N-甲酰吗啉抽提芳烃体系相平衡及过程模拟研究
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摘要
本文以优良的新型芳烃抽提剂N-甲酰吗啉(NFM)在萃取抽提过程中的应用为背景,实验测定了大量的相平衡数据,全面地考察了NFM抽提性能;以相平衡的条件为依据,建立了NFM抽提体系平衡数据关联模型,通过优化方法得到了热力学模型方程的作用参数;在此基础上围绕相平衡组成、临界点以及抽提过程模拟计算等方面,探讨了热力学模型方程在抽提体系中的应用。
1、相平衡的测定及实验数据可靠性分析。实验测定了不同温度下NFM分别与庚烷、环己烷以及甲基环己烷之间的相互溶解度,以及烷烃(庚烷,环己烷,甲基环己烷)+芳烃(苯,甲苯)+NFM六个体系在多个温度下的三元相平衡数据。相互溶解度实验结果表明,温度升高,NFM与烷烃(庚烷,环己烷,甲基环己烷)之间的相互溶解增大,相互溶解度顺序为环己烷＞甲基环己烷＞庚烷。以实验数据所建立的三元液液平衡相图表明,该类相图具有热力学相平衡类型Ⅰ的特征,NFM与芳烃和烷烃组成的体系存在较大的相平衡区域,从而NFM能满足抽提溶剂的要求。Othmer-Tobias和Bachman方程对三元体系相平衡实验数据关联的结果表明实验数据具有较好的一致可靠性。
2、N-甲酰吗啉抽提性能研究。系统地研究了NFM的抽提性能,考察了分配系数,选择性以及分离因子随温度和进料中芳烃含量之间的变化关系。结果表明NFM对芳烃具有良好的抽提性能,苯的分配系数、分离因子和选择性分别高达0.99,12.4和5.2;对于甲苯,也能达到0.85,9.6和3.4。温度升高,有利于芳烃的分配系数增加,而分离因子和选择性却呈下降的趋势;在两相共存区域内,进料中芳烃的含量增加使芳烃的分配系数增大,但其选择性随之减小。
3、相平衡的热力学模型研究与组成计算。以相平衡稳定性条件为出发点,建立了NFM抽提体系平衡数据关联模型;针对非线性目标函数难以得到全局最优解的问题,采用相平衡体系的Gibbs自由能最小原则,给定多个初值的方法以及共轭梯度算法回归等措施,求出了各体系的热力学模型方程(改进的NRTL和UNIQUAC)的参数,确保了所获得的参数为全局近似最优解。在此基础上,结合物料守恒方程用Broyden算法对各体系平衡组成进行了计算,结果发现,计算值与实验值非常吻合。对于烷烃-NFM二元体系,NRTL方程的偏差在0.0104～0.0817之间,UNIQUAC方程的偏差在0.0182～0.7105之间,而在烷烃-芳烃-NFM的三元体系中,NRTL和UNIQUAC方程的偏差分别在0.0110～0.0937和0.0133～0.1471之间,大大低于文献中规定的1.37的值。由此可见,改进的NRTL方程比UNIQUAC方程更能有效地描述体系的相行为。
4、平衡体系临界点的估算。以上述热力学模型回归参数为基础,对二元体系和三元体系临界点计算进行了理论研究,分别用NRTL和UNIQUAC两个模型方程给出了的临界点处温度和组成关系的数学表达式,从理论上获得了各体系相平衡曲线上的临界点值,为实际抽提过程中避免在临界点附近操作提供参考依据。
5、热力学模型在抽提过程模拟计算。将NRTL和UNIQUAC方程与经典的萃取塔模型和流率加和算法相结合,对NFM萃取抽提芳烃过程进行模拟计算,结果表明:在优化条件下,NFM能从烷烃中很好地分离出芳烃;在能产生液液相分离的前提下,温度升高和溶剂比增加有利于抽提过程;在给定进料条件下,在溶剂比为2.875时,庚烷-NFM溶剂体系内,温度为353K,理论板数为8,芳烃的回收率可达95%以上;在环己烷-NFM溶剂内,温度在298K,理论板为8时芳烃回收率达到96%以上;在温度为353K、理论塔板数为15,芳烃在甲基环己烷-NFM溶剂体系中的回收率在92%以上。
As one of the new and excellent aromatics extractants, N-formylmorphoiline(NFM) was investigated through measuring experimentally the liquid-liquid equilibrium (LLE) data for aromatics extraction from hydrocarbon (heptane, cyclohexane, methylcyclohexane), and its extraction capability was studied thoroughly. According to the conditions of phase equilibrium, the mathematical model was established to correlate liquid-liquid equilibrium data and the parameters of the model were obtained by optimization method. Then the applications of the two thermodynamic equations in the extraction systems were carried out by calculation of phase equilibrium, critical points and simulation of extraction process. The main conclusions are as follows.
