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Salicyladoxime 에 의한 금속 추출에 관한 연구
신정호,박상욱,박대원,이경수,정갑섭 ( Jeong Ho Shin,Sang Wook Park,Dae Won Park,Kyung Soo Lee,Kap Seop Jeong ) 한국공업화학회 1993 공업화학 Vol.4 No.1
salicylaldoxime에 의한 Cu의 용매추출에 있어서 추출평형 및 추출속도 등을 고찰하였다. 흡광도 측정으로부터 oxime의 분배정수와 해리정수를 구하고, oxime-Cu착화합물의 안정도 상수와 분배정수, 분자흡광계수 및 추출평형정수를 결정하였다. chloroform 및 benzene 용매하에 salicylaldoxime에 의한 Cu의 추출 화학종은 1:2의 형태인 CuR_2였으며, 초기 추출속도실험으로부터 salicylaldoxime-chloroform에 의한 Cu의 총괄추출속도는 R=k[Cu^(2+)][HR]^(0.5)/[H^+]^(0.4)로 표시되었다. The kinetic and equilibrium characteristics of copper extraction by salicylaldoxime in chloroform and benzene were investigated. Equilibrium constants such as dissociation constant, distribution coefficient of salicylaldoxime and stability constant, distribution coefficient and molar extinction coefficient of oxime-Cu chelate were determined from absorbance. Extracted species of Cu-chelate were found to be CuR_2. Overall initial extraction rate of copper by salicylaldoxime in chloroform was expressed by the following equation : R=k[Cu^(2+)][HR]^(0.5)/[H^+]^(0.4).
박상욱,문진복,신정호,박대원,김종현 ( Sang Wook Park,Jin Bok Moon,Jeung Ho Shin,Dae Won Park,Jong Hyeon Kim ) 한국공업화학회 1993 공업화학 Vol.4 No.1
교반기를 사용하여 n-butyl acetate의 알카리 가수분해반응의 액-액 불균일계에서 n-butyl acetate의 총괄물질전달속도를 측정하여 실험변수와의 관계를 고찰하고, 화학반응을 수반한 물질전달기구를 경막설에 적용하여 용질에 대한 확산방정식의 근사해로부터 구한 n-butyl acetate의 반응촉진계수의 이론값과 측정값을 비교하여 물질전달계수를 구하였다. 이로부터 분산용액의 액적 면적을 산출할 수 있었다. The rates of overall mass transfer of n-butyl acetate in the alkaline hydrolysis of n-butyl acetate were measured by using a mechanically agitated vessel in order to get the relationship between the mass transfer rates and experimental variables. The interfacial area between liquid-liquid heterogeneous phases could be obtained by comparing the theoretical values of reaction enhancement factor from an approximated solution of a diffusion equation based on the film theory with the experimental data.
폴리에틸렌글리콜 상이동 촉매상에서 니트로벤젠과 Fe(Co)5 로부터의 아닐린 합성
오소영,천승우,박대원,박상욱,신정호 ( So Young Oh,Sung Woo Chun,Dae Won Park,Sand Wook Park,Jung Ho Shin ) 한국공업화학회 1992 공업화학 Vol.3 No.4
Ironpentacarbonyl에 의한 니트로벤젠의 환원반응에 PEG를 상이동 촉매로 사용한 결과 상온에서 90% 이상의 아닐린 수율을 얻을 수 있었다. 니트로벤젠의 반응속도는 PEG의 사슬길이와 결합점의 수에 의존하였으며 NaOH의 농도가 높고 용매의 극성이 커질수록 증가하였다. 그러나 아닐린의 수율은 NaOH농도가 2N일때 최대였으며 그 이상의 농도에서는 감소하였다. PEG phase transfer catalyzed reduction of nitrobenzene with Fe(CO)_5 afforded aniline up to over 90% yield at room temperature. The reaction rate of nitrobenzene was dependent on the chain length and number of binding sites of PEG, and it was increased with the concentration of NaOH and solvent polarity. But the yield of aniline was maximum with 2N NaOH solution and it was decreased at higher concentrations.
