Biodiesel Production Using Reactive Distillation Column Based on Intensification Processes

Kinetics and structural design of ZSM-5@SiC foam catalytic packing in RD column for ethyl levulinate synthesis

Economic optimization of a reactive distillation column with multiple reactive sections for silane production

Fatty acid methyl esters derived from renewable sources such as vegetable oils has gained importance nowadays as an alternative fuel for diesel engines. The present study is aimed to produce biodiesel from non-edible oil (Karanja oil of Indian origin) both in batch and continuous reactors. The purpose of the study is the comparison of Karanja biodiesel production with different reactor types under variable reaction characteristics. Therefore, two types of continuous reactors were used: helical tube reactor and reactive distillation (RD) column. Experiments were carried out to obtain suitable operating parameters in batch- and continuous-flow reactors. For batch reactor, suitable operating conditions obtained are: 7:1 methanol-to-oil molar ratio, 0.8% (by weight of oil) catalyst (KOH), 65°C reaction temperature, and 1-h reaction time, at which the maximum yield obtained is 96%. In continuous helical tube reactor, maximum yield of 92.6% was obtained at 6.6 mL/min of flow rate at the same operating conditions of batch reactor. In continuous RD column, maximum yield of biodiesel 96.6% was obtained at the same operating conditions except methanol-to-oil molar ratio (5:1) because of recycling of methanol into the column. The residence times in the helical tube reactor and RD column were 4 and 8 min, respectively, as compared to 1 h in the batch reactor for almost the same yield.

Optimization and heat integration of hybrid R-HIDiC and pervaporation by combining GA and PSO algorithm in TAME synthesis

This paper aims to present the feasibility of conducting the transesterification of propylene glycol ether (PM) with methyl acetate (MeAc) in a reactive distillation (RD) column to improve the reaction conversion. The essential thermodynamic and reaction kinetic data of the reaction system were measured for the feasibility study. There is only one azeotrope, MeAc–MeOH, in the reaction system, and the NRTL model could describe well the thermodynamic behavior of this system. The transesterification of PM with MeAc is an endothermic reaction with activation energy E = 55.704 kJ·mol–1. The feasibility was analyzed by residue curve maps (RCM), showing that full conversion of PM could be realized by RD with a mole ratio of MeAc–PM larger than 2.882. The intensification effect was experimentally verified in a batch RD column. Finally, some important parameters are given through the conceptual design to develop a continuous RD column for the transesterification of PM with MeAc.

Reactive distillation (RD) in the face of azeotrope(s) in the separation of a mixture from an RD column might need debottlenecking design and more columns to obtain high-purity products. Under such circumstances, the integration of heat with the process becomes an effective consideration for reducing costs. In this study, an RD process to produce ethyl acetate and n-butanol from ethanol and n-butyl acetate by conducting a transesterification reaction is presented. The products from the RD column include n-butanol and an ethanol/ethyl acetate mixture. Designs with alternative configurations are used to illustrate plantwide designs of the process with heat integration/coupling. Among these alternatives are two with three columns and one with two columns. In the three-column configurations, separation of ethanol/ethyl-acetate mixtures from the top product of the RD column is conducted by extractive distillation or pressure-swing distillation. The other configuration consists of an RD column followed by a conventional distillation column operated at high pressure. Systematic design procedures are used to optimize the flowsheets of different configurations by minimizing the total annual cost. Heat integration and thermal coupling technologies are used in these three configurations to attempt to provide more economical designs. The results show that the selection of separation system depends on whether heat integration/coupling is considered. In this case, the two-column reactive distillation process with heat integration yields high-purity products and the lowest total annual cost.

This paper introduces multiple esterification reactions of three alcohols occurring in a single reactive distillation (RD) column and reports significant energy savings by combining three reactions in the single unit. To realize a feasible integration of the three reactions, the removal of the common water product from the unstable heterogeneous azeotrope should be possible through liquid–liquid decantation in the eight-component system. For this multireaction system, only the direct sequence can produce three esters with a purity higher than 99.0 mol % due to the behavior of liquid–liquid phase equilibrium. We demonstrate an economic evaluation of the direct sequence of a single RD column simultaneously producing the three esters by comparing the direct sequence with the two parallel RD sequences in the same design basis. The total annual cost of the triple esterification direct sequence is reduced by 21.3–25.2% compared to that of the parallel esterification system.

Kinetic analysis for the acid-catalyzed dimerization of C4 olefins was performed in a batch reactor, and a suitable rate model was developed. It was further used in the rate-based simulation model of a continuous reactive distillation (RD) column. The results obtained were compared with the experimental observations made on a pilot-scale high-pressure RD column. An important outcome of the present work is that RD can be used efficiently to enhance the selectivity of C8 dimers, thereby avoiding the formation of trimers and tetramers. The use of polar components (such as water or alcohols), as selectivity enhancers, is not necessary.

