• Bulletin of the Korean Chemical Society
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• 제22권7호
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• pp.678-684
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• 2001

Porous silica-pillared montmorillonites were prepared by simultaneous intercalation of dodecylamine-TEOS [tetraethylorthosilicate, Si(OC2H5)4] into the H-montmorillonite and intragallery amine-catalyzed hydrolysis of TEOS. Mixtures of the H-montmorillonite, dodecylamine and TEOS at molar ratios of 1 : 2 : 15-30 and 1 : 2-6 : 20 resulted to swollen and viscous gel once at room temperature, allowing intercalation compounds which dodecylamine and TEOS were simultaneously intercalated into interlayer of H-montmorillonite. The hydrolysis of the gallery TEOS was conducted in water solution for 40 min at room temperature, affording siloxane-pillared H-montmorillonite. Calcination of samples at 500 $^{\circ}C$ in air resulted in silica-pillared montmorillonite with large specific surface areas between 403 and 577 m2 /g, depending on the reaction stoichiometry. The reaction at H-montmorillonite : dodecylamine : TEOS reaction stoichiometries of 1 : 2 : 15 and 1 : 4 : 20 resulted in high specific surface areas and mesopores with a narrow pore size distribution. Result indicates that the intragallery-amine catalyze the hydrolysis of gallery-TEOS and simultaneously have a role of gallery-templated micellar assemblies.

• 한국광물학회지
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• 제15권4호
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• pp.273-282
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• 2002

국내산 Ca-몬모릴로나이트와 이것으로부터 이온치환에 의하여 합성된 Al-가교몬모릴로나이트의 특성을 비교하였다. Ca-몬모릴로나이트와 Al-가교몬모릴로나이트를 저면간격, 비표면적, 탈수 및 이온치환 등의 관점에서 그 특성을 비교 연구하였다. d(001) 간격은 Ca-몬모릴로나이트에서는 15.1 $\AA$이었으나 Al-가교몬모릴로나이트에서는 18.3 $\AA$으로 나타났다. 탈수는 Ca-몬모릴로나이트에서는 $350^{\circ}C$ 이하에서 일어났지만, Al-가교몬모릴로나이트에서는 $550 ^{\circ}C$까지도 선형적으로 일어났다. BET 비표면적은 Al-가교몬모릴로나이트( $192\m^2$/g)가 Ca-몬모릴로나이트보다 5～6배 높은 값을 보여주었다. Ca-Na 이온 용액과의 반응에서 Ca-몬모릴로나이트는$ Na^{＋}$ 에 대하여, 그리고 Al- 가교몬모릴로나이트는 $Ca^{2＋}$ 에 대하여 선택성을 보여주었다. Ca-몬모릴로나이트는 $Na^{＋}$ /가 증가할수록 d(001)간격이 감소하다가 $Ca^{ 2＋}$와 $Na^{＋}$ /가 같은 양일 경우에 구조적으로 불규칙한 혼합층구조 상태를 보여주었으며 Al-가교몬모릴로나이트는 $Ca^{2＋}$ 의 증가와 함께 d(001) 간격이 선형적으로 감소한 양상을 보여주었다.

• 한국광물학회지
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• 제15권4호
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• pp.315-327
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• 2002

벤토나이트에 포함된 몬모릴로나이트의 층간에 Al산화물의 기둥(pillar)을 만든 Al-층간가교 점토를 합성하였다. 이 Al-층간가교점토에 대해 XRD, DTA, 화학분석 등을 실시하여 광물학적 특성을 검토하였으며, 그리고 이 가교점토에 대하여 Batch법의 흡착실험을 통하여 인산이온의 흡착성을 검토하였다. X-선 회절분석의 결과, Al-층간가교점토는 상온에서 층간격이 $18.03 \AA$으로 증가되어 나타났고, $550\AA$가열에서도 약 $17\AA$을 나타내어 열적 안정성이 크며, 글리세롤에 의한 층간격의 팽윤은 매우 미약한 것으로 나타났다. 열분석 결과, 이 점토에는 pillar부분에 관련된 물의 탈수에 의한 것으로 보이는 $270^{\circ}C$와 $420^{\circ}C$의 특징적인 흡열반응이 나타났다. Al-층간가교 점토의 인산 이온에 대한 흡착실험의 결과, 몬모릴로나이트는 거의 흡착능력을 보이지 않는데 비하여 월등히 우수한 인산이온($PO_{4}^{3－}$ /)성을 나타냈다. 시료 2 g에 용액 20 mL의 실험에서 300 mg/L 이하의 인산 농도에서는 거의 100%의 흡착효율을 나타냈다. 그리고 인산 이온에 흡착된 시료를 $500^{\circ}C$로 가열한 후 재차 흡착실험을 행한 결과, 역시 매우 높은 흡착효율을 나타냈다. 따라서 Al-층간가교 점토의 인산 이온 흡착에 대한 재활용의 가능성이 큰 것으로 나타났다

