FCC汽油萃取精馏深度脱硫过程研究
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摘要
为控制汽车尾气对环境的污染,生产低硫汽油已成为炼油工业21世纪面临的迫切任务。在诸多生产低硫汽油的技术中,汽油萃取精馏深度脱硫技术具有过程条件温和、产品辛烷值损失小、能耗低、环境友好等优势。因此,深入研究汽油萃取/萃取精馏深度脱硫过程的相关问题具有重要的理论意义和应用价值。本文以FCC汽油(fludized catalytic cracking gasoline,通称为FCC汽油)和模拟汽油为原料,分别对萃取、萃取精馏过程的溶剂筛选、溶剂萃取性能评价和过程条件优化,含硫化合物和萃取溶剂的液液、汽液相平衡以及FCC汽油连续萃取精馏过程的模拟分析进行了研究。
以FCC汽油和三种模拟汽油(分别由硫醇、硫醚、噻吩+C6～C8烷烃组成)为原料,考察了初选溶剂环丁砜、二甲基亚砜、四甘醇和二甘醇的萃取脱硫性能,确定了环丁砜可作为FCC汽油萃取/萃取精馏脱硫的首选溶剂。FCC汽油连续萃取精馏脱硫的研究结果表明,以环丁砜为溶剂,在回流比4、剂油比0.3条件下,脱硫率达到88.5%;随着剂油比的增加,脱硫率增加,剂油比>0.3后脱硫率变化缓慢,剂油比在0.3～0.8之间较为适宜。进一步的研究结果表明,以环丁砜为萃取剂对FCC汽油中馏分进行脱硫脱芳,在回流比4、剂油比0.55的条件下,萃余油硫含量<30μg/g,苯含量<0.5%,芳烃含量<3%,可作为优质的重整原料;减压蒸馏回收的环丁砜热稳定性较好,回收后的环丁砜仍有很好的脱硫脱芳效果,可循环使用。
采用平衡釜法测定了常压下40、50、60℃时七个含硫化合物-正辛烷-萃取溶剂三元体系的液液相平衡数据:1)噻吩-正辛烷-二甲基亚砜体系,2)噻吩-正辛烷-环丁砜体系,3)噻吩-正辛烷-四甘醇体系,4)正丁基硫醇-正辛烷-环丁砜体系,5)正丁基硫醇-正辛烷-四甘醇体系,6)正丁基硫醚-正辛烷-环丁砜体系,7)正丁基硫醚-正辛烷-四甘醇体系。用NTRL、UNIQUAC模型对相平衡数据进行了热力学关联。关联时以摩尔分数偏差平方和最小为目标函数,用单纯形和拟牛顿优化法及混合吉布斯自由能最小的热力学平衡准则,确定了相应的模型参数。结果表明,NRTL模型对噻吩体系的预测误差最小,噻吩质量百分数的平均绝对偏差在0.005左右;正丁基硫醇和正丁基硫醚的质量百分数平均绝对偏差分别在0.04和0.0342左右。这表明NRTL模型能较好的描述上述三元体系的液液相平衡。
采用双循环汽液平衡釜法测定了四个常压下两类含硫化合物-正辛烷/环丁砜体系的二元汽液平衡数据:1)噻吩-正辛烷,2)噻吩-环丁砜,3)正丁基硫醇-正辛烷,4)正丁基硫醇-环丁砜体系。采用var Laar、Wilson、NTRL、UNIQUAC模型对汽液相平衡数据进行了热力学关联。UNIQUAC模型的预测结果优于其它三个模型的预测结果,其噻吩和正丁基硫醇的质量分数平均绝对偏差分别为0.0614和0.0505。四个体系的汽液相平衡数据基本符合Herrington的热力学一致性检验。
采用SRK-KD和NRTL方程,结合ProII新增的含有环丁砜部分性能的系统补丁,增补由实验平衡数据拟合得到的组分间交互作用参数(采用NRTL模型,结合UNIFAC活度系数方程对实验得到的VLE与LLE数据计算得到),用ProII软件对萃取精馏过程进行了模拟计算,模拟结果与实验结果吻合较好。萃取精馏的适宜条件为理论板数10～15、剂油比0.5、回流比4,溶剂进料位置在第4块理论板,原料油在下数第3～4板进料。在此基础上提出了萃取精馏+加氢脱硫组合工艺流程。
In order to control the pollution resulted from vehicle exhaust the production of gasoline with ultra-low sulfur content has become an urgent mission for the oil refining industries in the 21st century. Extractive distillation (ED) deep desulfurization of FCC gasoline has many potential advantages over the other desulfurization techniques, such as mild process conditions, low loss of octane number, low energy consumed, environmentally friendly, and etc. The study of extraction/extractive distillation deep desulfurization is of significantly economic and social interesting.
