• Korean Chemical Engineering Research
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• v.46 no.1
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• pp.142-146
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• 2008

Titanium silicalite-1 catalyst was prepared using a $SiO_2-TiO_2$ xerogel and applied to allylchloride (ALC) epoxidation by $H_2O_2$ as oxidant in a batch reactor. The reaction temperature was varied from 25 to $55^{\circ}C$, and the concentrations of ALC and $H_2O_2$ were changed from 0.2 to 3 M and from 0.2 to 1.5 M, respectively. The kinetic data obtained were applied to the power rate law, Eley-Rideal, and a Langmuir-Hinshelwood model, and power rate law fits the experimental data best. Activation energy was 27.9 kJ/mol, and the reaction orders with respect to $H_2O_2$ and ALC were determined to be 0.41 and 0.52, respectively.

• Korean Chemical Engineering Research
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• v.44 no.3
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• pp.243-247
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• 2006

MFI zeolite membranes were prepared on anodic alumina (Anodisc) as support. First, silicalite-1(${\approx}1.2{\mu}m$) seed crystals were attached to the surface of the support via chemical bonding, and the a- and b-axis oriented zeolite membranes could be synthesized on the support coated with the monolayer of the seed crystals by secondary growth hydrothermal synthesis. The zeolite membranes prepared were characterized using scanning electron microscope and analyzed by X-ray diffraction.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.48-48
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• 2003

미세기공(microporous)을 가진 제올라이트는 다양한 유기질 분리의 촉매제 및 광학, 화학 센서, 기체 분리 등의 고기능 소재로서 크게 주목받고 있으며, 비표면적의 증가, 새로운 기능의 발현 둥으로 최근 들어 나노크기를 갖는 제올라이트 합성에 관한 연구가 활발히 진행되고 있다. 본 연구에서는 기체 분리에 응용하기 위한 제올라이트 분리막 개발에 앞서 분리막 제조에 유리할 것으로 판단되어지는 적합한 크기와 형상을 갖춘 나노크기의 제올라이트를 합성하였으며 그 특성을 분석하였다. 출발물질로서 실리카 원으로는 TEOS, LUDOX AS-40, Cab-O-SIL 등을 사용하였으며, 템프레이트(TPAOH)와 함께 특정조성의 TPAOH/SiO$_2$,/$H_2O$ 겔을 만들었다. 합성시간을 단축할 수 있는 방법의 연구로서 저온하의 2단계 온도 변화법을 적용하였으며, 결정성장속도의 향상을 목적으로 NaH$_2$PO$_4$, H$_2$SO$_4$, NH$_4$OH 등의 결정화 촉진제로 사용하여 수열합성법으로 Silicalite-1를 합성하였다.

• Membrane Journal
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• v.25 no.5
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• pp.422-430
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• 2015

The present study announces that the pH value of seed coating solution makes a significant effect on the microstructure of silicalite-1 zeolite layer formed on ${\alpha}$-alumina support. Seed with an average diameter of 75 nm was dispersed in ethanol to prepare three kinds of seed coating solutions with different pH values, and dip-coated on the support. The pH value was controlled to be 2.2, 7.0, and 9.3, respectively. In the secondary growth process, pH 7 seed solution resulted an uniform, 3 to $4{\mu}m$ thick, completely covered, and 100 nm grained silicalite-1 zeolite separation layer. The uniformity and completeness were explained by a uniform, closely packed, multi-layered, and completely covered seed coating in the pH 7 condition. In the condition, ${\alpha}$-alumina support and seed are oppositely charged: support is positively charged (8.4 mV) and seed, negatively (-1.7 mV). The opposite charging induced a strong electrostatic attraction between seed and support, which made the good seed coating state. On the other hand, pH 2.2 and pH 9.3 seed solutions resulted non-uniform, partially covered, and around $1{\mu}m$ grained zeolite separation layer, since seed and support are the same sign charged in the conditions. The same sign charging induced a strong electrostatic repulsion between seed and support which caused a low coverage of seed. It could be concluded that the pH value of seed coating solution is a key parameter to determine the microstructure of silicalite-1 zeolite separation layer.

• Korean Chemical Engineering Research
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• v.51 no.4
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• pp.476-481
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• 2013

Ethylbenzene (EB) which has a similar physical properties with p-xylene (pX) was separated from EB/pX mixture by using MFI-type zeolite (TS-1, ZSM-5, and Silicalite-1) coated membranes. The zeolites were synthesized by microwave method to reduce the synthesis time and uniformly formed zeolite particles were coated on the ${\alpha}$-almina tubular support with a thickness of $3-4{\mu}m$. Separation factor and permeation flux of the synthesized zeolite coated membranes were measured to survey the best performance of ethylbenzene separation from different composition of EB/pX mixtures. When the EB/pX mixture of 5:5 molar ratio applied for the separation experiment, it represented the highest separation factor. We also have studied about the effect of the atomic composition of zeolites on the separation performance within the temperature range from 160 to $220^{\circ}C$. TS-1 showed the highest permeation flux of $1,666mol/m^{2*}s^*Pa$ and Silicate-1 showed the highest separation factor of 1.73 at $200^{\circ}C$ respectively.

