불화된 γ-Al<SUB>2</SUB>O<SUB>3</SUB>상에서 아세틸렌으로부터 1,1-difluoroethane의 합성

이윤우; 이경환; 임종성; 김재덕; 이윤용

Journal of the Korean Industrial and Engineering Chemistry, Vol.9, No.5, 629-633, October, 1998

Export Citation

불화된 γ-Al₂O₃상에서 아세틸렌으로부터 1,1-difluoroethane의 합성

1,1-Difluoroethane Synthesis from Acetylene over Fluorinated γ-Al₂O₃

이윤우, 이경환, 임종성, 김재덕, 이윤용

초록

γ-Al₂O₃을 불화한 촉매상에서 아세틸렌으로부터 1,1-difluoroethane을 합성하는 실험을 반응물질의 몰비와 접촉시간, 그리고 반응온도를 변화하여 실시하였다. 촉매의 불화는 무수 불화수소로 고온에서 행하였다. 제조된 시료는 XRD에 의한 결정성, 질소 흡착에 의한 세공성, 그리고 피리딘-IR과 암모니아-TPD에 의한 산 특성을 측정하였다. 촉매의 활성은 γ-Al₂O₃가 불화됨에 따라 향상되었고 반응온도 200℃ 정도에서 원하는 생성물인 1,1-difluoroethane의 분율이 90% 이상이었다. 불화된 γ-Al₂O₃ 촉매상에서 얻은 중간생성물인 vinylfluoride에 비해 원하는 물질인 1,1-difluoroethane의 비는 불화수소/아세틸렌 몰비가 높고 접촉시간이 큰 경우에서 높았고 반응온도 210℃에서 최대의 값을 얻었다.

The synthesis of 1,1-difluoroethane from acetylene as a function of HF/acetylene ratio, cantact time and reaction temperature was studied on a fluorinated γ-Al₂O₃. The fluorination of γ-Al₂O₃ was treated with pure HF gas at high temperature. The crystallinity, the porosity, and the acid properties of the prepared samples were examined using XRD, the nitrogen adsorption, pyridine-IR and ammonia-TPD respectively. The activity was enhanced by further fluorination of alumina. The fraction of 1,1-difluoroethane was obtained above 90% at reaction temperature of about 200℃. The ratio of 1,1-difluoroethane to vinylfluoride over fluorinated γ-Al₂O₃ catalyst was increased with the mole ratio of HF/acetylene and contact time, and was found to be the highest ratio at reaction temperature of 210℃.

Keywords:1;1-difluoroethane;Fluorinated γ-Al₂O₃;Vinylfluoride;Acetylene

[References]

Molina RT, Roland FS, Nature, 249, 810 (1974)
UNEP, "Montreal Protocol on Substance that Deplete the Ozone Layer," Final act (1987)
이윤우, 이윤용, 공기조화, 냉동공학, 108, 11 (1992)
이윤용, 이윤우, "HFC-152a 제조공정개발," KIST연구보고서 BSN888(3)-4687-6 (1992)
Manzer LE, Rao VNM, Adv. Catal., 39, 329 (1993)
Joint Committe on Powder Diffraction Standards, Number 29-63 (18-24 and 20-6) (1979)
Ghosh AK, Kydd RA, Catal. Rev.-Sci. Eng., 27, 539 (1985)
Bautista FM, Campelo JM, Garcia A, Luna D, Marinas JM, Romero AA, Navio JA, Macias M, J. Catal., 145(1), 107 (1994)
Farrokhnia A, Sakakini B, Waugh KC, J. Catal., 174(2), 219 (1998)
Pazderskii YA, Agroskon II, Flid RM, Kinet. Katal., 10, 415 (1969)

[Referenced By]

[1] Molina RT, Roland FS, Nature, 249, 810 (1974)

[2] UNEP, "Montreal Protocol on Substance that Deplete the Ozone Layer," Final act (1987)

[3] 이윤우, 이윤용, 공기조화, 냉동공학, 108, 11 (1992)

[4] 이윤용, 이윤우, "HFC-152a 제조공정개발," KIST연구보고서 BSN888(3)-4687-6 (1992)

[5] Manzer LE, Rao VNM, Adv. Catal., 39, 329 (1993)

[6] Joint Committe on Powder Diffraction Standards, Number 29-63 (18-24 and 20-6) (1979)

[7] Ghosh AK, Kydd RA, Catal. Rev.-Sci. Eng., 27, 539 (1985)

[8] Bautista FM, Campelo JM, Garcia A, Luna D, Marinas JM, Romero AA, Navio JA, Macias M, J. Catal., 145(1), 107 (1994)

[9] Farrokhnia A, Sakakini B, Waugh KC, J. Catal., 174(2), 219 (1998)

[10] Pazderskii YA, Agroskon II, Flid RM, Kinet. Katal., 10, 415 (1969)