Process design and control optimization: A simultaneous approach by multi‐parametric programming

We present a framework for the application of design and control optimization via multi‐parametric programming through four case studies. We develop design dependent multi‐parametric model predictive controllers that are able to provide the optimal control actions as functions of the system state and the design of the process at hand, via our recently introduced PAROC framework (Pistikopoulos et al, Chem Eng Sci. 2015;136:115–138). The process and the design dependent explicit controllers undergo a mixed integer dynamic optimization (MIDO) step for the determination of the optimal design. The result of the MIDO is the optimal design of the process under optimal operation. We demonstrate the framework through case studies of a tank, a continuously stirred tank reactor, a binary distillation column and a residential cogeneration unit. © 2017 American Institute of Chemical Engineers AIChE J, 2017     

Optimization‐based support for process design under uncertainty: A case study

The use of two‐stage stochastic optimization for the support of the solution of process design problems in the early phase of process development where the different potential elements of the production process can only be described with significant uncertainty is discussed. The first stage variables are the design decisions which are fixed after the process has been built, while the second stage variables are the operational parameters which can be adapted to the realization of the uncertainties. The application of the approach to the design of a hydroformylation process in a thermomorphic solvent system is demonstrated. The proposed designs which are computed using the software framework FSOpt are analyzed and compared using different graphic representations which provide insight into what the most important design decisions are. Finally, the experience with the proposed formulation and solution techniques and point out where further advances are needed is reviewed. © 2016 American Institute of Chemical Engineers AIChE J, 62: 3404–3419, 2016     

Design and Control of Ionic Liquid‐Catalyzed Reactive Distillation for n‐Butyl Acetate Production

A simulation study of n‐butyl acetate production with the [Hpy][HSO₄] ionic liquid catalyst was performed. Due to the lack of phase equilibrium data, the binary interaction parameters of the NRTL model for ionic liquid and reactive species were calculated by the COSMO‐RS technique. A reactive distillation process with recycled ionic liquid stream was proposed, and the column configuration was optimized by minimization of the total annual capital. The novel process is considerably efficient and economic compared to the traditional reactive distillation process of nonionic liquids. With the steady‐state parameters, a plant‐wide control structure was further developed to evaluate the robustness of the control system by exerting the disturbances of feed flow rate and feed composition. Dynamic simulation results suggest that the control scheme with a composition controller is timely and effective.     

Conceptual design of distillation processes for mixtures with distillation boundaries. II. Optimization of recycle policies

Geometric design methods for the conceptual design of azeotropic distillation processes are fast and efficient tools for the economic screening of different process alternatives. The second article of this two‐part series presents a novel optimization‐based conceptual design framework for azeotropic distillation processes, which allows a rapid screening of the different process alternatives with respect to feasibility and economic incentive. The design framework is based on the economic assessment of distillation columns by the rectification body method. The feasibility limits imposed by the azeotropes are incorporated using the split feasibility test introduced in the first part of this series. The application of the framework is highlighted with several ternary and quaternary process alternatives for the production of high‐purity alcohols. © 2010 American Institute of Chemical Engineers AIChE J, 2011     

A concept of reactive compatibilizer‐tracer for studying reactive polymer blending processes

A concept called reactive compatibilizer‐tracer is proposed. The latter bears reactive groups capable of reacting with its counterpart on forming a copolymer for in situ compatibilization, and fluorescent labels allowing determining very small amounts of the in situ formed compatibilizer and formation of micelles when it occurs. Owing to this concept, it is shown that a reactive compatibilizer may be very efficient at the beginning of a reactive blending process and may suddenly become completely inefficient, resulting in an abrupt and drastic increase in size of the dispersed phase domains. © 2015 American Institute of Chemical Engineers AIChE J, 62: 359–366, 2016     

Cyclic distillation technology – a mini‐review

Process intensification in distillation systems has received much attention during past decades, with the aim of increasing both energy and separation efficiency. Various techniques, such as internal heat‐integrated distillation, membrane distillation, rotating packed bed, dividing‐wall columns and reactive distillation were studied and reported in the literature. All these techniques employ the conventional continuous counter‐current contact of vapor and liquid phases. Cyclic distillation technology is based on an alternative operating mode using separate phase movement which leads to key practical advantages in both chemical and biochemical processes. This article provides a mini‐review of cyclic distillation technology. The topics covered include the working principle, design and control methods, main benefits and limitations as well as current industrial applications. Cyclic distillation can be rather easily implemented in existing columns by simply changing the internals and the operating mode, thus bringing new life to old distillation towers by significantly increasing the column throughput, reducing the energy requirements and offering better separation performance. © 2016 Society of Chemical Industry     

