Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer

doi:10.1016/j.cjche.2023.06.004

中国化学工程学报 ›› 2023, Vol. 64 ›› Issue (12): 9-17.DOI: 10.1016/j.cjche.2023.06.004

• Full Length Article • 上一篇下一篇

Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer

Wenlong Xiao¹, Yonglin Li³, Zhengming Yi¹, Sheng Yang², He'an Luo¹

1. School of Chemical Engineering, Xiangtan University, Xiangtan 411105, China;
2. School of Energy Science and Engineering, Central South University, Changsha 410083, China;
3. College of Materials and Chemical Engineering, Hunan Institute of Engineering, Xiangtan 411105, China

收稿日期:2023-02-11 修回日期:2023-05-27 出版日期:2023-12-28 发布日期:2024-02-05
通讯作者: Zhengming Yi,E-mail:yizm@xtu.edu.cn;Sheng Yang,E-mail:ceshyang@csu.edu.cn
基金资助:
The authors gratefully acknowledge the financial support by China Hunan Provincial Education Department Innovation Platform Project (20k125), Postgraduate Scientific Research Innovation Project of Hunan Province (CX20210518), and Postgraduate Scientific Research Innovation Project of Xiangtan University (XDCX2021B169).

Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer

Wenlong Xiao¹, Yonglin Li³, Zhengming Yi¹, Sheng Yang², He'an Luo¹

1. School of Chemical Engineering, Xiangtan University, Xiangtan 411105, China;
2. School of Energy Science and Engineering, Central South University, Changsha 410083, China;
3. College of Materials and Chemical Engineering, Hunan Institute of Engineering, Xiangtan 411105, China

Received:2023-02-11 Revised:2023-05-27 Online:2023-12-28 Published:2024-02-05
Contact: Zhengming Yi,E-mail:yizm@xtu.edu.cn;Sheng Yang,E-mail:ceshyang@csu.edu.cn
Supported by:
The authors gratefully acknowledge the financial support by China Hunan Provincial Education Department Innovation Platform Project (20k125), Postgraduate Scientific Research Innovation Project of Hunan Province (CX20210518), and Postgraduate Scientific Research Innovation Project of Xiangtan University (XDCX2021B169).

摘要/Abstract

摘要： With the increasing demand for high-purity products, the industrial application of melt crystallization technology has been highly concerned. In this study, the purification process of nitrochlorobenzene binary eutectic system (NBES) and naphthalene–benzothiophene solid solution system (NBSSS) in tower melting crystallizer is analyzed, and a mathematical model of crystallization process is established. The key parameters in terms of feed concentration, crystal bed height, reflux ratio and stirring speed efficiency on purification effects were discussed by the established model. The results show that the concentration of p-nitrochlorobenzene was purified from 90.85% to 99.99%, when the crystal bed height is 600 mm, the reflux ratio is 2.5, and the stirring speed is 12 r·min^-1. The naphthalene concentration is purified from 95.89% to 99.99%, when the crystal bed height is 400 mm, the reflux ratio is 1.43, and the stirring speed is 16 r·min^-1. The quality of the model is evaluated by the ARD (average relative deviation). The minimum ARD values of the NBES and NBSSS are 2.39% and 5.22%, respectively, indicating the model satisfactorily explains the purification process.

关键词: Crystallization, Separation, Mathematical modeling, Crystallizer, Purification

Abstract: With the increasing demand for high-purity products, the industrial application of melt crystallization technology has been highly concerned. In this study, the purification process of nitrochlorobenzene binary eutectic system (NBES) and naphthalene–benzothiophene solid solution system (NBSSS) in tower melting crystallizer is analyzed, and a mathematical model of crystallization process is established. The key parameters in terms of feed concentration, crystal bed height, reflux ratio and stirring speed efficiency on purification effects were discussed by the established model. The results show that the concentration of p-nitrochlorobenzene was purified from 90.85% to 99.99%, when the crystal bed height is 600 mm, the reflux ratio is 2.5, and the stirring speed is 12 r·min^-1. The naphthalene concentration is purified from 95.89% to 99.99%, when the crystal bed height is 400 mm, the reflux ratio is 1.43, and the stirring speed is 16 r·min^-1. The quality of the model is evaluated by the ARD (average relative deviation). The minimum ARD values of the NBES and NBSSS are 2.39% and 5.22%, respectively, indicating the model satisfactorily explains the purification process.

