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고병열,최기혁,이호인 ( Byoung Youl Coh,Ki Hyouk Choi,Ho In Lee ) 한국공업화학회 1994 공업화학 Vol.5 No.1
Temprature-programmed desorption method is a very useful technique for the research of heterogeneous catalysts. In most cases, the experimental condition is atmospheric. However, recently TPD experiments under vacuum conditions using powder catalysts give lots of very important results that can`t be obtained otherwise. In this paper, the interpretation method of TPD results and the experimental technique under vacuum conditions are introduced briefly.
축합반응에 의한 기체상의 아세톤으로부터 3,3,5-trimethyl-2-cyclohexene 의 합성에 쓰이는 불균일계 고체 염기성 Ni/CaO 촉매에 관한 연구
이호인,고병열,허진목,오호진 한국공업화학회 1999 응용화학 Vol.3 No.2
The Ni/CaO catalyst for the synthesis of 3,3,5-trimethyl-2-cyclohexene (isophorone) from acetone was studied. CaO and CaO incorporated with Co, Fe, and Cu did not show the activity. However, when 4 wt% Ni was incorporated into CaO, isophorone was much detected suggesting that Ni played an important role in catalytic activity. The 4 wt% Ni/CaO reduced at 700℃ showed 8∼50% of acetone overall conversion and 69∼85% of isophorone selectivity. With the increase of Ni loading to 20 wt%, the acetone overall conversion and the selectivity, for isophorone were decreased to 6∼24% and 40∼73%, respectively.
탄소 및 Ni 의 함유량에 따른 CaO 촉매의 표면 특성분석
이호인,조규호,고병열 한국공업화학회 1999 응용화학 Vol.3 No.2
Carbon dioxide and hydrogen adsorptions on the Ni-CaO catalyst have been investigated using temperature-programmed desorption technique under ultra-high vacuum condition. The CaO made from calcium acetate and citric acid has higher surface area with more mesopore than that made from calcium acetate only. The main factor giving these differences was carbon because the amounts of desorbed CO₂ from both surfaces were almost same. With the increase of Ni loading, the CO₂ desorption temperature increased suggesting the increase of basic strength of the catalyst. Because of the interaction between Ni and CaO, H₂ adsorbed on Ni-CaO desorbed at higher temperature than that adsorbed on nickel only catalysts.
아세톤으로부터 MIBK 의 1 단계 합성반응시 반응중간체의 거동
고병열,허진목,이호인 한국공업화학회 1998 응용화학 Vol.2 No.2
Behaviors of reaction intermediates, diacetone alcohol (DAA) and mesityl oxide (MSO) during one step synthesis of methyl isobutyl ketone (MIBK) from acetone and their relations to the catalytic activity were studied. 2wt%Ni-CaO catalyst showed very high catalytic activity, while pure CaO did not. The main factor giving this difference was the equilibrium constant, but not basic strength change by adding Ni. The condensation equilibria (K₁ = [DAA]/[acetone]² and K2 = [MSO][H₂O]/[DAA]) did not favor MSO formation, but the bifunctional Ni-CaO catalyst made it possible by both shifting the equilibrium of condensation to MSO and simultaneously hydrogenating it into MIBK. Ni site acted as dehydration site as well as hydrogenation one, and was deactivated rapidly in case of high feed rate.
승온열탈착에 의한 Ni-CaO 촉매에서의 아세톤의 흡착특성 분석
고병열,이호인,홍성진,조규호 한국공업화학회 1998 응용화학 Vol.2 No.2
Acetone adsorption on the Ni-CaO catalyst has been investigated using temperature-programmed desorption technique under ultra-high vacuum condition. Acetone adsorbed on the 2 wt%Ni-CaO catalyst decomposes mainly to carbon monoxide and hydrogen at 380℃, 590℃ and 790℃ simultaneously. With the increase of Ni loading, the acetone decomposition temperature shifts to higher temperature region suggesting that the catalyst basicity change due to Ni addition causes the weaker interaction between acetone and Ni-CaO than in case of pure CaO. So we could suggest that the added Ni decreases the Ni-CaO catalyst basicity to make the internal acetone bond strong resulting in less dissociation of acetone to hydrogen.
CaCO3 의 분해를 통한 CaO 의 제조시 Ni 의 첨가영향 및 아세톤으로부터 MIBK 의 1단계 합성반응에의 적용
이호인,고병열,허진목 한국공업화학회 1998 응용화학 Vol.2 No.1
Ni effect on the thermal decomposition of CaCO₃ into CaO and its application to single step synthesis of MIBK (methyl isobutyl ketone) from acetone was studied. Bulk calcium acetate decomposed into CaCO₃ and acetone at 450℃, and CaCO₃ into CaO and CO₂ at 700℃. When 2 wt% Ni was incorporated into calcium acetate, the decomposition temperature of CaCO₃ was decreased to 500℃ and, in case of 20 wt% Ni, this phenomenon was more drastic. From X-ray diffraction experiment, we found out that Ni-incorporated CaCO₃ did not decompose directly into CaO but via Ca(OH)₂, and consequently, into CaO. The crystallinity of CaCO₃ affected its decomposition rate. When we used 2 wt% Ni-CaO reduced at 500℃ for single step synthesis of MIBK, 60 ∼ 80% acetone overall conversion and 48∼60% MIBK selectivity were shown. But when the Ni loading was increased to 20 wt%, 73∼82% acetone overall conversion and 13∼16% MIBK selectivity were shown because of the formation of 2-propanol, one of by-products from hydrogenation at Ni site.