• Proceedings of the KSME Conference
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• 2004.11a
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• pp.1323-1328
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• 2004

This paper shows the study on the design of the spray-freeze dryer for the production of the pulmonary inhalation powders. Powder production and handling has been an integral part of pharmaceutical processing because of the wide use of oral dosage forms. There are a few commonly used powder preparation methods including mechanical milling, precipitaion, spray drying, freeze drying, and so on. In general, methods available for preparing inhalation powders are limited due to certain inhalation powder's sensitive nature to the processing environments. This is particularly true for preparing dry powder aerosols where the aerodynamic particle size$(<5{\mu}m)$ and the size distribution are pivotal. Supercritical fluid antisolvent and spray freeze drying have recently emerged as promising techniques for producing powders for use in microcapsulation. However, the aerosol applications of these powders are yet to be explored. The purpose of this study is to test the feasibility of using spray freeze-dried pulmonary inhalation powders for aerosolization.

• KSBB Journal
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• v.26 no.1
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• pp.69-77
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• 2011

In this study, poly (L-lactic acid) (PLLA) microparticles containing gemcitabine hydrochloride were prepared by a supercritical fluid process, called aerosol solvent extraction system (ASES), utilizing supercritical carbon dioxide as antisolvent. The influence of process parameters such as temperature, pressure, $CO_2$ and solution flow rate, solution concentration, and feed ratio of drug to polymer on the morphology and characteristics of the microparticles was studied in detail. The gemcitabine-loaded microparticles exhibited a spherical shape with a smooth surface. The entrapment efficiency of gemcitabine increased with increasing temperature, solution concentration and $CO_2$ flow rate and with decreasing drug/polymer feed ratio. The maximum drug loading obtained from the ASES process was found to be about 11%. The ASES-processed PLLA microparticles containing gemcitabine showed a relatively high initial burst due to the presence of surface pores on the microparticles and the poor affinity between drug and polymer.

• Proceedings of the Korea Committee for Ocean Resources and Engineering Conference
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• 2004.11a
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• pp.1-6
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• 2004

This paper shows the study on the design and another applications of the spray-freeze dryer for the production of valuable material powders. Powder production and handling has been an integral part of material extracting processing and pharmaceutical processing because of the wide use of oral dosage forms. There are a few commonly used powder preparation methods including mechanical milling, precipitaion, spray drying, freeze drying, and so on. In general, methods available for preparing inhalation powders are limited due to certain inhalation powder's sensitive nature to the processing environments. This is particularly true for preparing dry powder aerosols where the aerodynamic particle size($<5{\mu}m$) and the size distribution are pivotal. Supercritical fluid antisolvent and spray freeze drying have recently emerged as promising techniques for producing powders for use in microcapsulation. However, the aerosol applications of these powders are yet to be explored. The purpose of this study is to test the feasibility of using spray freeze-dried valuable material powders for aerosolization.

• Clean Technology
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• v.19 no.3
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• pp.212-218
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• 2013

The microparticles of 2-hydroxypropyl-${\beta}$-cyclodextrin (HP-${\beta}$-CD) were prepared using aerosol solvent extraction system (ASES) by employing supercritical carbon dioxide as an antisolvent, The effects of various process parameters such as temperature, pressure, solution concentration and solution flow rate on the formation of HP-${\beta}$-CD microparticles were investigated. The HP-${\beta}$-CD microparticles prepared by the ASES process were observed to consist of agglomerates of nano-sized (50-200 nm) particles. When an aqueous solution of ethanol was used as a solvent for HP-${\beta}$-CD, the HP-${\beta}$-CD particles were found to be spherical in shape and to become larger as the water content increased. It was confirmed that the micronization of HP-${\beta}$-CD using the ASES process could enhance the inclusion efficiency of ibuprofen/HP-${\beta}$-CD complexes significantly.

• Clean Technology
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• v.15 no.4
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• pp.233-238
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• 2009

Supercritical fluid processes have gained great attention as a new and environmentally-benign method of preparing the microparticles of energetic materials like explosives and propellants. In this work, RDX (cyclotrimethylenetrinitramine) was selected as a target explosive. The microparticle formation of RDX using supercritical anti-solvent (SAS) recrystallization process was performed and the effect of operating variables on the size and morphology of prepared particles was observed. N,N-Dimethylformamide was used as organic solvent for dissolving the RDX. The size of the RDX particles decreased remarkably up to less than $10\;{\mu}m$ by SAS recrystallization. In the range of operating conditions of the SAS process studied in this work, the finest RDX particles were obtained at 313.15K, 150 bar, and 15wt% RDX concentration in feed solution.

