• Title/Summary/Keyword: 경막결정화

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Study on the Selection of Solvent for Purificatino of p-Dioxanone by Crystallization Method (결정화에 의한 파라디옥산온의 정제를 위한 용매선정에 관한 연구)

  • kim, Sung-Il;Koh, Joo-young;Kim, Chul-Ung;Koh, Jae-Cheon;Park, So-Jin;Seo, Young-Jong;Choi, Byung-Ryul
    • Applied Chemistry for Engineering
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    • v.16 no.4
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    • pp.581-587
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    • 2005
  • In order to obtain a highly purified p-dioxanone (PDX) as monomer of biodegradable polymer, suitable solvent must be selected. The selection was based on the solubility of impurities, and partial layer melt crystallization were carried out under the presence of solvent. The solubility of PDX in various solvents such as ethyl acetate, tetrahydrofuran, acetone, alcohols (methanol, ethanol, 1-propanol, 1-butanol and 1-pentanol) were measured over the temperature range of $-10{\sim}15^{\circ}C$. As solubility parameters, the mixing and dissolution enthalpy between the PDX and the solvents was studied based on empirical equations and the regular solution theory. The solubility and the temperature dependency of the solubility with the solvents of acetone, ethylacetate, and tetrahydrofuran of PDX were shown to have relatively high values compared to the alcohol type solvents. Also, in same alcohols, the smaller molecules and higher polarity gave higher solvency. In partial layer melt crystallization, small amount of ethylacetate selectively dissolved impurities and gave highly purified p-dioxanone, over 99.9% purity.

Purification of p-Dioxanone from p-Dioxanone and Diethylene Glycol Mixture by a Layer Melt Crystallization (경막형 용융결정화에 의한 파라디옥사논과 디에틸렌글리콜 혼합물로부터 파라디옥사논의 정제)

  • Kim, Sung-Il;Kim, Chul-Ung;Park, So-Jin
    • Korean Chemical Engineering Research
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    • v.43 no.5
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    • pp.595-602
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    • 2005
  • In order to purify diethylene glycol as main impurity included in p-dioxanone, SLE (solid-liquid equilibria) and mixture density on two components system of p-dioxanone and diethylene glycol were measured and a layered melt crystallization with seed has been applied. The SLE of p-dioxanone and diethylene glycol were a simple eutectic system and the temperature and PDX concentration at eutectic point were 0.08 and 246 K, respectively. Densities of their binary mixtures were well fitted by the best correlation equation, ${\rho}_l=0.405+1.361x+0.002T-0.004xT$. In the melt crystallization, the growth rate (G) was proportional to the 1.5th power of the subcooling degree. The effective distribution coefficient ($K_{eff}$) as the degree of impurity removal was observed to increase with increasing the growth rate and initial p-dioxanone concentration. And also, $K_{eff}$ was correlated with Z function using Wintermantel's model such as $K_{eef}=-0.0604+6.392{\times}Z$. Finally, PDX purity through the optimization of this process can be obtained over 99%.

Removal of CO2 in Syngas using Li2ZrO3 (Li2ZrO3를 이용한 합성가스내의 CO2 제거)

  • Park, Joo-Won;Kang, Dong-Hwan;Yoo, Kyung-Seun;Lee, Jae-Goo;Kim, Jae-Ho;Han, Choon
    • Applied Chemistry for Engineering
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    • v.17 no.3
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    • pp.250-254
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    • 2006
  • Reaction of $CO_2$ with $Li_{2}ZrO_{3}$ has been investigated in a TGA and the effects of $H_{2}$ and CO on the removal of $CO_{2}$ using $Li_{2}ZrO_{3}$ were evaluated in a packed bed reactor. The initial rate of $CO_{2}$ removal reaction of $Li_{2}ZrO_{3}$ increased with the increase of gas flow rate up to 100 mL/min and then was maintained, which implied the disappearance of the gas film resistance. The reaction of $CO_{2}$ with $Li_{2}ZrO_{3}$ took place as the first order and the range of optimum temperature was found to be about $500{\sim}600^{\circ}C$. XRD and SEM analysis showed the formation of crystalline $Li_{2}ZrO_{3}$ and porous $Li_{2}ZrO_{3}$/$ZrO_{2}$. The presence of $H_{2}$ did not affect the adsorption of $CO_2$ with $Li_2ZrO_3$. On the other hand, CO inhibited the sorption of $CO_{2}$ into $Li_{2}CO_{3}$(L) on $Li_{2}ZrO_{3}$.