V2O5 - TiO2 및 황산으로 개질된 V2O5 - TiO2 의 특성

배영일,도임자,박은희,손종락 ( Young Il Pae,Im Ja Doh,Eun Hee Park,Jong Rack Sohn ) 한국공업화학회 1995 공업화학 Vol.6 No.5

Ti(OH)₄ 분말을 NH₄VO₃ 수용액에 함침시킨 후 공기중에 소성하여 V₂O_5-TiO₂ 촉매를 제조하였으며 또한 NH₄VO₃로 함침된 Ti(OH)₄ 분말을 황산으로 개질한 후 소성하여 V₂O_5-TiO₂/SO₄^(2-) 촉매를 제조하였다. 제조된 촉매의 특성을 FTIR, DSC-TGA, XRD 및 표면적 측정에 의하여 연구하였다. V₂O_5-TiO₂표면에 결합된 황산기는 V₂O_5함량이 많을수록 낮은 온도에서 분해되었다. 그리고 V₂O_5함량이 8∼10㏖%까지는 V₂O_5가 TiO₂ 표면에 잘 분산되어 900℃의 소성온도에서도 V₂O_5의 결정이 XRD pattern상에 나타나지 아니하였으나 V₂O_5함량이 10㏖% 및 그 이상에서는 400℃의 소성온도부터 V₂O_5 결정이 나타났다. IR과 XRD의 결과를 근거로 하면 V₂O_5표면을 monolayer로 완전히 입히는 데 필요한 V₂O_5의 함량은 8∼10㏖%임을 추측할 수 있다. V₂O_5-TiO₂ catalysts were prepared by dry impregnation of powdered Ti(OH)₄ with an aqueous solution of NH₄VO₃ followed by calcining in air, and V₂O_5-TiO₂/SO₄^(2-) catalysts were prepared by modifying impregnated Ti(OH)₄ with H₂SO₄ followed by calcining in air. The characterization of prepared catalysts was performed by using FTIR, DSC-TGA, and XRD, and by the measurement of surface area. The higher the content of V₂O_5 the lower the decomposition temperature of sulate bonded to the TiO₂-V₂O_5 surface. Since V₂O_5 was dispersed on the surface of TiO₂ up to 8㏖% of V₂O_5, any crystal phase of V₂O_5 even at the calcination temperature of 900℃ was not observed on the XRD patterns. However, in the case of sample containing 10㏖% and more than 10㏖% of V₂O_5, V₂O_5 crystal phase appeared on XRD pattern from the calcination temperature of 400℃. On the basis of results of IR and XRD, it is guessed that the content of V₂O_5 monolayer covering most of the available TiO₂ is 8∼10㏖%.

황산으로 개질된 TiO2 촉매의 특성

배영일,박만영,이준희,손종락 ( Young Il Pae,Man Young Park,Joon Hee Lee,Jong Rack Sohn ) 한국공업화학회 1992 공업화학 Vol.3 No.1

TiCl_4,-HCI 혼합용액으로부터 침전법으로 TiO_2를 만들고 이를 황산으로 개질하여 TiO_2/SO_4^(2-) 촉매를 제조하였으며 제조된 촉매의 특성을 IR, XPS, XRD 및 DT-TGA로 조사하였다. 개질된 촉매의 산의 세기는 적어도 H_0≤-14.52로 초강산 성질을 나타내었으며 이 성질은 TiO_2와 황산이온에 의하여 형성된 착물의 S=O 결합성질에 기인하였다. TiO_2/SO_4^(2-)의 IR spectra를 조사한 결과 황산이온은 TiO_2 표면에 2자리 ligand 로 배위하였다. TiO_2/SO_4^(2-)는 황산으로 개질하지 아니한 순수한 TiO_2에 비하여 표면적이 상당히 컸으며 또한 무정형에서 anatase상으로 되는 전이온도도 높았다. 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 H_0≤ -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.

Preparation and Characterization of Chromium Oxide Supported on Zirconia

배영일,Sohn, Jong Rack,Ryu, Sam Gon,Park, Man Young,Pae, Yeong Il 대한화학회 1992 Bulletin of the Korean Chemical Society Vol.13 No.6

Chromium oxide/zirconia catalysts were prepared by dry impregnation of powdered $Zr(OH)_4$ with ($NH_4$)$_2$CrO$_4$aqueous solution. The characterization of prepared catalysts was performed using FTIR, XPS, XRD and DTA methods, and by the measurement of surface area. The addition of chromium oxide to zirconia shifted the transitions of $ZrO_2$ from amorphous to tetragonal phase and from tetragonal to monoclinic phase to higher temperature due to the strong interaction between chromium oxide and zirconia, and the specific surface area of catalysts increased in proportion to the chromium oxide content. Since the $ZrO_2$ stabilizes supported chromium oxide, chromium oxide was well dispersed on the surface of zirconia, and ${\alpha}$-$Cr_2O_3$ was observed only at the calcination temperature above 1173 K. Upon the addition of only small amount of chromium oxide (1 wt% Cr) to $ZrO_2$, both the acidity and acid strength of catalyst increased remarkably, showing the presence of two kinds of acid sites on the surface of $CrO_x$/$ZrO_4$-Bronsted and Lewis.

