循环全回流间歇精馏过渡馏分新操作方式的研究
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摘要
间歇精馏由于其高纯度、易操作等优点在制药、精细化工等化工行业广为应用。循环全回流间歇精馏操作方法可以减少间歇精馏时间，提高产品纯度，可在最短的时间内将轻组分从塔顶馏出，具有分离效率高、控制简便、对扰动不敏感、易于操作等优点。目前循环全回流间歇精馏的研究基本上集中在操作方法的理论研究方面，并且仅限于二元物系的研究，而使其在工业应用中受到局限。
本文针对已有研究的不足，进行了三元物系循环全回流间歇精馏的操作方法的研究的模拟研究和实验研究，采用理论板辅助设定控制参数，并在塔中增加一个中间储罐用于过渡馏分阶段的采出和回流过程，通过模拟计算方法确定回流罐的设计参数及带中间回流罐循环全回流间歇精馏多温控制的控制策略用于三元物系的分离过程的可行性。
实验结果表明：本文以甲醇-乙醇-正丙醇为实验物系，采用加有中间回流罐的循环全回流间歇精馏多温控制策略，使精馏塔的利用率更高，过渡馏分的采出量和采出时间都较恒回流比更短。采用这种新的控制策略，使甲醇的产量提高了26.2%，过渡馏分采出量减少了39.3%。确定了采用塔中回流罐的循环全回流间歇精馏操作策略的可行性。
Cyclic total reflux operation is one of the new operating modes of batchdistillation. This operation is one of the most promising modes of batch distillation forits unique advantages over conventional partial reflux mode in highest enrichingefficiency under total reflux and fastest product collection under total withdrawal,together with high efficiency, energy saving and convenient controlling. Fewresearches are focused on the development and optimization of the control method forthis new operation mode which needs more precise and optimized control in order togive full play to its potential.
Operation strategy of cycle total reflux batch distillation with middle reflux drumwas studied in this paper. Operation steady flat was put forward and tri-componentmethanol-ethanol-propanol was adopted as the experimental mixture to validate theseparation process. According to this new operation strategy, tri-temperature controlstrategy was referred with multi-temperature sensors. Combined with systemidentification and predictive control theory, an on-line control platform wasconstructed and experiment as well as simulation was executed in order to getfeasibility verifying.
Contrast simulation and experiment of constant reflux ratio withmulti-temperature control strategies were carried out. Seven temperature sensors,equally distribute along the column, were used to control the alternation of the statesof total reflux and total withdrawal of the column and in result to keep the column runwith the highest enrichment efficiency,。The results indicated that with this newoperation and control strategy, the productivity increased 26.2%, the amount ofcollecting slop cut decreased 39.3%.The product yield increases and the amount ofslop cut decreases significantly with the same product specification. Therefore,multi-temperature control strategy holds obvious advantage over the other strategy.
本文针对已有研究的不足，进行了三元物系循环全回流间歇精馏的操作方法的研究的模拟研究和实验研究，采用理论板辅助设定控制参数，并在塔中增加一个中间储罐用于过渡馏分阶段的采出和回流过程，通过模拟计算方法确定回流罐的设计参数及带中间回流罐循环全回流间歇精馏多温控制的控制策略用于三元物系的分离过程的可行性。
实验结果表明：本文以甲醇-乙醇-正丙醇为实验物系，采用加有中间回流罐的循环全回流间歇精馏多温控制策略，使精馏塔的利用率更高，过渡馏分的采出量和采出时间都较恒回流比更短。采用这种新的控制策略，使甲醇的产量提高了26.2%，过渡馏分采出量减少了39.3%。确定了采用塔中回流罐的循环全回流间歇精馏操作策略的可行性。
Cyclic total reflux operation is one of the new operating modes of batchdistillation. This operation is one of the most promising modes of batch distillation forits unique advantages over conventional partial reflux mode in highest enrichingefficiency under total reflux and fastest product collection under total withdrawal,together with high efficiency, energy saving and convenient controlling. Fewresearches are focused on the development and optimization of the control method forthis new operation mode which needs more precise and optimized control in order togive full play to its potential.
Operation strategy of cycle total reflux batch distillation with middle reflux drumwas studied in this paper. Operation steady flat was put forward and tri-componentmethanol-ethanol-propanol was adopted as the experimental mixture to validate theseparation process. According to this new operation strategy, tri-temperature controlstrategy was referred with multi-temperature sensors. Combined with systemidentification and predictive control theory, an on-line control platform wasconstructed and experiment as well as simulation was executed in order to getfeasibility verifying.
