• Title/Summary/Keyword: Layer melt crystallization

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Crystallization of Benzene from Benzene-Cyclohexane Mixtures by Layer Melt Crystallization - Phenomena of Impurity Inclusion in Crystal - (경막형 용융결정화에 의한 벤젠-사이클로헥산 혼합물로부터 벤젠의 결정화-결정의 불순물 내포현상-)

  • Kim, Kwang-Joo;Lee, Jung-Min;Ryu, Seung-Kon
    • Applied Chemistry for Engineering
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    • v.8 no.3
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    • pp.389-394
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    • 1997
  • The distribution of impurity included in benzene layer crystal was explored in layer crystallization of cyclohexane and benzene mixtures. The influence of crystal growth rate on crystal purity was investigated. All experimental results for bezene-cyclohexane system obtained in layer crystallizer have been evaluated with the criterion of Wintermantel. The purity of crystal decreases with increasing degree of subcooling, decreasing feed concentration and increasing crystal growth rate. The crystal growth rate was a key parameter to determine the inclusion of impurity in crystals. The results obtained from runs performed at increasing crystallization time(i.e. crystal thickness) have clearly shown that migration of inclusions within crystal layer to the melt, leading to the removal of impurity occurs. The diffusion of impurity which takes place during the crystallization from the beginning, enhances a further purification of the crystal layer if that underwent a thermal gradient after growth of the layer crystal stops.

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Purification of Naphthalene from Naphthalene and 2-methylnaphthalene System by Layer MelMelt-Crystallization (경막형 용융결정화에 의한 나프탈렌과 2-메틸나프탈렌 혼합물로부터 나프탈렌의 분리)

  • Koh, Joo-Young;Kim, Chul-Uog;Park, So-Jin
    • Clean Technology
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    • v.12 no.3
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    • pp.157-164
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    • 2006
  • In order to purify 2-methylnaphthalene as main impurity included in naphthalene, SLE (solid-liquid equilibria) on two components system including naphthalene and 2-methylnaphthalene were measured and a layered melt crystallization has been studied. SLE in the present system is shown a simple eutectic mixture and the experimental results using DSC method is similar to the static method. Purity and yield of naphthalene in crystal depended mainly on the cooling rate: Increasing cooling rate, the purity of naphthalene in crystal increase, whereas the yield of that decrease. The effective distribution coefficient (Keff) as the degree of impurity removal was observed to decrease with decreasing of cooling rate. Therefore, the purity of naphthalene by melt crystallization can be enhanced to 5~7 %.

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Stability of the growth process at pulling large alkali halide single crystals

  • V.I. Goriletsky;S.K. Bondarenko;M.M. Smirnov;V.I. Sumin;K.V. Shakhova;V.S. Suzdal;V.A. Kuznetzov
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.1
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    • pp.5-14
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    • 2003
  • Principles of a novel pulse growing method are described. The method realized in the crystal growing on a seed from melts under raw melt feeding provided a more reliable control of the crystallization process when producing large alkali halide crystals. The slow natural convection of the melt in the crucible at a constant melt level is intensified by rotating the crucible, while the crystal rotation favors a more symmetrical distribution of thermal stresses over the crystal cross-section. Optimum rotation parameters for the crucible and crystal have been determined. The spatial position oi the solid/liquid phase interface relatively to the melt surface, heaters and the crucible elements are considered. Basing on that consideration, a novel criterion is stated, that is, the immersion extent of the crystallization front (CF) convex toward the melt. When the crystal grows at a <> CF immersion, the raised CF may tear off from the melt partially or completely due to its weight. This results in avoid formation in the crystal. Experimental data on the radial crystal growth speed are discussed. This speed defines the formation of a gas phase layer at the crystal surface. The layer thickness il a function of time a temperature at specific values of pressure in the furnace and the free melt surface dimensions in the gap between the crystal and crucible wall. Analytical expressions have been derived for the impurity component mass transfer at the steady-state growth stage describing two independent processes, the impurity mass transfer along the <> path and its transit along the <> one. The heater (and thus the melt) temperature variation is inherent in any control system. It has been shown that when random temperature changes occur causing its lowering at a rate exceeding $0.5^{\circ}C/min$, a kind of the CF decoration by foreign impurities or by gas bubbles takes place. Short-term temperature changes at one heater or both result in local (i.e., at the front) redistribution of the preset axial growth speed.

