[논문]Kinetics and Optimization of Dimethyl Carbonate Synthesis by Transesterification using Design of Experiment

Lee, Kilwoo; Yoo, Kye Sang

doi:10.9713/kcer.2018.56.3.416

Kinetics and Optimization of Dimethyl Carbonate Synthesis by Transesterification using Design of Experiment 원문보기

Korean chemical engineering research = 화학공학, v.56 no.3, 2018년, pp.416 - 420

Lee, Kilwoo (Department of Chemical & Biomolecular Engineering, Seoul National University of Science & Technology) , Yoo, Kye Sang (Department of Chemical & Biomolecular Engineering, Seoul National University of Science & Technology)

Abstract ▼ AI-Helper

A comprehensive kinetic study has been conducted on dimethyl carbonate synthesis by transesterification reaction of ethylene carbonate with methanol. An alkali base metal (KOH) was used as catalyst in the synthesis of DMC, and its catalytic ability was investigated in terms of kinetics. The experiment was performed in a batch reactor at atmospheric pressure. The reaction orders, the activation energy and the rate constants were determined for both forward and backward reactions. The reaction order for forward and backward reactions was 0.87 and 2.15, and the activation energy was 12.73 and 29.28 kJ/mol, respectively. Using the general factor analysis in the design of experiments, we analyzed the main effects and interactions according to the MeOH/EC, reaction temperature and KOH concentration. DMC yield with various reaction conditions was presented for all ranges using surface and contour plot. Furthermore, the optimal conditions for DMC yield were determined using response surface method.

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가설 설정

Furthermore, the interaction which is the effect of one factor depending on the level of the other factor is illustrated in Fig. 6. The interaction effect was higher in the condition where the main effect degree of each factor was small. The second-order polynomial equation was selected to predict the yield of DMC according to the reaction conditions.
In this work, we proposed kinetic performance of KOH catalyst and estimated the rate constants and the reaction orders in DMC synthesis, for both forward and backward reactions. Moreover, the effects of reaction conditions and their interactions on the catalytic performance were studied simultaneously on the responses using design of experiments.

제안 방법

The results will be informative for developing the reaction process of DMC synthesis. In this study, the optimum reaction process for synthesizing DMC was proposed using experimental design method. In the analysis using general factorial experiments, MeOH / EC, reaction temperature and catalyst concentration were found to be major factors.
In general, the experimental design method is designed to obtain maximum information at a low cost in an experiment. The experiment consists of a design step, an analysis step of the experimental data, and an optimization step [6]. In the design stage of the experiment, the selection of the experiments and the randomization, which is the order of the experiment, are determined to achieve the purpose of the experiment efficiently and practically.
To analyze the main effects and interactions of the reaction conditions in the synthesis of DMC, the MeOH/EC molar ratio, reaction temperature, and KOH concentration were used as experimental parameters. First, we performed Minitab 17 using the general factorial method, which is used when the level of all the factors is not 2 level.

대상 데이터

Starting materials used in this work were methanol (purity ≥ 99.5%) produced by Daejung Chemicals & Metals Co., and ethylene carbonate (≥ 98% from Aldrich), dimethyl carbonate (≥ 99%, Acros) and ethylene glycol (EG) (≥ 99%, Daejung) without further purification.

이론/모형

For that reason, the equation derived here is limited to the quadratic equation. The correlation coefficient was calculated by the nonlinear regression method (using Minitab 17 program) as Equation (10).

참고문헌 (7)

Pacheco, M. A. and Marshall, C. L., "Review of Dimethyl Carbonate (DMC) Manufacture and Its Characteristics as a Fuel Additive," Energ. Fuels, 11, 2-29(1997).

상세보기
Tatsumi, T., Watanabe, Y., Koyano, K. A., "Synthesis of Dimethyl Carbonate from Ethylene Carbonate and Methanol Using TS-1 as Solid Base Catalyst," Chem. Commun, 19, 2281-2282(1996).
Watanabe, Y., Tatsumi, T., "Hydrotalcite-type Materials as Catalysts for the Synthesis of Dimethyl Carbonate from Ethylene Carbonate and Methanol," Micropor. Mesopor. Mater., 22, 399-407(1998).

상세보기
Knifton, J. F., Duranleau, R. G., "Ethylene Glycol-dimethyl Carbonate Cogeneration," J. Mol. Catal., 67, 389-399(1991).

상세보기
Han, M. S., Lee, B. G., Ahn, B. S., Park, K. Y. and Hong, S. I., "Kinetics of Dimethyl Carbonate Synthesis from Ethylene Carbonate and Methanol using Alkalimetal Compounds as Catalysts," React. Kinet. Catal. Lett., 73, 33-38(2001).

상세보기
Walpole, R. E., Ye, K. E., Raymond, H. M. and Myers, S. L., Probability and Statistics for Engineers and Scientists, 9th ed., 639-652, Prentice Hall, Boston, USA(2012).
Mason, R. L., Gunst, R. F. and Hess, J. L., Statistical Design and Analysis of Experiments, with Applications to Engineering and Science, 2nd ed., 568-597, Wiley-Interscience, New Jersey, USA (2003).

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DOI : 10.9713/kcer.2018.56.3.416 [무료]
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