• Title/Summary/Keyword: Organic monolith particles

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Ground Organic Monolith Particles Having a Large Volume of Macropores as Chromatographic Separation Media

  • Lee, Jin Wook;Ali, Faiz;Kim, Yune Sung;Cheong, Won Jo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.7
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    • pp.2033-2037
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    • 2014
  • A reaction mixture was developed for formation of soft organic monolith that was easily smashed, rinsed, refluxed, filtered, and dried to give monolith particles having high pore volume of macropores. This phase was almost without mesopores. The reaction mixture was composed of methacrylic acid, ethylene glycol dimethacrylate, polyethylene glycol (porogen), and an initiator in a mixed solvent of toluene and isooctane. The selection of porogen and its amount was carefully carried out to obtain the optimized separation efficiency of the resultant phase. The median macropore size was 1.6 ${\mu}m$, and the total pore volume was 3.0-3.4 mL/g. The median particle size (volume based) was 15 ${\mu}m$, and the range of particle size distribution was very broad. Nevertheless the column (1 ${\times}$ 300 mm) packed with this phase showed good separation efficiency (N~10,000-16,000) comparable to that of a commercial column packed with 5 ${\mu}m$ C18 silica particles.

Effect of Heat Treatment on the Morphology and Transparency of Thick Inorganic-Organic Hybrid Films Prepared by the Electrophoretic Sol-Gel Deposition of Polyphenylsilsesquioxane Particles

  • Hasegawa, Koichi;Katagiri, Kiyofumi;Matsuda, Astunori;Tatsumisago, Masahiro;Minami, Tsutomu
    • The Korean Journal of Ceramics
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    • v.6 no.1
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    • pp.15-20
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    • 2000
  • Thick inorganic-organic hybrid films were prepared on ITO-coated glass substrates by the electrophoretic sol-gel deposition of polyphenylsilsesquioxane particles. The morphology of the deposited films changed from the aggregate of the spherical particles to monolith by heat treatment at temperatures higher than $200^{\circ}C$. Transparency of the films was significantly improved accompanied by the morphological change of the particles. The degree of the morphological change was governed by two factors; maximum heat treatment temperature and heating rate. Transparent thick films of ca. 3$\mu\textrm{m}$ in thickness were obtained only by heat treatment at $400^{\circ}C$ for 2h with rapid heating from room temperature to $400^{\circ}C$. These films obtained were strongly adhered to the ITO-coated glass substrates and has a very smooth surface.

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Preparation of Silica Monoliths with Macropores and Mesopores and of High Specific Surface Area with Low Shrinkage using a Template Induced Method

  • Guo, Jianyu;Lu, Yan;Whiting, Roger
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.447-452
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    • 2013
  • In this study we report a new method for the synthesis of a silica monolithic column bed with bimodal pores (throughpores and mesopores). The template induced synthesis method was used to direct bimodal pores simultaneously instead of the usual post base-treating method. Block polymer Pluronic F127 was chosen as a dual-function template to form hierarchically porous silica monolith with both macropores and mesopores. This is a simplification of the method of monolithic column preparation. Poly(ethylene glycol) was used as a partial substitute for F127 can effectively prevent shrinkage during the monolith aging process without losing much surface area (944 $m^2/g$ to 807 $m^2/g$). More importantly, the resultant material showed a much narrower mesopore size (centered at 6 nm) distribution than that made using only F127 as the template reagent, which helps the mass transfer process. The solvent washing method was used to remove the remaining organic template, and it was proved to be effective enough. The new synthesis method makes the fabrication of the silica monolithic column (especially capillary column) much easier. All the structure parameters indicate that monolith PFA05 prepared by the above method is a good material for separation, with the merits of much higher surface area than usual commercial HPLC silica particles, suitable mesopore volume, narrow mesopore size distribution, low shrinkage and it is easily prepared.