결정화에 의하여 Naphthalene-Benzothiophene-Methanol 계로부터 Naphthalene의 분리

김광주; 김정우; 이정민; 박소진

HWAHAK KONGHAK, Vol.37, No.5, 692-698, October, 1999

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결정화에 의하여 Naphthalene-Benzothiophene-Methanol 계로부터 Naphthalene의 분리

Separation of Naphthalene from Naphthalene-Benzothiophene-Methanol System by Solution Crystallization

김광주, 김정우, 이정민, 박소진

초록

메탄올을 이용한 용액결정화에 의하여 고용계를 이루고 있는 이성분계 유기물 naphthalene-benzothiophene 혼합물의 분리에 관한 연구가 수행되었다. 결정화 조건에 따라 나프탈렌 결정에 함유된 불순물의 내포현상이 조사되었다. 결정속에 불순물의 내포는 과냉각정도, 냉각속도 및 용매비에 대하여 조사되었으며 유효분배계수 개념에 의해 나타내었다. 결정의 순도에 미치는 결정성장속도, 물질전달계수 및 유기 혼합물의 조성비의 영향이 조사되었다. Methanol-naphthalene-benzothiophene계로부터 나프탈렌의 결정성장속도는 과포화의 3.2승에 비례하였다. 냉각속도에 따른 결정의 표면을 관찰할 때 냉각속도가 늦을수록 조밀한 표면의 결정을 얻을 수 있었고 불순물 내표가 감소함을 알 수 있었다.

Separation of naphthalene from naphthalene-benzothiophene mixture has been studied by crystallization using methanol as a solvent. The phenomena of inclusions trapped in naphthalene crystals were explored. The inclusion of impurity in crystals was investigated through process variables like the cooling rate, the subcooling degree and the ratio of solvent to organic mixtures. The purity of crystals was related to the crystal growth rate, mass transfer coefficient, residual concentration and feed concentration. The crystal growth rate of naphthalene from naphthalene-benzothiophene mixture with methanol as a solvent is proportional to the supersaturation to the 3.2 power. Morphological study proved that inclusion of impurity in crystals can be controlled by the cooling rate.

Keywords:Crystallization;Separation;Naphthalene;Growth Rate;Subcooling Degree

[References]

Ulrich J, Process Technol. Proc., 6, 585 (1989)
Marjatta LK, Chem. Technol. Ser., 241, 112 (1996)
Kirk RE, Othmer DF, Overberger CG, Seaborg GT, "Encyclopedia of Chemical Technology," 3rd ed., John Wiley and Sons, Inc., 15, New York (1979)
Wintermantal K, Wellinghoff G, Int. Chem. Eng., 34, 171 (1974)
Jancis ST, "Tech. Rev.," Sulzer, Winterthur, Switz (1986)
Mullin JW, Whiting MJL, J. Cryst. Growth, 58, 304 (1982)
van den Berg EPG, Greertman RM, Bennema P, 12th Symposium on Industrial Crystallization Proceedings, Warsaw, Poland, 3, 111 (1993)
ter Horst JH, Geertman RM, van der Heijden AE, van Rosmalen GM, "Proceedings of 13th Symposium on Industrial Crystallization," Toulouse, France, 1, 313 (1996)
Garside J, Chem. Eng. Sci., 40, 3 (1985)
Kim KJ, Kim MJ, Yeom CK, Lee JM, Choi HS, Kim HS, Park BS, J. Korean Ind. Eng. Chem., 9(7), 974 (1998)
Mersmann A, "Crystallization Technology Handbook," Mercel Dekker, New York (1995)
Schubert H, Mersmann A, Chem. Eng. Res. Des., 74(7), 821 (1996)
Karpinski PH, Chem. Eng. Sci., 40, 641 (1985)
Tai CY, Lin CH, J. Cryst. Growth, 82, 377 (1987)
Mullin JW, "Crystallization," 3rd ed., Butterworth Heinemann, Oxford (1993)
Nyvlt J, Kocova H, Cerny M, Collection Czechoslov. Chem. Commun., 38, 3199 (1973)
Meyerson AS, Decker SE, Weiping F, Ind. Eng. Chem. Process Des. Dev., 25, 925 (1986)
Kim KJ, Mersmann A, Sep. Sci. Technol., 31, 1589 (1996)
Kim KJ, Mersmann A, Chem. Eng. Res. Des., 75(2), 176 (1997)
Kim KJ, Lee CH, Ryu SK, Ind. Eng. Chem. Res., 33(1), 118 (1994)
Kim KJ, Kim MJ, Lee JM, Kim SH, Kim HS, Park BS, Fluid Phase Equilib., 146(1-2), 261 (1998)

[Referenced By]

[1] Ulrich J, Process Technol. Proc., 6, 585 (1989)

[2] Marjatta LK, Chem. Technol. Ser., 241, 112 (1996)

[3] Kirk RE, Othmer DF, Overberger CG, Seaborg GT, "Encyclopedia of Chemical Technology," 3rd ed., John Wiley and Sons, Inc., 15, New York (1979)

[4] Wintermantal K, Wellinghoff G, Int. Chem. Eng., 34, 171 (1974)

[5] Jancis ST, "Tech. Rev.," Sulzer, Winterthur, Switz (1986)

[6] Mullin JW, Whiting MJL, J. Cryst. Growth, 58, 304 (1982)

[7] van den Berg EPG, Greertman RM, Bennema P, 12th Symposium on Industrial Crystallization Proceedings, Warsaw, Poland, 3, 111 (1993)

[8] ter Horst JH, Geertman RM, van der Heijden AE, van Rosmalen GM, "Proceedings of 13th Symposium on Industrial Crystallization," Toulouse, France, 1, 313 (1996)

[9] Garside J, Chem. Eng. Sci., 40, 3 (1985)

[10] Kim KJ, Kim MJ, Yeom CK, Lee JM, Choi HS, Kim HS, Park BS, J. Korean Ind. Eng. Chem., 9(7), 974 (1998)

[11] Mersmann A, "Crystallization Technology Handbook," Mercel Dekker, New York (1995)

[12] Schubert H, Mersmann A, Chem. Eng. Res. Des., 74(7), 821 (1996)

[13] Karpinski PH, Chem. Eng. Sci., 40, 641 (1985)

[14] Tai CY, Lin CH, J. Cryst. Growth, 82, 377 (1987)

[15] Mullin JW, "Crystallization," 3rd ed., Butterworth Heinemann, Oxford (1993)

[16] Nyvlt J, Kocova H, Cerny M, Collection Czechoslov. Chem. Commun., 38, 3199 (1973)

[17] Meyerson AS, Decker SE, Weiping F, Ind. Eng. Chem. Process Des. Dev., 25, 925 (1986)

[18] Kim KJ, Mersmann A, Sep. Sci. Technol., 31, 1589 (1996)

[19] Kim KJ, Mersmann A, Chem. Eng. Res. Des., 75(2), 176 (1997)

[20] Kim KJ, Lee CH, Ryu SK, Ind. Eng. Chem. Res., 33(1), 118 (1994)

[21] Kim KJ, Kim MJ, Lee JM, Kim SH, Kim HS, Park BS, Fluid Phase Equilib., 146(1-2), 261 (1998)