Optimal programming of ideal and extractive batch distillation: single vessel operations

This work addresses the problem of optimal programming of multi-component batch distillation columns with a single vessel (batch rectifier, batch stripper, middle vessel and extractive middle vessel) so as to maximize an annualized profit function. A smooth price function is formulated for product valuation, allowing to release traditional purity constraints. The solution is the optimal batch policy of top/bottom withdrawals. A simplified cascade model is developed for separation calculations, offering several operational patterns. Ideal and non-ideal mixtures can be handled with this model that is proposed as a substitute for traditionally used Fenske–Underwood–Gilliland cascades. Batch separations of ideal quaternary feeds are optimally programmed for the first three operations aforementioned. The extractive middle vessel column was optimally programmed for production of anhydrous ethanol from hydrated, nearly azeotropic, alcohol with ethylene–glycol as entrainer. All applications considered fixed number of stages, heat duty, and, in the extractive system, fixed pump-around rate of entrainer.     

带有中间储罐的塔用于间歇萃取精馏

Batch extractive distillation was studied in a column with a middle vessel. The process was simulated by a constant holdup model and solved by two point implicit method. Acetone and methanol mixture was separated in such a setup using water as solvent. The simulation agrees well with experimental results. The experimental and simulation results show that the solvent at the bottom and the product at the top of the column can be withdrawn simultaneously for a long period of time. It needs more time for the solvent to reach high purity than that required for the more volatile component to reach high purity, so that the time to withdraw solvent from the bottom is delayed.     

带中间贮槽的间歇精馏塔的模拟计算

带中间贮槽的间歇精馏塔由２个分离段及其中间的贮槽组成。假定液体持液量和待分离的体系的相对挥发度均保持不变,建立了该塔的一个简化的模型,由此得到各组分在整个塔中的分布情况。在此基础上,又考察了各个操作参数对分离效果的影响。     

Batch‐Rektifikation azeotroper Gemische in Verstärkungs‐ und Abtriebskolonnen

Batch distillation is an efficient unit operation which allows the separation of a multicomponent mixture into its pure constituents in a single column. However, the separation of azeotropic mixtures by distillation is quite difficult because at the azeotrope the liquid and the gas have the same composition and, in turn, the driving force for distillation disappears. A systematic presentation of batch distillation processes for the separation of binary azeotropic mixtures using an entrainer is given.     

Batch Extractive Distillation in a Column with a Middle Vessel

Batch extractive distillation was studied in a column with a middle vessel. The process was simulated by a constant holdup model and solved by two point implicit method. Acetone and methanol mixture was separated in such a setup using water as solvent. The simulation agrees well with experimental results. The experimental and simulation results show that the solvent at the bottom and the product at the top of the column can be withdrawn simultaneously for a long period of time. It needs more time for the solvent to reach high purity than that required for the more volatile component to reach high purity, so that the time to withdraw solvent from the bottom is delayed.     

拟稳态模型用于间歇萃取精馏的数值模拟

Batch extractive distillation (BED) is a special method used in the distillation process by adding a solvent into the batch distillation column to alter the relative volatility of the components and improve the separation. A comprehensive design and simulation method is required due to the complexity of BED. In this study, a quasi-steady-state model for BED is proposed, the derivation and solution of the model are presented. This shortcut model can be used to simulate the composition and temperature of the reboiler, the top and other plates of the column in a batch extractive distillation operation. The calculated values are in good agreement with the experi-mental data. The results show that the quasi-steady-state model is a practical method because of some advantages such as high precision and fast calculation.     

反置式间歇蒸馏塔的设计程序(Ⅰ)多组分理想物系

Inverted batch distillation column(stripper) is opposed to a conventional batch distillation column(rectifier). It has a storage vessel at the top and products leave the column at the bottom. The batch stripper is favourable to separate mixtures with a small amount of light components by removing the heavy components as bottom products. In this paper, we are presenting a shortcut procedure based on our earlier work for design and simulation of the inverted batch distillation column, which is equivalent to the Fenske-Underwood-Gilliland procedure for continuous distillation. Given a separation task, we propose to compute the minimum number of stages(Nbmin) and the minimum reboil ratio(Rbmin) required in a batch stripper,which are the stages and reboil ratio required in a hypothetical inverted batch distillation column operating in total reboil ratio or having an infinite number of stages,respectively. Then, it is shown that the performance of inverted batch columns with a finite number of stages and reboil ratios could be correlated in Gilliland coordinates with the minimum stages Nbmln and the minimum reboil ratio Rbmin.     