Contrast simulation and experiment of constant reflux ratio withmulti-temperature control strategies were carried out. Seven temperature sensors,equally distribute along the column, were used to control the alternation of the statesof total reflux and total withdrawal of the column and in result to keep the column runwith the highest enrichment efficiency,。The results indicated that with this newoperation and control strategy, the productivity increased 26.2%, the amount ofcollecting slop cut decreased 39.3%.The product yield increases and the amount ofslop cut decreases significantly with the same product specification. Therefore,multi-temperature control strategy holds obvious advantage over the other strategy.
引文
[1]晋正茂，王维德，间歇精馏模拟及操作方式的研究进展，化工技术与开发，2006，35(9)：35~37
[2]Chiotti O J，Iribarren O A．Simplified models for binary batch distillation[J ] .Comput Chem Eng，1991，15 (1)：1~5
[3]Barolo M ,Guarise G B,Rienzi S A.Understanding the dynamic of a batchdistillation column with a middle vessel .Comput ChemEng ,1998 ,22:37~44
[4]Barolo M ,Guarise, GBRibon S ,et al. Some issues in the design and operationof a batch distillation column witha middle vessel . Comput Chem Eng ,1996 ,20( supply)：37~42
[5]Davidyan A G,Kiva V N ,Meski GA,et al.Batch distillation in a column with amiddle vessel.Chem Eng Sci,1994 ,49 (18)：3033~3051
[6]Meski G A ,Morari M. Design and operation of a batch distillation column with amiddle vessel .Comput Chem Eng ,1995,19 (supply)：s597~s602
[7]Barolo M,Guarise G Bx,Rienzi S A,et al.Running batch distillation in a columnwith a middle vessel .Ind Eng Chem Res ,1996 ,35 (12)：4612~4618.
[9]Arthur Rose R L，Williams T J，and Charles Prevost．Holdup in BatchDistillation[J ]．Industrial and Engineering Chemistry，1950，42(9)：1876~1879
[10]Pigford J B．Effect of Column Holdup in Batch Distillation．Industrial andEngineering Chemistry，1951，43(11)：2592~2602
[11]白鹏，张健，姜志等，间歇精馏新型操作方式的研究进展.化学工业与工程，2000，17（4）：226~230
[12]Trilleros Villaverde J A，Otero de la Gandara J L．Analogical Study of theUnsteady State in A Rectifying Column Operating under Total Reflux(I)ThereticalAspects．International Chemical Engineering AIChE，1994，34(3)：320~327.
[13]Mori Hideki，Ito Chikara，and Oda Akiyoshi，et al．Total Reflux Simulation ofPacked Column Distillation．Journal of Chemical Engineering of Japan，1999，32(1)：69~75
[14]Distefano.G..P. Mathematical Modeling and Numerical Integration ofMulticomponent Batch Distillation Equations. AIChE Jounal，1968，14 (1)：190~199
[15]时钧，汪家鼎，余国琮等.化学工程手册(上册) (第2版) .北京：化学工业出版社，1996
[16] Furlonge HI，Pantelides CC.Optimal Operation of Multivessel Batch DistillationColumns. AIChEJounal，1999，45 (4)：781~801
[17] Hasebe S．Kurooka T'and Hashimoto I。Comparisons of the SeparationPerformances of a Multi-effect Batch DistiIlation System and a ContinuousDistillation Systern．Proceedings DYCORD.1995：249
[18] Diwekar U M．and Madhavan K P．MulticomponentBatch Distillation ColumnDesign．Ind．Eng．Chem．Res．1991．30：713
[19]童景山．化工热力学，北京：清华大学出版社，1995
[20]汤恩旗，梁文才，徐世昌．间歇精馏的操作分析及设计．天津纺织工学院学报，1996，15(4)：76~80
[21]刘佳，循环全回流间歇精馏操作和模拟计算研究：[硕士学位论文]，天津：天津大学，2006
[22]李文秀，间歇精馏塔理论板数的一种确定方法，化工设计，1995，5(4)：28~31
