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.     

Reactive pressure swing batch distillation by a new double column system

Ethyl-acetate is generally produced by the esterification reaction of ethanol with acetic-acid. Since the reaction is equilibrium-limited, the use of reactive distillation is an attractive option. A new double-column system is suggested for ethyl-acetate production by applying reactive pressure swing batch distillation. The system was investigated by a feasibility study based on the analysis of reactive and non-reactive residue curve maps. Two different process options were found to be feasible. In the first option, the reactive column operates at the lower pressure (1.01 bar), and the non-reactive column that removes ethyl-acetate from the system operates at the higher pressure (10 bar). The second option allows the reactive column to operate at the higher pressure (10 bar), and the non-reactive column removes water at the lower pressure (1.01 bar). The first process option was studied by rigorous simulation based on less simplifying assumptions using a professional dynamic simulator. The influence of the most important operation parameters was also studied.     

热集成变压精馏乙二醇脱水系统的控制方案优化

针对热集成变压精馏乙二醇脱水再生系统存在的操作不稳定等问题,基于Aspen Plus和Aspen Dynamics软件,在全流程稳态模拟的基础上,对其进行了动态模拟及控制方案优化。设计了改进型控制方案CS2,与常规控制方案CS1相比,两个塔的操作压力的控制回路是相互独立的,高压塔的塔釜液位由再沸器的导热油流量控制,低压塔的塔釜温度由塔釜的采出流量控制,再分别对进料流量和进料组成中乙二醇含量的阶跃变动的动态响应特性进行分析。结果表明,控制方案CS1基本能够抵抗进料流量和进料组成扰动对系统的影响,但相关控制响应会出现一定的滞后性,难以保证产品满足要求。改进的控制方案CS2对相同的进料流量和进料组成扰动有更好的抵抗能力,控制性能显著提高,保证乙二醇的质量分数不低88%,趋于稳定时产品质量变化幅度小于2%,且该方案在实际应用中涉及到的操作相对简单。本文为相关双塔耦合过程的稳定控制提供了一种新思路,对于双塔耦合在其他体系的工程应用也有借鉴作用。     

热泵变压精馏分离乙二胺水溶液的模拟

基于乙二胺和水物系共沸组成随压力变化显著的特点,采用变压精馏工艺分离乙二胺和水物系;为了降低变压精馏工艺的能耗,提出了热泵变压精馏新工艺。使用Chem CAD软件,对变压精馏工艺和热泵变压精馏工艺进行了模拟。结果表明:采用变压精馏工艺和热泵变压精馏工艺都能实现乙二胺和水共沸物的高纯度分离,每个产品的纯度(质量分数)都可以达到99%;与变压精馏工艺相比,采用热泵变压精馏工艺,加热公用工程可节能62.24%;冷却公用工程可以节能49.51%。     

热集成变压精馏分离吡啶-水的控制研究

对于吡啶-水的分离,与传统的变压精馏工艺相比,热集成变压精馏工艺更加节能经济,进料流量为3 000 kg/h时,可以节约能耗43.52%,节省年度总费用40.70%。为了将该工艺应用在实际生产中,必须解决其控制的问题。在最优设计基础上,提出2种基于PI控制器的控制结构,并采用动态模拟软件Aspen Dynamics检验了存在进料流量和进料组成干扰情况下控制结构的有效性。模拟结果表明:扰动存在时,由于基本控制结构CS1中二塔均存在压力效应,并且控温板温度稳定在设定值,导致水和吡啶产品质量存在较大稳态余差。进而,在CS1基础上引入温差控制策略和压力补偿温度控制策略,提出一种改进的控制结构CS2。模拟结果显示,针对相同的进料流量和进料组成扰动,控制结构CS2的动态控制性能显著提高,产品质量的稳态余差均较小。     

热集成变压精馏分离甲苯-异丙醇的模拟

甲苯-异丙醇混合物的共沸组成对压力较为敏感,为此提出了热集成变压精馏工艺分离该共沸物.利用ASPEN PLUS化工模拟软件,以修正的WILSON活度系数方程作为物性计算模型,以甲苯和异丙醇的纯度作为约束变量,以分离过程能耗最低为目标函数,对主要工艺参数进行了模拟优化,得到了热集成变压精馏分离甲苯-异丙醇体系的最佳工艺操...     

变压精馏分离丙酮和环己烷的动态特性

基于丙酮-环己烷共沸体系的压力敏感性,利用Aspen Plus软件,以年度总费用(TAC)最小为目标函数对常规、部分及完全热集成变压精馏工艺进行稳态模拟与优化,并以经济最优的完全热集成变压精馏工艺为基础,借助Aspen Plus Dynamics软件建立多种不同控制结构,通过改变进料流量和进料组成考察了控制结构的有效性,并提出塔底热负荷/进料量比例控制与组成-温度串级控制相结合的改进控制结构。稳态模拟与优化结果表明,常规、部分和完全热集成三种工艺的最小TAC分别为3.64×105, 2.83×105, 2.76×105 $/y,经济最优工艺为完全热集成变压精馏。动态响应结果表明固定回流量/进料量控制结构在响应时间方面优于固定回流比控制结构,但产品纯度未达到设计值99.9wt%;而塔底热负荷/进料量比例控制与组成-温度串级控制相结合的改进控制结构能够有效保证产品纯度在99.9wt%及以上。     

Analysis of closed multivessel batch distillation of ternary azeotropic mixtures using elementary VLE cells

Introducing the concept of elementary topological cells, we illustrate how vapor-liquid equilibrium (VLE) diagrams like distillation lines and isotherms maps may be used in analysis of the closed (total reflux) multivessel batch distillation column. An indirect level control strategy is implemented that eliminates the need for pre-calculated vessel holdups and makes the closed operating policy flexible and simple to implement in practice.     

