Strategies for Starting Up Azeotropic Distillation Columns with Multiple Steady States

The operability of azeotropic distillation columns with multiplicity is analysed during start‐up by dynamic simulation. Different steady states can be reached by applying different start‐up configurations and/or policies. The well‐known benzene‐heptane‐acetone (BHA) system is studied. The process by which the column reaches these steady states can be seen through the examination of profile evolutions corresponding to the given start‐up policies. Indeed, a clear partition of the start‐up policies space yielding different solutions is achieved. Some properties of this space are explained and start‐up critical values can be identified. Finally, some guidelines for start‐up supervision are outlined for the study case.     

Analysis of the Start‐up Process for Reactive Distillation

The start‐up procedure of a distillation column is a time‐ and energy‐consuming process. Further, the products during the start‐up time are off specification and cannot easily be recycled as for conventional distillation but must costly be disposed of. In this paper, a process model to simulate the barely analyzed start‐up procedure for a reactive distillation from the cold and empty state to steady state is presented. The start‐up of a reactive distillation column has been modeled with gPROMS. The advantage of a cold and empty start‐up is the consistent and reproducible initialization. Commercial simulators do not give the opportunity to start form a cold and empty state, e.g., a column modeled with Hysys must be shut down from a steady state to be able to model the complete start‐up process, which is not possible, for example, for a batch process. Also, a change in the describing equations and discontinuities in process variables is difficult to handle within the simulation. In this paper, the start‐up strategies normally used for distillation without reaction are examined and applied to reactive distillation. It will be shown that the widely used strategy of total reflux is not suitable for reactive distillation. A simplified model to derive a time constant which describes the influence of parameter setting changes, like heating power, reflux ratio and feed composition on the start‐up time, is introduced and validated.     

Dynamic analysis and open‐loop start‐up of an integrated radiant syngas cooler and steam methane reformer

The transient performance of an integrated radiant syngas cooler (RSC) of an entrained‐bed gasifier and steam methane reformer (SMR) is investigated. Base‐case designs using either co‐current or counter‐current configurations are subjected to operating transients to evaluate the feasibility to transition to new steady states. Each system, under open loop, is subjected to changes in key variables of the SMR feed on the tube side and disturbances to variables of the coal‐derived syngas on the RSC side to determine the dynamics and stability of the integrated system. The results indicate that the co‐current configuration is flexible to move to new operating steady states and more safe than the counter‐current configuration, although it provides less cooling and has poorer methane conversion. The variables likely to violate the design limit in the event of a disturbance are identified. A start‐up procedure is also established based on industrial practices employed for entrained‐bed gasifiers and methane reformers. © 2016 American Institute of Chemical Engineers AIChE J, 63: 1602–1619, 2017     

Effects of Liquid Holdup in Condensers on the Start‐Up of Reactive Distillation Columns

Compared with start‐ups in conventional distillation columns, those in reactive distillation (RD) columns are much more time and energy consuming, and generate a large amount of by‐products which are not easy to deal with together. For several years, researchers have been trying out different methods to shorten the time required to lower the cost of the start‐up. In this work, a rigorous dynamic model in the ChemCAD simulator is applied to model the start‐up process for the esterification of ethyl acetate in a reactive distillation column. In the model, two sets of equations are employed: one for the fill‐up and heating stage and the other for the equilibration process which follows. In the fill‐up and heating stage, fluctuation curves of the reboiler temperatures with respect to time which are similar to those for conventional distillation columns are observed, while in the equilibration process it is found that the increase of the liquid holdup volume in the condenser reduces the time required to reach steady state for the reactive column and decreases the liquid holdup volume in the reboiler at the equilibrium state. This shows that the liquid holdup volume in the condenser has an important effect on the start‐up of reactive distillation columns.     

Heterogen katalysierte Reaktivdestillation: Design und Scale‐up am Beispiel von Methylacetat

Reactive Distillation by Heterogeneous Catalysis: Design and Scale‐up Using Methyl Acetate as an Example Methyl acetate synthesis and hydrolysis is used to exemplify the design and scale‐up of heterogeneously catalyzed reactive distillations using Katapak‐S/‐SP. Different equilibrium and non‐equilibrium stage models and a rate‐based model are compared in order to clarify the level of complexity needed to predict the process behavior. An equilibrium stage model accounting for reaction kinetics is the best choice for methyl acetate reactive distillation. Reliable information on fluid dynamics of the used reactive distillation packing is needed for the fluid dynamic design in order to assure a wide operation range of the reactive distillation column. To verify the process model, experiments on the synthesis of methyl acetate have been performed in columns with different diameters. As a case study, the model‐based scale‐up is described for an industrial methyl acetate hydrolysis process.     