1、Measurement of LLE and consistency of experimental data. The LLE data were measured for three binary systems (NFM + heptane or cyclohexane or methylcyclohexane) and six ternary systems (NFM+hydrocarbon (heptane, cyclohexane, methylcyclohexane) +aromatics (benzene, toluene)) using custom-built liquid-liquid equilibrium cell. It was found that the mutual solubilities increased in the higher temperature for the three binary systems. The mutual solubilities for NFM with different hydrocarbons satisfied the following relationship: cyclohexane > methylcyclohexane > heptane. The LLE diagrams obtained showed that they were type I and there exsited the large immiscibility regions, ensuring NFM to meet the demand of extraction solvent. The reliability of experimentally measured tie-line data was correlated by the Othmer-Tobias and the Bachman equations, and it was shown that the correlation coefficients had satisfactory degree of consistency.
2、The extraction capabilities of NFM. The extraction capabilities of NFM were studied systematically. Distribution coefficients, separation factors and selectivity were evaluated for the immiscibility region, and their connections with temperature and the concentration of aromatic hydrocarbon were studied respectively. The results showed that NFM had excellent extraction capabilities. The values of distribution coefficient, separation factor and selectivity for benzene in these systems are 0.99, 12.4 and 5.2 respectively; and 0.85, 9.6 and 3.4 are also obtained for toluene. It was also found that with temperature increasing, the distribution coefficients of aromatic hydrocarbon increased, while the separation factors and the selectivity decreased. In the two phase coexistence area, as the concentration of aromatic hydrocarbon increased, distribution coefficients became higher and selectivity lower.
3、The correlation of thermodynamic equations and the LLE calculation. Based on phase stability conditions, the objective function was established to correlate the LLE data. Because the solution of the global optimization is difficult to be obtained for the non-linear equations, several measurements had been employed, such as the minimization of Gibbs free energy of multi-component systems, feasible initial guess for a new minimization, conjugate Gradient method. The parameters of the two thermodynamics equations (NRTL and UNIQUAC) were guaranteed to be near the solution of global optimization. The correct solutions were obtained by the equality of chemical potentials, materiel conservation, and the Broyden method. It was found that NRTL and UNIQUAC used for LLE could provide a good prediction, and the former model was more suitable for the studied systems. In hydrocarbon-NFM binary systems, the root mean square deviation (RMSD) values of NRTL are in the range of 0.0104-0.0817, and those of UNIQUAC are between 0.0182-0.7105. In the ternary systems, the RMSD values are 0.0110-0.0937 for NRTL, 0.0133-0.1471 for UNIQUAC, showing that all RMSD values are lower than 1.37 prescribed by the literature.
4、Critical points of the equilibrium. Based on the parameters of two thermodynamics equations and thermodynamics principle, the critical points of the binary and ternary systems were studied. Non-linear equations for calculating the critical points are given using the NRTL and the UNIQUAC models, respectively. The critical points can be determined by solving these non-linear equations through Broyden method. These results can be applied in practical extraction process to operate in the conditions far from critical points.
5、Simulation of extraction process using thermodynamics equations. Simulation of extraction process using NFM as solvent to separate aromatics from hydrocarbon was carried out by adopting classical extraction tower model and Isothermal Sum Rates method. The two thermodynamics equations(NRTL and UNIQUAC) were used to calculate equilibrium constants of components. The optimization results obtained by the two equations show that aromatics can be separated effectively by NFM in extraction tower, and the relative temperature and solvent ratio are favorable on the condition of liquid-liquid phase separation. In the given conditions, in Heptane-NFM solvents system, when theoretical tray is 8, solvent ratio is 2.875, the recovery of aromatics can reach 95% at 353K. In the case of Cyclohexane-NFM, the recovery of aromatics is higher than 96% at 298K, in the conditions of theoretical tray=8, solvent ratio=2.875; As for Methylcyclohexane-NFM, the recovery of aromatics is as high as 92% at 353K, when theoretical tray is 15, solvent ratio is 2.875.
