Optimal design,dynamics and control of a reactive DWC for biodiesel production

Reactive separation technologies were proposed recently for fatty acid methyl esters (FAME) production, providing significant benefits such as minimal capital and operating cost savings. One approach is to use a reactive dividing-wall column (R-DWC) for the biodiesel production process. However, since the R-DWC is designed for a quaternary reactive system – two reactants (one in excess) and two products – more difficulties concerning the process control may be expected considering the high degree of integration of the process.     

Control analysis of an extractive dividing-wall column used for ethanol dehydration

This paper deals with design and control of an extractive dividing-wall distillation column (EDWC) for ethanol dehydration using ethylene glycol as entrainer. An initial design, based on a section analogy procedure for a conventional extractive distillation sequence, was obtained and then used in an optimization process to minimize the total annual cost. It was shown that the EDWC can result in significant savings over the conventional process. As these savings sometimes go along with a decrease in the control properties, an investigation of two control structures for the EDWC and one for the conventional column configuration was performed next.It was observed in closed-loop simulations that the EDWC with an appropriate structure exhibited good control properties and that its closed-loop responses were similar to those obtained for the operation of a conventional extractive distillation system.     

A disjunctive programming approach for the optimal design of reactive distillation columns

A generalized disjunctive programming formulation is presented for the optimal design of reactive distillation columns using tray-by-tray, phase equilibrium and kinetic based models. The proposed formulation uses disjunctions for conditional trays to apply the MESH and reaction kinetics equations for only the selected trays in order to reduce the size of the nonlinear programming subproblems. Solution of the model yields the optimal feed tray locations, number of trays, reaction zones, and operating and design parameters. The disjunctive program is solved using a logic-based outer-approximation algorithm where the MILP master problem is based on the big-M formulation of disjunctions, and where a special initialization scheme is used to reduce the number of initial NLP subproblems that need to be solved. Two examples are presented that include reactive distillation for the metathesis reaction of 2-pentene and for the production of ethylene glycol. The results show that the proposed method can effectively handle these difficult nonlinear optimization problems.     

Design and control of acetic acid dehydration system via heterogeneous azeotropic distillation

Acetic acid dehydration is an important operation in the production of aromatic acid, such as terephthalic acid or in the manufacture of cellulose acetate. Although acetic acid and water does not form azeotrope, but using simple distillation to separate these two components is not practical. The reason is because the system has tangent pinch on the pure water end, thus it is more customary in industry to use an entrainer via a heterogeneous azeotropic distillation column system for the separation. In this study, a suitable entrainer is selected from three candidate acetates through rigorous steady-state simulation of this system. Optimum process design and operating condition are determined to keep high-purity bottom acetic acid composition and also keep a small acetic acid loss through top aqueous draw. Furthermore, the overall control strategy of this column system is proposed to hold both bottom and top product specifications in spite of feed rate and feed composition load disturbances. The proposed overall control strategy is very simple requiring only one tray temperature control loop inside the heterogeneous azeotropic column.     

Vapor recompressed dividing-wall distillation columns: Structure and performance

Due to the topological structure of double columns and multiple separating sections in dividing-wall distillation columns (DWDCs), the development of vapor recompressed dividing-wall distillation columns (DWDC-VRHPs) represents a challenging issue with great complexities and tediousness. For the separations of light-component dominated and wide boiling-point ternary mixtures, because the purification of the light-component from the intermediate-and heavy-components incurs the primary energy dissipation, the application of vapor recompressed heat pumps (VRHP) should be aimed to reduce the irreversibility and this leads to the generation of the optimum topological structures of the DWDC-VRHPs, i.e., a DWDC plus a two-stage VRHP. The first-stage VRHP is to preheat feed, not only taking the advantages of the small temperature elevation available but also favoring the mass transfer between the vapor and liquid phases through feed splitting. The second-stage VRHP is to reduce further separation irreversibility. The philosophy can be applied to any DWDCs no matter where the dividing wall locates. Two case studies on the separations of ternary mixtures of benzene, toluene, and o-xylene and n-pentane, n-hexane, and n-heptane demonstrate the economic optimality of the proposed DWDC-VRHPs and reveal the inherent interplay between internal and external process integration.     

