Quantitative Extraction Analysis of Brominated Flame Retardant Substances Using Supercritical-Fluid Method for Environmental Assessment

초임계추출법을 이용한 브롬계 난연제 화합물 환경성 평가 추출효율 분석 연구

  • Oh, Min-Kyung (Department of Polymer Science and Engineering, SAINT, Sungkyunkwan University) ;
  • Yoon, Sang-Hwa (Department of Polymer Science and Engineering, SAINT, Sungkyunkwan University) ;
  • Lee, Young-Kwan (Department of Chemical Engineering, SAINT, Sungkyunkwan University) ;
  • Han, Jae-Sung (SGS Testing Korea Co., Ltd.) ;
  • Won, Sung-Ho (Microelectronic Packaging R&D Center, Sungkyunkwan University) ;
  • Nam, Jae-Do (Department of Polymer Science and Engineering, SAINT, Sungkyunkwan University)
  • 오민경 (성균관대학교 고분자공학과) ;
  • 윤상화 (성균관대학교 고분자공학과) ;
  • 이영관 (성균관대학교 화학공학과) ;
  • 한재성 ;
  • 원성호 (성균관대학교 마아크로전자패키징연구소) ;
  • 남재도 (성균관대학교 고분자공학과)
  • Published : 2008.01.31

Abstract

For the evaluation of brominated flame retardants included in polymeric electronic devices, we investigated the extraction methods and solvent systems for four different types of polymers of PC (polycarbonate), PP (polyropylene), PET (poly(ethylene terephthalate)) and PBT (poly(butylene terephthalate)) using different solvent systems of hexane/acetone, THF, toluene, and THF/toluene. In order to compare the extraction efficiency of different methods and solvent systems, the deca-BDE (decabromo diphenyl ether) flame retardant was included in PC, PP, PET and PBT systems and subsequently extracted by soxhlet, ultrasonic, accelerated solvent, microwave and supercritical fluid extraction methods. The amount of the extracted flame retardant was monitored to evaluate the extraction efficiency. The ultrasonic extraction method was found not to be acceptable as an extraction method for the polymer systems mainly due to a low salvation efficiency of the organic solvents. Soxhlet, accelerated solvent and microwave extraction methods exhibited over 80% of extraction efficiency for toluene. The supercritical fluid extraction method, which has been used as an extraction method for flame retardants in polymers, showed the extraction efficiencies of ca. 100% for PC and PP in the optimal extraction conditions of $60^{\circ}C$ and 120 bar.

전기 전자재료 중 고분자에 포함된 브롬계 난연제의 분석에 있어 용출이 어려운 4가지 재질 PC(polycar-bonate) PP(polypropylene), PET(poly(ethylene terephthalate)), PBT(poly(butylene terephthalate))에 대하여 추출방법 및 헥산/에세톤, THF, 톨루엔, THF/톨루엔에 대한 용매 특이성과 그 특성을 고찰하였다. 각 고분자에서의 deca-BDE(decabromo diphenyl ether)의 함량을 속슬렛, 초음파. 가속용매, 마이크로파, 초임계 유체 추출법을 사용하여 이들 방법의 효율을 정량분석 하였다. 초음파 추출은 낮은 고분자의 용해도 때문에 낮은 추출효율을 보여 사용한 고분자의 경우에 있어서 추출방법으로는 적합하지 않았으며, 나머지 3가지 방법에서는 톨루엔 사용시 약 80% 이상의 높은 추출효율을 보였다. 초임계 유체 추출은 고분자의 난연제 추출에 시도되지 않았던 방법이었으나, 본 실험에서 PP와 PC의 추출에서는 100%에 가까운 매우 높은 추출효율을 보였다.

Keywords

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