• Journal of the Korean Applied Science and Technology
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• v.21 no.3
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• pp.231-237
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• 2004

Ga-MFI was synthesized by a hydrothermal process at atmospheric pressure. The effect of mole ratios of reactants on crystallization was also investigated thoroughly. The characteristics of synthesized Ga-MFI was compared with ZSM-5. The synthesis of Ga-MFI was carried out with five different mole-compositions of $\underline{a}SiO_2-\underline{b}Ga_2O_3-\underline{c}Na_2O-\underline{d}TPA_2o-\underline{e}H_2O$. The synthesized Ga-MFI and ZSM-5 were characterized by XRD and FT-IR. The inorganic cation ($Na^+$) and water played an important role in crystallinity and the organic cation ($TPA^+$) as a template played a great influence on yields. With the increase in the amount of $Ga^{3+}$, crystallization time was increased. With a fixed $SiO_2/Ga_2O_3$ ratio of 400, the optimum reaction condition was obtained at $H_2O/SiO_2$=30${\sim}$35, $Na_2O/SiO_2$=0.5${\sim}$0.6, and $TPA_2O/Na_2O$=1${\sim}$1.25. In these cases, the crystallinity and yield were more than 95% and 90%, respectively. By comparing IR spectrum of Ga-MFI with those of ZSM-5 and silicalite, it was found that Ga-MFI showed a unique peak at 970 $cm^{-1}$, which may be used to identify Ga-MFI from ZSM-5 and silicalite.

• KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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• v.11 no.1
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• pp.53-58
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• 2005

Titanoalumino silicalite (TAS) was prepared hydrothermally, and the effects of synthesis parameters such as silica/alumina sources, $SiO_2/TiO_2$ ratio, and aging treatment were investigated. The structure, crystal size, and shape were examined by XRD and SEM, and the extent of titanium incorporation into the zeolite framework was examined using UV-vis DRS spectroscopy. For TAS preparation, aging of ca. 24h was essential, and the faster crystallization rates were achieved with Cab-O-Sil than with Ludox or TEOS as a silica source. In addition, the higher crystallinity and faster crystallization rate were obtained using sodium aluminate as an aluminum source.

• Proceedings of the Korean Ceranic Society Conference
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• 2003.04a
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• pp.201.1-201
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• 2003

• Bulletin of the Korean Chemical Society
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• v.25 no.5
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• pp.634-638
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• 2004

Titanium silicalite-1 (TS-1) molecular sieve was produced by microwave heating of amorphous titanium-containing solid precursors after impregnation with aqueous TPAOH solution. $SiO_2-TiO_2$ xerogel, sub-micron sized $SiO_2-TiO_2$ prepared by thermal plasma process, and Ti-containing mesoporous silica, Ti-HMS, were tested as the solid phase substrates. Highly crystalline product was obtained within 30 min. after microwave irradiation with yields over 90% using $SiO_2-TiO_2$ xerogel, which showed essentially identical physicochemical properties to TS-1 prepared by conventional hydrothermal method. Excellent catalytic activity was also obtained for 1-hexene epoxidation using $H_2O_2.\;SiO_2-TiO_2$ particles prepared by thermal plasma and Ti-HMS were found inferior as a substrate for TS-1, probably due to difficulties in wetting the surface uniformly with TPAOH.

• Journal of the Korean Ceramic Society
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• v.33 no.9
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• pp.1064-1072
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• 1996

The synthetic conditions and characteristics of ZSM-5 type zeolites (ZSM-5/silicalite) for the preparation of the zeolite composite membranes for gas separation were investigated. ZSM-5 zeolites could be synthesized by the hydrothermal treatment of the mixture of colloidal silica sol aluminum nitrate sodium hydroxide and TPABr at a temperature range of 150-17$0^{\circ}C$ in the autoclave. Silicalties were done from the solution of water glass water and TPABr. Their crystalline structures transformed from orthorhombic to monoclinic from and their pore structures of three-dimensional channels were opened as TPABr filling channels was burned off at the calcination temperature of 50$0^{\circ}C$. The specific surface area of the calcined zeolite was about 360 m3/g and its surface property was hydrophobic. Crystal sizes of ZSM-5 and silicalite were 0.5-1.0${\mu}{\textrm}{m}$ and 8-10${\mu}{\textrm}{m}$ respectively having no change due to the calcination. In particular the shape and the size of the ZSM-5 type zeolite were sensitively varied with silica sources and concentrations of reaction solutions/sols.