间歇萃取精馏操作过程的实验研究

采用复合式精馏塔实现了萃取精馏的间歇操作,塔顶产品物质的量分数达95%以上。以取得合格产品的量与时间之比作为目标函数,研究了回流比R、中间回流量Vm(中间罐向提馏段进料流量)、萃取剂用量S对萃取精馏过程的影响,在R=5～10,Vm=3.2～7.2mL/min,S=1.2～2.2mL/min范围内,随以上操作参数的增大,目标函数均呈先增大后减小的趋势。     

间歇萃取精馏过程模拟计算

提出了一种可用于间歇萃取精馏过程模拟计算的快捷模型－准稳态模型，并对该方法的数学模型进行了推导。用此方法对间歇萃取精馏过程中塔顶、塔釜浓度，各塔板温度随时间的变化进行模拟，其结果与实验值吻合较好。它具有计算精度高、计算速度快等优点。     

拟稳态模型用于间歇萃取精馏的数值模拟

Batch extractive distillation (BED) is a special method used in the distillation process by adding a solvent into the batch distillation column to alter the relative volatility of the components and improve the separation. A comprehensive design and simulation method is required due to the complexity of BED. In this study, a quasi-steady-state model for BED is proposed, the derivation and solution of the model are presented. This shortcut model can be used to simulate the composition and temperature of the reboiler, the top and other plates of the column in a batch extractive distillation operation. The calculated values are in good agreement with the experi-mental data. The results show that the quasi-steady-state model is a practical method because of some advantages such as high precision and fast calculation.     

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.     

分隔壁萃取精馏塔分离醋酸水溶液的模拟

提出了一种新的单塔萃取精馏精制醋酸水溶液的新工艺,该工艺采用分隔壁萃取精馏塔(DWC-E)替代常规萃取精馏流程的萃取精馏塔及溶剂回收塔,不仅节省了设备投资,而且降低了总能耗。利用Aspen Plus模拟软件,对DWC-E塔及常规萃取流程进行了模拟。DWC-E塔的操作条件:塔板数40块,侧线精馏段的板数10块,回流比2,溶剂摩尔比2.5,在此条件下,比较了常规萃取精馏流程与分隔壁精馏塔内温度、液相组成及汽液相流量的变化。结果表明,DWC-E塔比常规的2塔萃取精馏流程节能23.91%。     

带有中间储罐的间歇萃取精馏的模拟研究

本文提出了带有中间储罐塔间歇萃取精馏过程计算模型,将中间罐看成一块理论板,萃取剂看成第三组份进行建模,利用调节因子和泡点法相结合对整个塔进行迭代计算,经实例模拟表明,本模型只需较简单的赋初值,能以较快的速度收敛,本模型对带有中间储罐间歇萃取精馏操作及模拟具有一定的指导作用。     

Enhanced separation of highly non-ideal mixtures with extractive heterogeneous-azeotropic distillation

The distillation based separation can be extremely complex if highly non-ideal mixtures are to be separated. In spite of different successfully applied unit operations there is still a possible way to improve the distillation technique and widen its toolbar. A new improvement in this area is the development of the extractive heterogeneous-azeotropic distillation (EHAD). This unit operation includes the merits of extractive- and heterogeneous-azeotropic distillations in one unit without extra material addition. Our work supports EHAD features with successful experiments compared with modelling and comparison with other separation structures proving that the application of EHAD makes the separation of extremely non-ideal mixtures possible on an easy, powerful, energy saving, and cost efficient way.     

萃取精馏法分离乙二胺和H_2O的共沸物

研究了萃取精馏工艺对乙二胺和水共沸物的分离。通过Aspen Plus模拟计算了水对乙二胺(EDA)的相对挥发度,以此建立了一种快速筛选萃取剂的方法,确定最佳萃取剂为1,4-丁二醇。以1,4-丁二醇为萃取剂,选用Aspen Plus中的RadFrac严格精馏模型,进一步对萃取工艺操作参数进行了模拟优化,确定了脱水塔及EDA精制塔的最佳操作条件,即脱水塔理论塔板数为27,原料进料位置为第7块理论板,萃取剂进料位置为第3块理论板,萃取剂用量为300 kg/h,回流比为0.5;EDA精制塔理论板数为29,回流比1.5,进料位置在第5块理论板。在最优工艺条件下,水的理论纯度(质量分数)可达99.90%,EDA纯度大于99.90%,回收1,4-丁二醇纯度大于99.90%;对1,4-丁二醇的萃取效果进行了实验验证,水纯度达到99.99%,EDA纯度达到99.92%,实际萃取结果与模拟结果相当。     

萃取精馏分离四氢呋喃-乙醇共沸物系

首先根据汽液平衡实验数据采用UNIFAC法进行VLE关联。然后通过定性判断、基团贡献法定量估算选择该二元物系的合适萃取剂为乙二醇。通过气液平衡实验对萃取剂的有效性进行验证．比较了不同溶剂比对四氢呋喃,乙醇相对挥发度的影响,当溶剂比为3时,相对挥发度为2．26。最后进行精馏实验验证过程的可行性。     

