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。     

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。     

三元混合物分壁塔精馏分离的研究

提出了甲醇-乙醇-正丙醇三元混合物分壁塔精馏分离的新工艺。通过模拟和灵敏度分析,考察了分壁塔的进料位置、隔板位置、液体分配比、回流比等工艺参数对分离效果的影响,确定了分壁塔的最佳操作条件,并对分壁塔的能耗进行了分析。结果表明,单个分壁塔能达到常规三元混合物分离的要求,并且比常规精馏流程的分离过程节能约30%。     

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。     

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。     

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...     

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。     

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。     

Experimental operation of a reactive dividing wall column and comparison with simulation results

Reactive dividing wall columns (RDWC) are a special type of distillation column that allow for the targeted realization of chemical reactions and the separation into multiple product fractions in one shell. However, despite their huge economical and ecological potentials for certain fields of application, this innovative technology has not found its way into industrial production processes yet. The very limited availability of experimental research studies verifying the prediction capabilities of respective modeling concepts for this type of distillation column might be one decisive reason for that. Therefore, the present study puts its focus on the detailed comparison between experimental operation of RDWC and the corresponding simulation results for steady‐state. For the first time, the mentioned comparison is carried out for a chemical system with non‐negligible side reactions. It is shown that even for this highly complex system, the mathematical model is capable of predicting the column operation. © 2016 American Institute of Chemical Engineers AIChE J, 63: 1036–1050, 2017     

Nonlinear model predictive control for dividing wall columns

Dividing wall columns (DWCs) are practical, effective, and promising among distillation process intensification technologies. Nonlinear model predictive control (NMPC) schemes are developed in this study to control the three-product DWCs. As these systems are intensely interactive and highly nonlinear, NMPC may be more suitable than the traditional PI control. The model is established based on Python and Pyomo platforms. As the original mathematical model of the column section is ill-posed, index reduction is used to avoid a high-index differential-algebraic equation (DAE) system. The well-posed index-1 system after index reduction is employed for the steady-state simulation and dynamic control in this study. Case studies with three DWC configurations to separate the mixture of ethanol (A), n-propanol (B), and n-butanol (C) show that the NMPC performs very well with small maximum deviations and short settling times. This demonstrates that the NMPC is a feasible and very effective scheme to control three-product DWCs.     

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。     

间壁塔萃取精馏制取植物油抽提溶剂的研究

针对植物油抽提溶剂萃取精馏系统存在的萃取剂结焦问题展开研究,分析了萃取剂结焦的原因,提出了间壁塔萃取精馏制取植物油抽提溶剂的思路,并应用工艺模拟软件对比了间壁塔萃取精馏工艺和常规精馏工艺。模拟结果表明,间壁塔主塔合适的理论塔板数为30,侧线塔塔板数为10,剂油比为1.1(体积比),侧线采出位置为第27块板。与常规两塔精馏相比,再沸器热负荷降低约10%,冷凝器热负荷降低15%,且设备投资也有所减少。     

Control of reactive dividing wall column for selective hydrogenation and separation of C3 stream

In our previous work, the reactive dividing wall column (RDWC) was proposed and proved to be effective for selective hydrogenation and separation of C3 stream. In the present paper, the dynamics and control of the proposed RDWC are investigated. Four control structures including composition and temperature controls are proposed. The feed forward controllers are employed in the four control strategies to shorten the dynamic response time, reduce the maximum deviations and offer an immediate adjustment. The control structures are compared by applying them into the RDWC system with 20% disturbances in both the feed flow rate and the feed compositions, and the results are discussed.     