Studies in this work focused on selection and performance evaluation of the solvents for extraction desulfurization of FCC and modeling gasolines, optimization for continuous extraction/extractive distillation process of FCC gasoline, measurement and correlation of liquid-liquid, vapor-liquid phase equilibrium of three sulfides (thiophene, n-butyl mercaptan and n-dibutyl sulfide in FCC gasoline)– solvent, and simulation and analysis of FCC gasoline ED desulfurization process.
In the experimental study of extraction desulfurization, FCC gasoline and modeling gasolines which were prepared by respectively added mercaptan, sulfide, thiophene into C6～C8, used as feeds, the performance of the four selected solvents (sulfolane, dimethyl sulfoxide, tetraethylene glycol and diethylene glycol) were investigated, and finally sulfolane was considered as a best solvent for FCC gasoline extraction distillation desulfurization. The experimental results showed that using sulfolane as solvent, under the conditions of reflux ratio 4, solvent/oil ratio 0.3, the FCC gasoline desulfurization percentage reached to 88.5%, the desulfurization percentage increased with the increasing of solvent/oil ratio as solvent/oil ratio< 0.3, and the desulfurization percentage increased slightly with the increasing of solvent/oil ratio as solvent/oil ratio > 0.3 and a suitable solvent/oil ratio could be in a range of 0.3 ~ 0.8. Further experimental results of FCC gasoline medium fraction ED desulfurization-dearomation with sulfolane indicated that under the conditions of reflux ratio 4 and solvent/oil ratio 0.55, in the raffinate, the sulfur content could be reduced to less than 30μg/g, the benzene content less than 0.5% and the aromatics content less than 3%. The results of stability experiments showed that the recovered sulfolane with a good chemical stability can be reused.
Liquid-liquid equilibria (LLE) data of seven ternary systems of sulfide - octane - solvent at 40,50 and 60℃under atmospheric pressure were measured using an equilibria cell,the systems included: 1) thiophene- octane - dimethyl sulfoxide, 2) thiophene - octane - sulfolane, 3) thiophene- octane - teraethylene glycol, 4) n-butyl mercaptan -octane -sulfolane, 5) n-butyl mercaptan- octane - teraethylene glycol, 6) n-dibutyl sulfide- octane- sulfolane, 7) n-dibutyl sulfide- octane- teraethylene glycol. NRTL and UNIQUAC models were used to correlate and predict the LLE data of the ternary systems. The model parameters were estimated using the simplex optimization method and the quasi-Newton method with an objective function of mass fraction deviation square and the rule of minimum Gibbs free energy in a closed thermodynamic equilibrium system. The results indicated that NRTL model was better than UNIQUAC model, and the average absolute deviation of thiophene mass percentage is ca 0.0050, n-butyl mercaptan ca 0.0400, and n-dibutyl sulfide ca 0.0342. This implies that NRTL model is more suitable for describing the Liquid-liquid equilibria of the ternary systems studied.
Vapour-liquid equilibria (VLE) data of four binary systems of the sulfides-octane/ sulfolane were measured using a dual-circulating VLE cell, and the systems included: 1) thiophene- octane, 2) thiophene-sulfolane, 3) n-butyl mercaptan-octane, 4) n-butyl mercaptan -sulfolane. var Laar, Wilson, NRTL and UNIQUAC models were employed to correlate the VLE data and predict phase composition. Prediction of the UNIQUAC model was better than those of the other three models, and average mass fraction absolute deviations of thiophene and n-butyl mercaptan are respectively ca 0.0614 and ca 0.0505. The VLE data of the four systems were satisfied with Herrington thermodynamic consistency.