Investigating the need of a pre-concentrator column for acetic acid dehydration system via heterogeneous azeotropic distillation

In our previous study [Chien, I.L., Zeng, K.L., Chao, H.Y., Liu, J.H. (2004). Design and control of acetic acid dehydration system via heterogeneous azeotropic distillation. Chemical Engineering Science 59(21), 4547-4567.], an acetic acid dehydration system has been designed. The suitable entrainer selected for that system is iso-butyl acetate. Design and control of the system has been studied in detail to maintain high-purity bottom acetic acid concentration and also keep a small acetic acid loss through top aqueous draw. In that previous study, the feed composition is assumed to contain equal molar of acetic acid and water. However, in a typical waste acid recovery application, the above assumption may be too rich in acetic acid. In this paper, a feed stream containing 80 mol% water and 20 mol% of acetic acid is investigated. Several design alternatives can be deduced including one commonly used in industry by adding a pre-concentrator column in the upstream of a heterogeneous azeotropic distillation column. The necessity of this pre-concentrator column from design and control view points will be thoroughly investigated in this paper. The final recommended process design is a tradeoff between total annual cost (TAC) and operability of the system. The recommended design is a single heterogeneous azeotropic distillation column with aqueous reflux stream. Very wide feed composition and flow rate changes can be handled by this design with proper choice of the overall control strategy.     

Synthesis of dividing-wall columns (DWC) for multicomponent distillations—A systematic approach

Dividing-wall columns (DWC) are intensified distillation systems for multicomponent separations. They have the potential to save significantly both energy and capital costs than conventional simple column configurations. In this paper, it is shown that the DWC columns can be systematically generated from the conventional simple column configurations. Because of the simple column sequences with sharp splits are the simple and widely studied conventional schemes for multicomponent distillation, the purpose of this work is to formulate a procedure for systematic synthesis of DWC columns for such simple conventional schemes. A four-step procedure is formulated which systematically generates all the possible DWC columns from the simple column sequences. First, the subspace of the original thermally coupled configurations corresponding to the simple column configurations is generated. Then, the subspace of the thermodynamically equivalent structures corresponding to the original thermally coupled configurations is produced. Finally, the subspace of the DWC columns corresponding to the thermodynamically equivalent structures is achieved. An example of quaternary distillation is used to illustrate the synthesis procedure which is applicable to a mixture with any number of components.     

基于粒子群算法的隔离壁精馏塔的综合与设计

隔离壁精馏塔（dividing-wall distillation column,DWDC）是提高两个或者多个传统精馏塔热力学效率的有效手段。由于隔离壁精馏塔内部结构复杂、相互作用强,传统的序贯优化方法计算时间长,很难达到全局最优解。标准粒子群算法应用广泛、易于实现,但易于早熟、易于陷入局部极值点。因此,本工作采用改进的元胞粒子群算法对Kaibel隔离壁精馏塔进行综合与设计研究。元胞粒子群算法通过改进粒子的学习策略,采用元胞邻域的方法可有效地将粒子分散在多个子空间。对比标准粒子群优化和元胞粒子群优化两种方法的50次优化效果,结果表明,两种粒子群算法能够对内部结构复杂、相互作用强的四组分Kaibel隔离壁精馏塔这一复杂分离系统进行优化,优化效果显著。     

Design of entrainer-enhanced reactive distillation for the synthesis of butyl cellosolve acetate

An innovative entrainer-enhanced reactive distillation (RD) process is presented, which aims to the production of high-purity butyl cellosolve acetate from butyl cellosolve and acetic acid via an esterification reaction. This entrainer-enhanced RD process can procure technical advantages from both heterogeneous azeotropic distillation and RD. Solvents such as cyclohexane, ethylene dichloride, toluene, and octane are considered as candidates in this esterification RD process. The function of entrainers is to simplify the separation between water and acetic acid. For this purpose, the proper entrainer to use is thus evaluated based on its mutual solubility with water in two liquid phases. Simulation results reveal that total annual cost can be substantially reduced when cyclohexane, toluene, and octane are used as entrainers in the RD column. The octane-enhanced RD provides the most economical design in this studied case.     