• Korean Chemical Engineering Research
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• v.47 no.6
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• pp.740-746
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• 2009

In the present study, the drowning-out crystallization of L(+)-calcium lactate was investigated in order to develop the crystallization separation process. The crystallization of the calcium lactate was induced by injecting the alcoholic anti-solvent into the aqueous solution of calcium lactate and the control of the calcium lactate crystal size during the crystallization was primarily investigated under the consideration of the anti-solvent species, anti-solvent composition and agitation speed as the key operating factors. Alcohols of methanol, ethanol, n-propanol and i-propanol were used as the anti-solvent for the drowning-out crystallization. Prior to the crystallization experiment, the solubility of calcium lactate in the water-alcohol mixture was measured along with the variation of the alcohol species and composition, which was necessary to estimate the supersaturation level of the crystallization. By the drowning-out crystallization, the calcium lactate crystals of the fabric shape were obtained. Using the ethanol as the antisolvent, the fabric crystals close to the needle shape were produced. However, the hairy crystals were obtained by using the propanol as the anti-solvent. Due to such morphological features, the crystals was highly apt to form the aggregates. The aggregation of the crystals was intensified as increasing the alcohol fraction in the water-alcohol mixture. Meanwhile, the agitation caused the breakage of crystals, resulting in the decrease of the crystal size. Therefore, the crystal size in the crystallization was predominantly determined by the competition between the crystal aggregation and breakage.

• Korean Chemical Engineering Research
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• v.46 no.5
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• pp.958-964
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• 2008

In this work, micro-sized dextran particles, which have recently been focused as one of the candidate materials for the Drug Delivery System(DDS), were prepared by means of the Supercritical Antisolvent (SAS) process with $CO_2$. With dimethyl sulfoxide(DMSO) as the solvent, effects of the operating variables such as temperature (308.15~323.15 K), pressure(90~130 bar), solute concentration(10~20 mg/ml), and the molecular weight of the solute(Mw=37,500, 450,000) on the size and morphology of the resulting particles were thoroughly observed. The higher solute concentration led to the larger particles, however, the injection velocity of the solution and pressure did not show significant effects on the resulting particle size. With dextran of the lower molecular weight, the smallest particles were obtained at 313.15 K. On the other hand, the size of the particles from the high molecular weight dextran ranged between $0.1{\sim}0.5{\mu}m$ with an incremental effect of the temperature and pressure. For the solute concentration of 5 mg/ml, the lower molecular weight dextran did not form discrete particles while aggregation of the particles appeared when the solute concentration exceeded 15 mg/ml for the higher molecular weight dextran. It is believed that if the solute concentration is too low, the degree of the supersaturation in the recrystallization chamber would not be sufficient for initiation of the nucleation and growth mechanism. Instead, the spinodal decomposition mechanism leads to formation of the island-like phase separation which appears similar to aggregation of the discrete particles. This effect would be more pronounced for the smaller molecular weight polymer system due to the narrower phase-splitting region.

• Polymer(Korea)
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• v.31 no.2
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• pp.168-176
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• 2007

The sub-micron particles of poly ($\gamma-glutamic$ acid) (PGA) containing lysozyme have been prepared using supercritical antisolvent (SAS) precipitation process at various experimental conditions such as pressure, temperature, inner diameter of nozzle, and concentration. As overall results of the application of SAS process to this system, the smaller size powder has been produced as (i) increasing pressure, (ii) decreasing temperature, (iii) decreasing the inner diameter of nozzle, and (iv) decreasing the concentration of PGA and lysozyme. It is found by means of FT-IR analysis that during SAS process, the composition has changed from the original composition of PGA : lysozyme=50 : 50 into PGA : lysozyme=33 : 67 at final product powder. It means that PGA has higher solubility for the mixed solvent of carbon dioxide and dimethyl sulfoxide (DMSO). Due to such difference of solubility, this particle forms the core-shell structure of which the core consists mainly of lysozyme. It is also found that the residual DMSO amount of $7.8\times10^{-3}wt%$ exists inside the powder.