FIBONACCI SEARCH FOR OPTIMAL FEED LOCATION

A Fibonacci search technique is used in conjunction with a rigorous mullicomponenl distillaiion computer module to find the optimal feed location within a section of a distillation column. The function lo be minimized can be one of the following:

*key component ratio difference

*reflux ratio or reboiler ratio

*condenser duty or reboiler duty

This technique has been used successfully in the relocation of feed stages of many existing distillation columns and thus saved energy consumption. We shall describe this technique with a sample problem.     

Synthesis of High‐Purity Methylal via Extractive Catalytic Distillation

An integrated continuous process, which combines catalytic distillation and extractive distillation in one column, is investigated for the synthesis of high‐purity methylal from methanol and formalin in the presence of a cation‐exchange resin catalyst. A feed with methanol:formaldehyde 2:1 molar ratio is chosen to evaluate the effects of operating parameters, such as extractant feeding position, ratio of extractant to feed, reflux ratio, and reboiler temperature, on the continuous synthesis of methylal. Under the optimum operating conditions and with water as extractant, the extractive catalytic distillation process operated continuously, producing a methylal purity of 98.7 % (H₂O: < 1.30 %) with 98.0 % formaldehyde conversion.     

Analysis of Ternary Distillation Column Sequences

Abstract

Eight complex distillation column configurations for a ternary feed mixture are modeled and studied. A modified complex method is used to minimize the cost of the configurations. Optimum regions for each configuration depending on the feed composition are derived. The result provides guidelines for the synthesis of distillation column configurations.     

Reactive distillation for biodiesel production from soybean oil

Biodiesel, which is regarded as a promising alternative to a conventional petroleum-based diesel fuel, can be produced from transesterification of vegetable oils and alcohol in conventional batch and continuous reactors. Since the transesterification is an equilibrium-limited reaction, a large excess of reactants is usually used to increase the production of biodiesel, thereby requiring more expensive separation of unreacted raw materials. This study proposed the use of a reactive distillation for transesterification of soybean oil and methanol catalyzed by sodium hydroxide to produce biodiesel. The simulation results showed that a suitable configuration of the reactive distillation column consists of three reactive stages. The optimal conditions for the reactive distillation operation are at the molar feed ratio of methanol and oil at 4.5: 1, reflux ratio of 3, and reboiler duty of 1.6×10⁷ kJ h⁻¹. Methanol and soybean oil should be fed into the column at the first stage. The effect of important operating and design parameters on the performance of reactive distillation was also presented.     

2,3-丁二醇分离纯化中反应精馏的实验和模拟

对反应萃取-水解精馏法分离发酵液中2,3-丁二醇工艺中的水解精馏进行了实验和模拟研究。实验验证了4,5-二甲基-2-丙基-1,3-二氧戊环(DPD)水解精馏得到2,3-丁二醇的可行性。采用Aspen Plus建立反应精馏模型,以UNIFAC为热力学方程,RadFrac为反应精馏模块,对常压下DPD的水解精馏进行模拟,模拟结果与实验结果吻合较好。以2,3-丁二醇的收率为主要优化目标,考察最佳塔板数、进料位置、进料比、回流比和塔顶馏出比。模拟结果表明,在最佳操作条件下,塔釜2,3-丁二醇的收率为0.981,摩尔分率为0.150。     

Separation of Ethylbenzene from Mixed Xylenes by Continuous Adsorptive Processing

Abstract

Separation of ethylbenzene at high purity from its mixtures with xylenes has been accomplished commercially by superfractionation. Because of the low relative volatility (1.05) between ethylbenzene and para-xylene, this operation is difficult and energy-intensive, requiring the use of several hundred fractionation trays at a reflux/feed ratio of about 18.

To improve economics and reduce energy usage, a process has been developed to accomplish this separation by selective adsorption from the liquid phase onto a solid adsorbent. In this operation, ethylbenzene is separated from the mixed xylenes within the adsorbent bed, and the two products are recovered from the adsorbent by displacement with a liquid of different boiling point, referred to as desorbent. Desorbent is recovered from the net products by distillation and is recycled.

Results of liquid chromatographic tests used to screen various adsorbents are presented. Adsorbents have been developed that show a higher separation factor than the 1.05 existing in distillation, with ethylbenzene being the least strongly adsorbed component.