隔壁式空分精馏塔应用性能研究

为了降低空气低温分离过程的设备投资和能耗,在分析空分体系的热力学性质及流程特点的基础上,提出了一种新型的隔壁式空分精馏塔流程。应用Aspen Plus模拟软件,对空气分离的传统流程和隔壁塔流程进行了模拟对比,考察了隔壁式空分精馏塔各结构参数与操作参数对其年总成本的影响,并分析比较了空分传统流程和隔壁式空分精馏塔流程的热力学效率。结果表明,隔壁式空分精馏塔的建模合理可行,通过年总成本优化得到了该隔壁塔的最优结构参数与操作参数,分别为:液氧流量为3 kmol/h,气相分配比(体积比)为0.05,精馏段理论板数为33,侧线精馏段理论板数为30,公共提馏段理论板数为22。与传统空分流程相比,隔壁式空分精馏塔流程的有效能损失降低并且在热力学效率方面高出4.7%。     

Experimental and simulation of the reactive dividing wall column based on ethyl acetate synthesis

Reactive dividing wall column(RDWC) is a highly integrated unit which combines reaction distillation(RD) with dividing wall column separation technology into one shell, and it realized the chemical reaction and the separation of multiple product fractions simultaneously. In this paper, the reaction of esterification with acetic acid and ethanol to produce ethyl acetate was used as the research system, experiments and simulations of the RDWC were carried out. This system in the traditional process mostly used the homogeneous catalyst(e.g. sulfuric acid). However, in view of the corrosion of the equipment caused by the acidity of the catalyst, we used the heterogeneous catalysts – iron exchange resins – Amberlyst15 and proposed a novel catalyst loading method. Firstly,the reliability of the model of the simulation was verified by the experimental study on the change of liquid split ratio and reflux ratio. After that, the four-column model was established in Aspen Plus to analyze the effects of the amount of azeotropic agent, reflux ratio and acetic acid concentration. Finally, for a fair comparison, the economic analysis was conducted between traditional RD column and RDWC. The results showed that RDWC can save34.7% of total operating costs and 18.5% of TAC.     

热泵精馏隔壁塔分离宽沸程物系的模拟

将中间换热和热泵精馏两种精馏节能技术应用到隔壁塔中,提出了带中间换热器的热泵精馏隔壁塔流程,以解决隔壁塔在分离宽沸程物系时出现的塔顶与塔底温差过高而不宜应用热泵精馏的问题。利用精馏塔总复合曲线图,可确定中间产品塔板采出流股的相态,从而得到不同类型的热泵精馏隔壁塔流程。宽沸程物系分离实例的模拟计算结果表明,该类流程在主塔气液相流量较大的情况下具有较高的节能效率。     

Experimental study and CFD numerical simulation of an innovative vapor splitter in dividing wall column

The vapor split ratio (R_V) adjustment plays an important role on energy efficiency during dividing wall column (DWC) operation. In order to achieve active control of R_V, this aticle presents an innovative vapor splitter driven by hydraulics. The vapor flows into main tower from prefractionation section through the rectangle hole located at the end of the partition. Vapor splitting is implemented by the change of flow resistance at the rectangular hole caused by adjusting the liquid level on the bottom plate. This design makes full use of the hydraulic properties in DWC, employing simpler construction with single tunable parameter. Numerical simulations and laboratory tests were both carried out to validate its performance in the DWC with a diameter of 600 mm. The results demonstrate that the desired R_V can be handled effectively in the approximate range from 0.5 to 2, basically satisfying the industrial demand for the gas distribution.     

隔壁塔内半圆填料层中壁流与返混特性研究

在填料塔三参数壁流模型的基础上,提出了应用于隔壁塔半圆型填料层的壁流模型。通过实验对模型参数进行了估计。模型计算值与实验值吻合较好。在内径为580 mm、高2800 mm的半圆冷模塔内,常温常压下以空气-水为介质,测取了散堆填料的壁流曲线,分析了气液速率变化对壁流的影响。以氯化钠溶液为示踪剂,通过脉冲注入扰动响应技术获得停留时间分布曲线。发现气液速率变化均对停留时间分布产生不同程度影响。同时比较了同一填料层高度塔壁区和整体区的平均停留时间,在壁流充分发展阶段,塔壁区的平均停留时间明显小于整体区。从另一方面量化了壁流效应的影响。应用线性回归得到单相流和气液逆流时计算Pe_d的关联式。对于新型填料及塔内件的开发、改进隔壁塔的设计方法,从而实现安全有效放大具有参考意义。