Distillation pressure control troubleshooting—The hidden pittfalls of overdesign

The operating pressure of a distillation column is one of the main handles with which to control and optimise separation as it affects most other parameters as well as the overall stability of the column. It is therefore one of the most important parameters to control.Controlling a distillation column, designed to be operated under a vacuum, at the intended operating pressure can prove to be much more difficult than for positive pressure columns especially during the initial start-up of the column. Determining the cause of pressure instability can be a daunting task as the column will most likely be under turndown conditions, the inventory might differ from the intended composition, the control loops will be in manual or not tuned yet or the cause might even be from an equipment design perspective.During the initial start-up of a vacuum operated distillation column several problems were encountered that prohibited the column from being operated at its intended pressure. This caused severe instabilities in the column and also affected the downstream sections of the plant. This paper focuses on these problems and the troubleshooting to determine the causes of the pressure instability.During troubleshooting a number of key factors that contributed to the pressure instability were identified, with the main cause being the design and expected air ingress into the column. This influenced the design of several pieces of equipment in and around the column. A deviation from the design air ingress meant that several design parameters had to be re-evaluated in order to eventually reach the intended operating pressure.A conventional pressure control philosophy was implemented, but changes to this were required in order to achieve the necessary stability in the column. The improved control philosophy has several benefits, such as a reduced number of variables to be manipulated by the operator, smoother change over between the primary pressure controller and the setpoint high controller, as well as optimising the product losses to the vacuum system.     

“背包式”反应精馏集成过程研究进展

“背包式”反应精馏是一种反应器与精馏塔既相互独立又相互耦合的离散集成技术。由于反应与分离处于不同空间位置，能够突破传统反应精馏对工况的限制，拓宽应用范围，且便于工程放大。本文综述了国内外“背包式”反应精馏从基础到应用的研究概况。从转化率、选择性、塔内温度、组成分布等方面，分析了“背包式”反应精馏与传统反应精馏的等效性，指出“背包式”反应精馏的优势在于工况的灵活选择利于实现反应与分离能力的最佳匹配。介绍了“背包式”反应精馏在稳态模拟与优化、动态模拟及控制等方面的研究进展，并从不同工况反应与精馏集成技术的应用、便捷的催化剂装填与反应器设计应用两个角度归纳了该技术的应用进展。最后，从优化设计理论、先进控制方法、能量综合利用以及强化酶催化反应等方面对“背包式”反应精馏进一步的研究与应用进行展望。     

间歇提馏塔的操作

A stripping batch distillation column is preferred when the amount of the light component in the feed is small and the products are to be recovered at high purity. The operation modes of a batch stripping are believed to be the same as those of a rectifier. However, the control system of a stripper is different. In this paper, we explore three different control methods with Hysys (Hyprotech Ltd. 1997) for a batch stripper. The main difference is the control scheme for reboiler liquid level: (a) controlled by reflux flow; (b) controlled by reboiler heat duty; (c)controlled by bottom product flow. The main characteristics of operating a batch stripper with different control scheme are presented in this paper. Guidelines are provided for the startup of a batch stripper, the effects of some control tuning parameters on the column performance are discussed.     

Design and control of butyl acrylate reactive distillation column system

In this study, the design and control of a reactive distillation column system for the production of butyl acrylate has been investigated. The proposed design is quite simple including only one reactive distillation column and an overhead decanter. The optimal design is selected based on the minimization of total annual cost (TAC) for the overall system. At this optimized flowsheet condition, output multiplicity was found with reboiler duty or feed ratio as the bifurcation parameter. The highest purity stable steady state was selected as the base case condition for the control study. The overall control of this system can be achieved with no on-line composition measurements. Simple single-point tray temperature control loop is designed to infer final product purity. From results of dynamic simulation, the proposed control strategy performs very well in rejecting various disturbances while maintaining butyl acrylate product at high purity. One of the important finding in this paper is that it is better to operate this reactive distillation column not at the exact feed stoichiometric balance point for better operability reason. The control performances of the proposed operating point and the operating condition right at the exact stoichiometric balance point will be compared.     

