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Received June 8, 2013
Accepted September 3, 2013
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N-vinyl-2-pyrrolidone과 2-pyrrolidone 혼합물의 고-액 상평형 및 용융결정화를 이용한 N-vinyl-2-pyrrolidone의 결정성장속도 연구
Studies of Solid-Liquid Phase Equilibria for Mixtures of N-vinyl-2-pyrrolidone+2-pyrrolidone and Growth Rate of N-vinyl-2-pyrrolidone Crystal Using Melt Crystallization
고려대학교 화공생명공학과, 136-713 서울시 성북구 안암동 5-1 1경희대학교 화학공학과, 446-701 경기도 용인시 기흥구 서천동 1번지
Department of Chemical and Biological Engineering, Korea University, 5-1 Anam-dong, Sungbuk-gu, Seoul 136-713, Korea 1Department of Chemical Engineering, Kyung Hee University, 1 Seocheon-dong, Giheung-gu, Yongin-si, Gyeonggi 446-701, Korea
jwkang@korea.ac.kr
Korean Chemical Engineering Research, October 2013, 51(5), 587-590(4), 10.9713/kcer.2013.51.5.587 Epub 1 October 2013
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Abstract
N-vinyl-2-pyrrolidone (NVP)에 포함된 불순물인 2-pyrrolidone을 제거하기 위해 용융결정화가 이용될 수 있으며, 그 기본 연구로써 두 물질의 고-액 상평형을 측정하였다. 시차주사 열량계(DSC)와 결정화기를 이용하여 얻어진 두 실험 결과는 비슷한 경향을 보였으며, NVP와 2-pyrrolidone으로 구성된 2성분계 혼합물이 공융계를 형성함을 보였다. 간단한 열역학 식을 이용하여 혼합물의 상평형과 공융점(eutectic point)을 계산하였으며 실험결과와 비교적 잘 일치하였다. 결정화 공정의 설계에 중요한 요소인 결정성장속도를 알기 위해 판형 결정화기를 이용하여 시간에 따른 NVP 결정의 두께를 측정하였다. 냉각온도가 낮을수록 NVP의 결정성장속도가 증가하였다. 실험데이터로부터 상관된 열전달계수는 결정의 성장 거동을 잘 설명하였다.
Solid-liquid equilibria for mixtures composed of n-vinyl-2-pyrrolidone (NVP) and 2-pyrrolidone were measured as a basic study for the melt crystallization process to remove 2-pyrrolidone as impurity included in NVP. A differential scanning calorimeter (DSC) and a crystallizer were used and the experimental results obtained from two methods were similar. The mixture showed a eutectic system which has a single composition at the minimum melting temperature. Calculation results from simple thermodynamic equations were found in general agreements with present data. To determine the growth rate of NVP crystal which is important for the design of crystallization process, thicknesses of the crystal were measured with the time using a layer melt crystallizer. The growth rates increased as cooling temperatures decreased. Heat transfer coefficient correlated from present data was found to successfully describe the crystal growth behavior.
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References
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Lide DR, CRC Handbook of Chemistry and Physics, 78th ed., CRC Press, Boca Raton, New York (1997)
