SCI和EI收录∣中国化工学会会刊

Chinese Journal of Chemical Engineering ›› 2023, Vol. 58 ›› Issue (6): 163-169.DOI: 10.1016/j.cjche.2022.10.010

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Sulfonation of 1, 4-diaminoanthraquinone leuco by chlorosulfonic acid: Kinetics and process intensification

Bing Liu1,2, Yingjiao Li1,2, Moses Arowo3, Guangwen Chu1,2, Yong Luo1,2, Liangliang Zhang1,2, Haikui Zou1,2, Baochang Sun1,2   

  1. 1. State Key Laboratory of Organic-Inorganic Composites, Beijing University of Chemical Technology, Beijing 100029, China;
    2. Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, Beijing 100029, China;
    3. Department of Chemical & Process Engineering, Moi University, Eldoret 3900-30100, Kenya
  • Received:2022-07-20 Revised:2022-10-01 Online:2023-08-31 Published:2023-06-28
  • Contact: Guangwen Chu,E-mail:chugw@mail.buct.edu.cn;Baochang Sun,E-mail:sunbc@mail.buct.edu.cn
  • Supported by:
    This work was financially supported by the National Key Research and Development Program of China (2016YFB0301500) and the National Natural Science Foundation of China (21878009).

Sulfonation of 1, 4-diaminoanthraquinone leuco by chlorosulfonic acid: Kinetics and process intensification

Bing Liu1,2, Yingjiao Li1,2, Moses Arowo3, Guangwen Chu1,2, Yong Luo1,2, Liangliang Zhang1,2, Haikui Zou1,2, Baochang Sun1,2   

  1. 1. State Key Laboratory of Organic-Inorganic Composites, Beijing University of Chemical Technology, Beijing 100029, China;
    2. Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, Beijing 100029, China;
    3. Department of Chemical & Process Engineering, Moi University, Eldoret 3900-30100, Kenya
  • 通讯作者: Guangwen Chu,E-mail:chugw@mail.buct.edu.cn;Baochang Sun,E-mail:sunbc@mail.buct.edu.cn
  • 基金资助:
    This work was financially supported by the National Key Research and Development Program of China (2016YFB0301500) and the National Natural Science Foundation of China (21878009).

Abstract: The work herein employed a rotating packed bed (RPB) to intensify the sulfonation process of 1,4-diaminoanthraquinone leuco (DL) in an attempt to improve the yield of the product 1,4-diaminoanthraquinone-2-sulfonic acid (DSA). First, the effects of operating conditions in a stirred tank reactor (STR), including stirring speed, chlorosulfonic acid/DL molar ratio (η), solvent/DL mass ratio (ζ), reaction temperature and dropping speed of chlorosulfonic acid, on the yield of DSA were investigated. The yield of DSA can reach 87.34% under the optimal operating conditions: stirring speed of 500 r·min-1, η of 4.5, ζ of 7, reaction temperature of 150 ℃, dropping speed of 0.61 ml·min-1. In addition, the kinetics of the sulfonation process via the shrinking core model revealed that the reaction is controlled by diffusion via a product layer under the reaction temperature of 140 ℃. Furthermore, the RPB was employed to intensify the mass transfer between liquid and solid phases during the sulfonation reaction process. The results showed that the DSA yield of 92.69% obtained by RPB was 5.35% higher than that by STR, indicating that RPB can significantly intensify the mass transfer in the liquid-solid phase sulfonation reaction process.

Key words: Sulfonation, 1,4-Diaminoanthraquinone-2-sulfonic acid, Kinetics, Rotating packed bed (RPB), Chlorosulfonic acid

摘要: The work herein employed a rotating packed bed (RPB) to intensify the sulfonation process of 1,4-diaminoanthraquinone leuco (DL) in an attempt to improve the yield of the product 1,4-diaminoanthraquinone-2-sulfonic acid (DSA). First, the effects of operating conditions in a stirred tank reactor (STR), including stirring speed, chlorosulfonic acid/DL molar ratio (η), solvent/DL mass ratio (ζ), reaction temperature and dropping speed of chlorosulfonic acid, on the yield of DSA were investigated. The yield of DSA can reach 87.34% under the optimal operating conditions: stirring speed of 500 r·min-1, η of 4.5, ζ of 7, reaction temperature of 150 ℃, dropping speed of 0.61 ml·min-1. In addition, the kinetics of the sulfonation process via the shrinking core model revealed that the reaction is controlled by diffusion via a product layer under the reaction temperature of 140 ℃. Furthermore, the RPB was employed to intensify the mass transfer between liquid and solid phases during the sulfonation reaction process. The results showed that the DSA yield of 92.69% obtained by RPB was 5.35% higher than that by STR, indicating that RPB can significantly intensify the mass transfer in the liquid-solid phase sulfonation reaction process.

关键词: Sulfonation, 1,4-Diaminoanthraquinone-2-sulfonic acid, Kinetics, Rotating packed bed (RPB), Chlorosulfonic acid