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     

From simulation studies to experimental tests in a reactive dividing wall distillation column

The design and control of thermally coupled distillation sequences have been studied since many years, but the real implementation occurred until middle of the 1980s using a single shell divided by a wall named dividing wall distillation column. In this work, experimental results for the production of ethyl acetate in a reactive dividing wall distillation column are presented for first time. The experimental results are in agreement with those obtained using steady state simulations with AspenONE Aspen plus. These experimental results are important since it is possible to validate most of the previous results generated using simulations.     

Influence of heat transfer across the wall of dividing wall columns on energy demand

The implementation of a vertical dividing wall (DW) into a distillation column is a well‐known concept which can result in considerable energy savings for the separation of multicomponent mixtures. It is commonly known that heat streams across the DW, which are present due to temperature differences between both sides, may either increase or decrease the energy demand for a certain separation task. However, no work has been published so far which explains the maximum influence on energy demand. This article derives the maximum extent to which the minimum energy demand for a given column design can change due to heat transfer across the DW. Additionally, it is illustrated how energy‐efficient column operation can be assured even if the total amount of transferred heat is unknown. These results show that the phenomenon of heat transfer across the DW can be handled very well with a suitable control strategy. © 2015 American Institute of Chemical Engineers AIChE J, 61: 1648–1662, 2015     

Feed distribution in distillation: Assessing benefits and limits with column profile maps and rigorous process simulation

This contribution describes the column profile map (CPM) methodology for designing distributed feed distillation columns. For non‐sharp product distributions, a case study shows that energy savings of approximately 35% can be obtained if the feed stage(s) are designed optimally. Feed distribution allows capital cost savings, expands operating leaves, and can obtain greater separation feasibility. However, this column only has benefits in ternary and higer‐order systems and when product distributions are non‐sharp. To validate these counter‐intuitive claims, a real Benzene, p‐Xylene, Toluene system is modeled using CPMs, and the resulting design parameters are transported to Aspen Plus^®. Using a sum of squared errors objective function to quantify savings, a cost saving trend very similar to the one predicted by the CPM method is obtained. This article therefore describes a complete design methodology for distributed feed systems and provides convincing evidence of benefits of such a system. © 2012 American Institute of Chemical Engineers AIChE J, 59: 1668–1683, 2013     

乙酰丙酸乙酯的反应精馏模型及隔壁塔节能优化设计

乙酰丙酸乙酯是一种潜在的生物质基平台化合物,在工业上具有很高的应用价值。乙酰丙酸乙酯传统的生产方法主要为间歇反应法,效率较低,产物分离困难且工艺流程较长。因此,本文提出了反应精馏工艺生产乙酰丙酸乙酯,在以中试实验结果为依据的基础上,使用Aspen Plus模拟软件建立了工艺流程,并考察了回流比、进料位置、进料摩尔比以及理论塔板数等关键参数,得到了常规单塔反应精馏工艺生产乙酰丙酸乙酯的最优配置。而后,为了得到纯度大于99.9%的乙酰丙酸乙酯,本文进一步提出了反应精馏双塔精制流程以及反应精馏隔壁塔流程,并通过对两种流程所得到的产品纯度以及能耗的对比,验证了反应精馏隔壁塔工艺生产乙酰丙酸乙酯的有效性以及在节能方面较大的优势。     

Experimental study on pressure drops in a dividing wall distillation column

Previous studies in the fields of process design and process control [1] have shown the potential benefits that can be achieved through the implementation of thermally coupled distillation sequences, in particular, the dividing wall distillation column. The dividing wall distillation column meets important goals of process intensification, including energy savings, reduction in carbon dioxide emissions and miniaturization. In this paper, an experimental study on the hydrodynamic behavior of a dividing wall distillation column is presented. Several different values for gas and liquid velocities were tested in order to measure pressure drops and identify operational regions; the air/water system was used as the basis for the experimental setup. Results regarding pressure drops (fitted to the model of Stichlmair et al.) provide operational limits for the operation of the packed dividing wall distillation column. According to the results, the experimental dividing wall column can be operated at turbulent regime that is associated to proper mass transfer.     

