and extractive distillation process, this method can greatly reduce the energy consumption and is also consistent with the development of low-carbon. When the salt is added into the miscible azeotropic organic/water system, the interaction between the ions of salt and solvent molecules will change the LLE of this system and the partition coefficient of solvents to get the mixture separated. This is the salting-out effect of inorganic salts. Until now there are not so many reports about the research of partially miscible of azeotropic organic/water system by salting-out extraction exist and the LLE data of organic/water system is short, which brings a lot of difficulties to its research and application. In this paper the LLE of cyclohexanone-water-salts and n-butanol-water–salts systems are studied, providing the basic data and theoretical basis for the salting-out extraction’s application in industry. So it has an important academic theoretical significance and industrial application. The research works have been performed in this paper as follows:
1 The selection of inorganic salt used in the process of salting-out extraction. By the combined methods of theoretical calculations, literature data and experimental study, the salts used in the separating process of cyclohexanone-water and 1-butanol-water systems are selected. The theoretical models of salt selection are studied by the experimental verification method and its scope of application is determinated, which provides theoretical data for the selection of inorganic salt in the process of salting-out extraction.
2 Research on the LLE of cyclohexanone - water - salts and n-butanol - water - salts systems.The LLE data of the systems of cyclohexanone - water - potassium carbonate, cyclohexanone - water - potassium fluoride, n-butanol - water - potassium fluoride, n-butanol - water - potassium carbonate are experimentally measured, providing basis data for the separation of cyclohexanone/water and n-butanol/water systems by salting-out extraction.
3 Study on the mathematical model for the LLE of cyclohexanone - water - salts and n-butanol - water - salts systems. The LLE data of the systems of cyclohexanone - water - potassium carbonate, cyclohexanone - water - potassium fluoride, n-butanol - water - potassium fluoride, n-butanol - water - potassium carbonate are calculated by the Pitzer electrolyte solution theory and NRTL, Wilson or UNIQUAC equations, respectively. It provides a theoretical basis for the separation of cyclohexanone - water and n-butanol - water systems by using inorganic salts.
4 The technical study on the separation of n-butanol - water system by Salting-out extraction ways. According to the experimental results of liquid - liquid equilibrium, the potassium carbonate is selected and used to separate n-butanol/water system by salting-out extraction. The stability of aqueous potassium carbonate and mass ratio of aqueous potassium carbonate to raw materials on the extraction efficiency are investigated, and the optimum extraction ratio is obtained. Then the utilization process of high concentrations of n-butanol effluent with lower energy consumption is established. To compare the energy consumption of azeotropic distillation process and the salting-out extraction process, the processes are simulated and calculated by Aspen Plus simulation software and result shows that salting-out extraction process can be greatly reduced energy consumption in the separating process of this system.
目前在工业上采用盐效萃取分离部分互溶的恒沸有机溶液体系具有重要的应用背景,相对于传统的共沸精馏或萃取精馏工艺,该方法能大幅度的降低能耗,符合低碳发展的趋势。所谓盐析效应是指将无机盐加入到互溶或部分互溶的恒沸有机物水溶液中时,由于无机盐与溶剂分子之间的相互作用,从而引起体系液-液相平衡的变化,即溶剂间分配系数的变化,从而实现混合体系的分离提纯。目前采用无机盐分离部分互溶的恒沸体系的相关研究报道较少,相平衡数据较为缺乏,给盐效萃取分离恒沸体系的研究和应用带来了许多的困难。本文主要研究了环己酮-水体系和正丁醇-水体系在加盐时的液-液相平衡,为其在工业中的应用提供了基础数据和理论依据,具有较高的理论价值和工业应用价值。具体完成了以下几个方面的工作:
1盐效萃取工艺中盐析剂的选择:通过理论计算、文献查阅及实验研究相结合的方式分别确定了适用于环己酮-水体系和正丁醇-水体系的盐析剂,并通过实验验证比较了几种选盐理论模型的优缺点,得出了其各自的适用范围,为盐效萃取工艺中盐析剂的选择提供了理论依据。
2环己酮-水-无机盐体系及正丁醇-水-无机盐体系液-液相平衡实验研究:系统的测定了环己酮-水-碳酸钾、环己酮-水-氟化钾、正丁醇-水-氟化钾、正丁醇-水-碳酸钾体系的液-液相平衡数据,为采用无机盐分离环己酮-水和正丁醇-水恒沸体系提供了基础数据。
3环己酮-水-无机盐及正丁醇-水-无机盐体系液-液相平衡数学模型的研究:分别采用Pitzer理论和NRTL、Wilson或UNIQUAC方程计算了环己酮-水-碳酸钾、环己酮-水-氟化钾、正丁醇-水-氟化钾、正丁醇-水-碳酸钾体系的液-液相平衡数据,为采用无机盐分离环己酮-水和正丁醇-水恒沸体系提供了计算依据。
