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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.
이호인,허진목,오호진 한국공업화학회 1999 응용화학 Vol.3 No.2
Coupling reaction of methane and acetonitrile to form high value-added material was studied. The coupling reaction was conducted in non-oxidative condition to attain the target material with high selectivity by preventing the reactants from oxidation. As a result, propionitrile, coupled form of methane and acetonitrile, was produced on Ni/MgO catalyst with about 35% yield. In this non-oxidative condition, the byproduct due to the oxidation of reactants was not observed and so the selectivity to propionitrile amounted to nearly 100%. Li/MgO catalyst which has been known as a active catalyst for this model reaction in oxidative condition showed less than 0.2% acetonitrile conversion in the range of 400 ℃ ∼ 650 ℃ reaction temperature. Whereas, in this case, the main product was acrylonitrile, dehydrogenated form of propionitrile. In the non-oxidative coupling reaction of methane and acetonitrile, the rate-determining step was methane activation, and the Ni component doped played a major role in methane activation.
K 이온이 첨가된 MgO 촉매에 의한 아크릴로니트릴 합성
이호인,허진목 한국공업화학회 2000 응용화학 Vol.4 No.2
K ion-added MgO catalysts were prepared by using KOH, KNO₃ or KCl as the precursor of K ion and applied to the coupling reaction of methanol and acetonitrile to form acrylonitrile. The reaction proceeds via acetonitrile carbanion intermediate which is formed on surface base site. The catalytic activity calculated by acetonitrile conversion was in the order KOH-added MgO > KNO₃-added MgO > KCl-added MgO which was in agreement with the trend of basic strength of the catalysts measured by CO₂-TPD. However, the selectivity to acrylonitrile was in the opposite order and the main by-product was propionitirle, the hydrogenated form of acrylonitrile. This suggests that hydrogenation also occurred an base site in this reaction. When CO₂ was introduced in the reaction system, acetonitrile conversion was increased suggesting that CO₂ played a role of mild oxidant in this reaction. Acetonitrile conversion and acrylonitrile selectivity over KNO₃-added MgO were 22.3% and 79.0%, respectively.
K/MgO 촉매상에서의 메탄올과 아세토니트릴의 결합반응
이호인,허진목 한국공업화학회 2000 응용화학 Vol.4 No.1
K/MgO-catalyzed coupling reaction of methanol and acetonitrile to form acrylonitrile was studied. In non-oxidative atmosphere, the doping of K enhanced the catalytic activity of MgO resulting in the increase of acetonitrile conversion. However, propionitrile, the hydrogenated form of acrylonitrile, was the main product. Thermodynamic analysis showed that oxidative condition is necessary to suppress the production of propionitrile and raise the acrylonitrile selectivity. When oxygen was introduced in the reaction system, both acetonitrile conversion and acrylonitrile selectivity were increased. Oxygen facilitated acrylonitrile synthesis reaction and prevented the hydrogenation of acrylonitrile to propionitrile. However, introduced oxygen caused overoxidation of reactants and products to COx. In case of using carbon dioxide as a mild oxidant, overoxidation was not appreciably observed and catalytic activity was also enhanced.
고체 염기촉매에 의한 메탄올과 아세토니트릴로부터의 아크릴로니트릴 생성에 있어서 산소의 영향
이호인,고병열,허진목 한국공업화학회 1998 응용화학 Vol.2 No.1
We have studied the catalytic combustion of soot particulate over perovskitetype oxides prepared by malic acid method. The catalysts were modified to enhance the activity by substitution of metal into A or B site of perovskite oxide. In addition, the reaction conditions, such as temperature, O₂ concentration, space velocity have been studied. The effect of SO₂ pretreatment and water introduced into reactants were also examined. In the LaCoO₃ catalyst, the partial substitution of alkali metals into A site enhanced the catalytic activity in the combustion of soot particulate and the activity was shown in the order: Cs$gt;K$gt;Na; In the Lao_0.6Cs_(0.4)CoO₃ catalyst, the substitution of Fe or Mn showed no effect on the ignition temperature. The ignition temperature decreased with increasing O₂ concentration and contact time. The introduction of water into reactants feed decreased the ignition temperature and the pretreatment of SO₂ showed no effect on the catalytic activity.
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.