The process has been demonstrated by operation of a pilot plant in which a simulated moving-bed technique is used to obtain the process characteristics of continuous countercurrent flow of adsorbent and process fluid, without actual movement of solids. Results of these operations are presented.

The adsorptive process requires less than half of the energy input required by superfractionation. An economic comparison of the two operations is presented.     

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。     

Transesterification of palm oil with methanol in a reactive distillation column

The higher feedstock and processing costs for biodiesel production can be reduced by applying reactive distillation (RD) in transesterification process. The effects of reboiler temperature, amount of KOH catalyst, methanol to oil molar ratio and residence time on the methyl ester purity were determined by using a simple laboratory-scale RD packed column. The results indicated that from the empty column, the system reached the steady state in 8 h. Too high reboiler temperature and the amount of catalyst introduce more soap from saponification in the process. The optimal operating condition is at a reboiler temperature 90 °C, a methanol to oil molar ratio of 4.5:1.0, KOH of 1 wt.% respect to oil and 5 min of residence time in the column. This condition requires the fresh feed methanol 25% lower than in the conventional process and produces 92.27% methyl ester purity. Therefore this RD column can be applied in small or medium biodiesel enterprise.     

The Role of Recycle in Countercurrent Recycle Distillation Cascades. I. Constant Reflux,Ideal, and Squared-Off Cascades

Abstract

In most textbooks concerned with countercurrent multistage separations, minimum reflux ratio for continuous distillation is usually defined only in terms of a graphical construction on a McCabe—Thiele diagram: it is the recycle ratio (liquid flow rate) associated with the operating line that touches the equilibrium curve at the feed point. However, it is easily shown that minimum recycle ratio depends on local α and composition, as well as product compositions, and thus, it is a stage-composition phenomenon. As a result, for a specified separation, each ideal stage in a continuous distillation cascade has a specific minimum recycle ratio associated with it. For constant α, the minimum recycle ratio increases as the stage compositions depart more from product (distillate or bottoms) compositions. As a result, the textbooks only consider the maximum minimum recycle ratio. This paper presents the results of some theoretical calculations which illustrate how minimum recycle ratio varies with stage α, stage and product compositions, and presents an example of distillation cascade behavior when minimum recycle ratio is approached at a composition other than the feed point. An example is also presented which shows how the separation is effected when the reflux ratio is reduced below the design value in a distillation column containing a fixed number of ideal stages. A brief comparison is also made between constant reflux, ideal, and squared-off cascades in terms of number of stages, total interstage flow, and relative energy requirements for the different designs to illustrate and emphasize the consequences of the stagewise behavior of minimum recycle ratio.     

间歇减压精馏分离2-甲基吡啶/2-羟乙基吡啶

采用间歇减压精馏法实现了2-甲基吡啶和2-羟乙基吡啶这一热敏性混合物的分离,并考察了投料组成与操作压力对减压精馏过程的影响。结果表明,高真空条件降低了塔釜温度从而避免了物料在塔釜中受热变性,对于热敏物料2-羟乙基吡啶,减压精馏过程中压力应控制在4325 Pa以下,此时塔釜产品2-羟乙基吡啶的质量分数均能大于97%,同时收率能保持在86%以上。在压力为1325 Pa时,不同投料组成下塔顶产品2-甲基吡啶的质量分数和塔釜产品2-羟乙基吡啶的质量分数均高于98%,两者的收率也均在85%以上,能够很好地满足工业生产要求。     

萃取精馏分离苯/环己烷共沸体系的控制策略

将常规萃取精馏、差压热耦合萃取精馏以及隔壁塔萃取精馏技术应用于以糠醛为萃取剂的苯和环己烷共沸物分离过程。在稳态模型的基础上,利用Aspen Dynamics软件进行控制研究,对三工艺流程提出了若干控制策略。结果表明,对于常规萃取精馏过程,再沸器热负荷与进料量比值控制结构在降低控制过程超调量方面表现出明显优势;对于差压热耦合萃取精馏过程,带有压力-补偿控温策略的方案控制效果更佳;而对于隔壁塔,则选择了无隔板下方气液分离比控制的结构来作为较优的控制策略。     