Aliquat 336에 의한 액 - 액 불균일계에서 n - butyl acetate 의 가수분해 및 상전이 촉매의 물질전달
박상욱,문진복,박대원,신정호 ( Sang Wook Park,Jin Bok Moon,Dae Won Park,Jeung Ho Shin ) 한국화학공학회 1993 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.31 No.1
Constants of the distribution and dissociation equilibria of tricaprylmethyl ammonium chloride (Aliquat 336; Q^+Cl^-) were measured for the organic phase(toluene, n-butyl acetate)-aqueous phase(water, NaCl, NaOH) system. The enhancement factors of Q^+Cl^- were measured with a Lewis cell, and compared with those predicted from the theoretical model based on the film theory corrected by the Leveque model. A diffusion-reaction model was proposed to explain the mechanism of n-butyl acetate hydrolysis with a phase transfer catalyst(Aliquat 336), and the overall reaction rates observed were compared with those calculated by the proposed model. The reaction rate constant evaluated by fitting the rate data to model prediction was 36 ㎥/kmol·s at 298 K, which was about 100 times greater than that of alkaline hydrolysis in the aqueous phase without using a catalyst.
PEG/γ-Al<sub>2</sub>O<sub>3</sub> 상이동 촉매상에서 니트로벤젠과 Fe(CO)<sub>5</sub>로부터의 아닐린 합성
오소영,이화수,박대원,박상욱,신정호,Oh, So-Young,Lee, Hwa-Su,Park, Dae-Won,Park, Sang-Wook,Shin, Jung-Ho 한국공업화학회 1993 공업화학 Vol.4 No.1
${\gamma}-Al_2O_3$, ${\alpha}-Al_2O_3$, $SiO_2$, $TiO_2$등에 고정화된 폴리에틸렌글리콜을 $Fe(CO)_5$에 의한 니트로벤젠의 상온 환원반응에 상이동 촉매로 사용하였다. 고정화된 PEG의 몰수는 담체의 비표면적에 따라 증가하였고 PEG/${\gamma}-Al_2O_3$가 가장 좋은 활성을 나타내었다. PEG의 사슬길이가 길고 NaOH 농도가 높을수록 반응속도가 증가하였다. 적외선분광기를 이용하여 반응기구에 대한 고찰도 함께 실시하였으며 폴리에틸렌글리콜 상이동 촉매는 본 반응의 활성물질로 알려진 $HFe(CO)_4{^{-}}$이온의 생성과 이의 유기상으로의 이동을 촉진시키는 것으로 판단되었다. Immobilized polyethylene glycols onto metal oxides such as ${\gamma}-Al_2O_3$, ${\alpha}-Al_2O_3$, $SiO_2$ and $TiO_2$ were used as phase transfer catalysts for the room temperature synthesis of aniline from nitrobenzene and ironpentacarbonyl. The amount of attached PEG molecules increased with specific surface area of metal oxides. Among the immobilized catalysts tested PEG/${\gamma}-Al_2O_3$ showed the highest activity. The reaction rate increased with the chain length of PEG mole-cules and the aqueous NaOH concentration. Mechanistic study carried out using infrared spectrometer revealed that the role of PEG was to increase the formation of $HFe(CO)_4{^-}$ ion, which is known as active species, and its movement from aqueous to organic phase.
Aliquat 336의 분배 , 해리 평형 및 물질전달
박상욱,문진복,박대원,신정호 ( Sang Wook Park,Jin Bok Moon,Dae Won Park,Jeung Ho Shin ) 한국화학공학회 1992 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.30 No.5
The distribution and dissociation equilibria of tricaprylmethyl ammonium chloride(Aliquat 336; Q^+Cl^-) were measured for the system of organic phase(toluene, n-butyl acetate)-aqueous phase(water, NaCl, NaOH, Na₂S₂O₄). The enhancement factors of Q^+Cl^- were measured with a Lewis cell, and compared with those predicted from the theoretical model based on the film theory corrected by the Leveque model. The aqueous-phase mass transfer of Q^+Cl^- in the toluene-water system and toluene-NaOH aqueous solution system could be quantitatively explained as that with an instantaneous reversible dissociation reaction.