The SRK-KD and NRTL equations were used to simulate the ED process of FCC gasoline desulfurization using Pro II software. The inter-action parameters used in the simulation were determined using NRTL and UNIFAC activity coefficient models with the experimental VLE and LLE data. The simulated and the experimental results of the ED process were in fairly agreetment. Optimal operation conditions of FCC gasoline extraction distillation desulfurization were obtained as follows: theory stage number NT 10～15, solvent/oil ratio 0.5, reflux ratio 4, solvent feeded in the 4th tray, and oil feeded in the 3rd or 4th tray from bottom. Based on the experimental and simulated results, a combined deep desulfurization process of ED- HDS was suggusted.
以FCC汽油和三种模拟汽油(分别由硫醇、硫醚、噻吩+C6～C8烷烃组成)为原料,考察了初选溶剂环丁砜、二甲基亚砜、四甘醇和二甘醇的萃取脱硫性能,确定了环丁砜可作为FCC汽油萃取/萃取精馏脱硫的首选溶剂。FCC汽油连续萃取精馏脱硫的研究结果表明,以环丁砜为溶剂,在回流比4、剂油比0.3条件下,脱硫率达到88.5%;随着剂油比的增加,脱硫率增加,剂油比>0.3后脱硫率变化缓慢,剂油比在0.3～0.8之间较为适宜。进一步的研究结果表明,以环丁砜为萃取剂对FCC汽油中馏分进行脱硫脱芳,在回流比4、剂油比0.55的条件下,萃余油硫含量<30μg/g,苯含量<0.5%,芳烃含量<3%,可作为优质的重整原料;减压蒸馏回收的环丁砜热稳定性较好,回收后的环丁砜仍有很好的脱硫脱芳效果,可循环使用。
采用平衡釜法测定了常压下40、50、60℃时七个含硫化合物-正辛烷-萃取溶剂三元体系的液液相平衡数据:1)噻吩-正辛烷-二甲基亚砜体系,2)噻吩-正辛烷-环丁砜体系,3)噻吩-正辛烷-四甘醇体系,4)正丁基硫醇-正辛烷-环丁砜体系,5)正丁基硫醇-正辛烷-四甘醇体系,6)正丁基硫醚-正辛烷-环丁砜体系,7)正丁基硫醚-正辛烷-四甘醇体系。用NTRL、UNIQUAC模型对相平衡数据进行了热力学关联。关联时以摩尔分数偏差平方和最小为目标函数,用单纯形和拟牛顿优化法及混合吉布斯自由能最小的热力学平衡准则,确定了相应的模型参数。结果表明,NRTL模型对噻吩体系的预测误差最小,噻吩质量百分数的平均绝对偏差在0.005左右;正丁基硫醇和正丁基硫醚的质量百分数平均绝对偏差分别在0.04和0.0342左右。这表明NRTL模型能较好的描述上述三元体系的液液相平衡。
采用双循环汽液平衡釜法测定了四个常压下两类含硫化合物-正辛烷/环丁砜体系的二元汽液平衡数据:1)噻吩-正辛烷,2)噻吩-环丁砜,3)正丁基硫醇-正辛烷,4)正丁基硫醇-环丁砜体系。采用var Laar、Wilson、NTRL、UNIQUAC模型对汽液相平衡数据进行了热力学关联。UNIQUAC模型的预测结果优于其它三个模型的预测结果,其噻吩和正丁基硫醇的质量分数平均绝对偏差分别为0.0614和0.0505。四个体系的汽液相平衡数据基本符合Herrington的热力学一致性检验。
采用SRK-KD和NRTL方程,结合ProII新增的含有环丁砜部分性能的系统补丁,增补由实验平衡数据拟合得到的组分间交互作用参数(采用NRTL模型,结合UNIFAC活度系数方程对实验得到的VLE与LLE数据计算得到),用ProII软件对萃取精馏过程进行了模拟计算,模拟结果与实验结果吻合较好。萃取精馏的适宜条件为理论板数10～15、剂油比0.5、回流比4,溶剂进料位置在第4块理论板,原料油在下数第3～4板进料。在此基础上提出了萃取精馏+加氢脱硫组合工艺流程。
In order to control the pollution resulted from vehicle exhaust the production of gasoline with ultra-low sulfur content has become an urgent mission for the oil refining industries in the 21st century. Extractive distillation (ED) deep desulfurization of FCC gasoline has many potential advantages over the other desulfurization techniques, such as mild process conditions, low loss of octane number, low energy consumed, environmentally friendly, and etc. The study of extraction/extractive distillation deep desulfurization is of significantly economic and social interesting.
