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。     

Exploration of a heat-integrated pressure-swing distillation process with a varied-diameter column for binary azeotrope separation

The pressure-swing distillation (PSD) processes with varied-diameter columns (VDCs) for separating methanol–chloroform and n-heptane–isobutanol are studied. Furthermore, two heat-integrated PSD processes, partial integration and full heat integration, are discussed with ordinary and VDCs. The results show that whether it is heat integrated or non-heat integrated, the processes using VDC have an advantage in the economy. Based on the minimum total annual cost (TAC), the dynamic controllability without and with full heat integration for an azeotrope system methanol/chloroform is explored. The dynamic controllability without and with partial heat integration for the azeotrope system n-heptane/isobutanol is discussed. The results indicated that compared with the dynamic responses without heat integration process, the heat-integrated PSD with a VDC did not increase the control difficulty while maintaining its economy. More azeotropic systems should be studied to investigate their economics and control effects, which will benefit PSD design and industrial application.     

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...     

空分精馏系统最佳氩馏分位置的确定

指出在同时生产高纯度的氢、氮及粗氩产品，并带粗氩塔的空气分离双级精馏系统中，双级精馏塔的上塔存在最佳抽氩馏分位置，并介绍其确定方法。     

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.     

Feasible separation regions for distillation I: Structure

A feasible separation region is determined for only four special combinations of a saturated vapor/liquid feed and total/partial condenser or reboiler. This work addresses the construction of a feasible separation region for a general case where the feed is a mixture of vapor and liquid in equilibrium and where the column is equipped with a partial/total condenser and reboiler. The analysis reveals that the product composition sets (which are defined for various reflux and reboil ratios and a fixed number of stages in each column section) are the main elements of the feasible separation region. The application of the geometric model of the column in combination with the shape of the distillation line led to the conclusion that the feasible separation region is the union of two product composition sets for both enriching and stripping columns both with an infinite number of stages. The boundary of the feasible separation region consists of several curves related to specific types of operating modes in the column. Some of these curves create a well‐known product composition multitude, whereas other curves form a generalized distillation limit. © 2017 American Institute of Chemical Engineers AIChE J, 2017     

用分隔壁精馏塔分离三组分混合物的节能研究

为了比较分隔壁精馏塔与常规精馏流程能耗,确定其应用范围,采用Aspen plus软件中的精馏严格模型,对2种常规精馏流程和3种分隔壁精馏塔进行模拟计算,比较了各种分隔壁精馏塔序的节能效果。结果表明,中间组分的摩尔分数越高,分隔壁精馏塔的节能效果越好,分隔壁精馏塔可用于分离中间组分摩尔分数较高的混合物,且适于分离指数在0.61至2.1之间的物系。分隔壁侧线精馏塔适用于分离指数≥1、轻组分摩尔分数较高的混合物。分隔壁侧线提馏塔适于重组分摩尔分数较高的混合物。     

液化天然气分离的多效蒸馏工艺

采用化工过程模拟软件Aspen Plus计算模型,模拟研究了液化天然气分离得iC4,nC4和C5+的过程,比较了现有常规蒸馏工艺和采用双效蒸馏以及热集成新工艺的能耗情况。结果表明,在相同的处理量和塔板数下,双效蒸馏和热集成新工艺的能耗都比常规蒸馏工艺有大幅度降低,而尤以热集成的节能效果最好。双效蒸馏工艺比常规蒸馏方案节能31.9%,热集成工艺节能达35.8%左右。对于此分离过程,采用双效蒸馏以及热集成新工艺都有应用前景,值得进一步推广应用。     

Comparing three configurations of the externally heat-integrated double distillation columns (EHIDDiCs)

In terms of separation of a binary mixture of ethylene and ethane, three configurations of externally heat-integrated double distillation columns (EHIDDiCs), including a symmetrical EHIDDiC (S-EHIDDiC), an asymmetrical EHIDDiC (A-EHIDDiC), and a simplified asymmetrical EHIDDiC (SA-EHIDDiC), are compared with respect to aspects related to process design and controllability. It has been found that the A-EHIDDiC and SA-EHIDDiC are superior to the S-EHIDDiC in terms of thermodynamic efficiency as well as in terms of process dynamics and controllability. As for the comparison between the A-EHIDDiC and SA-EHIDDiC, the latter shows somewhat comparable behaviors with the former in terms of process design and controllability. These results demonstrate that the asymmetrical configuration should generally be favored over the symmetrical one for the development of the EHIDDiC. It is feasible to approximate external heat integration using three heat exchangers between the high- and low-pressure distillation columns involved.     

