Applied Chemistry for Engineering (공업화학)

The Korean Society of Industrial and Engineering Chemistry (한국공업화학회)
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High-Purity Purification of Indole Contained in Coal Tar Fraction - Separation of Close Boiling Mixtures of Indole by Solute Crystallization -

콜타르 유분 중에 함유된 인돌의 고순도 정제 - 용액 결정화에 의한 인돌 유사 비점 혼합물의 분리 -

  • Kim, Su Jin (Department of Materials Science and Applied Chemistry, Chungwoon University) ;
  • Kang, Ho-Cheol (Green Chemistry Division, Korea Research Institutes of Chemical Technology) ;
  • Jeong, Hwa Jin (Department of Fashion & Textile Engineering, Chungwoon University)
  • 김수진 (청운대학교 신소재응용화학과) ;
  • 강호철 (한국화학연구원 그린화학연구단) ;
  • 정화진 (청운대학교 패션섬유공학과)
  • Received : 2010.01.24
  • Accepted : 2010.02.04
  • Published : 2010.04.10
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Abstract

The purification of indole from 54.3wt% indole fraction (temperature range of distillate: $250{\sim}255^{\circ}C$) recovered by extraction-distillation combination of coal tar fraction (temperature range of distillate: $240{\sim}265^{\circ}C$) was examined by solute crystallization. The feed consists of eight components such as quinoline, iso-quinoline, indole, quinaldine, 1-methylnaphthalene, 2-methylnaphthalene, biphenyl and phenyl ether. Hexane and an aqueous solution of methanol (50 : 50 vol%) were used as the crystallization solvent and the coolant, respectively. A batch stirred tank of glass material was used as a crystallization apparatus. By increasing the operation temperature and the volume ratio of solvent to feed at initial, the purity of indole increas ed, but yields of indole showed a decreasing tendency. Solute crystallization method using hexane as a solvent was excellent because the purity of 99.3 wt% indole was recovered at the yield of 50% without washing operation.

콜타르 유분(유출온도범위: $240{\sim}265^{\circ}C$)으로부터 추출-증류의 조합에 의해 회수한 54.3 wt% 인돌 유출액(유출온도범위 $250{\sim}255^{\circ}C$)을 원료로 사용하여 용액 결정화 조작을 행해 인돌의 고순도 정제를 검토했다. 원료 유출액은 8성분(quinoline, iso-quinoline, indole, quinaldine, 1-methylnaphthalene, 2-methylnaphthalene, biphenyl, phenyl ether)으로 구성되어 있다. 결정화 조작의 용매로서는 노말헥산을, 냉매로서는 메탄올 수용액(50 : 50 vol%)을 각각 사용하였으며, 결정화 장치로서는 재킷이 부착된 pyrex제 유리 회분 교반기를 사용했다. 결정화 온도와 용매/원료의 초기 체적비의 증가는 인돌의 순도를 향상시켰으나, 역으로 수율을 저하시켰다. 석출된 결정의 세정조작 없이, 노말헥산을 용매로 사용한 용액 결정화 조작에 의해 고순도(99.3 wt%)의 인돌을 고수율(50%)로 회수할 수 있었다.

Keywords

Acknowledgement

Supported by : 청운대학교

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