• Korean Chemical Engineering Research
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• v.46 no.4
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• pp.739-746
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• 2008

The aim of this study is finding the optimal design parameters and the optimal operation variables of a reactive distillation column. Different from steady state optimization, dynamic optimization makes it possible considering operation ability as well as design problems at process design step. For performing dynamic optimization, dynamic simulation should be done first. If dynamic simulation is already finished, dynamic optimization can be performed with less effort than that of dynamic simulation.Reactive distillation systems involving reaction and separation in a single unit have the potential to reduce capital and operating costs, particularly when reaction have conversion constraint or when azeotropes exist making conventional separation difficult and expensive. This study here present work on the continuous distillation process, the homogeneous catalyzed esterification of methanol and acetic acid, the synthesis of methyl acetate. Based on an equilibrium stage model of a reactive distillation column a dynamic optimization problem was formulated and solved. And the results were verified by performing dynamic simulation and showing the variation of conversion and purity as the variation of the operation variables. As the results of dynamic optimization, this study found optimal feed ratio, reflux ratio and reboiler duty of this system. And as this study applied it to dynamic simulations the dynamic characteristics of a reactive distillation column are showed under optimal operating condition.

• KSBB Journal
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• v.14 no.2
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• pp.220-224
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• 1999

Lactic acid was reacted with alcohol into lactate ester, and lactate ester produced in esterification reaction was distilled simultaneously with hydrolysis reaction into lactic acid. When the yields of lactic acid recovered by batch reactive distillations with various alcohols were compared, the yield of lactic acid was increased as the volatility of lactate ester was increased. In this batch reactive distillation, because the mixtures condensed in partial condensor were flown to reboiler through distillation column, the recovery yield of lactic acid was affected by operation temperature of partial condensor. Hydrolysis reaction into lactic acid in distillation column rarelyoccurred because of short retention time of lactate ester and water. Lactate ester was reacted into lactic acid in reboiler.

• The Korean Journal of Food And Nutrition
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• v.15 no.4
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• pp.295-299
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• 2002

The esterification of alcohols with acetic acid, lactic acid and citric acid was carried out in batch during the second distillation. Effect of various parameters, e.g. pH of reactant base spirit, temperature of distillation, time of distillation were studied. The parameter of distillation temperature was modified by atmospheric distillation and pressure distillation. The pressure(1.9 atm.) distillation was used in order to react and distill at high temperature. Compared with the base spirit concentration, ethyl acetate, ethyl lactate and iso-amyl acetate in esterification distillate increased by 2,890%, 6,410% and 52%, respectively. Major factors of the esterification with organic acids in distilled spirit making were molecular weight of the organic acid and pH of reactant base spirit.

• Korean Chemical Engineering Research
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• v.52 no.6
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• pp.713-719
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• 2014

When multiple reactions of quaternary mixtures take place in a reactive distillation column, the behavior of composition trajectory is analyzed by a visual-aided method. By adding additional vectors of multiple reactions and visualizing them in composition space, the composition of each component and extent of each reaction on an arbitrary stage can be easily estimated in terms of the composition trajectory and reaction cascade difference points. Moreover, for a given operating conditions, the number of total stages and position of optimum reaction zone can be determined by the visual-aided method. In this study, ethylene glycol synthesis with a side reaction is taken as an example and analyzed by the proposed graphical method. Through this method, the quaternary reactive distillation with multiple reactions can be analyzed without numerous experiments and simulations.

• Korean Chemical Engineering Research
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• v.55 no.3
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• pp.341-352
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• 2017

Butyl acetate is produced from acetic acid and butanol via an esterification reaction in a reactive distillation column. Entrainer can be used for efficient removal of produced water from the reaction region, leading to significant improvement of the column performance. Batch reactive distillation has clear advantages over continuous one in terms of flexibility and adaptability in a small plant. We studied batch and semi-batch reactive distillation processes through process simulation and pilot-scale experiments. We investigated process configuration and type of entrainer for improvement of the column performance and suggested a novel cyclic operation strategy using the semi-batch reactive distillation column. The cyclic strategy was shown to give relatively high production rate and stable operation.