Identification and Control of an Industrial Binary Distillation Column: A Case Study

The challenging problem of identification and control of an industrial binary distillation column is addressed in this paper. Process identification represents an alternative to modeling and is shown to be the appropriate procedure for predictive control design. The predictive controllers based on the identified model ensure stability and high performance for a wide operating range of the industrial distillation column.     

Operational optimization of crude oil distillation systems using artificial neural networks

A new methodology for optimizing heat-integrated crude oil distillation systems is proposed in this work. The new procedure considers an artificial neural networks (ANN) model for representing the distillation column. Models of the distillation column and the associated existing heat exchanger network are incorporated in an optimization framework to systematically determine the operating conditions that improve the overall process economics. Of particular interest is the problem of optimizing the net value of the products obtained from the column by increasing the yield of higher-value products at the expense of less valuable products, while taking into account feasibility of the distillation specifications, heat recovery, energy and equipment constraints. A two-stage procedure is applied to first optimize the column operating conditions based on minimum utility requirements. In the second stage the heat exchanger network is designed.     

Quantitative comparison of dynamic controllability between a reactive distillation column and a conventional multi-unit process

A comparison of the steady-state economic optimum designs of two alternative chemical processes was presented in a previous paper [Kaymak, D. B., & Luyben, W. L. (2004). A quantitative comparison of reactive distillation with conventional multi-unit reactor/column/recycle systems for different chemical equilibrium constants. Industrial & Engineering Chemistry Research, 43, 2493–2507]. A generic exothermic reversible reaction A + B ↔ C + D occurs in both flowsheets, which consist of a conventional multi-unit reactor/separator/recycle structure and a reactive distillation column. Results showed that the reactive distillation process is significantly less expensive than the conventional process for a wide range of the chemical equilibrium constant when there is no mismatch between the temperature favorable for reaction and the temperature favorable for vapor–liquid separation.

A reactive distillation column has fewer control degrees of freedom than a conventional multi-unit system. Therefore a reactive distillation column may have worse dynamic response than a conventional process. The purpose of this paper is to compare the dynamic controllability of these two alternative processes.

Three different chemical equilibrium constants are considered. Several control structures are developed for each flowsheet, and their effectiveness is evaluated. Disturbances in production rate and fresh feed compositions are considered.

The conventional multi-unit process provides significantly better control. The operability region is much larger, there is less variability in product quality and the dynamic responses are faster than those of the reactive column. Thus, these results demonstrate that there is a significant trade-off in this system between optimum economic steady-state design and dynamic controllability.     

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™.     

反应精馏隔壁塔生产乙酸正丁酯的优化与控制

对反应精馏隔壁塔生产乙酸正丁酯过程进行了模拟、优化与控制的系统研究。利用Aspen Plus软件模拟乙酸甲酯与正丁醇的酯交换反应过程,以年总费用（TAC）为目标函数进行过程优化,通过稳态敏感性分析及相对增益矩阵（RGA）判据得到不同的操纵变量与控制变量匹配关系,以此为基础,在Aspen Dynamics平台建立了若干控制结构并进行分析对比。结果表明,利用两股反应物呈比例进料可较为有效地抵抗进料扰动,最后提出的无再沸器热负荷与混合物进料量比值（Q_r/F）控制的改进控制结构CS3,在降低反应精馏隔壁塔控制过程超调量方面有较大的优越性。     

Plantwide control for optimal operation of industrial-scale crude distillation unit processes

