• 한국환경과학회지
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• 제13권3호
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• pp.319-325
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• 2004

An experimental study on the preparation of monolithic porous polymers by environmentally friend process in supercritical carbon dioxide has been carried out. Polymerization mixture composed of a cross-linking monomer, initiator and functional co-polymer was charged in the reactor with sapphire window. After the system was purged with a flow of $CO_2$ for 15 min, the reactor was pressurized with liquid $CO_2$ up to 100 bars. The reactor was isolated from and placed back to the system via quick connector for shaking until the mixture had become fully homogeneous. The reactor was then heated and pressurized to the required reaction conditions and left overnight. After cooling and $CO_2$ evacuation, the polymer was removed from the reactor as dry, white, continuous monoliths. The effect of experimental conditions on the physical properties of porous polymer was systematically examined, and it was found that monomer content had a major effect on the physical properties of the polymers.

• Korean Chemical Engineering Research
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• 제43권1호
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• pp.21-26
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• 2005

초임계 이산화탄소를 이용하여 다공성 고분자 모노리스를 제조하는 실험적 연구를 행하여, 단량체의 종류와 중합반응 조건들이 생성되는 고분자 모노리스의 물성에 미치는 영향을 실험적으로 조사하였다. 중합반응은 반응이 진행되는 동안 반응물의 상변화를 관찰할 수 있도록 사파이어 창을 부착한 고압 반응기 내에서 진행되었으며, 단량체의 농도가 매우 낮은 경우를 제외하고는 반응기 내부형태와 동일한 형상의 건조하고 다공성인 고분자 모노리스를 얻었을 수 있었다. 생성되는 고분자 모노리스의 비 표면적은 반응혼합물 중의 단량체 농도와 중합반응 압력에 따라 증가하였으며, 기계적 강도는 경도 보강제 MMA를 첨가하여 증대시킬 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제27권1호
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• pp.71-76
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• 2006

Porous polymer monolithic columns were prepared by the direct free radical copolymerization of methacrylic acid and ethylene glycol dimethacrylate within the confines of a chromatographic column in the presence of toluene-dodecanol as a porogenic solvent. The separation characteristics of the monolithic columns were tested by a homologous series of xanthine derivatives, theophylline and caffeine. The effects of the polymerization mixture composition and polymerization condition, mobile phase composition, flow rate and temperature on the retention times and separation efficiencies were investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and temperatures. Hydrogen-bonding interaction played an important role in the retention and separation. Compared with conventional particle columns, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency and fast analysis.

• Bulletin of the Korean Chemical Society
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• 제34권2호
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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.