Modeling and in-depth analysis of the start-up of dividing-wall columns

Saving potentials of up to 30% in capital and operating costs are the driving forces behind the increase in the application of dividing-wall columns in industry. However, a lack of knowledge still exists when dealing with the start-up of dividing-wall columns, which is inherently a strongly nonlinear process. Here, for the first time the start-up of dividing-wall columns is explored, where the starting point is an empty column at ambient conditions. A model is presented which is capable of predicting the dynamic discrete-continuous changes which are characteristic of dividing-wall columns. The proposed process model takes into account the heat transfer across the dividing wall as well as the vapor distribution below the dividing wall. The degree of accuracy of the model is clearly determined by comparing different simplifications, e.g. a constant vapor distribution ratio equal to the steady-state value. The detailed studies were carried out with strict product specifications so that the influence of process parameters could be quantified. The rigorous process model and the obtained simulation results presented in this study provide a promising basis for developing and applying optimal start-up policies for dividing-wall columns.     

工业醋酸脱水过程五元体系非均相共沸精馏的流程模拟

针对以醋酸正丙酯为共沸剂的醋酸脱水过程,考虑醋酸溶剂中未反应的前体对二甲苯以及反应的副产物醋酸甲酯的影响及回收利用,分别选用HOC和UNIQUAC模型来修正体系中五元混合物系的汽液非理想性,通过拟合醋酸甲酯-对二甲苯和醋酸正丙酯-对二甲苯两体系的二元汽液平衡实验数据获得了该两组体系UNIQUAC模型的二元交互作用参数,借助模拟软件Aspen Plus,结合软件内置其他二元体系参数,对工业醋酸脱水塔系包括溶剂脱水塔、PX回收塔、共沸剂回收塔在内的三塔体系进行系统的分析模拟,得到了与工艺数据误差小于±6%的能正确描述工业醋酸脱水塔系操作特性的工艺机理稳态模型,为工业醋酸脱水过程工艺的进一步研究提供理论基础和依据。     

Fatty acid esterification by reactive distillation. Part 1: equilibrium-based design

Esters of fatty acids are currently produced in batch processes. In this study we present an innovative process based on reactive distillation (RD). The synthesis of a several fatty esters is possible in the same RD set-up, making possible the development of a continuous multipurpose process. Conceptual design is presented as a systematic methodology based on thermodynamic analysis combined with computer simulation. This approach sets also targets for limited experimental work. The methodology is illustrated by the esterification of lauric acid with 2-ethylhexanol and methanol, the heaviest and lightest alcohol in the C₁-C₈ series. The first part presents the design of a RD set-up based on chemical equilibrium. Both reactions can be accommodated in the same hardware, but with different operation procedures. The alternative with alcohol reflux is suitable for heavy alcohols that form heterogeneous azeotropes with water. Another alternative with acid reflux can accommodate both light and heavy alcohols, and may be seen as a generic process for fatty acid esterification.     

隔离壁精馏塔水平传热设计与研究

通过将隔离壁精馏塔(DWC)的隔板两侧进行水平传热,可以进一步降低DWC的能量消耗。本文以假想的三组分混合物A,B,C为例,在三塔简捷计算初值的基础上,利用Mathematica对DWC进行最终的优化设计,并进行了主塔和副塔间水平传热的研究。结果表明,与未耦合的DWC对比,耦合DWC最大能够节能0.9%,且耦合塔板数与耦合面积能够影响DWC的节能效果。     

规整填料精馏塔的设计计算

通过大量的文献调研，比较了规整填料精馏塔和板式塔的优缺点，对规整填料精馏塔内压降、传质及液泛时压降的计算公式进行了比较，总结出设计计算规整填料精馏塔的步骤与方法，为规整填料精馏塔的应用提供了基础。     

Optimal design of extractive dividing-wall column using an efficient equation-oriented approach

The extractive dividing-wall column(EDWC)is one of the most efficient technologies for separation of azeotropic or close boiling-point mixtures,but its design is fairly challenging.In this paper we extend the hybrid feasible path optimisation algorithm(Ma Y,McLaughlan M,Zhang N,Li J.Computers&Chemical Engineering,2020,143:107058)for such optimal design.The tolerances-relaxation integration method is refined to allow for long enough integration time that can ensure the solution of the pseudo-transient continuation simulation close to the steady state before the required tolerance is used.To ensure the gradient and Jacobian information available for optimisation,we allow a relaxed tolerance for the simulation in the sensitivity analysis mode when the simulation diverges under small tolerance.In addition,valid lower bounds on purity of the recycled entrainer and the vapour flow rate in column sections are imposed to improve computational efficiency.The computational results demonstrate that the extended hybrid algorithm can achieve better design of the EDWC compared to those in literature.The energy consumption can be reduced by more than 20%compared with existing literature report.In addition,the optimal design of the heat pump assisted EDWC is achieved using the improved hybrid algorithm for the first time.     

