• 공업화학
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• 제19권5호
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• pp.559-567
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• 2008

SAPO-34 촉매는 메탄올에서 올레핀 전환반응에서 세공크기가 작아 코크침적에 대한 비활성화가 촉진됨에 따라 촉매의 수명증진이 요구된다. 본 연구에서는 촉매의 수명증진을 위해 다양한 구조 유도제로 합성된 SAPO-34 촉매의 특성을 비교하기 위하여 질소 흡착-탈착 등온선, X-선 회절 분석(XRD), 주사 전자현미경(SEM), 암모니아 승온탈착(NH3-TPD) 등을 이용하여 분석하였으며, 또한 MTO 전환반응 실험을 수행하였다. 합성시 구조 유도제에 따른 결정크기의 감소와 산특성의 변화와, 결정크기가 MTO 전환반응에 미치는 영향을 관찰할 수 있었다. 특히 DEA와 TEAOH 구조 유도제를 혼합 사용한 SAPO-34 촉매는 $0.5{\mu}m$ 정도의 균일한 결정크기를 갖으며, 산특성의 최적화로 가장 우수한 MTO 반응성을 보였으며 촉매의 수명이 향상됨을 알 수 있었다.

• Korean Chemical Engineering Research
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• 제48권6호
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• pp.684-689
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• 2010

본 연구에서는 다양한 구조 유도제로 합성된 SAPO촉매를 이용하여 자일로오스의 탈수화 반응을 진행하였다. 구조 유도제로는 테트라에틸암모늄수산화물(TEAOH), 디프로필아민(DPA), 디에틸아민(DEA), 몰포린(Morpholine) 그리고 디에탄올아민(DEtA)을 사용하였다. 촉매의 특성을 파악하기 위하여 질소 흡착-탈착 등온선, 암모니아 승온탈착($NH_3$-TPD), 그리고 승온산화분석(TPO)을 이용하였다. 구조 유도제로 몰포린(Morpholine)을 사용하여 제조한 SAPO-34를 촉매로 사용하였을 경우 사용한 촉매중에서 푸르푸랄 수율이 가장 높았다. 고체산 촉매의 외부 표면적과 산농도가 자일로오스의 탈수화 반응에 영향을 주는 것으로 나타났다.

• Macromolecular Research
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• 제17권9호
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• pp.697-702
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• 2009

Mesoporous ethanesilica thin film was prepared using PEO-PLGA-PEO triblock copolymers as structure-directing agents and (1,2-bis(triethoxysilyl) ethane BTESE; bridged organosilicates) as inorganic precursors via one-step sol-gel condensation of ethanesilica precursors. The mesostructure of ethanesilica films is critically dependent on the processing experimental parameters after the hydrolyzed silica sol mixture was spin-cast. This study examined the effects of the block copolymer template/organosilica precursor ratio in the casting solution and aging period before calcination of the mesostructure. It was further demonstrated that mesoscopic ordering of organosilicate thin films is induced by the rearrangement of block copolymer template/organosilica hybrid during thermal decomposition of the PEO-PLGA-PEO triblock copolymer. The mesoporous structure and morphology were characterized by SAXS, TEM and solid-state NMR measurement.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1562-1566
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• 2006

Mesoporous silica films with three different pore sizes were prepared by using cationic surfactant, non-ionic surfactant, or triblock copolymer as structure directing agents with tetramethylorthosilicate as silica source in order to control the pore size and wall thickness. They were synthesized by an evaporation-induced self-assembly process and spin-coated on Si wafer. Mesoporous silica films with three different pore sizes of 2.9, 4.6, and 6.6 nm and wall thickness ranging from $\sim$1 to $\sim$3 nm were prepared by using three different surfactants. These materials were optically transparent mesoporous silica films and crack free when thickness was less than 1 m m. The photoluminescence spectra found in the visible range were peaked at higher energy for smaller pore and thinner wall sized materials, consistent with the quantum confinement effect within the nano-sized walls of the silica pores.