A Study on the Efficient Purification Process of Dimethyl carbonate (Dimethyl Carbonate의 효율적인 정제공정 연구)

  • Lee, Sang-Won;Kim, Sung-Il;Chun, Suk-Keun;Park, Du-Goan;Park, Keun-Ho;Lee, Soo;Park, So-Jin
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.4
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    • pp.383-392
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    • 2007
  • This paper is studied on the efficient purification process of dimethyl carbonate (DMC) from the melt layer crystallization combining crystallization process, sweating process and distillation recovery process. Purity and yield of DMC crystal depended mainly on the crystallization temperature, cooling rate, sweating termperature sweating rate. Through the optimization of crystallization and sweating operation, DMC crystal can be upgraded to very high purity over 99.9% and high yield over 85%.

Effect of Cooling Rate and Crystallizer Type on the Separation of Naphthalene Mixture by Layer Melt Crystallization (경막형 용융결정화에 의한 나프탈렌 혼합물의 분리에 관한 냉각속도와 결정화기 형태의 영향)

  • Kang, So-Rim;Koh, Joo-Young;Kim, Chul-Ung;Park, So-Jin
    • Clean Technology
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    • v.13 no.1 s.36
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    • pp.72-78
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    • 2007
  • As a basic research fur the separation of effective components included in pyrolysis gas oil, the crystallization on each system of naphthalene with 2-methylnaphthalene, indene and 1-methylnaphthalene as impurity has been carried out in column and cold-finger type crystallizer, respectively. In crystallization operation, the purity of naphthalene has been a tendency of increase with decreasing of cooling rate and in the presence of impurity with lower melting point. In comparison of crystallizer types, naphthalene purity in column type crystallizer was a higher value than that in cold-finger type due to effective sweating operation after crystallization.

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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%.

Crystallization of $K_2O-SiO_2-TiO_2$ Glasses ($K_2O-SiO_2-TiO_2$ 계 유리의 결정화)

  • 김성식;박현수
    • Journal of the Korean Ceramic Society
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    • v.22 no.2
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    • pp.44-50
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    • 1985
  • The crystallization behavior of $K_2O-SiO_2$ glasses with added $TiO_2$ and the effect of $TiO_2$ on internal nuleation at temperature in the range of 875 to 121$0^{\circ}C$ have been investigated by means of X-ray diffractometry optical microscopy and scanning electron microscopy. The crystalline phase of these glasses identified by X-ray diffractometry is cristbalite. The scanning electron microspcopy reveals a two-phase layer of dendritic crystals and intersitial melt which grow from the surface at a constant rate, The observed crystallization rates are consistent with a diffusion-controlled mechanism. An equation relating viscosity and undercooling to growth rate is presented.

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A Study on the Sweating Process for High Purification of p-Dioxanone (파라디옥사논의 고순도 정제를 위한 발한(sweating) 공정에 관한 연구)

  • Kim, Sung-Il;Chun, Suk-Keun;Park, Du-Goan;Park, Keun-Ho;Park, So-Jin;Kim, Chul-Ung
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.2
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    • pp.140-148
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    • 2007
  • As an additional high purification method of p-dioxanone monomer for a high molecular weight polymer, the sweating operation of crystalline layer obtained by layered melt crystallization from p-dioxanone-diethylene glycol system was studied. Purity and yield of p-dioxanone crystal depended mainly on the sweating temperature and sweating time. Increasing sweating time and sweating temperature, the purity of p-dioxanone crystal increase, whereas the yield of that decrease, respectively. Through the optimization of sweating operation, p-dioxanone crystal can be upgraded to very high purity over 99.9 % suited to monomer for polymerization.