황산으로 개질된 TiO₂ 촉매의 특성

배영일,박만영,이준희,손종락,Pae, Young-Il,Park, Man-Young,Lee, Joon-Hee,Sohn, Jong-Rack 한국공업화학회 1992 공업화학 Vol.3 No.1

$TiCl_4-HCl$ 혼합용액으로부터 침전법으로 $TiO_2$를 만들고 이를 황산으로 개질하여 $TiO_2/SO_4{^{2-}}$ 촉매를 제조하였으며 제조된 촉매의 특성을 IR, XPS, XRD 및 DT-TGA로 조사하였다. 개질된 촉매의 산의 세기는 적어도 $H_0{\leq}-14.52$로 초강산 성질을 나타내었으며 이 성질은 $TiO_2$와 황산이온에 의하여 형성된 착물의 S=O 결합성질에 기인하였다. $TiO_2/SO_4{^{2-}}$의 IR spectra를 조사한 결과 황산이온은 $TiO_2$ 표면에 2자리 ligand로 배위하였다. $TiO_2/SO_4{^{2-}}$는 황산으로 개질하지 아니한 순수한 $TiO_2$에 비하여 표면적이 상당히 컸으며 또한 무정형에서 anatase상으로 되는 전이온도도 높았다. $TiO_2/SO_4{^{2-}}$ 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 $H_0{\leq}-14.52$, 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 occurred at a higher temperature, as compared with pure $TiO_2$.

Titania 에 담지된 NiO 의 촉매특성과 촉매성질에 관한 연구

배영일,도임자,손종락 ( Young Il Pae,Im Ja Doh,Jong Rack Sohn ) 한국공업화학회 1995 공업화학 Vol.6 No.6

일련의 NiO-TiO₂ 촉매를 NiCl₂와 TiCl₄ 혼합 용액을 공침전시켜 제조하였으며 이중에서 일부의 촉매는 H₂SO₄로 처리하여 촉매 표면을 개질하였다. 제조된 촉매의 특성을 FTIR, DSC-TGA, XRD 및 표면적 측정에 의하여 연구하였다. TiO₂에 NiO를 첨가 할수록 표면적 및 산의 양이 중가하였으며 NiO함량이 25㏖%에서 최대의 값을 나타내었다. 그리고 NiO의 함량이 25㏖%에서 propene의 부분산화반응과 1-butene의 이성화반응의 촉매활성도 최대를 보여 주었다. H₂SO₄로 개질된 NiO-TiO₂/SO₄^(2-)촉매는 미개질된 NiO-TiO₂촉매에 비하여 1-butene의 이성화반응에서 월등히 향상된 촉매활성을 나타내었다. NiO 함량이 많을 수록 anatase가 rutile로 전이되는 온도가 NiO와 TiO₂의 상호작용으로 높게 나타났으며 600℃ 이상의 소성온도에서 NiO와 TiO₂가 결합하여 rhombohedral구조를 갖는 NiTiO₃화합물이 생성되었다. A series of NiO-TiO₂ catalysts were prepared by coprecipitation from the mixed solution of nickel chloride and titanium tetrachloride. Some of the samples were modified by treatment with H₂SO₄. The characterization of prepared catalysts was performed by using FTIR, DSC-TGA, and XRD, and by the measurment of surface area. The addition of NiO to TiO₂ caused the increase of surface area and acidity, showing a maximum at 25㏖% of NiO. Catalytic activites for prepene partial oxidation and 1-butene isomerization reactions also exhibited a maximum at 25㏖% of NiO. NiO-TiO₂/SO₄^(2-) modified whth H₂SO₄ exhibited remarkably enhanced catalytic activity for 1-butene isomerization compared with unmodified NiO-TiO₂. The addition of NiO to TiO₂ shifted the phase transition of TiO₂ from anatase to rutile towards higher temperatures due to the interaction between NiO and TiO₂. NiTiO₃ compound from NiO and TiO₂ was formed at calcination temperature above 600℃.

