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손종락,이동진 한국화학공학회 1983 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.21 No.6
각각 다른 출발물질로부터 네 종류의 수산화니켈을 제조하여 이들의 성질을 X-선회절, 열분석, 적회선스펙트라를 이용하여 조사하였다. 그리고 수산화니켈을 진공분해시켜 산화니켈촉매를 얻었으며 이들의 콩기름 수소화에 대한 활성을 비교 검토하였다. 그 결과 요소의 가수 분해로 제조된 수산화니켈은 반결정성의 수화된 구조였으며, 암모니아수나, 수산화나트리움으로 침전시켜 제조된 것은 brucite 형의 육방정계의 구조를 하고 있었다. 그리고 수산화니켈의 제조 방법 및 출발물질의 상이에 따라 여러 종류의 흡착종 즉 질산기, 황산기, 이산화탄소, 요소, 암모니아에 의한 흡수띠가 적외선스펙트라에 나타났으며, 이중에서 황산기종과 질산기 종은 430℃의 높은 진공온도에서도 상당히 남아 있었다. 이들 흡착종은 촉매활성에 상당히 영향을 미쳤다. 또한 NiO(N-U) 촉매가 가장 높은 촉매활성을 나타내었으며, 400℃에서 1.5시간 동안 진공시켰을 때에 촉매활성이 최고로 나타났다. Four kinds of nickel hydroxide were prepared from different starting materials, and their properties were studied by means of X-ray diffraction, thermal analysis, and IR spectra. The nickel oxide catalysts were prepared by decomposing these nickel hydoxides in vacuo and their catalytic activity was tested for the hydrogenation of soybean oil. Consequently, it was found that nickel hydroxide prepared by urea hydrolysis was semicrystalline of hydrated structure, while the others, three kinds of nickel hydroxide precipitated by ammonium hydroxide or sodium hydroxide were all the same hexagonal system of brucite type. The various adsorbed species including nitrate ion, sulfate ion, carbon dioxide, ammonia, and urea were observed in IR spectra. Among these species, nitrate and sulfate species were so stable that they remained considerably even after evacuation at 430℃. These adsorbed species affected the catalytic activity profoundly. Also, it was found that NiO (N-U) catalyst exhibited higher catalytic activity than any other catalysts and showed a maximum activity after evacuation at 400℃ for 1.5hrs.
孫宗洛,朴萬榮,裵永一 慶北大學校 1991 論文集 Vol.51 No.-
TiO_2/SO_4^2- was prepared by precipitation from the mixed solution of titanium chloride and hydrochloric acid followed by modification with sulfuric acid. The characterization of prepared catalyst was performed by using IR. XPS, XRD and DT-TGA. Infrared spectra of TiO_2/SO_4^2- showed bidentate sulfate ion coordinated to the surface of TiO_2. The acid strength of modified catalyst was at least Ho≤-14.52, showing the superacidic properties which are attributed to the double bond nature of S=O of the complex formed by the interaction of TiO_2 with sulfate ion. For TiO_2/SO_4^2-, the specific surface area increased and the transition from the amorphous to anatase phase occured at a higher temperature, as compared with pure TiO_2.
손종락,김해원,배영일 한국화학공학회 1989 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.27 No.3
ZrOCl₂ 용액으로부터 Zr(OH)₄ 침전물을 만들고 이어서 인산이나 붕산으로 표면을 변화시켜 ZrO₂/PO₄^(-3) 및 ZrO₂/BO₃^(-3) 촉매를 각각 제조하였다. 이들 촉매의 특성을 적외선 spectra, X-선 회절 및 시차열분석으로 조사하였다. 그 결과 순수한 ZrO₂에 비하여 산으로 표면이 변화된 ZrO₂ 촉매는 무정형에서tetragonal phase로 전이되는 온도가 150-200℃ 정도 높았으며 비포면적도 약 40-50㎡/g 정도 증가하였다. 그리고 산의 세기도 Hoscale로 2.6-5.2단위 증가하였다. ZrO₂/PO₄^(-3) and ZrO₂/BO^(-3) catalysts were prepared by precipitation from the solution of zirconium oxychloride followed by modification with phosphoric acid and boric acid, respectively. The characterization of prepared catalysts was examined by infrared spectra, X-ray diffraction and differential thermal analysis. On the basis of the results obtained from X-ray diffraction and DTA for ZrO₂ modified with acids, the transition temperature from amorphous to tetragonal phase was high by 150-200℃ and the specific surface area increased by about 40-5O ㎡/g, as compared with pure ZrO₂. The acid strength of modified catalysts increased by 2.6-5.2 unit as Ho scale.