间歇萃取精馏操作过程的实验研究

采用复合式精馏塔实现了萃取精馏的间歇操作,塔顶产品物质的量分数达95%以上。以取得合格产品的量与时间之比作为目标函数,研究了回流比R、中间回流量Vm(中间罐向提馏段进料流量)、萃取剂用量S对萃取精馏过程的影响,在R=5～10,Vm=3.2～7.2mL/min,S=1.2～2.2mL/min范围内,随以上操作参数的增大,目标函数均呈先增大后减小的趋势。     

Shortcut Procedure for Inverted Batch Distillation Column (Ⅰ) Multicomponent Ideal System

Inverted batch distillation colunm(stripper) is opposed to a conventional batch distillation column(rectifier). It has a storage vessel at the top and products leave the column at the bottom. The batch stripper is favourable to separate mixtures with a small amount of light components by removing the heavy components as bottom products. In this paper, we are presenting a shortcut procedure based on our earlier work for design and simulation of the inverted batch distillation column, which is equivalent to the Fenske-Underwood-Gilliland procedure for continuous distillation. Given a separation task, we propose to compute the minimum number of stages(Nbmin)and the minimum reboil ratio(Rbmin) required in a batch stripper,which are the stages and reboil ratio required in a hypothetical inverted batch distillation colnmn operating in total reboil ratio or having an infinite number of stages,respectively. Then, it is shown that the performance of inverted batch columns with a finite number of stages and reboil ratios could be correlated in Gilliland coordinates with the minimum stages Nbmin and the minimum reboil ratio Rbmin.     

Feasibility of new pressure swing batch distillation methods

The pressure swing distillation in different batch column configurations is investigated by feasibility study and rigorous simulation calculations. Besides studying the well known batch configurations (rectifier, stripper, middle vessel column) we also suggest two novel configurations such as double column batch rectifier (DCBR) and double column batch stripper (DCBS). The alternate application of a batch rectifier and a batch stripper is also studied. The feasibility method is based on the assumption of maximal separation. The results of the feasibility studies are verified by rigorous simulations based on less simplifying assumptions. The calculations are made by a professional dynamic flow-sheet simulator for the separation of a minimum (ethanol–toluene) and a maximum boiling (water–ethylene-diamine) azeotropic mixture. The different column configurations are compared. The DCBS (for the separation of the minimum azeotrope) and the DCBR (for the maximum azeotrope) showed several advantages (e.g. only one production step without pressure change, lower energy consumption) compared with the other configurations.     

Membrangestützte Flüssig/Flüssig‐Extraktion – Wo stehen wir heute?

Thanks to advancements in materials science and manufacturing technology, membranes are now available for stable liquid‐liquid extraction processes. Rigorous calculation models can be used to calculate the membrane areas required for a given separation task as well as to optimize the module design. In rapid tests, the basic suitability and kinetic parameters can be determined. Thus, the general requirements are for utilizing the specific advantages of this separation technology in technical applications are fullfilled.     

Operation and control of batch extractive distillation for the separation of mixtures with minimum-boiling azeotrope

Batch distillation is commonly used in the fine chemicals, specialty polymer, biochemical, pharmaceutical, and food industries. For separating mixtures with minimum-boiling azeotrope, a heavy entrainer is frequently added to the top section of the batch column to aid in the separation. This process is called batch extractive distillation. Most of the papers in open literature have only studied the first operating step of the batch extractive distillation which is the recovery of the light component without mentioning the later steps for the recovery of the other component and entrainer. In this paper, two real chemical systems, one separating acetone and methanol using water as entrainer and the other separating isopropyl alcohol (IPA) and water using dimethyl sulfoxide (DMSO) as entrainer, are studied for the feasible operation of the complete batch distillation sequence. The operating variables, including the pre-load amount with the mixture, continuous feed rate of the entrainer, and reflux ratio at each operating step are determined in the operating sequence. The constant reflux ratio and constant entrainer feed rate operating policy and another policy to allow these two operating variables to be varied will be compared in order to further improve the batch operation. All dynamic simulations that are performed directly mimic industrial situations from an empty column using a rigorous dynamic simulator, Aspen Dynamics™.     