Studies in this work focused on selection and performance evaluation of the solvents for extraction desulfurization of FCC and modeling gasolines, optimization for continuous extraction/extractive distillation process of FCC gasoline, measurement and correlation of liquid-liquid, vapor-liquid phase equilibrium of three sulfides (thiophene, n-butyl mercaptan and n-dibutyl sulfide in FCC gasoline)– solvent, and simulation and analysis of FCC gasoline ED desulfurization process.
In the experimental study of extraction desulfurization, FCC gasoline and modeling gasolines which were prepared by respectively added mercaptan, sulfide, thiophene into C6～C8, used as feeds, the performance of the four selected solvents (sulfolane, dimethyl sulfoxide, tetraethylene glycol and diethylene glycol) were investigated, and finally sulfolane was considered as a best solvent for FCC gasoline extraction distillation desulfurization. The experimental results showed that using sulfolane as solvent, under the conditions of reflux ratio 4, solvent/oil ratio 0.3, the FCC gasoline desulfurization percentage reached to 88.5%, the desulfurization percentage increased with the increasing of solvent/oil ratio as solvent/oil ratio< 0.3, and the desulfurization percentage increased slightly with the increasing of solvent/oil ratio as solvent/oil ratio > 0.3 and a suitable solvent/oil ratio could be in a range of 0.3 ~ 0.8. Further experimental results of FCC gasoline medium fraction ED desulfurization-dearomation with sulfolane indicated that under the conditions of reflux ratio 4 and solvent/oil ratio 0.55, in the raffinate, the sulfur content could be reduced to less than 30μg/g, the benzene content less than 0.5% and the aromatics content less than 3%. The results of stability experiments showed that the recovered sulfolane with a good chemical stability can be reused.
Liquid-liquid equilibria (LLE) data of seven ternary systems of sulfide - octane - solvent at 40,50 and 60℃under atmospheric pressure were measured using an equilibria cell,the systems included: 1) thiophene- octane - dimethyl sulfoxide, 2) thiophene - octane - sulfolane, 3) thiophene- octane - teraethylene glycol, 4) n-butyl mercaptan -octane -sulfolane, 5) n-butyl mercaptan- octane - teraethylene glycol, 6) n-dibutyl sulfide- octane- sulfolane, 7) n-dibutyl sulfide- octane- teraethylene glycol. NRTL and UNIQUAC models were used to correlate and predict the LLE data of the ternary systems. The model parameters were estimated using the simplex optimization method and the quasi-Newton method with an objective function of mass fraction deviation square and the rule of minimum Gibbs free energy in a closed thermodynamic equilibrium system. The results indicated that NRTL model was better than UNIQUAC model, and the average absolute deviation of thiophene mass percentage is ca 0.0050, n-butyl mercaptan ca 0.0400, and n-dibutyl sulfide ca 0.0342. This implies that NRTL model is more suitable for describing the Liquid-liquid equilibria of the ternary systems studied.
Vapour-liquid equilibria (VLE) data of four binary systems of the sulfides-octane/ sulfolane were measured using a dual-circulating VLE cell, and the systems included: 1) thiophene- octane, 2) thiophene-sulfolane, 3) n-butyl mercaptan-octane, 4) n-butyl mercaptan -sulfolane. var Laar, Wilson, NRTL and UNIQUAC models were employed to correlate the VLE data and predict phase composition. Prediction of the UNIQUAC model was better than those of the other three models, and average mass fraction absolute deviations of thiophene and n-butyl mercaptan are respectively ca 0.0614 and ca 0.0505. The VLE data of the four systems were satisfied with Herrington thermodynamic consistency.
The SRK-KD and NRTL equations were used to simulate the ED process of FCC gasoline desulfurization using Pro II software. The inter-action parameters used in the simulation were determined using NRTL and UNIFAC activity coefficient models with the experimental VLE and LLE data. The simulated and the experimental results of the ED process were in fairly agreetment. Optimal operation conditions of FCC gasoline extraction distillation desulfurization were obtained as follows: theory stage number NT 10～15, solvent/oil ratio 0.5, reflux ratio 4, solvent feeded in the 4th tray, and oil feeded in the 3rd or 4th tray from bottom. Based on the experimental and simulated results, a combined deep desulfurization process of ED- HDS was suggusted.
引文
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