[23]Pigford R L．Effect of Column Holdup in Batch Distillation．Ind．Eng．Chem．，1951，43(11)：2592
[24]王浩平，项曙光．间歇精馏过程模拟优化研究进展．计算机仿真，2004，2l(2)：4~6
[25]白鹏，张卫江，余国琮，动态累积分批精馏过程研究．化学工程，1994，22(5)：15
[26]颜清，彭小平，冷明伟，VBA实现恒馏出液组成间歇精馏的计算机模拟．计算机应用与软件，2008，25（12）：88~90，102
[27]颜青，彭小平，恒馏出液组成间歇精馏回流比的控制和调节．2008，25(10)：1248~1252[28杨海荣，薄翠梅，陆爱晶等，间歇精馏过程变回流比智能控制法的研究．化工自动化及仪表，2008，35(1)：12~16
[29]王为国，冯魏良，彭友瑞等，二元多段恒回流比常规间歇精馏的讨论．设计技术，2008，18（1）：7~9
[30]刘成军，刘登峰，薛发芳，精馏控制系统中灵敏板的求取．石油与天然气化工，1997，26（3）：179~181
[31]Converse A O，Gross G D．Optimal Distillate Rate Policy in Batch Distillation．Ind．Eng Chem．Fundum，1963，2：217
[32]曾舟华，不稳定精馏恒馏出液组成回流比的自动控制．黄冈师专学报，1997，1：70~72
[33]Steven E．Gallun，Charles D．Holland．Gear’s Procedure for the SimultaneousSolution of Differential and Application to Unsteady State Distillation Problems．Computers and Chemical Engineering，1982，6(3)：231~244
[34]白鹏，张卫江，尹波等，无返混动态累积分批精馏过程．化学工程，2000，28(5)：7~9
[35]刘成军，刘登峰，薛发芳，精馏控制系统中灵敏板的求取．石油与天然气化工，1997，26（3）：179~181
[36]Urmila M Diwekar，Madhavan K P．Multicomponent Batch Distillation ColumnDesign．Ind．Eng．Chem．Res．，1991，30：713~721
[37]Distefano G．P．Stability of Numerical Integration Techniques．AIChE Journal，1968，14(6)：946~955
[38]H．Sadotomo，Miyahara K．Calculation Procedure for Multicomponent BatchDistillation．International Chemical Engineering，1983，23(1)：56~64
[39]吴迪，分批精馏过程的模拟和设计计算方法的研究：[硕士生学位论文]，天津：天津大学，1992
[40]Bauerle G L，Sandall O C．Batch Distillation of Binary Mixtures at MinimumReflux．AIChE Journal，1978，33(6)：1034
[41]余国琮，杨志才，白鹏等．分批精馏优化策略与微机控制的研究．化工学报，1989，3(3)：271
[42]郭天仁，白鹏，曹吉林．间歇精馏过渡馏份的脉冲控制法．化工科技，1999，7(4)：15～18
[43]Ruiz C A．A Generalized Model Applied to Multieomponent Batch Distillation．Presented at the CHEMDATA 88 Conference．Gothenburg，Sweden，1988
[44]Diwekar U M．and Madhavan K P．MulticomponentBatch Distillation ColumnDesign．Ind．Eng．Chem．Res．1991．30：713
[2]Chiotti O J，Iribarren O A．Simplified models for binary batch distillation[J ] .Comput Chem Eng，1991，15 (1)：1~5
[3]Barolo M ,Guarise G B,Rienzi S A.Understanding the dynamic of a batchdistillation column with a middle vessel .Comput ChemEng ,1998 ,22:37~44
[4]Barolo M ,Guarise, GBRibon S ,et al. Some issues in the design and operationof a batch distillation column witha middle vessel . Comput Chem Eng ,1996 ,20( supply)：37~42
[5]Davidyan A G,Kiva V N ,Meski GA,et al.Batch distillation in a column with amiddle vessel.Chem Eng Sci,1994 ,49 (18)：3033~3051
[6]Meski G A ,Morari M. Design and operation of a batch distillation column with amiddle vessel .Comput Chem Eng ,1995,19 (supply)：s597~s602
[7]Barolo M,Guarise G Bx,Rienzi S A,et al.Running batch distillation in a columnwith a middle vessel .Ind Eng Chem Res ,1996 ,35 (12)：4612~4618.
[9]Arthur Rose R L，Williams T J，and Charles Prevost．Holdup in BatchDistillation[J ]．Industrial and Engineering Chemistry，1950，42(9)：1876~1879
[10]Pigford J B．Effect of Column Holdup in Batch Distillation．Industrial andEngineering Chemistry，1951，43(11)：2592~2602
[11]白鹏，张健，姜志等，间歇精馏新型操作方式的研究进展.化学工业与工程，2000，17（4）：226~230
[12]Trilleros Villaverde J A，Otero de la Gandara J L．Analogical Study of theUnsteady State in A Rectifying Column Operating under Total Reflux(I)ThereticalAspects．International Chemical Engineering AIChE，1994，34(3)：320~327.
