Applied Chemistry for Engineering (공업화학)

The Korean Society of Industrial and Engineering Chemistry (한국공업화학회)
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Optimization of MOF-235 Synthesis by Analysis of Statistical Design of Experiment

통계학적 실험계획법 해석을 통한 MOF-235 합성 최적화

  • Chung, Mingee (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)
  • 정민지 (서울과학기술대학교 화공생명공학과) ;
  • 유계상 (서울과학기술대학교 화공생명공학과)
  • Received : 2019.08.20
  • Accepted : 2019.09.04
  • Published : 2019.10.10
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Abstract

Statistical design of experiments was performed to optimize MOF-235 synthesis process. Concentrations of terephthalic acid (TPA), iron (III) chloride hexahydrate, N,N-dimethylformamide (DMF) and ethanol were important factors to develop the crystal structure of MOF-235. MOF-235 was synthesized with various concentrations of the listed chemicals above and the crystallinity was measured by XRD. The effect of the composition on the synthesis of MOF-235 was evaluated using a statistical analysis. For the variance analysis using F-test, the concentration of ethanol showed the greatest effect on the crystallinity and TPA the least influential. A regression model for predicting the crystallinity of MOF-235 was derived and the prediction results for two synthetic variables were presented using contour plots. Finally, the crystallinity was predicted by a mixture method with $FeCl_3$, ethanol and DMF.

통계학적 실험계획법을 이용하여 다공성 구조체인 MOF-235 합성 공정 최적화를 수행하였다. 합성에 사용되는 주성분인 terephthalic acid (TPA), Iron (III) chloride hexahydrate, N,N-dimethylformamide (DMF) 및 ethanol의 농도가 MOF-235의 결정구조를 형성하는데 중요한 요소가 되었다. 다양한 농도의 4가지 성분을 이용하여 MOF-235를 합성한 후 XRD를 이용하여 결정도를 측정하였다. 16가지 실험조건을 통해 합성한 MOF-235의 결정도 결과를 통계학적 해석을 통해 주성분의 조성이 입자의 합성에 미치는 영향을 분석하였다. F 검정법을 이용한 분산분석에서 에탄올의 농도가 입자의 결정도에 가장 큰 영향을 미치고 TPA가 가장 영향력이 작은 것으로 분석되었다. 결정도를 예측할 수 있는 회귀모델을 도출하였고 2가지 합성변수에 대한 예측결과를 등고선도를 이용하여 제시하였다. 마지막으로 혼합물법을 이용하여 3가지 합성인자가 미치는 결정도를 예측하여 제시하였다.

Keywords

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