共沈澱法에 依하여 調製한 酸化 Nickel-Silica系 觸媒의 Ethylene 二量化
孫宗洛 慶北大學校 1978 論文集 Vol.25-26 No.-
共沈澱方法에 依하여 酸化 nickel-silica觸媒를 調製하여 ethylene 二重化活性을 硏究하였다. ethylene二重化에 대한 酸化 nickel-silica의 活性은 脫水에 依한 것으로 증명되었다. 低溫의 眞空處理에 있어서는 觸媒의 活性點이 Bro¨nsted酸이었으나, 高溫의 경우에는 活性點이 Lewis酸이었다. 또한 觸媒의 活性能은 觸媒의 表面積과 酸化 nickel의 量에 依存되었다. The nickel oxide-silica catalysts were prepared by coprecipitation method and their activities of ethylene dimerization were studied by the conventional static apparatus. The activation of nickel oxide-silica for ethylene dimerization was proved to be due to the dehydration of catalyst. It was shown that the active site for dimerization was Bro¨nsted acid for the lower evacuation temperature but was Lewis acid for the higher evacuation temperature. The activity of catalyst was dependant on the specific surface area and nickel oxide % in the catalyst.
손종락,류삼곤 ( Jong Rack Sohn,Sam Gon Ryu ) 한국공업화학회 1992 공업화학 Vol.3 No.4
분말의 Zr(OH)_4를 (NH_4)2_CrO_4수용액에 함침시킨 후 공기중에 소성하여 질코니아에 담지된 산화크롬 촉매를 제조하였다. 제조된 CrO_x/ZrO_2 촉매상에 cumene을 반응시켜 산화-환원 거동을 연구한 결과 크롬의 산화상태가 +6인 chromate형태로 질코니아 표면에 존재할 때는 강한 산점이 생성되어 cumene의 탈알킬화 반응에 촉매활성을 나타내었다. 그러나 많은 양의 Cr^(6+)종은 반응중에 탈수소로 생성된 H_2에 의하여 환원되어 Cr^(3+)종으로 변화되었으며 Cr^(3+)종은 cumene을 탈수소화시켜 α-methyl styrene을 생성하는 반응에 활성점으로 작용하였다. 환원된 Cr^(3+)종은 0_2로 처리하면 다시 Cr^(6+)종으로 되고 따라서 산화된 촉매는 cumene의 탈알킬화 반응에 활성을 나타내었다. Chromium oxide/zirconia catalysts were prepared by dry impregnation of Zr(OH)_4 powder with aqueous solution of (NH_4)_2CrO_4 followed by calcining in air. The redox behavior of prepared catalysts were investigated by reacting cumene as test material over catalysts. As a result it was found that Cr^(6+) species(as chromate) on the surface of catalyst was responsible for the formation of strong acid site and the catalytic activity for the dealkylation of cumene. However, much of the Cr^(6+) species was reduced to Cr^(3+) species by H_2 formed during the catalytic reaction of cumene and the reduced Cr^(3+) species was an active site for dehydrogenation of cumene to form α-methyl styrene. The reduced Cr^(3+) species was also reoxidized to a Cr^(6+) species after treatment with O_2 and consequently the reoxidized catalyst exhibited catalytic activity for the dealkylation reaction of cumene.