Methyl acetatemethanol mixture separation by extractive. Reactive distillation extractive distillation buffalo. Control of a reactive distillation column for methyl acetate system using aspen plus satirtha kumar sarma1, kailash singh2 and rajeev kumar dohare3 m. Jul 05, 2016 production of npropyl acetate by reactive distillation experimental and theoretical study m. A novel intensification technologymicrowave reactive distillation mrd process was developed by coupling the microwave irradiation and reactive distillation rd process to break through the limitations of the rd process, such as low esterification reaction rate.
International journal of chemical reactor engineering. Conceptually, a rd column has three basic elements. Production of npropyl acetate by reactive distillation. Production process using ethylene, acetic acid and oxygen. Ethyl acetate is found in many foods such as kiwi fruit, guava fruit, roasted filberts, blue cheese and baked potatoes.
Investigations on the production of methyl acetate by. The production of methyl acetate in a reactive distillation process prior art for 15 years is often used as an example to study the basic phenomena of reactive distillation. While the derivative obtained from the reactive distillation of acetic acid can be further used in industries like foods, pharmaceuticals, explosives, medicinals and solvents. A reactive distillation column, combining the reaction and separation into a single stage, is proposed. Lee, design of reactive distillations for acetic acid esterification with different alcohols, aiche j. The acetic acid feed acts as a solvent in an extractive distillation section placed above the reaction section, breaking the methanolmethyl acetate azeotrope, and yielding a pure methyl acetate. The batch mrd process and rd process for acetic acid and ethanol esterification were compared by using a laboratoryscale rd. About the author kai sundmacher and achim kienle are the authors of reactive distillation. This reaction mixture is again added to the reactive distillation. The approach is illustrated for the production of methyl acetate because of its commercial importance, and because of the availability of adequate published data for comparison. The present invention is a reactive distillation process for methyl acetate hydrolysis comprising a rectifying section 2, a reaction section 3 and a stripping section 4. May 14, 2014 reactive distillation can be used in the separation of acetic acid from water. We have explored a hierarchy of methods and models for the design and simulation of a reactive distillation column for the production of methyl acetate.
The basic concept of reactive distillation has already been applied in the 1920s 1. Synthesis and design of reactive distillation columns a thesis submitted to the university of manchester institute of science and technology for the degree of doctor of philosophy by ramona manuela dragomir under the supervision of dr. Microwave reactive distillation process for production of. In first step ethanol with acetic acid is feed into the pre reactor column.
Ads l9 reactive distillation case studies part 1 youtube. Thermodynamic aspects of the considered system are discussed, and uniquac interaction parameters are given. Occurrence in wines edit ethyl acetate is the most common ester in wine, being the product of the most common volatile organic acid acetic acid, and the ethyl alcohol generated during the fermentation. The results are compared for both experimental and simulation studies.
A water stream is fed into the upper portion of the rectifying 2 or reaction zone 3 and a methyl acetate stream is fed into the lower portion of the reaction zone 3 which contains packings made of ion exchange resin. Reactive distillation process for the production of methyl. Control of reactive distillation process for production of. At the top of reactive distillation colmn, an azeotropic mixture of ethyle acetate, ethanol and water is obtained which is seperated with a decanter into water and an organic phase. Methyl acetate synthesis using a reactive distillation. Then, the reactive distillation process for methyl acetate synthesis is simulated by the aspen plus process simulator. Nevertheless, the recent progress in modelling and simulation, as well as impressive examples realised in industrial practice, such as methyl acetate production via reactive distillation 2, have led to. The raw material, a byproduct from the polyvinyl alcohol process is a mixture of methanol and methyl acetate 30 wt% methyl acetate. This work considered the use of this novel process to investigate how the purity of a fatty acid methyl ester oleic acid methyl ester methyl oleate, which is an alternative fuel that has a potential economic bedrock, vary with variations in reflux ratio. Reactive distillation processes to break azeotropes. To eliminate the azeotropes especially the methanolmethyl acetate oxylene is used as an entrainer. The experiments were conducted at various operating conditions like reboiler temperature, reflux ratio, and different feed flow rates of the acetic. Reactive distillation for methyl acetate production the models require increasingly sophisticated data needs as the hierarchy is implemented.
Thus the aim of these runs was to obtain experimental data. We found that when assuming reaction equilibrium, it is possible to design a column operating with stoichiometric feeds and producing highpurity methyl acetate as distillate, and water as bottom product. Review modeling of reactive distillation column for the. Control of a reactive distillation column for methyl acetate. Process for the production of methyl acetate from methanol. The use of dilute acetic acid for butyl acetate production in. The top nonreactive rectifying section performs the separation of inert gases and 4076 iii reactive distillation. Reactive distillation is a process where the chemical reactor is also the still. Reactive distillation experiments were carried out both in laboratory and semiindustrial scale with different catalytic packings. International journal of advanced technology and engineering exploration, vol 426 the condenser, stages 23 being the rectification section, followed by the reactive section with stages 437.