Impact of mass transfer coefficient correlations on prediction of reactive distillation column behaviour

A significant part of the safety analysis of a reactive distillation column is the identification of multiple steady states and their stability. A reliable prediction of multiple steady states in a reactive distillation column is influenced by the selection of an adequate mathematical model.For modelling reactive distillation columns, equilibrium (EQ) and nonequilibrium (NEQ) models are available in the literature. The accuracy of the nonequilibrium stage model seems to be limited mainly by the accuracy of the correlations used to estimate the mass transfer coefficient and interfacial area.The binary mass transfer coefficients obtained from empirical correlations are functions of the tray design and layout, or of the packing type and size, as well as of the operational conditions and physical properties of the vapour and liquid mixtures.In this contribution, the nonequilibrium model was used for the simulation of a reactive distillation column. For prediction of the binary mass transfer coefficient for a sieve tray, four correlations were chosen to show their impact on the prediction of the reactive distillation column behaviour. As a model reactive distillation system, the synthesis of methyl tertiary-butyl ether (MTBE) was chosen. The steady-state analysis and the dynamic simulation of the model system were done. Qualitative differences between the steady states were predicted using the chosen correlations.     

Experimental investigation of column efficiency for two ternary systems in a three‐phase packed distillation column

In this work, the effect of vapor load and initial feed concentrations on column efficiency and liquid hold‐up in a two‐ and three‐phase packed distillation column at total reflux was investigated. Results for the two investigated mixtures (n‐heptane, n‐hexane, water) and (ethyl acetate, 1‐butanol, water) reveal that column efficiency remains almost constant for the former mixture but changes significantly for the latter. Specific liquid hold‐up and water to organic‐phase volumetric ratio within the column affect the column efficiency due to variations in initial feed concentrations. Influence of vapor load on separation efficiency and specific liquid hold‐up is also studied.     

Packed‐bed reactor for short time gas phase olefin polymerization: Heat transfer study and reactor optimization

A specially conceived packed‐bed stopped flow minireactor (3 mL) suitable for short gas phase catalytic reactions has been used to study the start‐up of ethylene homopolymerization with a supported metallocene catalyst. Focus has been put on the heat transfer characteristics of the supported catalysts and on understanding the relationship between the initial rate and the relative gas/particle velocities and the influence of particle parameters in the packed bed. We performed a comprehensive study on the influence of various physical parameters on the heat transfer regime at start up conditions. The catalyst activity as well as the polymer morphology is shown to be dependent on heat transfer regime. The knowledge thus obtained is applicable to industrial problems like catalyst injection in fluidized beds and helps preventing experimental artifacts due to overheating in following studies. © 2011 American Institute of Chemical Engineers AIChE J, 2012     

Design and Control Comparison of Alternative Separation Methods for n‐Heptane/Isobutanol

The binary mixture of n‐heptane and isobutanol forms an azeotrope at atmospheric pressure, with a composition of 66.9 mol % n‐heptane and a temperature of 364 K. Several methods of separation are possible. This study compares the steady‐state economics and the dynamic controllability of three alternative separation techniques: a two‐column extractive distillation process, a two‐column pressure‐swing distillation process, and a single column with a refrigerated condenser.     

Effects of cationic polymer on start‐up and granulation in upflow anaerobic sludge blanket reactors

The upflow anaerobic sludge blanket (UASB) has been used successfully to treat a variety of industrial wastewaters. It offers a high degree of organics removal, low sludge production and low energy consumption, along with energy production in the form of biogas. However, two major drawbacks are its long start‐up period and deficiency of active biogranules for proper functioning of the process. In this study, the influence of a coagulant polymer on start‐up, sludge granulation and the associated reactor performance was evaluated in four laboratory‐scale UASB reactors. A control reactor (R1) was operated without added polymer, while the other three reactors, designated R2, R3 and R4, were operated with polymer concentrations of 5 mg dm^?3, 10 mg dm^?3 and 20 mg dm^?3, respectively. Adding the polymer at a concentration of 20 mg dm^?3 markedly reduced the start‐up time. The time required to reach stable treatment at an organic loading rate (OLR) of 4.8 g COD dm^?3 d^?1 was reduced by more than 36% (R4) as compared with both R1 and R3, and by 46% as compared with R2. R4 was able to handle an OLR of 16 g COD dm^?3 d^?1 after 93 days of operation, while R1, R2 and R3 achieved the same loading rate only after 116, 116 and 109 days respectively. Compared with the control reactor, the start‐up time of R4 was shortened by about 20% at this OLR. Granule characterization indicated that the granules developed in R4 with 20 mg dm^?3 polymer exhibited the best settleability and methanogenic activity at all OLRs. The organic loading capacities of the reactors were also increased by the addition of polymer. The maximum organic loading of the control reactor (R1) without added polymer was 19.2 g COD dm^?3 d^?1, while the three polymer‐assisted reactors attained a marked increase in organic loading of 25.6 g COD dm^?3 d^?1. Adding the cationic polymer could result in shortening of start‐up time and enhancement of granulation, which may in turn lead to improvement in the efficiency of organics removal and loading capacity of the UASB system. Copyright © 2004 Society of Chemical Industry     