Retrofit of Distillation Columns Using Thermodynamic Analysis

Abstract

Thermodynamic analysis provides the column grand composite curves and exergy loss profiles, which are becoming readily available for a converged distillation column simulation. For example, the Aspen Plus simulator performs the thermodynamic analysis through its Column–Targeting tool for rigorous column calculations. This study uses the column grand composite curves and the exergy loss profiles obtained from Aspen Plus to assess the performance of the existing distillation columns, and reduce the costs of operation by appropriate retrofits in a methanol plant. Effectiveness of the retrofits is also assessed by means of thermodynamics and economics. The methanol plant utilizes two distillation columns to purify the methanol in its separation Section. The first column operates with 51 stages, has a side heat stream to the last stage, a partial condenser at the top and a side condenser at stage 2, and no reboiler. The second column operates with 95 stages, has a side heat stream to stage 95, a total condenser, and high reflux ratio. Despite the heat integration of the columns with the other Sections and a side condenser in column 1, the assessment of converged base case simulations have indicated the need for more profitable operations, and the required retrofits are suggested. For the first column, the retrofits consisting of a feed preheating and a second side condenser at stage 4 have reduced the total exergy loss by 21.5%. For the second column, the retrofits of two side reboilers at stages 87 and 92 have reduced the total exergy loss by 41.3%. After the retrofits, the thermodynamic efficiency has increased to 55.4% from 50.6% for the first column, while it has increased to 6.7% from 4.0% for the second. The suggested retrofits have reduced the exergy losses and hence the cost of energy considerably, and proved to be more profitable despite the fixed capital costs of retrofits for the distillation columns of the methanol plant.     

Modeling of Fixed Adsorptive Distillation in Batch Operation

Abstract

This paper presents the modeling of fixed adsorptive distillation in batch operation. A combination of theoretical and empirical approaches is used to derive the model with the following procedures:

• (i)?modeling through each sub‐unit based on ideal concepts and assumptions,

• (ii)?addition of empirical correction factors into the model to eliminate assumptions.

The model is designated to predict the model parameter, which is the composition of the second column product, as a function of three process variables (i.e. time, feed composition, and flow ratio). It is found that the two above–mentioned approaches result in a representative model with an average error percentage of 5.46%.     

Vapor Permeate Characteristics of Membrane Distillation

Abstract

To study the permeate characteristics of membrane distillation considering heat and mass transfers and concentration polarization, theoretical and experimental studies were performed. To understand the effect of concentration polarization, concentrated solutions of LiBr and H₂SO₄ were used as feed. The permeate flux was found to be proportional to the vapor pressure difference between the feed and cooled surface and decreased with increasing concentration because of the concentration and temperature polarization. Furthermore, when considering the heat and mass transfers and concentration polarization, the permeate flux could be estimated accurately.     

Effect of Changes in Operating Variables on Stage-wise and Cumulative Separation in Binary Multistage Distillation

Abstract

The progressive separation that occurs stage-wise within a multistage distillation column is characterized by the cumulative extent of separation, ζ _N ; while the contribution of individual stages, δ _N , to the overall separation is given by the difference between ζ _N for successive stages. These indexes permit the “goodness” of separation for individual stages and for the entire column to be compared on an equivalent basis. This paper examines the effects of changing operating variables of reflux ratio, feed rate, feed composition, and feed stage location on the separation obtained in a distillation column containing a fixed number of ideal stages, and how the single-stage contribution changes when these variables are altered from the design value. The calculations show that the reflux ratio (R) is probably the most important variable in determining how well a column makes a separation. Separation declines rapidly as R is reduced below the design value, as the feed rate is increased at constant boil-up rate, and as the feed concentration drops below the design value. Changing the feed stage location of ±5 stages in a 50-stage column has a minimal effect on separation at all feed compositions. δ _N clearly shows how the contribution of individual stages changes when operating variables are varied from the design values.     

Facilitated Transport Membrane Hybrid Systems for Olefin Purification

Abstract

A new membrane system has been developed by BP for refinery and chemical plant olefin purification and recovery. This facilitated transport system, coupled with distillation, offers lower capital and operating costs than conventional distillation alone. Initial results on lab scale hollow fiber devices indicate membrane flux ranging from 8.75×10^?6 to 8×10^?5 m³/m²/sec (2.5 to 23 scfd/ft²) and selectivities from 150 to 300. Pilot plant experiments on propylene/propane and ethylene purge gas recovery over three to six months duration show membrane stability and product purity of 98.5% or greater using refinery grade propylene feed. Hybrid system optimization data for membranes and distillation indicate that using a side draw from the distillation tower provides advantages in terms of membrane area, purity of feed to the membrane, and low per-pass recovery coupled with high overall propylene recovery. Membrane performance data under various conditions will also be presented. In addition to performance data, economic evaluation and energy savings will be discussed.     

