Selective hydrogenation of 4-isobutylacetophenone over a sodium-promoted Pd/C catalyst

박융호,Hong-Baek Cho,Bae Uk Lee,Chung-Han Ryu,Tadachika Nakayama 한국화학공학회 2013 Korean Journal of Chemical Engineering Vol.30 No.2

The effect of sodium promotion on the selective hydrogenation of 4-isobutylacetophenone, 4-IBAP, was investigated over a Pd/C catalyst. A precipitation and deposition method was used to prepare the catalyst, and sodium was promoted on the Pd/C catalyst via post-impregnation while varying the sodium content. The sodium-promoted Pd/C catalyst resulted in a significantly improved yield greater than 96% of the desired product, 1-(4-isobutylphenyl)ethanol (4-IBPE), compared with the non-patented literature results under a mild hydrogenation condition. A detailed hydrogenation network over the Pd/C catalyst was suggested. The reaction mechanism for the yield and selectivity enhancement of 4-IBPE induced-by the promoted Pd/C was elucidated in relation to the geometric and electronic effects of reactant molecules in the microporous support depending on the reaction steps.

폴리에스터 연속 중합 공정의 전산모사 연구

박융호,강우철 漢陽大學校 工學技術硏究所 1999 工學技術論文集 Vol.8 No.1

Process modeling, though a very useful tool in optimizing chemical processes, is not utilized very much in Korea due to lack of modeling techniques and application experiences. Modeling of the complicated processes haven't been attempted very much due to the difficulties in using the process simulator and the lack of actual experiences in optimization of large processes. In the case of continuous process of PET polymerization, the modeling of the entire process has never been reported due to secret of commercial processes. In this works, a model for PET process has been bullit with a commercial simulator(Aspen Plus) with a detailed consideration of undissolved TPA particles in esterification step and mass transfer of EG in polycondensation step. The model was used in investigating the effect of the changes in the operating conditions of the process on the properties of polymer product and in studying the interaction among the process equipments. And practical techniques for process modeling and optimization have been suggested through the example of PET process modeling.

Ethylene 중합용 Pentamethylene Bridged Dinuclear Zirconocene 합성에 관한 연구

박융호,임선화 漢陽大學校 工學技術硏究所 2001 工學技術論文集 Vol.10 No.-

본 연구는 메탈로센 신촉매 공정 개발을 위하여 진행되었으며, 하나의 촉매에 두 개의 활성점을 갖는 pentamethylene bridged dinuclear zirconocene을 Noh 등의 protocol을 활용하여 합성하였고, 상업화시 가장 중요한 변수인 반응 수율을 향상시키기 위하여 각 합성 단계의 개선을 시도하였다. Biscyclopentadienyl pentane 합성시 silica gel chromatography column을 이용하여 순수한 ligand를 제조하였고, trimethyltin compound 합성시 용매 변환과 TEA 주입을 통하여 수율을 향상시켰다. 최종 메탈레이션 반응시에는 반응 온도의 변화를 통하여 촉매의 활성을 향상시킬 수 있었다. This study was done for the development of a new metallocene catalyst process. The pentamethylene bridged dinuclear zirconocene which have two active sites in one catalyst had been synthesized using Noh et al's protocol and each synthetic step was modified for the improvement of reaction yield which was the most important variable in commercialization. Pure biscyclopentadienylpentane was obtained by passing through silica gel chromatography column and the reaction yield of trimethyltin compound was improved by solvent change and TEA injection. A change in the reaction temperature during the final metallation process also improved the catalytic activity.