• Bulletin of the Korean Chemical Society
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• 제19권11호
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• pp.1185-1188
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• 1998

Layered nanocomposite, SiO2/TiO2 sol pillared clay, has been prepared by the ion exchange reaction of Na' ion in montmorillonite with positively charged mixed SiO2/TiO2 sol. The nanosized sol particles were synthesized by mixing SiO2 sol solution with TiO2 one, which is obtained by acidic hydrolysis of TEOS and TiCl4, respectively. From powder XRD, the basal spacing (d001) of the sample calcined at 400 ℃ was found to be ca. 60 Å, due to the multistacking of nanosized SiO2 and TiO2 sol particles, which was confirmed by the pore size analysis from 129Xe NMR and micropore analysis calculated from nitrogen adsorption. The BET specific surface area shows the value of 684 m2g-1 (Langmuir 1115 m2g-1), which is the highest among various pillared clays ever reported previously, and the total porosity is found to be 0.51 mlg-1, and the pores are mainly composed of micropore with a size of ca. 11.8 Å. This result agrees with the adsorption capacity obtained from water adsorption. According to diffuse reflectance ultraviolet-visible spectroscopy, it is found that the TiO2 particles stabilized in the interlayer space of montmorillonite are quantum-sized of ca. 20 Å.

• Bulletin of the Korean Chemical Society
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• 제34권10호
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• pp.3005-3012
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• 2013

The effect of Mn-promotion on high surface area Al-pillared montmorillonite (AlMMT) supported Co nanoparticles prepared by hydrothermal method have been investigated. A series of different weight% Mn-promoted Co nanoparticles were prepared and characterized by XRD, TPR, TGA, BET and SEM techniques. An increase in the surface area of MMT is observed with Al-pillaring. Fischer-Tropsch catalytic activity of the as prepared catalysts was studied in a fixed bed micro reactor at $225^{\circ}C$, $H_2/CO$ = 2 and at 1 atm pressure. The data showed that by the addition of Mn the selectivity of $C_1$ dropped drastically while that of $C_2-C_{12}$ hydrocarbons increased significantly over all the Mn-promoted Co/AlMMT catalysts. The $C_{13}-C_{20}$ hydrocarbons remained almost same for all the catalysts while the selectivity of $C_{21+}$ long chain hydrocarbons decreased considerably with the addition of Mn. The catalyst with 3.5%Mn showed lowest $C_{21+}$ and highest $C_2-C_{12}$ hydrocarbons selectivity due to cracking of long chain hydrocarbons over acidic sites of MMT.

• 한국물환경학회지
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• 제34권6호
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• pp.621-631
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• 2018

In this study, catalyst was made through incipient wetness method using palladium (Pd) as noble metal, indium (In) as secondary metal, and montmorillonite (MK10) and Al pillared montmorillonite (Al-MK10) as supporters. The nitrate reduction rate of the catalysts was measured by batch experiments where H2 gas was used as reducing agent and formic acid as pH controller. Transmission electron microscopy (TEM) equipped with energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were all used to determine the elemental distribution of Pd, In, Al, and Si on catalysts. It was observed that Al pillaring increased the Al/Si elemental composition ratio and point of zero charge of MK10, but decreased its BET specific surface area and pore volume. The nitrate reduction rate of Al-MK10 Pd/In was 2.0 ~ 2.5 times higher than that of MK10 Pd/In using artificial groundwater (GW) in ambient temperature and pressure. Nitrate reduction rates in GW were 1.2 ~ 1.7 times lower than those in distilled deionized water (DDW). Nitrate reduction rates in acidic conditions were higher than those in neutral condition in both GW and DDW. The amount of produced NH3-N over degraded NO3- at acid conditions was lower than that of neutral condition. Even though the leaching of Pd after reaction was measured in DDW it was not detected when both Al-MK10 Pd/In and MK10 Pd/In were used in GW. The modification of montmorillonite as a supporter significantly increased the reductive catalytic activities of nitrates. However, the ratio of producing ammonia by-products to degraded nitrates in ambient temperature and pressure was similar.