Heterogeneous extractive batch distillation of chloroform-methanol-water: Feasibility and experiments

A novel heterogeneous extractive distillation process is considered for separating the azeotropic mixture chloroform-methanol in a batch rectifying column, including for the first time an experimental validation of the process. Heterogeneous heavy entrainer water is selected inducing an unstable ternary heteroazeotrope and a saddle binary heteroazeotrope with chloroform (ternary diagram class 2.1-2b). Unlike the well-known heterogeneous azeotropic distillation process and thanks to continuous water feeding at the column top, the saddle binary heteroazeotrope chloroform-water is obtained at the column top, condensed and further split into the liquid-liquid decanter where the chloroform-rich phase is drawn as distillate. First, feasibility analysis is carried out by using a simplified differential model in the extractive section for determining the proper range of the entrainer flowrate and the reflux ratio. The operating conditions and reflux policy are validated by rigorous simulation with ProSim Batch Column^® where technical features of a bench scale distillation column have been described. Six reproducible experiments are run in the bench scale column matching the simulated operating conditions with two sequentially increasing reflux ratio values. Simulation and experiments agree well. With an average molar purity higher than 99%, more than 85% of recovery yield was obtained for chloroform and methanol.     

反应蒸馏分离技术进展

反应蒸馏分离是近年来发展起来的具有独特作用的新型分离技术。讨论了几个典型的反应蒸馏分离流程，指出了该技术的应用范围并分析了该分离过程的主要影响因素。     

分隔壁精馏塔分离醇类混合物的模拟

以分隔壁精馏塔分离乙醇、正丁醇及正己醇为例,建立分隔壁精馏塔稳态模型。用Aspen Plus软件进行模拟,模拟数据与实验数据吻合良好。同时考察了分隔壁精馏塔内液体分配比对产品含量的影响及正丁醇液相组成分布情况。比较了采用分隔壁精馏塔和常规二塔流程分离此物系的节能情况。结果表明,由于分隔壁精馏塔能极大地减少返混现象的产生,故达到相同的分离要求,分隔壁精馏塔比常规精馏的流程更节能,采用分隔壁精馏塔分离此物系时,中间组分的摩尔分数越高,节能效果越好,当进料组成为n(C2H5O)∶n(C4H10O)∶n(C6H14O)=1∶3∶1时,可节能25.9%。分隔壁精馏塔技术是一种节能、经济的新工艺。     

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%。     

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     

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.     

分子蒸馏技术在烟用香料提取分离中的应用

采用分子蒸馏技术富集烟叶碎片萃取物中的致香物质。通过正交试验优化得到最佳分离条件：压力0.1Pa、温度60℃、转子转速250r·min-1、进料流速70mL·h-1。卷烟加香试验表明：该馏出物能够增补卷烟香气中的清甜香韵,增加香气的透发飘逸感,是一种适宜卷烟加香的理想香精制品。     

Optimum design of Petlyuk and divided-wall distillation systems using a shortcut model

An optimization approach for fully thermally coupled distillation systems for the separation of ternary mixtures is presented. The thermally coupled schemes considered here can be implemented in the form of the original Petlyuk arrangement (with an external prefractionator) or the modified Kaibel arrangement (in the form of a divided-wall column). The approach uses a shortcut design method that allows the system to be modeled as a nonlinear programming problem. Given the practical interest in divided-wall column arrangements, special attention is given in this work to this type of structure. Several cases of study are presented to show the applicability of the proposed approach.     

反应精馏在裂解碳五分离中的应用

在分析现有萃取精馏碳五分离工艺流程的基础上,结合碳五馏分中双烯烃异戊二烯、间戊二烯和环戊二烯的反应动力学数据在AspenPlus中建立了反应精馏模型,结果表明反应精馏应用于碳五分离过程是可行的。     

氯仿精馏二塔流程探讨

分析由氯仿精馏塔和氯仿蒸出塔组成的氯仿精馏二塔流程中,氯仿蒸出塔的返回量对氯仿精馏塔操作性能、产品收率和蒸汽消耗量的影响。建议将二塔流程改成一塔流程。     

氢同位素的低温精馏分离及模拟技术

低温精馏分离氢同位素的技术,是可使聚变反应器燃料循环使用的有效方法。在研究低温精馏氢同位素的过程中,必须考虑到物系的特殊性,如氚具有衰变热、氢溶液的非理想性,以及严格的分离要求等。文章从理论及实际出发综述了氢同位素低温精馏体系的发展过程,并比较和讨论了各种流程的构造及特点,总结了氢同位素低温精馏模拟研究的发展历程和目前状况。提出进一步研究低温精馏分离氢同位素的必要性。