PET 공정 Ester화 반응기의 열전달 계수에 관한 연구

박융호 한양대학교 에너지·환경기술연구소 1998 에너지·環境技術論文集 Vol.4 No.-

반응기 설계능력을 높이기 위한 노력의 하나로서 국내에서 많이 운전되고 있는 Hitachi PET 공정 중에서 esterification반응기를 중심으로 실제 반응조건(260℃, EG:TPA = 1.5:1)에서 실시한 열전달 실험으로부터 열전달 계수를 확인하였다. 또한 교반공정 모사기인 Visimix를 이용하여 Esterification반응기와 같은 형태와 Dimension을 갖는 모델을 수립하여 반응기 설계시에 필요한 열전달 계수 관계식을 구하였다. In an effort to increase the ability for reactor design, the value of heat transfer coefficient were obtained from heat-transfer experiment in real reaction condition (260℃, EG:TPA = 1.5:1), for the esterfication reactor of Hitachi process for PET manufacture. A mixing model of the ES reactor has been built using Visimex, a mixing process simulator, and a correlation was obtained for the heat transfer coefficient which is necessary in calculation of heat transfer area of the reactor.

Polyester 축중합 공정 회분식 반응기의 전산 모사 및 운전 최적화 연구

박융호,강우철 漢陽大學校 工學技術硏究所 1996 工學技術論文集 Vol.5 No.1

A batch polycondensation reactor for polyester manufacture has been modeled based on plant data using a process simulator (Aspen Plus). Model includes major aspects of polycondensation reactions, side reaction, vapor liquid equilibria, and mass transfer and predicted correctly the dependency of the process performance on the temperature and the pressure of the reaction. Various profiles of the temperature and the pressure were tested for its performance and the profiles which improves significantly the degree of polymerization of the final product were found. The individual and combined effects of the temperature profile and pressure profiles were examined and a way to shorten the batch time using optimized profiles has been discussed.

에탄올 탈수 PSA 공정의 전산 모사 및 설계 최적화 연구

박융호,최재식 漢陽大學校 工學技術硏究所 1997 工學技術論文集 Vol.6 No.1

A model for scale-up of PSA process of ethanol dehydration was established using bench experimental data. LDF mass-transfer model, Langmuir adsorption isotherm and single-component adsorption were assumed in the model and the coefficients for heat and mass transfer in the beds were fitted against the experimental data. Model equations were solved using a DAE solver (Speed Up). The effects of cycle time, P/F ratio, adsorption pressure, bed length were examined, and the dimension and the operating condition which give optimum peformance for a commercial process were determined.

Montmorillonite에 담지된 Cp2ZrCl2 촉매를 이용한 에틸렌 중합특성 연구

박융호 ( Yeung Ho Park ),안성현 ( Sung Htun Ahn ),이성호 ( Sung Ho Lee ),최무석 ( Moo Seok Choi ),임준섭 ( Jun Seop Im ),( Rizwan Sheik ),조득희 ( Deug Hee Cho ) 한국공업화학회 2013 공업화학 Vol.24 No.1

Cp2ZrCl2 촉매를 Montmorillonite (MMT) 담체에 각기 다른 3가지 방법[MMT/Cp2ZrCl2, MMT/MAO/Cp2ZrCl2, MMT/ (MAO + Cp2ZrCl2)]을 적용하여 불균일 촉매를 제조하였고, 이를 이용하여 에틸렌 중합 특성을 조사하였다. 유기점토 인 30B-MMT에 담지한 불균일계 촉매가 자연점토인 Na + -MMT에 담지한 촉매보다 높은 담지율을 나타내었고, 에틸렌 중합에서 높은 활성을 보였다. 이는 유기점토의 층간사이에 존재하는 하이드록시기가 MAO 및 촉매와의 화학적 결합 을 유도한다고 할 수 있다. MMT에 직접 메탈로센을 담지하여 에틸렌 중합에 사용할 경우 균일계 촉매에 비해 낮은 활성을 보이지만, MMT를 MAO로 처리해서 만든 MMT/MAO/Cp2ZrCl2 촉매에 MMAO의 조촉매를 사용하여 중합시에 는 높은 활성을 나타내었다. MMT 담지촉매로 제조된 폴리에틸렌은 담지방법에 관계없이 균일계 촉매에 비해 높은 용융점, 분자량, 분자량 분포를 보였으며, 또한 입자형상에 있어 크기가 상당히 증가한 구형의 입자를 나타내었다. 또한 가장 안정적인 담지 반응과 높은 활성을 나타낸 30B-MMT/MAO/Cp2ZrCl2 촉매로 최적의 중합조건을 찾기 위해 공정변수에 따라 에틸렌 중합을 수행하였다. Heterogeneous metallocene catalysts supported on montmorillonite (MMT), [Cp2ZrCl2/MMT, Cp2ZrCl2/MAO/MMT, and Cp2ZrCl2 + MAO/MMT], were prepared with three different methods of immobilization and tested for ethylene polymerization. The heterogeneous catalysts immobilized on organo clay (30B-MMT) showed the higher metal loading and polymerization activity than those immobilized on natural clay (Na + -MMT). These results suggest that the hydroxyl groups of organo clay interlayers react with the MAO and catalyst through the chemical bond. The metallocene catalyst supported directly on MMT showed lower activity for ethylene polymerization compared to the homogeneous systems, while MMT/MAO/Cp2ZrCl2, catalysts treated with MAO before impregnation, showed a higher activity. The polymers obtained from MMT-supported catalysts have higher melting point, molecular weight and molecular weight distributions than those of homogeneous catalysts. The polymer particles with increasing significant size. Ethylene polymerization over 30B-MMT/MAO/Cp2ZrCl2 catalyst was also performed varying the process variables to optimize the process conditions.