[13]Mori Hideki，Ito Chikara，and Oda Akiyoshi，et al．Total Reflux Simulation ofPacked Column Distillation．Journal of Chemical Engineering of Japan，1999，32(1)：69~75
[14]Distefano.G..P. Mathematical Modeling and Numerical Integration ofMulticomponent Batch Distillation Equations. AIChE Jounal，1968，14 (1)：190~199
[15]时钧，汪家鼎，余国琮等.化学工程手册(上册) (第2版) .北京：化学工业出版社，1996
[16] Furlonge HI，Pantelides CC.Optimal Operation of Multivessel Batch DistillationColumns. AIChEJounal，1999，45 (4)：781~801
[17] Hasebe S．Kurooka T'and Hashimoto I。Comparisons of the SeparationPerformances of a Multi-effect Batch DistiIlation System and a ContinuousDistillation Systern．Proceedings DYCORD.1995：249
[18] Diwekar U M．and Madhavan K P．MulticomponentBatch Distillation ColumnDesign．Ind．Eng．Chem．Res．1991．30：713
[19]童景山．化工热力学，北京：清华大学出版社，1995
[20]汤恩旗，梁文才，徐世昌．间歇精馏的操作分析及设计．天津纺织工学院学报，1996，15(4)：76~80
[21]刘佳，循环全回流间歇精馏操作和模拟计算研究：[硕士学位论文]，天津：天津大学，2006
[22]李文秀，间歇精馏塔理论板数的一种确定方法，化工设计，1995，5(4)：28~31
[23]Pigford R L．Effect of Column Holdup in Batch Distillation．Ind．Eng．Chem．，1951，43(11)：2592
[24]王浩平，项曙光．间歇精馏过程模拟优化研究进展．计算机仿真，2004，2l(2)：4~6
[25]白鹏，张卫江，余国琮，动态累积分批精馏过程研究．化学工程，1994，22(5)：15
[26]颜清，彭小平，冷明伟，VBA实现恒馏出液组成间歇精馏的计算机模拟．计算机应用与软件，2008，25（12）：88~90，102
[27]颜青，彭小平，恒馏出液组成间歇精馏回流比的控制和调节．2008，25(10)：1248~1252[28杨海荣，薄翠梅，陆爱晶等，间歇精馏过程变回流比智能控制法的研究．化工自动化及仪表，2008，35(1)：12~16
[29]王为国，冯魏良，彭友瑞等，二元多段恒回流比常规间歇精馏的讨论．设计技术，2008，18（1）：7~9
[30]刘成军，刘登峰，薛发芳，精馏控制系统中灵敏板的求取．石油与天然气化工，1997，26（3）：179~181
[31]Converse A O，Gross G D．Optimal Distillate Rate Policy in Batch Distillation．Ind．Eng Chem．Fundum，1963，2：217
[32]曾舟华，不稳定精馏恒馏出液组成回流比的自动控制．黄冈师专学报，1997，1：70~72
[33]Steven E．Gallun，Charles D．Holland．Gear’s Procedure for the SimultaneousSolution of Differential and Application to Unsteady State Distillation Problems．Computers and Chemical Engineering，1982，6(3)：231~244
[34]白鹏，张卫江，尹波等，无返混动态累积分批精馏过程．化学工程，2000，28(5)：7~9
[35]刘成军，刘登峰，薛发芳，精馏控制系统中灵敏板的求取．石油与天然气化工，1997，26（3）：179~181
[36]Urmila M Diwekar，Madhavan K P．Multicomponent Batch Distillation ColumnDesign．Ind．Eng．Chem．Res．，1991，30：713~721
[37]Distefano G．P．Stability of Numerical Integration Techniques．AIChE Journal，1968，14(6)：946~955
[38]H．Sadotomo，Miyahara K．Calculation Procedure for Multicomponent BatchDistillation．International Chemical Engineering，1983，23(1)：56~64
[39]吴迪，分批精馏过程的模拟和设计计算方法的研究：[硕士生学位论文]，天津：天津大学，1992
[40]Bauerle G L，Sandall O C．Batch Distillation of Binary Mixtures at MinimumReflux．AIChE Journal，1978，33(6)：1034
[41]余国琮，杨志才，白鹏等．分批精馏优化策略与微机控制的研究．化工学报，1989，3(3)：271
[42]郭天仁，白鹏，曹吉林．间歇精馏过渡馏份的脉冲控制法．化工科技，1999，7(4)：15～18
[43]Ruiz C A．A Generalized Model Applied to Multieomponent Batch Distillation．Presented at the CHEMDATA 88 Conference．Gothenburg，Sweden，1988
[44]Diwekar U M．and Madhavan K P．MulticomponentBatch Distillation ColumnDesign．Ind．Eng．Chem．Res．1991．30：713