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。     

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。     

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。     

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%。     

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.     

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。     

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%。     

间歇萃取精馏分离碳酸二甲酯与甲醇恒沸物

采用过程模拟与实验结合的方法,选用碳酸乙烯酯作萃取剂,采取间歇萃取精馏的方法研究回流比、萃取剂进料温度等对分离甲醇-碳酸二甲酯恒沸物的影响.结果表明,模拟结果与实验结果相比,优化了最佳操作条件.萃取精馏段回流比为0.8～1.2;最佳溶剂进料温度为64.5℃,溶剂进料量与共沸物的最佳摩尔比在1.85～1.95.优化的结果可以为工业放大研究提供基础,指导实验的进一步操作.     

间歇萃取精馏分离环己烷-正丙醇的研究

首次研究了间歇萃取精馏方法分离环己烷-正丙醇二元共沸物。通过溶剂选择原理选出DMF作为分离此共沸物系的溶剂,采用UNIFAC模型对常压下环己烷-正丙醇物系和加入溶剂DMF后的物系进行气液平衡模拟,并进行了实验验证,其中模拟结果与实验数据吻合较好。通过间歇萃取精馏分离此共沸物的实验研究来进一步考察所选萃取剂的效果。结果表明,DMF能够消除环己烷-正丙醇共沸物系的共沸点,采用有30块理论板的填料塔,萃取剂进料位置为第4块板,溶剂质量比为1∶1,回流比为3∶1时,塔顶环己烷产品质量分数为96.2%,回收率为72.2%。     

带有中间贮罐间歇萃取精馏实验研究

使用一个带有中间贮罐的间歇萃取精馏实验装置,以能形成最低共沸物的乙酸乙酯-乙醇体系为分离对象,选用N,N-二甲基甲酰胺(DMF)为萃取剂,实验研究了中间贮罐持液量、中间贮罐持液温度、萃取剂加入速率等操作参数对分离过程的影响。实验结果表明:随着萃取剂流率的增加,中间贮罐持液量也相应增加,组分更易于分离;随着中间贮罐持液量的增加,中间贮罐持液温度也相应升高,且存在最佳分离持液温度;萃取剂流率对分离结果的影响最大,中间贮罐持液温度对分离结果的影响次之,中间贮罐持液量对分离结果的影响最小。     

New double column system for heteroazeotropic batch distillation

A new double column system (DCS) operated in closed mode is suggested for heterogeneous batch distillation. This configuration is investigated by feasibility studies based on the assumption of maximal separation and is compared with the traditional batch rectifier (BR). We study the configurations also by dynamic simulation based on a detailed model using a professional simulator. For the new configuration the minimal duration of the process is determined. The influence of the most important operational parameters is studied. The calculations and the simulations are performed for a binary (n-butanol–water) and for a ternary heteroazeotropic mixture (isopropanol–water + benzene as entrainer). One of the advantages of the DCS is that distillation of binary and ternary systems is performed in only one step. Furthermore the recovery of components is usually higher and the amount of byproducts is lower.     

Cyclic total reflux batch distillation with two reflux drums

The present work proposes a novel cyclic total reflux (CTR) operation of batch distillation with two reflux drums working alternatively. A mathematical model is set up for the process. The computational comparison of the novel policy with the regular constant reflux and non-cyclic total reflux (NCTR) operations is also presented. The experimental runs of the new mode show that it can be operated and controlled more easily. The novel operation is significantly time saving compared to the mode of regular constant reflux theoretically and experimentally. The two reflux drum mode of CTR is also suitable for the separation of the mixture containing a large amount of light component.     

萃取精馏分离环氧丙烷与甲醇混合物的模拟与优化

使用AspenPlus软件对HPPO法生产环氧丙烷新工艺中环氧丙烷的分离提纯进行了模拟计算,并使用灵敏度分析优化了水作为萃取剂进行萃取精馏的工艺条件。结果表明萃取剂用量在14 kg/h左右,质量回流比为8,萃取剂和原料进料位置分别在第10块和第35块塔板时,分离效果最好。     

旋转填料床间歇萃取精馏性能研究

为了寻找强化间歇萃取精馏过程的有效途径,在装填2mm×2mm三角形螺旋填料的旋转床中,以乙醇-水为实验物系,乙二醇为萃取剂,通过考察馏出液组成随时间的变化情况,产品的纯度和回收率随转速、回流比和溶剂比的变化情况,研究了旋转填料床间歇萃取精馏的性能。结果表明,旋转填料床中强大的离心力和高效填料的协同作用极大地强化了间歇萃取精馏过程,具有分离效果好、操作时间短、节能、小设备大生产能力等突出优点;存在最佳转速使产品的纯度和回收率最大;增加溶剂比和回流比均能使产品的纯度和回收率得到提高,但增加溶剂比的效果更显著。旋转填料床是强化间歇萃取精馏过程的有效途径。