Air separation by pressure swing adsorption

The original pressure swing air separation process, developed almost simultaneously by Exxon and Air Liquide, uses a nitrogen selective zeolite adsorbent to produce a high purity oxygen product. The same basic process is still widely used in small scale units although, for larger scale units, many modifications to the cycle have been introduced in order to reduce power consumption. Although nitrogen can in principle be recovered from the blowdown stream of such systems, if high purity nitrogen is the required product, it is more economic to use an oxygen selective adsorbent. Most adsorbents show either no selectivity or preferential adsorption of nitrogen. However, in small pore carbon molecular sieves or 4A zeolite there is a substantial difference in diffusion rates so that an efficient kinetic separation is possible. Somewhat different cycles are generally used in such processes. Progress in modelling the dynamic behaviour of both types of PSA system is reviewed and comparisons between experimental performance and the model predictions are shown. A simple linear driving force model provides a good overall prediction of the effects of process variables but the computationally more cumbersome diffusion model gives better quantitative agreement with experiment. Comparisons are drawn between the performance achieved (in nitrogen production) with two different kinetically selective adsorbents; RS-10 (a modified 4A zeolite) and Bergbau Forschung carbon molecular sieve.     

Feasibility of heterogeneous batch distillation processes

Synthesis of heterogeneous batch distillation is discussed, which aims at splitting azeotropic mixtures by adding an entrainer partially miscible with one of the initial binary mixture components. Key operational parameters are identified such as the amount of entrainer added in the ternary feed, the reflux policy, and the vapor line position by examples. Synthesis and operation are less straightforward for heterogeneous batch distillation than those for the homogeneous case, but offer many advantages: more design alternatives, simplified distillation sequences, a lower consumption of entrainer, and a crossing of distillation boundaries by the still path. Feasibility is assessed using simplified modeling and confirmed using a commercial batch process simulator package. Synthesis expectations and simulated results are verified throughout bench-plant experiments for the separation of the acetonitrile—water mixture using acrylonitrile as a light heterogeneous entrainer.     

Comparative analysis of sharp separation regimes in the distillation of ternary zeotropic mixtures

A comparative analysis of the direct and indirect splits and class-1 fractionation of ternary zeotropic mixtures has been carried out in terms of total vapor flow rate by means of a mathematical experiment. Composition regions in which a certain separation flowsheet minimizes the total vapor flow rate have been found.     

变压精馏分离乙酸甲酯和甲醇共沸物

乙酸甲酯和甲醇共沸物对压力变化敏感,因此采用变压精馏工艺对共沸物进行高效分离。低压塔和高压塔压力分别设置为101.325 kPa和810.600 kPa。基于相图分析,确定了精馏序列和工艺流程。以年度总费用(TAC)最小为原则,优化了进料位置、回流比、塔板数等设计变量,确定了最佳工艺参数。工艺优化完成后,通过调节双塔的回流比,对高压塔的冷凝器和低压塔的再沸器进行了完全热集成。由结果可知:在低压塔回流比为0.9,高压塔回流比为2.07时,完全热集成变压精馏工艺的TAC最小。相比无热集成的变压精馏工艺,完全热集成工艺的设备投资和能耗费用均明显降低,最终TAC费用节约31.40%,在经济上更合理,也为类似的共沸物分离工艺提供了一定的技术参考。     

热集成变压精馏分离吡啶-水的工艺模拟与优化

基于吡啶-水体系的共沸组成对压力变化敏感,提出了热集成变压精馏的新工艺。新工艺采用冷凝器-再沸器式热集成,利用高压塔塔顶蒸汽加热低压塔再沸器,以节省能耗和操作费用。选择NRTL活度方程为物性计算模型,使用Aspen Plus软件对该工艺流程进行严格稳态模拟。为了获得经济最优的工艺条件,提出了局部经济优化和全局经济优化相结合的优化方案,并建立了优化迭代流程。优化结果显示:当低压塔和高压塔的操作压力分别为16 kPa和1 200 kPa,总理论板数分别为12和14,新鲜原料和循环物流分别从低压塔第9块板和从第6块板进料,高压塔的物流进料位置为第8块板,高压塔质量回流比为0.59时,年度总费用(TAC)最小。与常规的变压精馏工艺相比,热集成变压精馏工艺更加节能经济,可以节约能耗43.52%,节省年度总费用40.70%。     

Gas separation by pulsed pressure swing adsorption

An experimental study of the separation of a binary mixture of methane and carbon dioxide by pulsed pressure swing adsorption in a single isothermal column packed with an activated carbon adsorbent revealed that a product containing 72% methane could be obtained from a feed mixture containing only 44% methane. When a 5A zeolite was used as adsorbent, the product contained more than 92% methane, the initial feed mixture being only 46% methane. A mathematical model of the process operation is shown to be in general agreement with the experimental results obtained.     

