Purification of 2-mercaptobenzothiazole by solvent extraction

Prakorn Ramakul; Milan Hronec; Ura Pancharoen

Korean Journal of Chemical Engineering, Vol.24, No.2, 282-287, March, 2007

DOI10.1007/s11814-007-5042-z Export Citation

Purification of 2-mercaptobenzothiazole by solvent extraction

Prakorn Ramakul, Milan Hronec¹, and Ura Pancharoen^†

Department of Chemical Engineering, Faculty of Engineering, Chulalongkorn University, Patumwun, Bangkok, Thailand
¹Department of Organic Technology, Faculty of Chemical and Food Technology, Slovak University of Technology, Bratislava, Slovakia (Slovak Republic)

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Purification of 2-mercaptobenzothiazole (91.9% purity) by solvent extraction was studied. The extraction of impurities present in crude 2-MBT (e.g. benzothiazole, sulfides and sulfur containing compounds) was carried out at temperatures between 70-180 ℃ using various solvents and their mixtures of different polarity. The highest purity of 2-MBT, above 99% was obtained using nitrobenzene, toluene and ethanol, even at a concentration of 2-MBT above 50 wt%. Increasing temperature and decreasing concentration of the raw material have a positive influence on the purification process. A comparable efficiency of purification was observed also with mixed solvents, (toluene with ethanol, acetone and aniline) possessing the same polarities. A correlation between the polarity indexes (PI) of mixed solvents and experimentally obtained purity of 2-MBT was found. The highest purity of 2-MBT provides extraction of the raw material with mixed solvents having PI 3.8-4.4

Keywords:Purification;Impurities;2-Mercaptobenzothiazole;Solvent Extraction;Polarity

[References]

Spies RB, Andresen BD, Rice D, Nature, 327, 697 (1987)
Alicot M, Tignol A, FR patent, 2450828 (1980)
Harman MW, US patent 2191656 (1940)
Chemical M, GB patent 642597 (1950)
Reinartz K, Schlesmann H, Dietl S, DE patent 4126992 (1992)
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Robert HP, US patent 2090233 (1937)
Leslie S, US patent 3030373 (1962)
Michel J, Alicot C, Adrien P, Tignol N, US patent 4371698 (1984)
Prakorn R, Kwanta N, Ura P, Korean J. Chem. Eng., 21(6), 1212 (2004)
Roger ES, Allan JS, Modern methods of pharmaceutical analysis 2nd edition, Volume II, Guided Wave, Inc., El Dorado Hills, CA, CRC Press (1991)

[Referenced By]

[1] Spies RB, Andresen BD, Rice D, Nature, 327, 697 (1987)

[2] Alicot M, Tignol A, FR patent, 2450828 (1980)

[3] Harman MW, US patent 2191656 (1940)

[4] Chemical M, GB patent 642597 (1950)

[5] Reinartz K, Schlesmann H, Dietl S, DE patent 4126992 (1992)

[6] Sakuma K, Hotsuta K, JP patent 60025979 (1985)

[7] Khamitov RN, Kononova TP, Osipova TF, Nagaev T, SU patent, 852869 (1981)

[8] Teshima M, Kifune T, Koizumi T, Kawaoka Y, DE patent 2652394 (1977)

[9] Ebel RH, GB patent GB734970 (1955)

[10] Robert HP, US patent 2090233 (1937)

[11] Leslie S, US patent 3030373 (1962)

[12] Michel J, Alicot C, Adrien P, Tignol N, US patent 4371698 (1984)

[13] Prakorn R, Kwanta N, Ura P, Korean J. Chem. Eng., 21(6), 1212 (2004)

[14] Roger ES, Allan JS, Modern methods of pharmaceutical analysis 2nd edition, Volume II, Guided Wave, Inc., El Dorado Hills, CA, CRC Press (1991)