Rigorous design and economic optimization of reactive distillation column considering real liquid hold-up and hydraulic conditions of industrial device

In this paper, design of a complete reactive distillation (RD) system has been developed. 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. A suitable NRTL model parameter set for calculating of liquid activity coefficients has been established with excellent prediction of the compositions and temperatures for the four azeotropes in this system. In the VLE calculations, vapor association of acetic acid due to dimerization has also been considered. A reactive distillation column with an overhead decanter can be designed to achieve over 93 wt% of ethyl acetate composition at organic phase top product stream while the bottom product stream is designed to be rich in acetic acid so that it can be recycled and mixed with fresh acid make-up stream to serve as acid feed to the reactive distillation column. Since the purity of the optimum top organic product is still not good enough for the ethyl acetate product specification in industry, an additional column is designed to purify the ethyl acetate product of the reactive distillation column to over 99.5 wt%. The top draw of the second column will be recycled back to the decanter. In summary, the overall optimum design of this ethyl acetate reactive distillation system includes two columns (including the reactive distillation column and the second column), one decanter, and two recycle streams. The optimum operating condition of the overall system will also be studied to minimize the total operating cost of the overall system while meeting product specifications.

In this study, the performance of a packed-bed reactive distillation (RD) column for the production of methyl acetate (MeOAc) using an ion-exchange catalyst and simulation of the same using CHEMCAD were analyzed. An ion-exchange catalyst, Indion 190, was used in this study. The performance of the RD column was evaluated based on the MeOAc concentration in the top product. Both steady- and unsteady-state behavior of the column was simulated using CHEMCAD, and the results were experimentally validated. The process parameters, viz., reboiler temperature, enriching temperature, reactor temperature, catalyst loading, molar ratio of the reactant, and flow rate of reactants, were studied, and the optimal values were found to be 73 °C, 56 °C, 72 °C, 100 g, 1:2, and 15 mL/min, respectively. Feed locations of acid and alcohol to the reactor that gave maximum MeOAc concentration in the top product were determined. A mathematical model based on the rigorous calculation using SCDS (used to calculate the nonideal K val...

Development of a dynamic nonequilibrium cell model for reactive distillation tray columns

Novel intensified process for di-isopropyl ether production from isopropanol etherification using reactive distillation technology

The study aims to reveal the possibility of reactive distillation (RD) in the 2-methoxy-2-methylheptane (MMH) production process. MMH is getting more industrial and academic interests as a gasoline additive to replace methyl tert-butyl ether. Traditionally, MMH is obtained by carrying out the reaction in the reactor followed by three distillation columns. The high yield of MMH could be achieved by keeping the large reactor size or by using the large excess of 2-methyl-1-heptene (MH). Both former and latter strategies are associated with the high capital and operating costs. To solve these problems, this study proposed an innovative RD configuration to take synergistic benefits of reaction and separation involved. This innovative RD configuration allows the production of MMH with significantly lower capital, operating and total annual costs. For desired MMH yield, the result demonstrates that the proposed RD configuration can reduce energy, capital, and total annual costs up to 7.7, 31.3, and 17.1%, respectively, compared to a conventional process. Furthermore, the influence of some important design parameters on the RD column performance was also explored to overcome the temperature limitation of acid resin catalyst inside the reactive zone of the RD column.

Most of the published studies have focused on the thermal integration of nonreactive distillation columns. The key limitation of reactive distillation (RD) technology is that the necessary conditions (such as pressure and temperature) for the reaction must match those of distillation. Owing to this constraint, the reaction conversion may be adversely affected at the elevated pressure in the reactive section of an internally heat integrated distillation column (HIDiC). This fact forces us to adopt an external heat integration approach for an industrial heterogeneously catalyzed ethyl tert‐butyl ether (ETBE) RD column. The direct vapor recompression column (VRC) is an external heat integration scheme that is successfully used as an energy efficient scheme for separating a close‐boiling mixture. Interestingly, there exists a large temperature difference between the two ends of the representative ETBE column, and it makes the external heat integration more challenging. Aiming to improve the thermal efficiency of the ETBE column under the VRC framework, various heat pump arrangements with intermediate reboiler(s) (IR(s)) are explored and analyzed with performing a comparative study in terms of energy consumption and economics. To improve further the thermal efficiency, in this contribution, a novel multistage vapor recompression RD column with IRs is introduced addressing a number of practical concerns. An algorithm for the proposed column is formulated showing the sequential steps involved in heat integration. It is inspected that the proposed multistage vapor recompression RD system appears overwhelmingly superior to the classical vapor recompression RD and its conventional stand alone column providing a significant savings in energy as well as cost. © 2012 American Institute of Chemical Engineers AIChE J, 59: 761–771, 2013