• 한국신재생에너지학회:학술대회논문집
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• 2011.11a
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• pp.113.2-113.2
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• 2011

동물성 오일을 이용한 바이오디젤 생산 반응 후 미반응된 메탄올과 염기촉매의 처리에 관한 연구로써 바이오디젤의 순도에 영향을 미친다. 메탄올과 염기촉매는 바이오디젤 생산 반응 후 상층인 메틸 에스터 층과 하층인 글리세롤 층에 각각 포함되어 있다. 1차적으로 각각의 층에서 메탄올을 증발하게 되며 메탄올 증발은 감압 증류 장치를 이용해 분리하게 된다. BD100을 기준으로 하여 메탄올의 함량은 0.2% 이하여야 하며 수분 함량은 0.05% 이하를 유지해야 한다. 메탄올 증발은 메탄올의 끓는 온도인 $65^{\circ}C$를 기준으로 하여 끓는점 보다 낮은 온도와 높은 온도에서 각각 증발을 실시하고 각각의 메탄올 증발 제거에 따른 FAME 함량에 미치는 영향에 대해 FAME 함량 분석을 통해 조사하였으며 메탄올 증발 후 증류수를 이용한 바이오디젤 내 잔류 촉매 및 자유 글리세린 세정 제거에 대해 조사하였다. 증류수 양과 증류수 온도 및 세정 시간에 따른 FAME 함량 변화를 알아보았으며 세정 후 증류수 증발에 따른 FAME 함량 변화에 대해서 분석을 실시하였다. 본 실험을 통해 동물성 오일을 이용한 바이오디젤 생산 후처리 공정인 메탄올 증발 및 세정, 수분 증발 공정의 최적 조건을 도출하고자 하였다.

• Clean Technology
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• v.17 no.1
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• pp.56-61
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• 2011

In this study, hydrocarcking of vacuum residue was carried out in an autoclave reactor at $450^{\circ}C$ and $500^{\circ}C$ with a commercial catalyst (HDM) and the quantitative product distributions were analyzed by GC-SIMDIS method or simple distillation. During catalytic hydrocracking, thermal cracking also occurred together with catalytic cracking and the higher conversion and selectivity of gasoline and naphtha were obtained at high reaction temperature. GC-SIMDIS and simple distillation revealed different results for the analysis of products produced at different hydrocracking temperatures; almost same results were obtained for the product produced at $500^{\circ}C$ but different ones for the product produced at $450^{\circ}C$. In the analysis of product produced at $450^{\circ}C$, the GC-SIMDIS showed that a main product was VGO while a main product in the simple distillation was diesel, which implies that the simple distillation for the $450^{\circ}C$ reaction was not accurate due to thermal cracking of the product by the simple distillation.

• Journal of the Korean Society of Food Science and Nutrition
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• v.38 no.11
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• pp.1559-1563
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• 2009

Scaled-up production of oil containing diacylglycerol (DAG), so called diacylglycerol-oil, was produced by lipase-catalyzed reaction. Mixture of soybean oil and glyceryl monooleate with 1:2 molar ratio was esterified with Lipozyme RMIM in a batch-type reactor at 55$^{\circ}C$ and 300 rpm during 6 hr. After short-path distillation for removal of monoacylglycerol and free fatty acid as reaction by-products, diacylglycerol-oil mainly consisted of DAG (29 area%) and TAG (71 area%). The major compositional fatty acids in diacylglycerol-oil were oleic (44.36 wt%), and linoleic acids (37.36 wt%). Acid value and iodine value of diacylglycerol-oil were 0.13 and 112.6, respectively. Solid fat content (SFC) of diacylglycerol-oil was observed after differential scanning calorimetry (DSC) analysis in which three melting peaks at -25.0, 0.1, and 11.2$^{\circ}C$ were shown.

• Resources Recycling
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• v.11 no.6
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• pp.38-46
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• 2002

Fundamental investigations were conducted far the recovery process of waste organic solvent by fractional distillation in the aspects of equilibrium and kinetics. Mixture of toluene and xylene, which were both being used in the largest amount as industrial organic solvent, was taken as the artificial waste organic solvent and their distillation behaviors were studied. The purity of recovered solvent was investigated by Cir Chromatography and shown to be in the range of 94～98%. Based upon equilibrium calculations, the changes in the Gibbs free energy, standard enthalpy, and standard entropy for distillation reaction have been estimated. The standard enthalpy changes for toluene and xylene were shown to be 44.833 and 47.044 kJ $mol^{-1}$ respectively, which were similar to their molar heats of evaporation. The activation energies of distillation fur toluene and xylene obtained from kinetic studies were 3.281 and 2.699 kJ $mol^{-1}$ and they were about one tenths of the standard enthalpy changes of distillation reaction. The highness of the purity of recovered organic solvents suggested the possibility that the recovered waste organic sol-vent could partly replace the original solvent.

• Proceedings of the Korean Society of Propulsion Engineers Conference
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• 2009.05a
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• pp.67-70
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• 2009

Because many research using rocket grade peroxide is studied, distillation method for domestic production of rocket grade hydrogen peroxide is required. Distillation methods are very various and divided by feeding method, distillation time, distillation pressure, and so on. Among these, vacuum distillation is a suitable method for hydrogen peroxide. This method can reduce thermal decomposition and reaction with impurities. Distillation condition is determined by Raoult's law. Low vacuum level and vacuum level control are appeared as important problems of the experiment equipment, which are solved by using less leakage vacuum chamber and metering valve.