A generic feasibility study of batch reactive distillation in hybrid configurations

A new graphical feasibility method is developed to investigate batch reactive distillation processes in middle vessel column. The suggested methodology can deal with fully reactive, nonreactive, and complex column configuration. A new formulation is suggested to describe the composition profiles in the reactive sections. Its application has made possible to develop a generic feasibility methodology containing the same model equations independently of the presence or absence of reaction. By combining the reactive and nonreactive models, not only the fully reactive and fully nonreactive but also hybrid configurations can be studied. Feasibility criteria related to the hybrid configurations are also presented. Application of the new methodology is demonstrated on the production of ethyl acetate in batch reactive distillation. Five configurations are found feasible; pure EtOAc is produced as distillate, and pure H₂O is produced at the bottom. In each case, continuous feeding of AcOH is necessary. © 2009 American Institute of Chemical Engineers AIChE J, 2009     

间歇共沸精馏分离乙醇一水体系的改进研究

间歇共沸精馏是分离共沸物的一种方法,适用于化工、制药、溶剂回收、天然产物提取等产量小、品种多的行业,因此间歇共沸精馏近年来已成为非常活跃的研究和开发热点.对已有的常规间歇共沸精馏的操作方式作了改进,即共沸剂改为在塔釜回流,以正己烷为共沸剂,对分离乙醇-水共沸体系进行了改进研究,并与常规间歇共沸精馏的实验结果进行比较.结...     

Verhalten gedehnter Flüssigkeitsfäden in viskosen Flüssig/Flüssig‐ Systemen

The stability of jets in elongational flow is exploited to receive thin threads before break up. Fine drops can be generated in suitable geometries with comparable large cross flow areas. The examination deals with the stability of liquid threads simultaneously extended with the continuous phase in convergent flow. Break up limits and regimes are discussed.     

基于样条插值模型的间歇精馏模拟与预测控制

以Aspen Batch Distillation（ABD）中的间歇精馏仿真系统为过程原型,提出了利用过程的模拟测试数据来建立间歇精馏过程的样条插值简化模型（spline interpolation model, SIM）。结合变回流比下的动态修正函数,构造出了一种简单实用的动态模型。该模型可有效模拟不同组分浓度下回流比发生变化时馏出液浓度和流量的动态变化情况。以该模型作为预测模型,进一步提出了一种变回流比的预测控制（model predictive control, MPC）算法来使馏出液浓度按照期望的设定值变化。控制仿真结果表明该控制方案计算简单,同时具有较好的控制效果。     

间歇精馏模拟及操作方式的研究进展

综述了间歇精馏模拟研究常用的数学模型,主要介绍了严格模型和简捷模型,简要讨论了各个模型的特点.较详细地介绍了国内外间歇精馏操作方式的研究进展,讨论了动态累积间歇精馏塔、反向间歇精馏塔、中间罐间歇精馏塔、多罐间歇精馏塔等新塔型的操作.     

间歇萃取精馏技术的研究进展

对间歇萃取精馏分离技术和进展进行了评述,主要从萃取精馏的溶剂选择与设计、模拟及优化、操作参数对分离过程影响及萃取精馏塔设备等几个方面,介绍了国内外关于间歇萃取精馏新兴分离技术的最新研究动态,最后指出了萃取精馏技术目前存在的问题和今后发展的方向。     

Online‐Analytik zur Prozessführung

Online Analyzers for the Process Control Save, efficient, and economical operation of chemical processes more and more relies on online analyzers. The use of component properties (e.g., concentrations) for control becomes even more common. The combination of online analyzers and advanced control technologies holds an enormous economic potential, though a rocky path is leading there. As a result the number of existing applications is only growing slowly, but steadily. The main part of this contribution shows the potential of the combination of advanced control technologies and online analyzers using some illustrative examples like a batch distillation column, a continuous isomer distillation unit and the automation of a complete fine chemicals unit. Based on the experiences and problems encountered in the past projects, some guidelines and requests are formulated to optimize the definition and implementation of these projects in an interdisciplinary team and the integration of the online analyzers in a distributed control system.     

间歇精馏技术及其模拟优化研究进展

间歇精馏技术是一种重要的化工分离手段。文章综述了国内外间歇精馏技术及其常用的数学模型，其中主要阐述了严格模型和简捷模型，简要讨论了降价模型、半严格模型，同时探讨了间歇精馏优化的发展及其应用，并展望了间歇精馏系统的发展趋势。