• Korean Chemical Engineering Research
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• v.58 no.1
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• pp.92-97
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• 2020

In this study, the solubilities of a pharmaceutical compound, nifedipine, in three mixed solvents were determined. In addition, the nifedipine, that was dissolved in solvents (acetone, DMF, methylene chloride), was recrystallized using antisolvents (water, hexane, carbon dioxide) The external shape, size, and melting point of the crystallized nifedipine were measured. As the mixed solvents, acetone+water, DMF+water, and methylene chloride+hexane were used, and the solubility of nifedipine decreased with increasing antisolvent concentrations in the mixtures. In case of acetone+water, the solubility maximum was observed due to the density anomaly of the mixture, and this phenomenon was not observed in other systems. The crystallized nifedipine particles exhibited the bladed, equant, and prismatic habits, and the particles size was significantly reduced compared to the raw material. The average particle size of raw nifedipine was 337 ㎛, and the size of crystallized particles was in the range of 11.6~69.8 ㎛. All the crystallized nifedipine particles had the same thermal behavior and this result was not influenced by the change of solvent and antisolvent.

• Clean Technology
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• v.14 no.4
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• pp.242-247
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• 2008

Poly(N-vinyl-2-pyrrolidone) (PVP) has been used as biocompatible and biodegradable polymer in cosmetics, pharmaceuticals and electronics. Micro-particles of PVP were produced using an aerosol solvent extraction system (ASES). Dichloromethane (DCM) and supercritical carbon dioxide were used as solvent and antisolvent, respectively. The mean diameter of the obtained polymer particles ranged from 0.184 to $0.249\;{\mu}m$. The relationship between particle size and initial drop size was also considered.

• Journal of the Korean Chemical Society
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• v.27 no.1
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• pp.1-8
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• 1983

Solvent effects on nucleophilic substitution reaction of naphthalene sulfonyl chlorides with pyridine in protic and aprotic solvent have been studied by means of conductometry. Results showed that the rate constants increased with dielectric constants for protic solvents, while they decreased with dielectric constants for aprotic solvents, except for acetonitrile which has a higher dielectric constant but had also greater rate constant. The rate constants were shown to be more susceptible to polarity-polarizability parameter, , than to hydrogen bond donor acidity parameter, ${\alpha}$, indicating that the pulling effect of hydrogen bonding solvent.

• Korean Chemical Engineering Research
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• v.55 no.2
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• pp.225-229
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• 2017

Micron-sized dextran particles, which now attract wide attention as a promising drug delivery systems, can be prepared via the supercritical anti-solvent (SAS) process. In SAS process, dextran particles are obtained as a result of recrystallization of dissolved dextran in dimethyl sulfoxide (DMSO) on addition of supercritical $CO_2$ as an anti-solvent. In this work, with an intention to provide information on the feasible operating conditions of the process, the phase behavior of Dexran/DMSO/$CO_2$ is observed by measuring the cloud point in favor of a variable volume cell. From the experimental study, it is concluded that a feasible operating condition of the SAS process for preparation of dextran particles would be 300.15 K~330.15 K and 90 bar~130 bar, respectively, and solute concentration ranges from 5mg/ml to 20 mg/ml.

• Applied Chemistry for Engineering
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• v.26 no.6
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• pp.730-736
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• 2015

Cyclotrimethylene trinitramine (RDX) is a high explosive commonly used for military applications. Submicronization of RDX particles has been a critical issue in order to alleviate the unintended and accidental stimuli toward safer and more powerful performances. The purpose of this study is to optimize experimental variables for drowning-out crystallization applied to produce submicron RDX particles. Effects of RDX concentration, anti-solvent temperature and anti-solvent mass were analyzed by the central composite rotatable design. The adjusted determination coefficient of regression model was calculated to be 0.9984 having the p-value less than 0.01. Response surface plots based on the central composite rotatable design determined the optimum conditions such as RDX concentration of 3 wt%, anti-solvent temperature of $0.2^{\circ}C$ and anti-solvent mass of 266 g. The optimum and experimental diameters of RDX particles were measured to be $0.53{\mu}m$ and $0.53{\mu}m$, respectively. The regression model satisfactorily predicts the average diameter of RDX particles prepared by drowning-out crystallization. Structure of RDX crystals was found to be ${\alpha}$-form by X-ray diffraction analysis and FT-IR spectroscopy.