In this article, a combination of the wavelet neural network framework and the line-up competition algorithm is used to solve the economic optimization algorithm for an industrial-scale atmospheric distillation column (ADC) process. Compared to the relevant measuring data from Sinopec Wuhan Petroleum Group Company, China, the first optimal operating conditions show that the increments of the duties of furnace and pump-arounds of the ADC can effectively improve oil production. In our approach, the preflash column (PFC) coupled with ADC is denoted as an industrial-scale crude distillation unit (CDU) process. Since the PFC can produce light naphtha and reduce the furnace duty and steam consumption of ADC, it is verified that the CDU process provides the higher economic potential than ADC. Based on the second optimal operating conditions, the plantwide control strategy is employed to operate the system safely as well as regulate the outputs of the plant in the presence of inlet perturbations. Within the plantwide control framework, the inventory control aims to keep the controlled variables close to the desired operating condition and the quality control loops use a combination of inferential predictions and feedforward ratios to effectively suppress the temperature spikes of trays and furnaces. Finally, the simulations show that the product quality is guaranteed due to no offset ASTM D86 distillation temperature responses.     

Hyperazeotropic ethanol salted-out by extractive distillation. Theoretical evaluation and experimental check

A distillation process for the production of hyperazeotropic ethanol from a dilute wine obtained from the fermentation of biomass has been studied. This process utilizes the coupling of a soft preconcentration stage and of a dehydration stage based on the salting-out effect produced by calcium chloride on the ethanol in an aqueous solution, with the disappearance of the azeotrope. The salt is employed in a close cycle, due to the presence of a regeneration stage, therefore no consumption of calcium chloride is noticed.

The distillation process utilizes one column consisting of two sections operating at different pressures in order to reach an efficient heat recovery.

In this paper, a simplified flow-sheet of the process and the principal operating conditions of the distillation column are illustrated. When compared with other processes, conventional or under development, this one is characterized by the promising reduction of the specific energy requirement.

The operating conditions chosen for the distillation with salt have been experimentally checked using a laboratory column running continuously with calcium chloride as salting-out agent. Moreover, the experiments confirmed the reliability of the mathematical model of the process. Further experiments are in progress with the aim of utilizing a mixture of salts which can be fed from the bottom of the dehydration section back to the fermentor, so that the salt regeneration stage can be reduced.     

REDUCING STATIC DEVIATIONS OF PRODUCT QUALITIES IN THE TEMPERATURE CONTROL OF AN IDEAL HEAT-INTEGRATED DISTILLATION COLUMN

Two strategies are proposed in this work for the reduction of static deviations of product qualities in the dual-point temperature control of a simulated ideal heat-integrated distillation column. The key to achieve this purpose is to sense the changes in operating conditions and make appropriate adjustments simultaneously to the set-points of the top and bottom control loops. The first method is based on the inferential signals extracted from the composition of products and the second one from the temperatures of the top and bottom stages. Both strategies are intensively studied through the operation of the simulated ideal heat-integrated distillation column separating a binary equimolar mixture of benzene and toluene, and it is found that they could work effectively to decrease the static deviations in product qualities. The strategies are characterized by great simplicity in principle and a relatively small effort in process modeling, thereby allowing wide applications in the operation of various distillation columns with a dual-point temperature control scheme.     

Experimental validation of a packed bed distillation model

A mathematical model of a packed bed distillation column is presented and applied to a binary system in a full scale industrial distillation column with structured packings. The model is reduced by orthogonal collocation to sets of ordinary differential and algebraic equations. A linearized large state space model is then obtained and further reduced by the optimal Hankel norm method in order to obtain a model of manageable size. The model is studied under three different operating conditions in order to cover the feasible operating ranges during the experiments. The experiments carried out with a monoethanolamine-diethanolamine system show a good agreement with the model implying that a control design based on the model is satisfactory. It is also shown that the control configuration to be used can be easily analyzed by the model, since different input and output structures can be studied. Furthermore, models based on one-film and two-film theories are compared in the frequency domain and show that, due to its simplicity, the one-film theory should be used in control design.     