Key words: Crystallization, Separation, Mathematical modeling, Crystallizer, Purification

Wenlong Xiao, Yonglin Li, Zhengming Yi, Sheng Yang, He'an Luo. Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer[J]. 中国化学工程学报, 2023, 64(12): 9-17.

参考文献

[1] J. Ulrich, Is melt crystallization a green technology? Cryst. Growth Des. 4 (5) (2004) 879–880.
[2] Q. Liu, Z.J. Li, B.S. Liu, H. Sun, A new melt crystallization process for efficient purification of chlorobromobenzene, Sep. Purif. Technol. 251 (2020) 117367.
[3] H. Feng, N. Wang, X. Huang, T. Wang, L.N. Zhou, H.X. Hao, Recent progress in melt crystallization, Chem. Eng. Res. Des. 190 (2023) 268–281.
[4] S.Z. Jia, B. Jing, Z.G. Gao, J.B. Gong, J.K. Wang, S. Rohani, Melt crystallization of 2,4-dinitrochlorobenzene: Purification and process parameters evaluation, Sep. Purif. Technol. 259 (2021) 118140.
[5] L. Gang, K. Chen, Y. Shao, B. Wu, L. Ji, Y. Wu, J. Zhu, Preparation of high purity phosphoric acid by layer melt crystallization, Inorg. Chem. Ind. 51 (01) (2019) 21-25. ((in Chinese)).
[6] T. Beierling, J. Osiander, G.Sadowski, Melt crystallization of isomeric long-chain aldehydes from hydroformylation, Sep. Purif. Technol. 118 (2013) 13–24.
[7] B.Y. Zhang, L. Yang, H.L. Wang, C.L. Shen, Y.Y. Li, J.C. Cheng, C. Yang, Experiment and modeling of static layer melt crystallization in a crystallizer with an inner cooling tube, J. Cryst. Growth 593 (2022) 126739.
[8] L. Chen, Progress in separation of para-xylene by suspension crystallization technology, Mod. Chem. Ind. 40 (02) (2020) 57-61. (in Chinese).
[9] W. Liu, S. Liu, Y. Ma, The latest development of zone melting technology, Rare Met. Cem. Carbides 41 (01) (2013) 66-71. (in Chinese).
[10] G.J. Arkenbout, Progress in continuous fractional crystallization, Sep. Purif. Method. 7 (1) (1978) 99–134.
[11] S. Münzberg, H. Lorenz, A. Seidel-Morgenstern, Multistage countercurrent crystallization for the separation of solid solutions, Chem. Eng. Technol. 39 (7) (2016) 1242–1250.
[12] K. Tamura, H. Tsuge, Characteristics of multistage column crystallizer for gas–liquid reactive crystallization of calcium carbonate, Chem. Eng. Sci. 61 (17) (2006) 5818–5826.
[13] K. Otawara, T. Matsuoka, Axial dispersion in a kureha crystal purifier (KCP), J. Cryst. Growth 237-239 (2002) 2246–2250.
[14] H. Kawachi, H. Ooshima, Crystallization of ergosterol from hexane solution by a continuous column crystallizer equipped with a water feeding system, J. Chem. Eng. Japan 39 (11) (2006) 1200–1205.
[15] J. Ulrich, T. Stelzer, Design examples of melt crystallization, In: Crystallization: Basic Concepts and Industrial Applications (Chap. 17), 2013, pp. 325-335. https://doi.org/10.1002/9783527650323.ch17.
[16] Q. Li, H. Liu, B. Wang, Y. Zhang, High purity separation of eutectic mixtures in a continuous moving crystal bed column crystallization, Chem. Eng. Res. Des. 81 (10) (2003) 1373–1378.
[17] Q. Li, W. Zhang, Melt crystallization technology and its application, Chem. Prod. Technol. 20 (2013) 29-31. (in Chinese).