反应精馏隔壁塔的模拟研究

以乙酸甲酯酯转换体系为例提出了一种反应精馏隔壁塔的设计和优化方法,应用该方法可将常规双塔反应精馏序列转化为反应精馏隔壁塔并保证各操作参数的最优值.首先通过在反应精馏塔与甲醇塔之间交换汽液相物流来实现反应精馏隔壁塔的简捷设计;然后利用Aspen Plus模拟软件,对常规反应精馏序列和反应精馏隔壁塔进行了模拟分析;最终以2...     

分壁式精馏塔精制丁二烯流程模拟

丁二烯是一种重要的石油化工烯烃原料,由于其生产过程能耗高,因此节能降耗成为丁二烯生产工艺的研究热点。利用Aspen Plus模拟软件对丁二烯精制工艺的两套流程进行了模拟研究,考察了分壁式精馏塔(DWC)中内部互连物流连接位置、预分离塔气液相流量和回流比对分离效果和热负荷的影响,对比了相同分离条件下DWC分离流程和传统顺序分离流程的能耗,并根据两套分离流程中塔内液相丁二烯浓度分布情况,分析DWC的节能原因。结果表明,当主塔理论板数105,预分离塔理论板数56,进入预分离塔气相流量1020kmol/h,液相流量890kmol/h,回流比7800时,DWC分离效果最好,丁二烯质量分数可达99.7%,这为DWC精制丁二烯工艺的工业化提供了理论依据。由于DWC有效减少了精馏过程中的返混效应,提高了能量利用率,使其冷凝器可节能29.36%,再沸器可节能29.19%,存在明显的节能优势。     

立板式隔板塔分离直馏汽油工艺

对利用一种新型立板式隔板精馏塔切割直馏汽油工艺进行了研究。首先,利用模拟软件HYSYS对该分离过程进行模拟,得到较优的工艺条件。在此基础上,利用立板式隔板塔实验装置,考察了塔顶总回流量、液体分配比等操作参数对产品的影响及装置的操作稳定性。结果表明,塔顶总回流量的增大有助于产品的分离,且液体分配比的选择范围更广。液体分配比的改变对中间侧线产品质量的影响较大,是操作的关键变量。     

反应精馏隔壁塔内合成乙酸甲酯的模拟

提出了一种应用反应精馏隔壁塔合成乙酸甲酯的新工艺流程,采用反应精馏隔壁塔替代常规反应精馏流程中的反应精馏塔及甲醇回收塔。利用Aspen Plus模拟软件,对反应精馏隔壁塔及常规流程进行了模拟,比较分析了两种流程塔内液相组成分布,并分析了塔顶回流比与气相分配比对反应精馏隔壁塔的影响。结果显示新流程可以节能11.9%,并能降低设备投资费用和操作费用。     

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。     

碳五隔壁反应精馏预处理工艺模拟及多目标优化

针对碳五综合利用预处理工段能耗较高的现状,在反应精馏(RD)预处理流程基础上提出了隔壁反应精馏(RDWC)预处理流程。首先,利用化工模拟软件Aspen Plus搭建RDWC四塔等效严格模型,并对其进行自由度和单变量分析。在此基础上,以响应面Box-Behnken Design(BBD)方法作为模型拟合工具,拟合出目标变量与决策变量之间的函数关系,并对拟合结果进行方差分析(ANOVA)。最后采用基于分解的多目标进化算法(MOEA/D)对RDWC预处理流程进行多目标优化,得到一系列Pareto最优解,选出其中年总成本(TAC)最小的一组解与RD预处理流程进行对比。结果显示：与RD预处理流程相比,RDWC预处理流程可以节约TAC 12.8%,节省再沸器负荷27.8%,选择性也有所提高。     

隔板塔共沸精馏分离二氯甲烷-乙腈-水-硅醚体系

以二氯甲烷-乙腈-水-硅醚为分离体系,采用自制隔板塔小试装置,研究了共沸剂回流比和液相分配比等操作参数对隔板塔分离效果的影响。实验结果表明,当气相分配比R_v为0.5,共沸剂回流比为3时,液相分配比R_l在[0.12,0.2]范围内,隔板塔分离效果较好。在实验的基础上,采用Aspen Plus软件对隔板塔共沸精馏工艺进行模拟,考察了隔板塔共沸精馏工艺最佳操作区域及节能效果。模拟结果表明,特定分离要求下,隔板塔存在一个使再沸器热负荷最小的最佳操作区域,在此最佳操作区域内,R_l和R_v相互关联,呈一一对应关系;与三塔串联简单精馏工艺相比,完成相同的分离任务,隔板塔共沸精馏工艺再沸器节能32.74%,冷凝器热负荷减少33.70%,乙腈回收率由66.47%提高到96.01%,且大幅降低设备投资。     