• 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.

• Journal of the Korean Chemical Society
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• v.39 no.8
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• pp.589-597
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• 1995

In water-ethanol systems, the limiting equivalent conductances of electrolytes were obtained using conductometric method. Using TATB method, the limiting equivalent ionic conductances of Li+, Na+, K+, Cl-, and Br- ions were also obtained. The effective radii of corresponding ions were determined using Nightingale method. From the volume of the solvation shell, the four solvation numbers were suggested. The reasonable solvation numbers (hH2O+hO) were estimated by comparing the values obtained by from the various suggested methods. The isosolvation point of ion in water-ethanol estimated was found to be larger than that of in water-methanol. This result agree with ET (solvent polarity) values of solvents. From the reasonable solvation numbers of ions in water-ethanol, the selective solvents of corresponding ions in water-ethanol were obtained.

• Journal of the Korean Chemical Society
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• v.37 no.3
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• pp.309-316
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• 1993

The limiting equivalent ionic conductances of Li$^+$, Na$^+$, K$^+$, Cl$^-$, and Br$^-$ ions were obtained with TATB[Tetraphenyl Arsonium Tetraphenyl Borate] method from limiting equivalent conductances of LiCl, NaCl, KCl and KBr measured in water-methanol systems by conductometric method. With those values and viscosity of water-methanol systems, the Stokes radii of corresponding ions have been extracted. The latter values corrected by calibration method of Nightingale and supplemented by the crystallographic radii were utilized to calculate the volume of solvation-shell that surrounds ions. The reasonable solvation numbers (h$_{H_2O}$ ＋ h$_0$) were estimated by comparing the values obtained by the various suggested methods. The selective properties of ion solvation were also discussed.

• Proceedings of the Membrane Society of Korea Conference
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• 1997.06a
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• pp.159-174
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• 1997

삼투현상이란 반투막을 사이에 두소 저농도의 용매가 고농도의 용액으로 이동하는 현상으로 막양측 용매의 화학포텐셜이 같아지게 되면 용매의 이동은 정지되고 수두차 만큼의 삼투압차가 발생한다. 이 때 고농도 용액측에 삼투압차 이상의 압력을 가하게 되면 삼투현상과는 반대로 고농도 용액측의 용매가 저농도의 용액측으로 역류하는데 이를 역삼투현상이라 한다. 역삼투현상을 이용하여 물질을 분리하는 역삼투 공정은 막의 물리화학적 특성, 분리대상물질의 물리화학적 특성, 그리고 압력차를 추진력으로 하는 세가지 요소의 조합에 의해 행하여 진다. 역삼투는 분자크기에 따른 분리조작이 아니므로 정밀여과나 한외여과에서와 같은 유기물질의 침착현상이 적으며 결과적으로 막의 수명도 길어진다. 역삼투막은 용존염을 분리제거할 뿐만 아니라 분자량이 적은 유기물 및 Aromatic hydrocarbon 등의 분리조작에도 그 이용가능성이 고조되고 있다.

• Journal of the Korean Chemical Society
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• v.16 no.6
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• pp.369-372
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• 1972

The dissociation constants of dibasic carboxylic acids $(HOOC(CH_2)_nCOOH$, n = 0~4] in methanol, N, N-dimethylformamide and acetonitrile have been determined by the potentiometric method with a glass electrode. The difference between over-all dissociation constants in each other solvent is found to be of the same order of magnitude, and the $K_1/K_2$ ratios in aprotic dimethylformamide and acetonitrile are much greater than those in protic methanol and water.