萃取精馏分离碳酸二甲酯-乙醇二元共沸物

测定了101.3 kPa下乙醇-碳酸二甲酯（DMC）和DMC-糠醛二元体系的汽液平衡数据,以及乙醇-DMC-糠醛体系在溶剂比为1∶1时的三元汽液平衡数据。结果表明,糠醛的加入可以改变乙醇和DMC的相对挥发度,并且当糠醛的摩尔分数大于0.25时,乙醇-DMC二元物系的共沸点消失。因此,可以采用萃取精馏的方法以糠醛为溶剂分离乙醇和DMC的混合物。采用Aspen Plus软件对连续萃取精馏分离乙醇-DMC共沸物的过程进行了模拟。结果表明,单塔带侧线采出的操作方式比双塔操作方式更有优势。     

间歇萃取精馏制备高纯甲醇模拟与实验研究

针对工业甲醇制备高纯甲醇的间歇萃取精馏过程,建立了准稳态模型,采用Newton迭代法进行求解。模拟分析了影响高纯甲醇收率的溶剂流率、溶剂加入位置、回流比等因素,并通过实验验证了模型的准确性和可靠性。在实验与模拟计算的基础上,确定了工业甲醇制备高纯甲醇的最佳工艺条件:总理论板数35,萃取剂二甲基亚砜在第10块理论板加入,萃取剂与原料甲醇的体积比0.3,前馏分段回流比8,产品段回流比5,此时,高纯甲醇单程收率可达60%。     

双溶剂进口的双釜间歇萃取精馏

提出了带有塔底回收釜及双溶剂进口的间歇萃取精馏操作方式。在新操作方式中,塔内回流液不流回塔釜,而是流入塔底回收釜,再经简单蒸馏气相返回塔釜,回收后的溶剂返回精馏塔中。以乙二醇作溶剂分离乙醇-水物系的实验结果表明,当间歇操作次数为2时,产品采出率最大,单位产品消耗的新鲜溶剂量最少。新操作方式具有塔釜温度变化平稳,新鲜溶剂用量相对较少等优点。     

分批萃取精馏回收无水乙醇的新工艺

针对分批萃取精馏法回收无水乙醇原有工艺流程中存在的问题,提出了优化方案。在原有流程的基础上,添加了一个溶剂回收釜,塔的下段液相流体直接流入溶剂回收釜。结果使得塔釜的温度变化降低,加热容易控制,操作时间变短。此方案对分批萃取精馏法回收无水乙醇的工艺改造有参考价值。     

Batch extractive distillation as a hybrid process: separation of minimum boiling azeotropes

The batch extractive distillation is compared with the hybrid process (absorption+distillation) by feasibility studies and rigorous simulation. A new method is presented for the assessment of feasibility of the hybrid batch extractive distillation. The limiting values of the operational parameters are determined. Calculations are presented for the separation of the minimum boiling azeotropic mixtures of acetone-methanol and ethanol-water by the application of water and ethylene glycol as heavy solvents, respectively.     

A note on the identification and control of batch distillation columns

A method for the identification and control of a batch distillation process is presented in this note. The proposed model consists of a first-order integrating process in composition with a high-frequency gain. The feedback controller is designed in the framework of robust nonlinear control with modeling error compensation techniques for the control of distillate composition via manipulations of the reflux ratio. The proposed identification and control procedures are illustrated via numerical simulations.     

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.     

加盐萃取精馏法制无水异丙醇过程模拟

对加盐萃取精馏法制备无水异丙醇过程进行了模拟计算,采用有序双液程(NRTL)模型对异丙醇-水-乙二醇-醋酸钾体系异丙醇-水气液平衡数据进行了回归,得到了该条件下的NRTL交互作用参数,在此基础上采用Aspen软件进行模拟计算;对理论塔板数、回流比(质量比)与进料位置进行了优化,模拟结果与现场数据吻合较好,说明采用的方法适用于加盐萃取精馏过程的模拟。     

萃取精馏分离三甲氧基硅烷和甲醇的模拟和优化

运用Aspen Plus对萃取精馏分离三甲氧基硅烷和甲醇进行了模拟研究。采用芳烃作溶剂,通过和传统的对二甲苯溶剂对比,发现异丙苯和均三甲苯作溶剂具有很好的节能效果,且均三甲苯效果十分显著。在均三甲苯作溶剂的基础上,分析了溶剂比、塔板数、进料位置、回流比等条件对分离效果的影响,并对参数进行优化。确定了最优的操作条件为萃取精馏塔共24块理论板,混合物进料位置为第15块塔板,溶剂进料位置为第11块板,溶剂比为0.4,回流比为0.6。溶剂回收塔共12块理论板,进料位置为第5块塔板,回流比为2.3。在此条件下,三甲氧基硅烷和甲醇的产品的质量分数均能达到99.6%。     

四氢呋喃-乙醇变压精馏分离

共沸混合物分离是化工过程中常见的分离难题。变压精馏是根据物系压力改变而使液体混合物共沸点组成发生变化,进而使共沸物系得以分离的一种有效分离方法。在热力学分析基础上,提出了四氢呋喃-乙醇液体混合物变压精馏分离双塔工艺流程。以NRTL-RK为物性计算方法,利用Aspen Plus模拟软件对变压精馏分离工艺过程进行分析及模拟,并对工艺参数进行优化。研究结果表明:在常压塔和0.8 MPa高压塔组成的双塔流程中变压精馏可将四氢呋喃-乙醇最低共沸混合物进行较好的分离。