1、相平衡的测定及实验数据可靠性分析。实验测定了不同温度下NFM分别与庚烷、环己烷以及甲基环己烷之间的相互溶解度,以及烷烃(庚烷,环己烷,甲基环己烷)+芳烃(苯,甲苯)+NFM六个体系在多个温度下的三元相平衡数据。相互溶解度实验结果表明,温度升高,NFM与烷烃(庚烷,环己烷,甲基环己烷)之间的相互溶解增大,相互溶解度顺序为环己烷＞甲基环己烷＞庚烷。以实验数据所建立的三元液液平衡相图表明,该类相图具有热力学相平衡类型Ⅰ的特征,NFM与芳烃和烷烃组成的体系存在较大的相平衡区域,从而NFM能满足抽提溶剂的要求。Othmer-Tobias和Bachman方程对三元体系相平衡实验数据关联的结果表明实验数据具有较好的一致可靠性。
2、N-甲酰吗啉抽提性能研究。系统地研究了NFM的抽提性能,考察了分配系数,选择性以及分离因子随温度和进料中芳烃含量之间的变化关系。结果表明NFM对芳烃具有良好的抽提性能,苯的分配系数、分离因子和选择性分别高达0.99,12.4和5.2;对于甲苯,也能达到0.85,9.6和3.4。温度升高,有利于芳烃的分配系数增加,而分离因子和选择性却呈下降的趋势;在两相共存区域内,进料中芳烃的含量增加使芳烃的分配系数增大,但其选择性随之减小。
3、相平衡的热力学模型研究与组成计算。以相平衡稳定性条件为出发点,建立了NFM抽提体系平衡数据关联模型;针对非线性目标函数难以得到全局最优解的问题,采用相平衡体系的Gibbs自由能最小原则,给定多个初值的方法以及共轭梯度算法回归等措施,求出了各体系的热力学模型方程(改进的NRTL和UNIQUAC)的参数,确保了所获得的参数为全局近似最优解。在此基础上,结合物料守恒方程用Broyden算法对各体系平衡组成进行了计算,结果发现,计算值与实验值非常吻合。对于烷烃-NFM二元体系,NRTL方程的偏差在0.0104～0.0817之间,UNIQUAC方程的偏差在0.0182～0.7105之间,而在烷烃-芳烃-NFM的三元体系中,NRTL和UNIQUAC方程的偏差分别在0.0110～0.0937和0.0133～0.1471之间,大大低于文献中规定的1.37的值。由此可见,改进的NRTL方程比UNIQUAC方程更能有效地描述体系的相行为。
4、平衡体系临界点的估算。以上述热力学模型回归参数为基础,对二元体系和三元体系临界点计算进行了理论研究,分别用NRTL和UNIQUAC两个模型方程给出了的临界点处温度和组成关系的数学表达式,从理论上获得了各体系相平衡曲线上的临界点值,为实际抽提过程中避免在临界点附近操作提供参考依据。
5、热力学模型在抽提过程模拟计算。将NRTL和UNIQUAC方程与经典的萃取塔模型和流率加和算法相结合,对NFM萃取抽提芳烃过程进行模拟计算,结果表明:在优化条件下,NFM能从烷烃中很好地分离出芳烃;在能产生液液相分离的前提下,温度升高和溶剂比增加有利于抽提过程;在给定进料条件下,在溶剂比为2.875时,庚烷-NFM溶剂体系内,温度为353K,理论板数为8,芳烃的回收率可达95%以上;在环己烷-NFM溶剂内,温度在298K,理论板为8时芳烃回收率达到96%以上;在温度为353K、理论塔板数为15,芳烃在甲基环己烷-NFM溶剂体系中的回收率在92%以上。
As one of the new and excellent aromatics extractants, N-formylmorphoiline(NFM) was investigated through measuring experimentally the liquid-liquid equilibrium (LLE) data for aromatics extraction from hydrocarbon (heptane, cyclohexane, methylcyclohexane), and its extraction capability was studied thoroughly. According to the conditions of phase equilibrium, the mathematical model was established to correlate liquid-liquid equilibrium data and the parameters of the model were obtained by optimization method. Then the applications of the two thermodynamic equations in the extraction systems were carried out by calculation of phase equilibrium, critical points and simulation of extraction process. The main conclusions are as follows.