Explicit Nonlinear Predictive Control of a Distillation Column Based on Neural Models

A nonlinear Model Predictive Control (MPC) algorithm and its application to a distillation column are described. The algorithm uses a neural model of the process that is linearized online around the current operating point. The algorithm is computationally efficient because the control policy is calculated explicitly without any optimization. The algorithm requires online repetition of a matrix decomposition task and the solution of linear equations. The obtained solution is projected onto the admissible set of constraints imposed on the magnitude and the increment of the manipulated variables. For the distillation column considered, the control accuracy is comparable not only to that obtained in MPC with online linearization and quadratic programming but also to that obtained in nonlinear MPC, which is based on full nonlinear optimization repeated at each sampling instant.     

The effects of thermal distillation on the performance of differential-contact distillation columns

It is shown for a differential-contact distillation column that when there is net evaporation or net condensation within the column the height of a transfer unit should be lower than it is for adiabatic conditions. However, this improvement in efficiency, which is due to thermal distillation occurring in addition to contact distillation, is detected experimentally only for net condensation. It is also shown that, for the same reflux ratio at the top of the column, when there is thermal distillation fewer transfer units are needed, seemingly giving a further improvement in the performance. However, operating under the more realistic criterion of the same heat load per unit of throughput, implying a higher reflux ratio for adiabatic conditions, a column gives about the same separation whether there is thermal distillation or not.     

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     

甲醇精馏热焓控制设计及Aspen实现

对甲醇精馏塔塔釜进行热焓控制方案设计并通过Aspen软件仿真验证。首先介绍了甲醇三塔精馏工艺背景,根据实际项目的工艺条件,精馏塔底部采用双换热器作为再沸器的特点,进行热焓控制方案的设计,然后,利用Aspen软件仿真,以出料杂质乙二醚的含量为参考标准,通过与甲醇精馏塔塔釜常规温度控制的对比验证了本控制方案中热焓控制的优势,在面对实际工况下常规的流量和组分变化扰动时,产品质量能达到工业生产的要求,具有一定的实际意义。     

无累积罐循环全回流间歇精馏三温控制操作

提出了通过塔顶、塔中上以及塔中3个温度控制进行操作状态转换的无累积罐循环全回流间歇精馏控制方法,并以理想物系--乙醇-正丙醇混合物为分离物系进行了实验研究。通过实验确定了温度控制条件为当塔顶温度稳定后且塔顶和塔中上温差为0.3 ℃时变全回流为全采出操作,当塔中温度升高1.0 ℃时停止全采出转为全回流操作。同时还考察了在不同乙醇投料浓度条件下这种操作的运行情况,发现不同投料浓度对塔顶产品平均纯度的影响并不显著,基本能保持在0.99。最后在相同的投料浓度和操作条件下,对比了这种新型控制方式和双温度控制方式,结果表明三温度控制方式比双温度控制方式操作时间减少了23.3 min,分离效率提高了23.95%,产品浓度提高了1.06%,产品收率提高了1.08%。     

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.     

Activity evaluation of a catalytic distillation packing for MTBE production

The octane enhancer methyl tertiary butyl ether (MTBE) can be produced very efficiently from methanol and isobutene in a reactive distillation column where the heterogeneous catalyst also acts as distillation packing. Some mathematical models have been published for the simulation of such a process but they focus on the physical transport processes between the vapour and liquid phases. However, the aim of this paper is to analyze the importance of the internal and external multicomponent mass and heat transfer phenomena on the catalyst under boiling conditions. Therefore, experiments were carried out in a reactive distillation column at different compositions of feed, column pressures and reflux ratios using a Raschig ring shaped acidic ion exchange resin as the catalyst. The temperature and composition of the liquid phase entering and leaving the catalytic column section were measured. These data were used to evaluate the effectiveness factor of the catalyst with a rigorous macrokinetic model. It is shown that the effectiveness factor varies significantly along the column length. Under certain operating conditions, decomposition of MTBE can occur accompanied by boiling processes inside the catalyst macropores.