파라핀 왁스의 산화반응조건의 최적화에 관한 연구

박융호,윤덕상 한양대학교 에너지·환경기술연구소 1998 에너지·環境技術論文集 Vol.4 No.-

파라핀 왁스를 산화시키고 최적의 반응조건을 찾기 위해 교반기, impeller,공기diffuser, temperature controller, silicon oil bath, silicagel dry trap 등으로 구성된 반응장치를 제작하였다. 촉매인 KMnO₄의 suspension을 형성하고 diffuser를 하향으로 하며 Rushton turbine impeller로 교반함으로써 미세한 공기방울을 형성하는 등 반응 조건을 개선하였다. 촉매의 양 및 성상 조절, 기액접촉 방법의 개선 그리고 반응기의 형태 변형 등을 통해 산화반응물의 비누화가 및 산가를 향상시킬 수 있었다. 반응물 GC/MS분석을 통해서 포화탄화수소의 일부가 지방산으로 분해되었음을 확인할 수 있었다. 이러한 노력에 의해 생성물의 비누화가 193, 산가 85를 주는 산화반응의 최적조건을 얻을 수 있었으며 100ℓpilot 반응기를 이용하여 그 상업적 생산 가능성을 확인하였다. In order to oxidize paraffin wax and to find out optimal reaction condition, reaction apparatus was set up with agitator, impeller, air diffuser, temperature controller, oil bath and silica gel dry trap etc. The catalyst, potassium permanganate, was added in the form of a concentrated aqueous solution, the diffuser head was toward the bottom of the reactor and Rushton turbine type impeller was selected. The saponification number and acid value of oxidation product increased by controling the amount and the state of catalyst, improving gas-liquid contact, and changing the set up of reactor. The analysis of reactants and products by FTIR and GC/MS confirmed the formation of fatty acid. As a result, saponification number of 193 and acid value of 85 were obtained at the optimum condition. Finally, the possibility of its commercial scale-up of the process was found from the experiment in 100ℓpilot reactor.

크로메이트 컨버젼 코팅 기술

박융호 ( Yeung Ho Park ),이현철 ( Hyon Chol Lee ),한명근 ( Myung Keun Han ) 대한금속재료학회 1997 大韓金屬學會會報 Vol.10 No.1

연구발표 초록 ( 촉매 및 반응공학 (Ⅶ) ) : 팔라디움 촉매상에서 아세틸렌의 선별적 수소화반응에 있어서의 포테시움 첨가제의 영향

박융호(Yeung Ho Park),G . L . Price(Geoffrey L . Price) 한국화학공학회 1991 추계학술발표회 Vol.- No.-