1、Measurement of LLE and consistency of experimental data. The LLE data were measured for three binary systems (NFM + heptane or cyclohexane or methylcyclohexane) and six ternary systems (NFM+hydrocarbon (heptane, cyclohexane, methylcyclohexane) +aromatics (benzene, toluene)) using custom-built liquid-liquid equilibrium cell. It was found that the mutual solubilities increased in the higher temperature for the three binary systems. The mutual solubilities for NFM with different hydrocarbons satisfied the following relationship: cyclohexane > methylcyclohexane > heptane. The LLE diagrams obtained showed that they were type I and there exsited the large immiscibility regions, ensuring NFM to meet the demand of extraction solvent. The reliability of experimentally measured tie-line data was correlated by the Othmer-Tobias and the Bachman equations, and it was shown that the correlation coefficients had satisfactory degree of consistency.
2、The extraction capabilities of NFM. The extraction capabilities of NFM were studied systematically. Distribution coefficients, separation factors and selectivity were evaluated for the immiscibility region, and their connections with temperature and the concentration of aromatic hydrocarbon were studied respectively. The results showed that NFM had excellent extraction capabilities. The values of distribution coefficient, separation factor and selectivity for benzene in these systems are 0.99, 12.4 and 5.2 respectively; and 0.85, 9.6 and 3.4 are also obtained for toluene. It was also found that with temperature increasing, the distribution coefficients of aromatic hydrocarbon increased, while the separation factors and the selectivity decreased. In the two phase coexistence area, as the concentration of aromatic hydrocarbon increased, distribution coefficients became higher and selectivity lower.
3、The correlation of thermodynamic equations and the LLE calculation. Based on phase stability conditions, the objective function was established to correlate the LLE data. Because the solution of the global optimization is difficult to be obtained for the non-linear equations, several measurements had been employed, such as the minimization of Gibbs free energy of multi-component systems, feasible initial guess for a new minimization, conjugate Gradient method. The parameters of the two thermodynamics equations (NRTL and UNIQUAC) were guaranteed to be near the solution of global optimization. The correct solutions were obtained by the equality of chemical potentials, materiel conservation, and the Broyden method. It was found that NRTL and UNIQUAC used for LLE could provide a good prediction, and the former model was more suitable for the studied systems. In hydrocarbon-NFM binary systems, the root mean square deviation (RMSD) values of NRTL are in the range of 0.0104-0.0817, and those of UNIQUAC are between 0.0182-0.7105. In the ternary systems, the RMSD values are 0.0110-0.0937 for NRTL, 0.0133-0.1471 for UNIQUAC, showing that all RMSD values are lower than 1.37 prescribed by the literature.
4、Critical points of the equilibrium. Based on the parameters of two thermodynamics equations and thermodynamics principle, the critical points of the binary and ternary systems were studied. Non-linear equations for calculating the critical points are given using the NRTL and the UNIQUAC models, respectively. The critical points can be determined by solving these non-linear equations through Broyden method. These results can be applied in practical extraction process to operate in the conditions far from critical points.
5、Simulation of extraction process using thermodynamics equations. Simulation of extraction process using NFM as solvent to separate aromatics from hydrocarbon was carried out by adopting classical extraction tower model and Isothermal Sum Rates method. The two thermodynamics equations(NRTL and UNIQUAC) were used to calculate equilibrium constants of components. The optimization results obtained by the two equations show that aromatics can be separated effectively by NFM in extraction tower, and the relative temperature and solvent ratio are favorable on the condition of liquid-liquid phase separation. In the given conditions, in Heptane-NFM solvents system, when theoretical tray is 8, solvent ratio is 2.875, the recovery of aromatics can reach 95% at 353K. In the case of Cyclohexane-NFM, the recovery of aromatics is higher than 96% at 298K, in the conditions of theoretical tray=8, solvent ratio=2.875; As for Methylcyclohexane-NFM, the recovery of aromatics is as high as 92% at 353K, when theoretical tray is 15, solvent ratio is 2.875.
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