• Bulletin of the Korean Chemical Society
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• 제21권10호
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• pp.1049-1051
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• 2000

A chromia-pillared clay has been prepared by ion exchange type intercalation reaction between the sodium ion in montmorillonite and the trimeric chromium oxyformate (TCF) ion, and by subsequent heat-treatment. The structural and thermal properties have been systematically studied by thermal analysis, powder XRD, IR spec-troscopy, and XAS. The gallery height of~6.8 $\AA$ upon intercalation of the TCF ion suggests that the $Cr_3O$ plane is parallel to the aluminosilicate layers. Even though the basal spacing of TCF intercalated clay decreases slightly upon heating, the layer structure was retained up to $550^{\circ}C$ as confirmed by XRD and TG/DTA. Ac-cording to the EXAFS spectroscopic analysis, it is identified that the (Cr-Cr) distance of 3.28 $\AA$ between vertex-linked CrO6 octahedra in TCF splits into 2.64 $\AA$, 2.98 $\AA$, and 3.77 $\AA$ due to the face-, edge-, and corner-shared CrO6 octahedra after heating at $400^{\circ}C$, implying that a nano-sized chromium oxide phase was stabilized within the interlayer space of clay.

• 한국세라믹학회지
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• 제41권1호
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• pp.81-85
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• 2004

점토를 이용한 나노 다공성 촉매 제조를 목적으로 $Ni^{2+}$ 이온으로 피복된 $SiO_2$ 나노 졸 입자를 2차원 충상점토 화합물의 층간에 삽입, 가교화 시켜 비표면적 및 다공도가 우수한 $NiO-SiO_2$ 가교화 점토($NiO-SiO_2$-PILM)를 합성하였다. 나노 크기의 실리카 졸 입자는 tetraethyl orthosilicate(TEOS)를 가수분해하여 합성하였고, 여기에 $Ni^{2+}$ 수용액을 첨가한 다음 NaOH 용액을 적정하여 $Ni^{2+}-SiO_2$ 혼합 나노 졸입자를 완성하였다. 이렇게 제조된 혼합 졸 용액을 1wt%의 점토 수분산액에 첨가하여 $60{\circ}C$에서 5h 이온교환 반응을 통해 층간에 삽입, 수세, 건조 후 $40^{\circ}C$에서 2시간 열처리 하므로써 다공성 가교화 점토를 제조하였다. 나노 졸 입자의 가교화에 따라 점토의 층간거리($d_{001}$)는 $45{\AA}$ 정도 크게 증가하였고 $600^{\circ}C$까지도 다공구조가 안정하게 유지되었다. 또한 질소 흡착-탈착 등온선 분석 결과 비표면적($S_{BET}$)이 최대 $760m^2/g$으로 다공 구조가 매우 잘 발달되어 있음을 확인하였고, $NiO-SiO_2$ 졸 가교화 점토의 경우 $NiO-SiO_2$ 나노입자가 층간에 이중층으로 배열되어 있음을 알 수 있었다.

• 한국철도학회:학술대회논문집
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• 한국철도학회 2011년도 정기총회 및 추계학술대회 논문집
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• pp.2870-2874
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• 2011

Soil pollution around railroad has been occurred mainly by diesel and lubricant oil, which is difficult to treat due to high carbon number. In this study, we investigated the feasibility of inorganic-inorganic nanohybrid photo-catalyst for the remediation of diesel-contaminated railroad soil. Generally, the $TiO_2$ nanoparticle easily removes organic pollutants due to photo and natural clay of layer structure. Also, montmorillonite (MMT) have an excellent absorption property with organic component. So, we prepared $TiO_2$ pillared MMT nanohybrid photo-catalyst as a chemical oxidant through the integration of theses advantage. As a result, the removal efficiency of diesel was more than 45% at a laboratory-scale test with diesel concentration and the amount of $TiO_2$-MMT. In future, we will improve the removal efficiency of diesel to optimize experimental parameters and apply the field soil The remediation method using photo-catalyst can be used to clean up the railroad soil polluted with high concentration instead of common methods such as soil washing, bioremediation, etc..