Optimization-based design of reactive distillation columns using a memetic algorithm

The design optimization of reactive distillation columns (RDC) is characterized by complex nonlinear constraints, nonlinear cost functions, and the presence of many local optima. The standard approach is to use MINLP solvers that work on a superstructure formulation where structural decisions are represented by discrete variables and lead to an exponential increase in the computational effort. The mathematical programming (MP) methods which solve the continuous sub-problems provide only one local optimum which depends strongly on the initialization. In this contribution a memetic algorithm (MA) is introduced and applied to the global optimization of four different formulations of a computational demanding real-world design problem. An evolution strategy addresses the global optimization of the design decisions, while continuous sub-problems are efficiently solved by a robust MP solver. The MA is compared to MINLP techniques. It is the only algorithm that finds the global solution in reasonable times for all model formulations.     

轻组分绝对占优的蒸汽再压缩隔离壁蒸馏塔的最优拓扑结构

隔离壁蒸馏塔（DWC）的双塔多段拓扑结构导致蒸汽再压缩热泵（VRHP）的应用具有多种可能性,包括单VRHP、多VRHP、多级VRHP以及它们的相互组合等复杂结构,这显著加剧了蒸汽再压缩隔离壁蒸馏塔（DWC-VRHP）综合与设计的复杂性与烦琐性。为解决这一问题,针对轻组分绝对占优的三元宽沸点物系的分离问题推演了DWC-VRHP的最优拓扑结构,由此能够有效回避系统综合与设计过程中的结构搜索问题并显著降低模型化与搜索计算的工作强度。轻组分绝对占优与宽沸点物性导致了塔顶冷凝器与预分离蒸馏塔的提馏段是主要的热源与热阱,也决定了DWC-VRHP的最优拓扑结构,即一个二级VRHP与DWC的耦合系统。第一级VRHP用于进料预热,既充分利用温度提升跨度小的特点,又可以通过进料分流强化气液相间的物质传递。第二级VRHP用于加热预分离蒸馏塔的提馏段（或公共提馏段）,能够最大限度地降低分离操作的非可逆性。采用苯/甲苯/邻二甲苯和正戊烷/正己烷/正庚烷两个物系的分离问题对所提出的DWC-VRHP的最优拓扑结构进行了分析与验证。通过与DWC以及DWC-VRHP其他潜在结构的系统性比较,显示了所提出系统结构在稳态性能方面的优越性。     

Conceptual design of single-feed hybrid reactive distillation columns

It is well known that reactive distillation offers benefits by integrating distillation and reaction within a single unit. While there are procedures available for the synthesis of non-reactive distillation processes and of reaction-separation systems, the design of reactive distillation columns is still a challenge. This work presents a new synthesis and design methodology for hybrid reactive distillation columns, featuring both reactive and non-reactive sections; reactive equilibrium is assumed. The approach is based on graphical techniques; therefore it is restricted to systems with two degrees of freedom according to Gibbs phase rule. The design method allows rapid and relatively simple screening of different reactive distillation column configurations. The results are useful for initialising more rigorous calculations. The methodology is illustrated for MTBE and ethyl formate production.     

Optimal operation of Kaibel distillation columns

The objective of this paper is to study the Kaibel distillation column from an operability point of view. Two different objectives, namely minimizing energy requirement at fixed product purities and maximizing product purities with a fixed boilup are considered. We have visualized the objective functions for the two cases as a function of operational degrees of freedom and conclude that operation with fixed product purities is the more difficult case from control point of view.     

应用液滴停留时间模型优化萃取塔设计

很多因素影响着萃取塔的工作效率,其中最为重要的为塔内液滴的空间分布和停留时间。文中基于欧拉-拉格朗日二相流模型,利用CFD技术,模拟了塔内的液滴空间分布和停留时间,提出了萃取塔优化设计和操作的原则。结果显示:在满足萃取塔优化设计原则的基础上,通过优化萃取塔设计和操作参数如塔单元高度、叶片转速等,可以有效提高萃取塔的效率。提出的优化方法简单易行,适合实际设计工作。