Undergraduate design of experiment laboratory on analysis and optimization of distillation column

A two-level full factorial design and/or a central composite design are used to optimize the operation of a distillation column by manipulating three variables: the feed flow rate, the reflux ratio and the steam flow to the reboiler. The response variable of interest is a profit function where the objective of this experiment is to examine the effect of each of the three factors and their interactions on this profit function. This is accomplished in a sieve tray type continuous distillation column operated at ambient pressure to separate a methanol–isopropanol mixture. Students were asked to determine the significant variables and the optimal operating conditions for steam rate, reflux ratio and feed rate such that the profit is maximized. As a result, this experiment not only exposes students to an industrially relevant unit operation but it also helps complement the classroom teaching on design of experiment concepts.     

Design and Control of Extraction Distillation for Dehydration of Tetrahydrofuran

Design and control of an extractive distillation system for tetrahydrofuran (THF) dehydration with ethylene glycol as entrainer is investigated. The main module is a two‐column system containing an extractive distillation column, whose top stream is the desired product THF, and an entrainer recovery column. Economic analysis with total annual cost as the objective function is developed. Two kinds of control strategies are explored for THF dehydration. The responses reveal that the control structure with fixed reflux ratio cannot maintain the bottom liquid level of the entrainer recovery column, while the control scheme with fixed reboiler heat duty/feed flow ratio exhibits good control performance in spite of large deviations in feed flow rate and feed composition.     

Recovery of Chloroform from Effluent with Solvent Extraction–Distillation Process

Abstract

A solvent extraction–distillation process for recovery of chloroform in aqueous effluent was developed. Sutfonated kerosene was used for extraction of chloroform. When the flow ratio of organic phase to aqueous phase is 0.1, the chloroform concentration in the aqueous effluent can be decreased from 10 g/L to about 100 mg/L by 3-stage countercurrent extraction. The distribution ratio of chloroform between sulfonated kerosene and water is about 50. Sodium sulfate in the aqueous effluent will enhance the distribution. A small amount of water was added to the distillation column for stripping chloroform in sulfonated kerosene. RPC was used as a commercial extractor. Scale-up from the data of the pilot test was based on the Karr correlation. Recovery of chloroform was over 90%, and residual kerosene in the aqueous effluent from the extraction was lower than 70 mg/L. It is expected that the technique can be used for the recovery of other organic solvents miscible with kerosene.     

Production of Motor Fuel Grade Alcohol by Concentration Swing Adsorption

Abstract

A new cyclic process concept called “concentration swing adsorption” for separation of bulk binary liquid mixtures is described. The process carries out the primary separation by selective liquid-phase adsorption of one of the components of the feed mixture on an adsorbent. The adsorbed component is then desorbed by a desorbent liquid which is equally or more strongly adsorbed than the slectively adsorbed component of the feed mixture. The desorbent liquid is removed from the adsorbent by displacing it with the less strongly adsorbed component of the feed mixture so that the adsorbent can be resused. The process also includes a complementary step where the adsorbent is rinsed with the more strongly adsorbed component of the feed mixture so that two essentially pure products are produced from the feed mixture with high recoveries of both components. At least one simple distillation is also required by the process which separates the desorbent liquid from the less strongly adsorbed component of the feed mixture. The process can be used to separate liquid mixtures with close boiling components or azeotropic mixtures which require energy intensive distillation. A very efficient separation can be achieved in these cases by spending only a fraction of the distillation energy. An example of such an application, viz., separation of a bulk ethanol–water mixture for motor fuel grade alcohol production, is described. A local equilibrium model of the process is used to evaluate the performance of the process for that separation using an activated carbon as the adsorbent and acetone as the desorbent liquid. Experimentally measured equilibrium adsorption characteristics for ethanol–water, acetone–water, and acetone–ethanol binary liquid mixtures on the carbon as well as adsorption column dynamics for the steps of the process are reported.