• Bulletin of the Korean Chemical Society
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• 제26권11호
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• pp.1653-1668
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• 2005

Assembly of hybrid mesophases through the combination of amphiphilic block copolymers, acting as structuredirecting agents, and silicon sources using low acid catalyst concentration regimes is a versatile strategy to produce large quantities of high-quality ordered large-pore mesoporous silicas in a very reproducible manner. Controlling structural and textural properties is proven to be straightforward at low HCl concentrations with the adjustment of synthesis gel composition and the option of adding co-structure-directing molecules. In this account, we illustrate how various types of large-pore mesoporous silica can easily be prepared in high phase purity with tailored pore dimensions and tailored level of framework interconnectivity. Silica mesophases with two-dimensional hexagonal (p6mm) and three-dimensional cubi (Fm$\overline{3}$m, Im$\overline{3}$m and Ia$\overline{3}$d) symmetries are generated in aqueous solution by employing HCl concentrations in the range of 0.1−0.5 M and polyalkylene oxide-based triblock copolymers such as Pluronic P123 $(EO_{20}-PO_{70}-EO_{20})$ and Pluronic F127 $(EO_{106}-PO_{70}-EO_{106})$. Characterizations by powder X-ray diffraction, nitrogen physisorption, and transmission electron microscopy show that the mesoporous materials all possess high specific surface areas, high pore volumes and readily tunable pore diameters in narrow distribution of sizes ranging from 4 to 12 nm. Furthermore, we discuss our recent advances achieved in order to extend widely the phase domains in which single mesostructures are formed. Emphasis is put on the first synthetic product phase diagrams obtained in $SiO_2$-triblock copolymer-BuOH-$H_2O$ systems, with tuning amounts of butanol and silica source correspondingly. It is expected that the extended phase domains will allow designed synthesis of mesoporous silicas with targeted characteristics, offering vast prospects for future applications.

• 대한전자공학회:학술대회논문집
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• 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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• pp.610-615
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• 2001

Over 800 thousand tons per year (TPY) agricultural biowastes, such as sugar cane bagasse, sugarcane leaf, rice straw, rice husk and corn leaf, are produced in Taiwan. These biomasses are the major types of agricultural wastes and are abundantly available. However, these biowastes cause disposal and landfill problems. Ossification ashes of the agricultural biowastes containing 70-95 % amorphous silica would make the utilization system of agricultural biowaste ashes become highly economically and environmentally attractive. Experimentally, high crystallinity (99%$^{+}$) zeolites ZSM-5 and ZSM-48 synthesized from the reaction mixtures containing a silica source from ashes of these biowastes gasification were investigated. Tetrapropylammonium bromide (TPABr) and 1,6-diamino-hexane (C$_{6}$ DN) were used as structure-directing agents in syntheses of ZSM-5 and ZSM-48, respectively. X-ray powder diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM/EDX) data indicated that ZSM-5 or ZSM-48 with a high crystallinity can be obtained within 48 hours of crystallization in the high pressure (15-20 atm) autoclave at 393-473 K. The Si/Al ratios of synthetic zeolite products were determined by X-ray fluorescence (XRF) and induced couple plasma/mass spectroscopy (ICP/MS). It was observed that the ZSM-5 crystals a.e composed of hexagonal rod-shaped crystals with typically 8-13 пm in size by SEM. In addition, ZSM-48 crystalline materials are composed of spherical aggregates of needle-shaped or rod-like crystals with typically 2-3 пm in diameter and 6-8 пm in length.h.

• 공업화학
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• 제26권2호
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• pp.217-223
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• 2015

DTO (dimethyl ether to olefin) 반응에서 촉매 성능을 향상하기 위하여 염산에 의한 SAPO-34 시료의 산 처리 영향을 연구했다. 먼저 TEAOH (tetraethylammonium hydroxide)와 DEA (diethylamine)를 구조유도제로 사용하여 정육면체 형태를 갖는 균일한 크기의 SAPO-34 시료를 수열 합성했다. 제조된 촉매는 염산의 농도 및 처리 시간을 변수로 하여 개조되었다. 그 결과, 우수하게 개조된 시료는 외부 표면의 침식과 함께 총 비표면적 및 마이크로 세공부피가 증가하였으며, 산점량이 다소 감소하는 것으로 나타났다. 특히, 개조된 SAPO-0.2 M (3 h) 시료 상에서의 DTO 반응에서 촉매 수명과 경질 올레핀 선택성은 모체 SAPO-34 시료와 비교하여 크게 향상되었다. 이것은 코크 형성에 의한 비활성화가 주로 결정 외부 표면의 기공 입구에서 상대적으로 빠르게 진행된다는 것을 의미한다. 따라서 산 처리는 SAPO-34 촉매의 외부 표면을 개조함으로써 촉매의 성능을 향상할 수 있는 단순한 방법임을 확인했다.