控制与工艺集成优化设计研究进展

控制与工艺集成优化设计是一种系统化的过程优化设计方法。以典型二元精馏塔设计为例阐述了其过程系统的数学描述，给出其最优工艺设计和控制设计的求解框架和求解策略，以及其中混合整数动态优化问题(MIDO)的求解方法。通过与传统的工艺与控制分步序贯设计比较，讨论了二者各自的优势和不足，指出控制与工艺集成优化设计具有良好的发展前景。     

Dynamic process intensification of binary distillation based on output multiplicity

Process intensification focuses largely on process and equipment design. Much less emphasis has been placed on operational changes to achieve cost savings and increased efficiency. This article introduces the concept of dynamic intensification, defined as changes to the dynamics, operating strategy and/or control of a process that lead to a substantially more efficient processing path. This idea is illustrated in the context of binary distillation. Output multiplicity properties are exploited to establish a new periodic operating mode based on switching between two auxiliary products, which, on a time-average basis, is more energy efficient than steady-state operation. An extensive case study is presented concerning the distillation of a propanol–acetic acid mixture, confirming the theoretical developments. In contrast to previous research (e.g., on cyclic distillation), the present concept has significant advantages as it relies on existing hardware and exploiting system nonlinearity, rather than using specialized equipment operated in a discontinuous fashion. © 2018 American Institute of Chemical Engineers AIChE J, 65: 1162–1172, 2019     

Enhancing mass and energy integration by external recycle in reactive distillation columns

The synthesis and design of reactive distillation columns separating reacting mixtures with the most unfavorable relative volatilities (i.e., the reactants are the heaviest and lightest components with the products being the intermediate ones) are described. The unfavorable thermodynamics poses great difficulties in combining the reaction operation and the separation operation involved and limits severely the potential of reactive distillation columns in the reduction of capital investment (CI) and operating cost. To remove the limitation, we propose two strategies for facilitating the synthesis and design of this kind of reactive distillation columns in this article. One is to arrange prudentially the reactive section so as to strengthen internal energy integration between the reaction operation and the separation operation involved; that is, while the reactive section should be placed at the bottom of the reactive distillation columns separating exothermic reactions, it should be at the top of the reactive distillation columns separating endothermic reactions. The other is to introduce an external recycle flow between the two ends of the reactive distillation columns to reinforce internal mass integration and internal energy integration between the reaction operation and the separation operation involved; that is, whereas the external recycle flow should be directed from the top to bottom of the reactive distillation columns separating exothermic reactions, it should be from the bottom to top of the reactive distillation columns separating endothermic reactions. Separation of four hypothetical ideal (i.e., two quaternary and two ternary systems, respectively) and two real nonideal (i.e., two quaternary systems) reacting mixtures is chosen to evaluate the proposed strategies. The results show that they can considerably lower energy requirement besides a further reduction in CI. © 2012 American Institute of Chemical Engineers AIChE J, 59: 2015–2032, 2013     

Enzymatic catalyzed reactive dividing wall column: Experiments and model validation

A novel process for the integration of chemical reaction and product separation is proposed: the enzymatic catalyzed reactive dividing wall column (eRDWC). The eRDWC combines the highly integrated and complex reactive dividing wall column (RDWC) with the use of a very selective enzymatic catalyst. This apparatus enables the simultaneous production and separation of up to 4 pure product streams. Comprehensive experiments with the reference system of a hexanol and butyl acetate transesterification in a DN 65 pilot scale column show the feasibility of stable steady state operations for this process. A rigorous model for the plant design of an eRDWC wall column is developed. The reaction kinetics and vapor‐liquid‐equilibria for the reference system are measured and implemented in the model. The model is successfully validated using the acquired experimental data. The application of enzymes in continuous reactive distillation processes has the potential to increase the selectivity at milder process conditions. © 2016 American Institute of Chemical Engineers AIChE J, 63: 2198–2211, 2017     