A globally convergent method for finding all steady‐state solutions of distillation columns

A globally convergent method is proposed that either returns all solutions to steady‐state models of distillation columns or proves their infeasibility. Initial estimates are not required. The method requires a specific but fairly general block‐sparsity pattern; in return, the computational efforts grow linearly with the number of stages in the column. The well‐known stage‐by‐stage (and the sequential modular) approach also reduces the task of solving high‐dimensional steady‐state models to that of solving a sequence of low‐dimensional ones. Unfortunately, these low‐dimensional systems are extremely sensitive to the initial estimates, so that solving them can be notoriously difficult or even impossible. The proposed algorithm overcomes these numerical difficulties by a new reparameterization technique. The successful solution of a numerically challenging reactive distillation column with seven steady‐states shows the robustness of the method. No published software known to the authors could compute all solutions to this difficult model without expert tuning. © 2013 American Institute of Chemical Engineers AIChE J 60: 410–414, 2014     

The start‐up of anaerobic sequencing batch reactors at 20 °C and 25 °C for the treatment of slaughterhouse wastewater

The objective of this research was to evaluate the feasibility, the stability and the efficiency of a start‐up at 20 °C and 25 °C of anaerobic sequencing batch reactors (ASBRs) treating slaughterhouse wastewater. Influent chemical oxygen demand (COD) and suspended solids concentrations averaged 7500 and 1700 mg dm^?3, respectively. Reactor start‐up was completed in 168 and 136 days at 20 °C, and 25 °C, respectively. The start‐up process was stable at both temperatures, except for a short period at 20 °C, when effluent volatile fatty acid (VFA) concentrations increased from an average of 40 to 400 mg dm^?3. Effluent quality varied throughout start‐up, but in the last 25 days of the experiment, as the ASBRs were operated under organic loading rates of 2.25 ± 0.21 and 2.86 ± 0.24 kg m^?3 d^?1 at 20 °C and 25 °C, respectively, total COD was reduced by 90.3% ± 1.3%. Methanogenesis was not a limiting factor during start‐up. At 20 °C, the limiting factor was the acidification of the soluble organics and, to a smaller extent, the reduction of propionic, isobutyric and isovaleric acids into lower VFAs. At 25 °C, the limiting factor was the hydrolysis of particulate organics. To minimize biomass loss during the start‐up period, the organic loading rate should be increased only when 75 –80% of the COD fed has been transformed into methane within the design hydraulic retention time. © 2001 Society of Chemical Industry     

工程建设项目的开车/开车服务管理

介绍工程公司在化工,石化或医药工程项目设计,采购,施工,开车及生产验收各阶段的开车／开车服务管理的工作职责,主要工作内容和方法以及所依据的标准／规范和作用文件。     

Phase Distribution Measurements during Transient Bubbly Two‐Phase Flow in a Vertical Pipe

An experimental procedure for investigating transient bubble flow for an adiabatic air/water system with vertical upward flow in a pipe is presented. The results of the measured local transient two‐phase flow parameters are shown along a pipe length of approx. four meters. From the measured radial phase distributions under steady and under transient conditions one can draw conclusions about the interfacial forces. Here, the effects indicate the action of forces such as a transverse lift force and a time dependent force like the virtual mass force during the transient. For modelling the transverse lift force which seems to play a dominant role for that flow regime the formulation of Zun was chosen and it was implemented into the commercial CFD‐Code Fluent Release 4.4.4 via user‐defined subroutines. Finally, results from the simulation of the steady states of start and end conditions of an experimental measured transient are shown.     

