Abstract
The synthesis of 1,1-difluoroethane from acetylene as a function of HF/acetylene ratio, contact time and reaction temperature was studied on a fluorinated ${\gamma}-Al_2O_3$. The fluorination of ${\gamma}-Al_2O_3$ 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 $200^{\circ}C$. The ratio of 1,1-difluoroethane to vinylfluoride over fluorinated ${\gamma}-Al_2O_3$ 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 $200^{\circ}C$.
${\gamma}-Al_2O_3$을 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 ${\gamma}-Al_2O_3$가 불화됨에 따라 향상되었고 반응온도 $200^{\circ}C$ 정도에서 원하는 생성물인 1,1-difluoroethane의 분율이 90% 이상이었다. 불화된 ${\gamma}-Al_2O_3$촉매상에서 얻은 중간생성물인 vinylfluoride에 비해 원하는 물질인 1,1-difluoroethane의 비는 불화수소/아세틸렌 몰비가 높고 접촉시간이 큰 경우에서 높았고 반응온도 $210^{\circ}C$에서 최대의 값을 얻었다.