막반응기에서 Aliquat 336 에 의한 n - butyl acetate 의 알칼리 가수분해반응 1. 이론적 고찰
박상욱,문진복,정영훈,박대원,신정호 ( Sang Wook Park,Jin Bok Moon,Young Hoon Jung,Dae Won Park,Jung Ho Shin ) 한국화학공학회 1994 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.32 No.2
A theoretical model about a phase transfer catalyzed liquid-liquid heterogeneous reaction system in a hydrophobic membrane reactor was developed by the chemical-diffusion equations from the mass transfer mechanism with the approximated pseudo 1st-order reaction, and the performance of the membrane reactor was analyzed with the interaction of mass transfer with chemical reaction from this simulation.
상 이동 촉매상에서 니트로벤젠과 Fe3(Co)12 로부터 아닐린의 합성
천승우,오소영,박대원,박상욱,신정호 ( Sung Woo Chun,So Young Oh,Dae Won Park,Sang Wook Park,Jung Ho Shin ) 한국공업화학회 1992 공업화학 Vol.3 No.2
Triirondodecacarbonyl에 의한 니트로벤젠의 환원 반응에 상 이동 촉매를 사용한 결과 상온에서 높은 수율의 아닐린을 합성할 수 있었다. Benzyltriethylammonium chloride, tricaprylmethylammonium chloride, 18-crown-6, polyethyleneglycol-400 등이 이 반응에 좋은 상 이동 촉매임을 알 수 있었고, 반응온도, 수용액상의 NaOH 농도, 유기용매가 반응속도 및 아닐린의 수율에 미치는 영향을 고찰하였다. The reduction of nitrobenzene by triirondodecacarbonyl over phase transfer catalysts was investigated. The phase transfer catalysts showed a good yield of aniline at room temperature. Benzyltriethylammonium chloride, tricaprylmethyl ammonium chloride, 18-crown-6 and polyethyleneglycol-400 were good phase transfer catalysts in this reaction. The effeet of reaction temperature, concentration of sodium hydroxide and organic solvents on the reaction rate and yield of aniline were studied in this work.
Aliquat 336 상이동 촉매하에서 디페닐메탄의 산화에 의한 벤조페논의 합성
박대원,이화수,문정열,박상욱,신정호 ( Dae Won Park,Hwa Soo Lee,Jeong Yeol Moon,Sang Wook Park,Jung Ho Shin ) 한국공업화학회 1994 공업화학 Vol.5 No.1
본 연구는 Aliquat 336 상이동 촉매와 potassium tert-butoxide 염기를 사용하여 상온에서 디페닐메탄올 산화시켜 벤조페논을 합성하는데 관한 것이다. 4급 암모늄염 촉매 존재하에서는 벤조페논이 합성되지 않는다고 보고된 다른 연구결과와는 달리 Aliquat 336 촉매로 상온에서 30% 이상의 벤조페논 수율을 얻었다. Aliquat 336 촉매의 양과 potassium tert-butoxide의 양이 증가할수록 디페닐메탄의 전화율이 증가하였다. 산소의 분압이 높을수록 유기용매에 녹아 있는 산소의 농도가 증가하여 전화율과 선택도가 상승하였다. 또한 A1iquat 336 촉매의 역할이 포함된 반응 메카니즘을 제시하였다. Synthesis of benzophenone by oxidation of diphenylmethane at room temperature is studied using Aliquat 336 as phase transfer catalyst and potassium tert-butoxide as base. No other study has shown that diphenylmethane can be oxidized to benzophenone with quaternary ammonium salt as phase transfer catalyst. However, in presence of Aliquat 336, higher than 30% of benzophenone was yielded. The conversion of diphenylmethane was increased with increasing amount of Aliquat 336 and potassium tart-butoxide. Higher partial pressure of oxygen favored conversion of diphenylmethane and selectivity of benzophenone by increasing the concentration of oxygen in organic solvent. A reaction mechanism involving the role of Aliquat 336 was also proposed.