[18] S.P. Ding, X. Huang, Q.X. Yin, Y.Y. Dong, Y.H. Bai, T. Wang, H.X. Hao, Heat transfer and its effect on growth behaviors of crystal layers during static layer melt crystallization, Chem. Eng. Sci. 233 (2021) 116390.
[19] B.H. Ryu, M.J. Jones, J. Ulrich, Crystallization of hen egg white lysozyme by solvent freeze-out: Effect of cooling rate on protein inclusion in the ice layer, Chem. Eng. Technol. 33 (10) (2010) 1695–1698.
[20] L.F. Zhou, M. Su, B. Benyahia, A. Singh, P.I. Barton, B.L. Trout, A.S. Myerson, R.D. Braatz, Mathematical modeling and design of layer crystallization in a concentric annulus with and without recirculation, AIChE J. 59 (4) (2013) 1308–1321.
[21] E. Temmel, S. Wloch, U. Müller, D. Grawe, R. Eilers, H. Lorenz, A. Seidel-Morgenstern, Separation of systems forming solid solutions using counter-current crystallization, Chem. Eng. Sci. 104 (2013) 662–673.
[22] K.J. Kim, J.W. Kim, J.S. Chae, S.K. Ryu, Purification of naphthalene from coal tar distillate by solution and melt crystallizations, Sep. Sci. Technol. 38 (11) (2003) 2407–2424.
[23] W. Li, A. Xuan, Y. Wu, L. Cheng, Advance of research on solid–liquid equilibrium, Petrochem. Technol. 36 (2007) 1067-1073. (in Chinese).
[24] W. Xiao, B. Huang, Y. Li, Z. Yi, Experimental investigation of continuous multistage countercurrent crystallizer for separation p-nitrochlorobenzene and o-nitrochlorobenzene, Sep. Purif. Technol. 267 (2021) 118648.
[25] Q.S. Li, Z.M. Yi, X.F. Sun, M.G. Su, Purification of naphthalene from eutectic mixture by continuous column crystallization, Korean J. Chem. Eng. 27 (2) (2010) 619–623.
[26] Jr.C. Moyers, J.H. Olson, Dense-bed column crystallizer: An experimental and analytical study. AIChE J. 20(6) (1974) 1118–1124.
[27] J.D. Henry, J.E. Powers, Experimental and theoretical investigation of continuous flow column crystallization, AIChE J. 16 (6) (1970) 1055–1063.
[28] M.A. van der Gun, O.S.L. Bruinsma, P.J. Jansens. Purification of polycrystalline ε-caprolactam particles, Chem. Eng. Sci. 60(1) (2005) 201-211.
[29] K. Funakoshi, H. Uchida, H. Takiyama, M. Matsuoka, Influences of reflux ratio on separation and purification of acrylic acid by inclined column crystallizer, J. Cryst. Growth 237-239 (2002) 2251–2256.
[30] L. Chen, J. Li, M. Matsuoka, Experimental and theoretical investigation of the purification process of organic materials in a continuous inclined column crystallizer, Ind. Eng. Chem. Res. 45 (8) (2006) 2818–2823.
[31] A.M. Chen, K. Chen, J.W. Zhu, B. Wu, L.J. Ji, Purification of phosphoric acid in a gravity wash column, Can. J. Chem. Eng. 91 (5) (2013) 944–949.
[32] M.A. van der Gun, O.S.L. Bruinsma, G.M. van Rosmalen, Pastille purification in a gravity wash column, Chem. Eng. Sci. 56 (7) (2001) 2381–2388.
[33] T. Chen, G. Zhang, Fundamentals of Chemical Transfer Processes (3rd ed.), Chemical Industry Press, Beijing, 2009, pp. 255–256. (in Chinese).

Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer

Experiments and model development of p-nitrochlorobenzene and naphthalene purification in a continuous tower melting crystallizer

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