Advanced control strategies for the multicolumn countercurrent solvent gradient purification process

The multicolumn countercurrent solvent gradient purification process (MCSGP) is a semicontinuous, chromatographic separation process used in the production of monoclonal antibodies) . The process is characterized by high model complexity and periodicity that challenge the development of control strategies, necessary for feasible and efficient operation and essential toward continuous production. A novel approach for the development of control policies for the MCSGP process, which enables efficient continuous process control is presented. Based on a high fidelity model, the recently presented PAROC framework and software platform that allows seamless design and in‐silico validation of advanced controllers for complex systems are followed. The controller presented in this work is successfully tested against disturbances and is shown to efficiently capture the process periodic nature. © 2016 American Institute of Chemical Engineers AIChE J, 62: 2341–2357, 2016     

Design and optimization of reactive distillation: a review

Reactive distillation process, a representative process intensification technology, has been widely applied in the chemical industry. However, due to the strong interaction between reaction and separation, the extension of reactive distillation technology is restricted by the difficulties in process analysis and design. To overcome this problem, the design and optimization of reactive distillation have been widely studied and illustrated for plenty of reactive mixtures over the past three decades. These design and optimization methods of the reactive distillation process are classified into three categories: graphical, optimization-based, and evolutionary/heuristic methods. The primary objective of this article is to provide an up-to-date review of the existing design and optimization methods. Desired and output information, advantages and limitations of each method are stated, the modification and development for original methodologies are also reviewed. Perspectives on future research on the design and optimization of reactive distillation method are proposed for further research.     

反应精馏过程耦合强化技术基础与应用研究述评

反应精馏技术是过程强化概念在化学工业成功应用的典范。由于反应与精馏耦合的高度复杂性和非线性,反应-精馏相互影响机制、耦合方式及其过程能效调控与优化成为制约该技术广泛应用的关键科学问题。综述了近二十年来国内外反应精馏技术从基础研究到工业应用的概况,包括反应精馏过程的可行性分析与概念设计方法、稳态模拟过程优化与动态模拟控制策略设计、兼具催化反应与气液传质的高效内构件开发以及反应精馏在各领域的应用。探讨了目前制约反应精馏广泛应用关键问题的解决方法与途径,阐明了普适性的反应精馏过程开发方法,总结了基于反应精馏过程耦合的新型过程强化技术,指出了反应精馏技术的发展趋势。     

Control‐relevant decomposition of process networks via optimization‐based hierarchical clustering

A systematic method is proposed for control‐relevant decomposition of complex process networks. Specifically, hierarchical clustering methods are adopted to identify constituent subnetworks such that the components of each subnetwork are strongly interacting while different subnetworks are loosely coupled. Optimal clustering is determined through the solution of integer optimization problems. The concept of relative degree is used to measure distance between subnetworks and compactness of subnetworks. The application of the proposed method is illustrated using an example process network. © 2016 American Institute of Chemical Engineers AIChE J, 62: 3177–3188, 2016     

A generalized method for the synthesis and design of reactive distillation columns

Owing to the combination between the reaction operation and the separation operation involved, it is extremely difficult to determine in advance the optimum configuration of a reactive distillation column and this makes process synthesis and design a great challenging task. Currently, no easy-to-use and yet effective methods are available to guide process synthesis and design, restricting considerably the applications and therefore the impacts of reactive distillation columns to the chemical process industry. In this paper, a generalized method is proposed for the synthesis and design of reactive distillation columns in terms of the insights from process intensification. The method is initiated from a simple process design with all feeds of reactants at the middle of the process and all stages as reactive ones. In terms of an economical objective function, it can be evolved into the optimum process design via sequential structure adjustments, including reactive section arrangement, feed stage relocation, feed splitting, and catalyst redistribution. The generalized method proposed is characterized by great simplicity in principle, the capability to tap the full potentials of process intensification, and the high robustness to the initial guess of process configuration as well as the thermodynamic properties of the reacting mixtures separated. Four example systems are employed to evaluate the generalized method proposed and the obtained outcomes demonstrate its effectiveness and applicability to the synthesis and design of various reactive distillation columns.     