Ethyl acetate is a volatile compound that is in wines, brandy, fruits like pineapple and essential oils obtained from fruits and flowers. Tech student, malaviya national institute of technology, jaipur, india1 associate professor, malaviya national institute of technology, jaipur, india2. The structured packing was filled with amberlyst 15 ion. The process parameters such as total feed flow rate. A batch reactive distillation column to produce the ethyl acetate studied in this work is shown in fig. Methyl acetate is considered low toxicity volatile solvent produced either as a byproduct during methanol carbonylation or via acetic acid esterification with methanol. The process is centered on the reaction between ethylene, oxygen and acetic acid in order to produce vinyl acetate and water. The question is how processes can be identified that exhibit potential for reactive distillation. Pervaporation coupled process for ethyl acetate production with water removal from reboiler and acetic acid recycle bida lv, gongping liu, xueliang dong, wang wei, and wanqin jin state key laboratory of materialsoriented chemical engineering, nanjing university of technology, 5 xinmofan road, nanjing. Process intensification, process design tavan, yadollah on. The use of dilute acetic acid for butyl acetate production in a reactive distillation.
Reactive distillation column synthesis springerlink. In this study a model and solution strategies are proposed for the optimization of a dividing wall batch and semibatch reactive distillation column. Novel reactive distillation pervaporation coupled process for. Investigations on the synthesis of methyl acetate in a. Methyl acetate production via reactive distillation is chosen as a case study. The aspen plus reactive distillation process model was developed and simulated using radfrac packed column the rectification and the stripping. Separation of the product from the reaction mixture does not need a separate distillation step which saves energy for heating and materials. Robin smith department of process integration manchester, united kingdom march 2004. Reactive distillation a very promising alternative to conventional reactiondistillation flow schemes. Is this an exception or does it stand for a type of process with a comparable potential for improvement. The column is fed with pure acetic acid and pure methanol at stages 2 and 36. Conventional batch reactive distillation high purity ethyl acetate production with.
Reactive distillation is used commercially to produce methyl tertbutyl ether, esters including methyl acetate, and nylon 6, 6. A profit maximization involving methanol esterification reaction for the production of methyl acetate as the main product is proposed. A novel energy saving procedure for the coproduction of ethyl acetate and nbutyl acetate by reactive distillation is simulated by aspen plus in this paper. The results show that the maximum recovery obtained for methyl acetate was 90. Investigations on reactive membrane separation have led huang and al. Production of highpurity ethyl acetate using reactive. Besides the homogeneously catalyzed systems as in the methyl acetate. Methyl acetate meoac can be made by the liquidphase reaction of acetic acid hoac and methanol meoh in the presence of an acid catalyst e. Ethyl acetate is normally produced by esterification of ethanol and acetic acid. We describe a hierarchy of methods, models, and calculation techniques that support the design of reactive distillation columns. Process for the production of methyl acetate from methanol and acetic acid last modified by.
The present invention relates to a process for the production of methyl acetate by reactive distillation. Reactive distillation, methyl acetate, control aspen plus dynamics. Keyes was among the first who studied a reactive distillation process for the production of ethyl acetate etac using a prereactor, two recovery columns, and one decanter. It has captured the imagination of many researchers due to the demonstrated potential over the. The potential of homogeneously catalyzed reactive distillation to increase conversion and improve selectivity has been highlighted by kenig et al. Control of reactive distillation process for production of ethyl acetate haoyeh lee a, hsiaoping huang a, ilung chien b a department of chemical engineering, national taiwan university, taipei 10617, taiwan, roc. Vinyl acetate from ethylene, acetic acid and oxygen. Recent trends 3 produced by the berkeley electronic press, 2004. Optimization of the ethyl acetate reactive distillation process. Also, a hybrid modelling approach, which can be easily implemented in radfrac, is proposed for this system.