分隔壁精馏塔分离裂解汽油

自制一套塔高8.3m可拆装10L釜分隔壁精馏塔小试装置分离裂解汽油,考察不同的出料位置、侧线采出量、液体分配比等参数对分离效果的影响。得出较佳工艺条件为:进料速度6L/h,进料温度56℃,塔顶出料1.1L/h,回流量为1.5L/h,液体分配比(主:副)为2:1及侧线出料量3.6L/h。在此条件下,塔顶C5的质量分数达到98.5%以上,侧线C5的质量分数小于2%,满足分离要求。该工艺缩短了流程,减少了设备投资。     

气相进料对隔板精馏塔优化设计的影响

隔板精馏塔（DWC）在节能和节省设备投资方面具有十分突出的优势,隔板精馏塔中隔板位置是重要的设计变量,影响分离效果及能耗,当进料中含有气相时这种影响更加显著。选用苯、甲苯和对二甲苯三元物系,研究了进料的气相分率对隔板位置的影响并确定最优隔板位置。采用严格模拟方法,以年度总费用（TAC）为评价指标,比较不同进料气相分率下隔板塔的经济性,其中气相进料较液相进料TAC最高可节省23.33%。并通过灵敏度分析展示了在进料中含有气相时确定最优隔板位置的重要性。     

气相进料对隔板精馏塔优化设计的影响

隔板精馏塔（DWC）在节能和节省设备投资方面具有十分突出的优势,隔板精馏塔中隔板位置是重要的设计变量,影响分离效果及能耗,当进料中含有气相时这种影响更加显著。选用苯、甲苯和对二甲苯三元物系,研究了进料的气相分率对隔板位置的影响并确定最优隔板位置。采用严格模拟方法,以年度总费用（TAC）为评价指标,比较不同进料气相分率下隔板塔的经济性,其中气相进料较液相进料TAC最高可节省23.33%。并通过灵敏度分析展示了在进料中含有气相时确定最优隔板位置的重要性。     

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     

三组分精馏隔板塔的操作柔性模拟与分析

隔板精馏塔作为完全热耦合精馏塔由于具有较强的耦合性,其操作与控制相比传统精馏塔更为复杂,同时由于具有更多的自由度表现出更多的操作柔性。选用正戊烷、正己烷、正庚烷混合物的分离为例,采用严格模拟方法,通过对7 种进料条件设计的隔板塔进行模拟,考察了不同进料条件下的操作柔性,同时考察进料组成对隔板精馏塔操作柔性的影响。     

Design and optimization of a dividing wall column for debottlenecking of the acetic acid purification process

The dividing wall column (DWC) has gained increasing application in a variety of chemical processes because of its potentiality in energy and capital cost savings in multicomponent separations. The main objective in this work is investigation of its use for removing the bottleneck phenomenon within the column when increasing the throughput of an existing distillation process, particularly, the acetic acid (AA) purification process. Optimal column sequence design, involving both conventional and DWC, is considered. The internal recycle flow distribution around the dividing wall was investigated as a primary optimizing variable. Several column arrangements were analyzed to show that the DWC requires less investment and energy costs than conventional distillation, the Petlyuk column, or the prefractionator arrangement.     

生物燃料乙醇分壁塔萃取精馏新工艺的研究

针对生物燃料乙醇生产中的"蒸馏-脱水"过程,建立基于分壁式萃取精馏塔的三塔工艺和两塔工艺,对2种工艺进行模拟计算,比较其分离效果和过程能耗。结果显示,在满足产品质量的前提下,三塔工艺比两塔工艺节约66.6%的冷凝器热负荷和77.9%的再沸器热负荷。对三塔工艺的分壁式萃取精馏塔的工艺条件进行优化,优化结果为,主塔回流比1.5,溶剂比1.0,原料进料位置为第22块板,隔板底端位置在第28块板,气相分配比为8.4。在优化工艺条件下对三塔工艺进行全流程模拟,可得到质量分数99.96%生物燃料乙醇和99.49%的水,回收萃取剂乙二醇质量分数为99.97%。