V2O5 - ZrO2 / WO3 촉매의 특성에 관한 연구

도임자,배영일,손종락 ( Im Ja Doh,Young Il Pae,Jong Rack Sohn ) 한국공업화학회 1997 한국공업화학회 연구논문 초록집 Vol.1997 No.0

Citrate Complexes of Alkaline Earth Metals in Aqueous, Acetone-Water and Ethanol-Water Solutions

최상업,배영일,제원목,Choi, Sang-Up,Pae, Young-Il,Jae, Won-Mok Korean Chemical Society 1970 대한화학회지 Vol.14 No.1

양이온 교환수지와 시트르산 이온($Cit^{3-}$)이 들어있는 용액에서 방사성 알칼리 토류 금속 이온이 수지와 용액 사이에 어떻게 분배되는가를 실온에서 조사함으로써 그들 금속 이온의 시트르산 착물형성에 관한 연구를 하였다. 용매로서 $H_2O$, 아세톤-$H_2O$ 및 에탄올-$H_2O$를 사용하였다. 용액의 pH는 7.2-7.5로 조절하였고 이온 강도는 0.10-0.12로 유지하였다. 본 연구의 결과 $Ba^{++}$과 $Sr^{++}$은 어떤 용매계에서도 1:1착물(M $Cit^-$)을 형성하는 것을 알았다. 그리고 $Ca^{++}$은 수용액에서는 1:1착물을 형성하지만 혼합 용매계에서는 1:1착물(Ca $Cit^-$)과 1:2착물(Ca $Cit_2^{4-}$)을 형성함을 알았다. 그리고 이들 착물의 안정도는 $Ba^{++}\;<\;Sr^{++}\;<\;Ca^{++}$ 의 순으로 커지며 또 혼합용매의 유기 성분의 농도 증가순으로 커짐을 알았다. Formation of the complexes of alkaline earths with citrate ions in aqueous, acetone-water and ethanol-water solutions was studied at room temperature by the equilibrium exchange technique. This technique involved the measurements of distribution of radioactivity between cation exchange resin and solution phase after the radioactive metal ions were equilibriated with the cation exchange resin in the presence of citrate ions ($Cit^{3-}$) of varying concentrations. The pH of the solutions was controlled to 7.2-7.5, and the ionic strength of the solutions was kept at 0.10-0.12. The present study revealed that both barium and strontium ions formed the one to one citrate complexes, $[M Cit]^-$ in all solvent systems examined. It was also observed that calcium ions formed the one to one citrate complex in aqueous solution. In acetone-water and ethanol-water solutions, however, calcium ions were observed to form both one to one and one to two complexes, $[Ca Cit]^-$ and $[Ca\;Cit_2]^{4-}$. The results of the present study indicated also that relative stabilities of the complexes increased in the order; $Ba^{++}\;<\;Sr^{++}\;<\;Ca^{++}$, and in the order of increasing concentration of the organic components in the mixed solvent systems.

포스터 발표 - 무기재료분과 / 전기화학분과 / 촉매분과 : V2O5 - ZrO2 / WO3 촉매의 특성에 관한 연구

도임자,배영일,손종락 ( Im Ja Doh,Young Il Pae,Jong Rack Sohn ) 한국공업화학회 1997 한국공업화학회 연구논문 초록집 Vol.1994 No.1

V2O5 - ZrO2 및 황산으로 개질된 V2O5 - ZrO2 의특성

손종락,배영일,조성국 ( Jong Rack Sohn,Young Il Pae,Sung Guk Cho ) 한국화학공학회 1993 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.31 No.6

V₂O_5- ZrO₂ catalysts were prepared by dry impregnation of powdered Zr(OH)₄ with an aqueous solution of NH₄VO₃ followed by calcining in air, and V₂O_5-ZrO₂/SO₄^(2-) catalysts were prepared by modifying impregnated Zr(OH)₄ with H₂SO₄ followed by calcining in air. The characterization of prepared catalysts was performed by using FTIR. DSC-TGA, and XRD, and by the measurement of surface area. The addition of V₂O_5 to ZrO₂ and modification with H₂SO₄ shifted the phase transition of ZrO₂ from amorphous to tetragonal and from tetragonal to monoclinic to higher temperatures due to the interaction between ZrO₂ and V₂O_5(or H₂SO₄). Since V₂O_5 was dispersed on the surface of ZrO₂ up to 10 ㏖% of V₂O_5, any crystal phase of V₂O_5 even at the calcination temperature of 900℃ was not observed on the XRD patterns. However, in the case of sample containing 15 ㏖% of V₂O_5, V₂O_5 crystal phase appeared on XRD pattern from the calcination temperature of 700℃.

연구논문 - 무기 / 촉매 : Titania 에 담지된 NiO 촉매의 특성

박준호,도임자,배영일,손종락 ( Joon Ho Park,Im Ja Doh,Young Il Pae,Jong Rack Sohn ) 한국공업화학회 1995 한국공업화학회 연구논문 초록집 Vol.1990 No.3