Nevertheless, the recent progress in modelling and simulation, as well as impressive examples realised in industrial practice, such as methyl acetate production via reactive distillation 2, have led to increasing interest in such processes. The ethyl acetate is always distilled and withdrawn out of the reaction zone. Optimization of the ethyl acetate reactive distillation process sungkyu lee and myungwan han department of chemical engineering, chungnam national university, daejeon 305764, korea received 2 july 2001. Simulation study on the application of reactive distillation. It has also been proposed for hydrolysis reactions, ethyl ene glycol synthesis, and cumene production. Reactive distillations for the production of ethyl acetate etac and isopropyl acetate ipac are classified as the typeii process where the first column consists of a reactive zone and a. Novel procedure for coproduction of ethyl acetate and n. Reactive distillation for methyl acetate production robert s. The production of butyl acetate and methanol via reactive. Pdf reactive distillation for methyl acetate production. The reaction involved is an esterification reaction between methanol and acetic acid to produce methyl acetate and water. The aim of this work is to synthesize, design, and study the dynamic behavior for the azeotropic separation, the reactive and extractive distillation unit, and the solvent recovery system.
Control of a reactive distillation column for methyl. Synthesis and design of reactive distillation columns. Simulation of reactive distillation column for nbutyl. The reactive distillation column is composed of three sections, the middle of which is a reactive zone packed with a solid catalyst. The production of highpurity ethyl acetate etac using reactive distillation rd is studied experimentally in a pilotscale plant. The reactive distillation column is followed by two purification columns operating in series to produce ethyle acetate. Production of tame and npropyl propionate by reactive. Lifetime evaluation of nkc9 was carried out to study the conversion rate of acetic acid and selectivity of methyl acetate during the longperiod running in the fixedbed reactor. Methyl acetate also arises by esterification of acetic acid with methanol in the presence of strong acids such as sulfuric acid. Recent trends in the experimental and theoretical investigations in this area are also outlined. Production of tame and npropyl propionate by reactive distillation dissertation presented to the faculty of engineering of the university of porto for the degree of doctor in chemical engineering by carlos filipe moreira duarte supervisor professor doutor jose miguel loureiro laboratory of reaction and separation engineering. The optimum operation conditions and all design parameters of the reactive distillation column are determined on the ground of the analyses carried out. In both cases, pure methyl acetate has to be isolated from the reaction mixture. The synthesis of methyl acetate was carried out in a packed rdc by catalytic esterification using acetic acid and methanol as reactants in a pilotscale experimental setup.
Soon after the invention and commercial application of this technology for methyl acetate synthesis it was used as a model system for testing a new design and synthesis framework that was developed for the limiting case of. The development of a heterogeneously catalyzed reactive distillation process for the production of nbutyl acetate by the esterification of nbutanol with acetic acid is presented. Catalysts, kinetics, and reactive distillation for methyl. The potential importance of reactive distillation in some industrial iii reactive distillation 4075. The reactive distillation system in the study is the production of ethyl acetate etac via esterification of acetic acid hac with ethanol etoh using sulphuric acid as homogeneous catalyst. Process alternative for methyl acetate conversion using. High purity ethyl acetate production with a batch reactive. Its feasibility is theoretically analyzed on the basis of the physical properties of ethyl acetate nbutyl acetate system. Modelling, simulation and sensitivity analysis of a fatty.
The modeling, simulation, and optimization of the reactive distillation esterification process used for the production of methyl acetate have been carried out in this work with the aid of aspen plus. Novel reactive distillation pervaporation coupled process. Reactive distillation, being an intensified process of combining reaction and distillation in a single vessel, is an ongoing research. An extensive body of literature exists on the subject of reactive distillation. However, a reactive distillation process for the production of pure methyl acetate has not hitherto been disclosed. Mar 06, 1984 the present invention relates to a process for the production of methyl acetate by reactive distillation. In the present study, methyl acetate has been synthesized using esterification of acetic acid with methanol in a continuous packed bed catalytic reactive distillation column in the presence of novel indion 180 ion exchange resin solid catalyst. Simulation studies of reactive distillation for ethyl acetate. Doherty department of chemical engineering, university of massachusetts, amherst, ma 01003, usa.
Methyl acetate can be obtained by reactive distillation. Reactive distillation, mathematical modeling, ethyl acetate, parametric analysis, reactive extractive distillation 1. Simulation study of reactive distillation column for the. The default solver for three phase columns is the sparse continuation solver which is an advanced solver designed. As a further example, the manufacture of methyl acetate uses reactive distillation, because reaction eliminates the azeotrope between water and methyl acetate. The process consists of one reactive distillation column, two distillation columns and one recycle stream with the product specification of 99 mol% acetic acid. Hiwale et al industrial applications of reactive distillation.
The new procedure not only significantly reduces energy consumption, but also eliminates the acetic acid. Wikisheet reactive distillation methyl acetate production, reactive distillation and conventional process. However, pure methyl acetate remains a saddle in the reactive system, and cannot be obtained as a pure component by simple reactive distillation. Pdf production of ethyl acetate using reactive distillation. Sep 29, 20 reactive distillation processes to break azeotropes. Rd process for methyl acetate and energy utilization using rd cumene production.
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