4盐效萃取分离正丁醇-水体系工艺研究:根据液-液相平衡实验所得到的结果,采用碳酸钾水溶液萃取分离正丁醇-水体系,考察了碳酸钾水溶液的稳定性及溶液萃取比对萃取效果的影响,并确定了最佳萃取比。建立高浓度正丁醇废液资源化利用节能技术的工艺流程,为了对该流程与传统恒沸精馏流程的能耗情况进行比较,采用Aspen Plus流程模拟软件对新旧流程进行了模拟计算,结果发现盐效萃取工艺可大幅度的降低分离正丁醇-水体系的能耗。
The separation of partially miscible cyclohexanone - water and n-butanol - water systems based on salting-out principle is studied by the combined methods of theoretical analysis and experimental research, including the selection of inorganic salts, the liquid-liquid equilibrium(LLE) experiments and salting-out extraction process, and a theoretical model is established by the calculation of LLE data.
Currently, it has an important application background for the salting-out extraction of partially miscible of azeotropic organic/water system in industry. Compared to conventional azeotropic distillation and extractive distillation process, this method can greatly reduce the energy consumption and is also consistent with the development of low-carbon. When the salt is added into the miscible azeotropic organic/water system, the interaction between the ions of salt and solvent molecules will change the LLE of this system and the partition coefficient of solvents to get the mixture separated. This is the salting-out effect of inorganic salts. Until now there are not so many reports about the research of partially miscible of azeotropic organic/water system by salting-out extraction exist and the LLE data of organic/water system is short, which brings a lot of difficulties to its research and application. In this paper the LLE of cyclohexanone-water-salts and n-butanol-water–salts systems are studied, providing the basic data and theoretical basis for the salting-out extraction’s application in industry. So it has an important academic theoretical significance and industrial application. The research works have been performed in this paper as follows:
1 The selection of inorganic salt used in the process of salting-out extraction. By the combined methods of theoretical calculations, literature data and experimental study, the salts used in the separating process of cyclohexanone-water and 1-butanol-water systems are selected. The theoretical models of salt selection are studied by the experimental verification method and its scope of application is determinated, which provides theoretical data for the selection of inorganic salt in the process of salting-out extraction.
2 Research on the LLE of cyclohexanone - water - salts and n-butanol - water - salts systems.The LLE data of the systems of cyclohexanone - water - potassium carbonate, cyclohexanone - water - potassium fluoride, n-butanol - water - potassium fluoride, n-butanol - water - potassium carbonate are experimentally measured, providing basis data for the separation of cyclohexanone/water and n-butanol/water systems by salting-out extraction.
3 Study on the mathematical model for the LLE of cyclohexanone - water - salts and n-butanol - water - salts systems. The LLE data of the systems of cyclohexanone - water - potassium carbonate, cyclohexanone - water - potassium fluoride, n-butanol - water - potassium fluoride, n-butanol - water - potassium carbonate are calculated by the Pitzer electrolyte solution theory and NRTL, Wilson or UNIQUAC equations, respectively. It provides a theoretical basis for the separation of cyclohexanone - water and n-butanol - water systems by using inorganic salts.
4 The technical study on the separation of n-butanol - water system by Salting-out extraction ways. According to the experimental results of liquid - liquid equilibrium, the potassium carbonate is selected and used to separate n-butanol/water system by salting-out extraction. The stability of aqueous potassium carbonate and mass ratio of aqueous potassium carbonate to raw materials on the extraction efficiency are investigated, and the optimum extraction ratio is obtained. Then the utilization process of high concentrations of n-butanol effluent with lower energy consumption is established. To compare the energy consumption of azeotropic distillation process and the salting-out extraction process, the processes are simulated and calculated by Aspen Plus simulation software and result shows that salting-out extraction process can be greatly reduced energy consumption in the separating process of this system.
引文
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