Mass transfer and hydrodynamic characteristics in a co‐current downflow contacting column

Hydrodynamic and mass transfer characteristics of water–air system in a co‐current downflow contacting column (CDCC) were studied for various nozzle diameters at different superficial gas velocities and liquid re‐circulation rates. Gas hold‐up and liquid‐side mass transfer coefficient increased with increasing superficial gas velocity and liquid flow rate but decreased with increasing nozzle diameter. It is shown that correlations developed, which are based on liquid kinetic power per liquid volume present in the column, and superficial gas velocity explains gas hold‐up and the mass transfer coefficient within an error 20% for all gas and liquid flow rates and nozzle diameters used. The constants of correlations for gas hold‐up and mass transfer coefficient were found to be considerably different from other gas–liquid contacting systems. © 2003 Society of Chemical Industry     

Predictions for Start‐Up Processes of Reactive Distillation Column via Artificial Neural Network

The time consumed in starting up the unit with appropriate holdups can form an important part of the total distillation time, particularly for reactive distillation systems with large holdups. Also, the products formed during the start‐up time are off specification, and are not easily recycled as for traditional distillation, but must be carefully disposed of, which can be very costly. A back‐propagation algorithm artificial neural network model is presented as a tool to assess the start‐up process for a given reactive distillation system. All the data required for training and testing the artificial neural network have been generated using the CHEMCAD simulator, version 5.2–0. The values for the learning rate, momentum term, and gain term of the artificial neural network have been taken as 0.01, 0.6, and 1.0, respectively. From the case studied in this work, it can be seen that a good start‐up policy can reduce both the energy and time requirements in the start‐up phase of reactive distillation processes. Results from predictions show the time consumed in the start‐up period has an average error of 2.833 %, and a maximum error of 7.600 %, for the case studied here. The accuracy of the model will depend upon the data available and the type of model being approximated.     

On the dynamics of distillation processes—IV Uniqueness and stability of the steady state in homogeneous continuous distillations

Recent numerical studies by Magnussen et al.[1] have shown that multiple steady state solutions can be exhibited by the constant molar overflow (CMO) model for ternary azeotropic distillation in a multistaged column. This has such important consequences for distillation control, design and startup that further experimental and analytical work is desirable.This paper addresses the problem of uniqueness and stability of the steady state in the continuous distillation of homogeneous mixtures. It is shown that multiple steady state solutions are not exhibited by either binary homogeneous distillations in a multistage CMO column or multicomponent homogeneous distillations in a single stage CMO column (flash distillation). Therefore, the multiplicity is a consequence of multicomponents and multiple stages.     

Multiple Analysis in a Reactive Distillation Column for the Synthesis of tert‐Amyl Methyl Ether

tert‐Amyl methyl ether (TAME) is produced via reactive distillation. A simulation is set up and controlled on Aspen HYSYS v 8.0 for generating the highest purity of TAME. This simulation includes a plug‐flow reactor and a reactive distillation column. Emphasis was put on finding the optimal operating conditions of the reactive distillation column in order to get the maximum purity of TAME. The operational parameters were reflux ratio, number of reactive stages in the distillation column, and condenser pressure. The results indicated the optimal reflux ratio and condenser pressure which could be adapted to industrial scale.     

厌氧膜床处理小型餐饮废水的启动研究

厌氧膜床最大的特点是用立体填料代替了传统的小粒径填料，首次以厌氧膜床处理小型餐饮废水的启动为研究对象，以满负荷的1／8，2／8，4／8，8／8逐步提高容积负荷，经过85d的启动运行，反应器达到满负荷。研究结果表明：进水pH较低，平均为5．06，经过厌氧膜床启动，出水在6．7左右；COD的去除率稳定在50％左右；启动后期的污泥上浮可能是颗粒污泥形成的预兆。     

Energy‐efficient complex distillation sequences: Control properties

Four thermally coupled distillation systems were designed for the separation of five‐component mixtures (the light‐ends separation section of a crude distillation plant); their steady‐state design was obtained by starting from a conventional distillation sequence and then optimizing for minimum energy consumption. The thermally coupled distillation systems were compared to sequence based on conventional columns design. Comparison was based on controllability properties under open and closed loop operation, following the dynamic behaviour after common industrial operating disturbances. Simulation results were analyzed by the singular value decomposition technique and with the performance examination of elimination of feed disturbances using PI controllers. It was found that thermally coupled distillation systems are controllable and, sometimes, they exhibit dynamic responses that are easier to manage than in the case of conventional distillation sequences; this result is innovative in the study of this kind of systems.