Combining extractive heterogeneous-azeotropic distillation and hydrophilic pervaporation for enhanced separation of non-ideal ternary mixtures

The separation of non-ideal mixtures using distillation can be an extremely complex process and there continues to be a need to further improve these techniques. A new method which combines extractive heterogeneous-azeotropic distillation (EHAD) and hydrophilic pervaporation (HPV) for the separation of non-ideal ternary mixtures is demonstrated. This improved distillation method combines the benefits of heterogeneous-azeotropic and extractive distillations in one column but no added materials are needed as is usually the case with pervaporation. The separation of water-methanol-ethyl acetate and water-methanol-isopropyl acetate mixtures were investigated to demonstrate the accuracy of the combined EHAD/HPV technique. There is not currently an established treatment strategy for the separation of the second mixtures in the literature. These separation processes were rigorously modelled and optimized using a professional flowsheet. The objective functions were total cost and energy consumption and heat integration was also investigated. The verification of the process modelling was carried out using laboratory-scale measurements. Extractive heterogeneous-distillation combined with methanol dehydration was found to be more efficient than conventional distillation for the separation of these highly non-ideal mixtures.     

热集成变压分离碳酸二甲酯-甲醇的优化与控制

利用Aspen Plus软件对碳酸二甲酯-甲醇物系,提出了热集成变压精馏新工艺,以年度总费用(TAC)最小为目标函数进行经济优化,优化结果显示可以节约能耗33.82%,TAC节省25.97%。在动态控制系统中,针对常压塔温度分布均匀、灵敏板选择困难的问题,给出一种简单有效的导斜率判据方法。在此基础上,研究了常压塔不同灵敏板以及不同控制结构对完全热集成工艺动态可控性的影响。结果表明:常压塔第29块塔板作为灵敏板的组成/温度串级控制结构CSC,可以有效处理±10%进料流量和进料组成扰动。对于超过10%进料流量和组成扰动,高压塔(HPC)压力波动大、产品不易控制的特点,在CSC基础上建立的压力-补偿温度控制结构CSD,使两塔产品的稳态余差较小,可以处理±20%的进料流量和组成扰动,实现更稳健的动态控制。     

Dynamic composition estimation for a ternary batch distillation

A novel Kalman estimator has been proposed to provide the estimates of dynamic composition in a ternary batch distillation process operated in an optimal-reflux policy. The estimator is formulated based on a sequence of reduced-order process models representing a whole batch behavior. Therefore, the full-order models are first developed around different pseudo-steady-state operating conditions along batch optimal profiles. Then they reduce their orders to achieve all state observability and controllability by a balanced truncation method. In the estimator scheme, the reduced models as well as relevant covariance matrices of process noise are pre-scheduled and switched according to any desired periods. Four important issues have been studied including selection of a sensor frequency, effects of an integrating step size, a state initialization and a measurement noise. The performances of the reduced estimator have been investigated and compared with those of a conventional nonlinear estimator. Simulation results have demonstrated that the performances of the novel linear estimator are reasonably good and almost identical to the nonlinear estimator in all cases, though the linear estimator performs rather sensitively to the effect of high measurement noise. Nevertheless, it has been found to be applicable to implement in real plants with much lower computation effort, easier state initialization and unrequired a priori knowledge of thermodynamics.     

差压精馏法分离甲醇与乙酸甲酯

研究了差压精馏法分离甲醇-乙酸甲酯共沸体系的工艺过程。通过模拟计算,着重针对精馏塔的理论板数、进料位置、回流比3个关键参数进行了讨论,分析和确定了最佳工艺条件,并给出了工艺流程和装置单耗。该工艺流程简单,产品纯度高,不需要向体系中加入第三组分。     

高浓度含酚废水的变压精馏分离过程研究

为了实现高浓度含酚废水中的苯酚回收和减少含酚废水处理量,针对苯酚水二元共沸物系的压力敏感性,利用Aspen软件对高浓度含酚废水的变压精馏分离进行了可行性研究,并以全年总成本TAC为目标函数,采用序贯迭代法对苯酚水混合物的变压精馏分离过程进行了流程优化。当高压塔操作压力1 418.55 k Pa,理论板数61,进料位置30,循环物流进料位置15,回流比2.09,低压塔操作压力101.325 k Pa,理论板数7,进料位置6,回流比0.19时,苯酚回收率可达到99.1%,水纯度为99.9%,再经生化处理后就可直接排放。在此基础上,对热集成工艺在含酚废水变压精馏过程中的经济性进行了分析,结果表明:对于苯酚质量分数为10%的含酚废水的变压精馏过程,部分热集成工艺可降低能源消耗1 137 k W,节约运行成本$283 709,且部分热集成变压精馏比完全热集成变压精馏具有更低的运行成本。     

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™.