Conceptual design of distillation processes for mixtures with distillation boundaries: I. Computational assessment of split feasibility

Geometric design methods for the conceptual design of azeotropic distillation processes are fast and efficient tools for the economic screening of different process alternatives. This two‐part series presents a fully automated conceptual design method for finding an optimal recycle policy for the separation of mixtures with distillation boundaries. It does not require visualization and graphical inspection of residue curve or pinch maps and is, hence, not limited to ternary mixtures. The first part introduces a fully computational geometric split feasibility test based on bifurcation analysis. This bifurcation‐based feasibility test can be used as a valuable stand‐alone tool for the assessment of different separation options. It is also one of the core elements of the recycle optimization discussed in the second part of this series. © 2010 American Institute of Chemical Engineers AIChE J, 2011     

A superstructure representation,generation, and modeling framework for chemical process synthesis

We present a framework for the efficient representation, generation, and modeling of superstructures for process synthesis. First, we develop a new representation based on three basic elements: units, ports, and conditioning streams. Second, we present four rules based on “minimal” and “feasible” component sets for the generation of simple superstructures containing all feasible embedded processes. Third, in terms of modeling, we develop a modular approach, and formulate models for each basic element. We also present a canonical form of element models using input/output variables and constrained/free variables. The proposed methods provide a coherent framework for superstructure‐based process synthesis, allowing efficient model generation and modification. © 2016 American Institute of Chemical Engineers AIChE J, 62: 3199–3214, 2016     

Design and Control Comparison of Alternative Separation Methods for n‐Heptane/Isobutanol

The binary mixture of n‐heptane and isobutanol forms an azeotrope at atmospheric pressure, with a composition of 66.9 mol % n‐heptane and a temperature of 364 K. Several methods of separation are possible. This study compares the steady‐state economics and the dynamic controllability of three alternative separation techniques: a two‐column extractive distillation process, a two‐column pressure‐swing distillation process, and a single column with a refrigerated condenser.     

Proactive fault‐tolerant model predictive control

Fault‐tolerant control methods have been extensively researched over the last 10 years in the context of chemical process control applications, and provide a natural framework for integrating process monitoring and control aspects in a way that not only fault detection and isolation but also control system reconfiguration is achieved in the event of a process or actuator fault. But almost all the efforts are focused on the reactive fault‐tolerant control. As another way for fault‐tolerant control, proactive fault‐tolerant control has been a popular topic in the communication systems and aerospace control systems communities for the last 10 years. At this point, no work has been done on proactive fault‐tolerant control within the context of chemical process control. Motivated by this, a proactive fault‐tolerant Lyapunov‐based model predictive controller (LMPC) that can effectively deal with an incipient control actuator fault is proposed. This approach to proactive fault‐tolerant control combines the unique stability and robustness properties of LMPC as well as explicitly accounting for incipient control actuator faults in the formulation of the MPC. Our theoretical results are applied to a chemical process example, and different scenaria were simulated to demonstrate that the proposed proactive fault‐tolerant model predictive control method can achieve practical stability and efficiently deal with a control actuator fault. © 2013 American Institute of Chemical Engineers AIChE J, 59: 2810–2820, 2013     

Horizontal reactive distillation for multicomponent chiral resolution

A novel horizontal reactive distillation apparatus and a new overall process scheme are proposed for continuous multicomponent chiral resolution via reversible enantioselective acylation of a chiral (racemic) substrate by a chiral (racemic) acyl donor. The process enables simultaneous production of up to four enantiomers with enhanced chiral purity. Kinetic studies, miniplant experiments, and process simulation results are described for a model lipase‐catalyzed reaction: (R)‐enantioselective transesterification of (R,S)‐1‐n‐butoxy‐2‐propanol with (R,S)‐1‐methoxy‐2‐acetoxypropane to produce (R)‐1‐n‐butoxy‐2‐acetoxypropane, (R)‐1‐methoxy‐2‐propanol, and the two unreacted (S)‐enantiomers of the (R,S)‐reagents. A horizontal, compartmentalized reactive distillation vessel is specified instead of a conventional reactive distillation column to provide longer liquid‐phase residence time needed for adequate conversion. Low vapor‐traffic pressure drop allows operation under vacuum at reduced temperatures for good enzyme stability and enantioselectivity. The general technology has potential as a means to producing a wide range of chiral synthons used in asymmetric syntheses of chiral pharmaceuticals and other biologically active products. © 2013 American Institute of Chemical Engineers AIChE J, 59: 2603–2620, 2013