Agglomeration Mechanisms and Kinetics during the Carbonation of a Suspension of Lime in a Pilot Batch Reactor
Author(s)
Mathilde Schnebelen1,2*,
Kevin Mozet1,
Alexandra Jakob2,
Didier Sy2,
Edouard Plasari1,
Hervé Muhr1
Affiliation(s)
1 Université de Lorraine, Laboratoire Réactions et Génie des Procédés, Nancy, France. 2 Solvay Spécialités France, Salin de Giraud, France.
1 Université de Lorraine, Laboratoire Réactions et Génie des Procédés, Nancy, France. 2 Solvay Spécialités France, Salin de Giraud, France.
ABSTRACT
The reaction studied in this work is the synthesis of nanometric size calcium carbonate particles by carbonation of a suspension of lime, which represents the most common industrial route. It consists in bubbling carbon dioxide in a suspension of lime to obtain precipitated calcium carbonate (PCC). PCC is a mineral filler with various applications: sealants, paints, paper, ink, pharmacy, cosmetics, food etc. However, there is a challenge related to the synthesis and the use of this precipitate: the agglomeration of the monoparticles. The aim of this work is then to understand the mechanisms of this phenomenon and to study its kinetics to improve the run of the process and the control of its impact on the final product. Experiments realized with a high concentration in sodium chloride (2 M) showed that the modification of the electrostatic environment did not change the particle size distribution and the morphology of the agglomerates. This indicates that the electrostatic interactions are not responsible for the agglomeration but the formation of crystalline bridges induced by the crystal growth. Thus, thanks to an agglomeration model including the crystal growth rate, the agglomeration kernel β and the agglomeration constant β0 can be determined using a mathematical treatment of the experimental particle size distributions. Finally, by varying the experimental conditions, it appears that the agglomeration constant increases with the temperature whereas there is an optimal value regarding the shear rate.
The reaction studied in this work is the synthesis of nanometric size calcium carbonate particles by carbonation of a suspension of lime, which represents the most common industrial route. It consists in bubbling carbon dioxide in a suspension of lime to obtain precipitated calcium carbonate (PCC). PCC is a mineral filler with various applications: sealants, paints, paper, ink, pharmacy, cosmetics, food etc. However, there is a challenge related to the synthesis and the use of this precipitate: the agglomeration of the monoparticles. The aim of this work is then to understand the mechanisms of this phenomenon and to study its kinetics to improve the run of the process and the control of its impact on the final product. Experiments realized with a high concentration in sodium chloride (2 M) showed that the modification of the electrostatic environment did not change the particle size distribution and the morphology of the agglomerates. This indicates that the electrostatic interactions are not responsible for the agglomeration but the formation of crystalline bridges induced by the crystal growth. Thus, thanks to an agglomeration model including the crystal growth rate, the agglomeration kernel β and the agglomeration constant β0 can be determined using a mathematical treatment of the experimental particle size distributions. Finally, by varying the experimental conditions, it appears that the agglomeration constant increases with the temperature whereas there is an optimal value regarding the shear rate.
Cite this paper
Schnebelen, M. , Mozet, K. , Jakob, A. , Sy, D. , Plasari, E. and Muhr, H. (2015) Agglomeration Mechanisms and Kinetics during the Carbonation of a Suspension of Lime in a Pilot Batch Reactor. Crystal Structure Theory and Applications, 4, 35-46. doi: 10.4236/csta.2015.43005.
Schnebelen, M. , Mozet, K. , Jakob, A. , Sy, D. , Plasari, E. and Muhr, H. (2015) Agglomeration Mechanisms and Kinetics during the Carbonation of a Suspension of Lime in a Pilot Batch Reactor. Crystal Structure Theory and Applications, 4, 35-46. doi: 10.4236/csta.2015.43005.
References
[1] Schnebelen, M., Ricaud, M., Jakob, A., Sy, D., Plasari, E. and Muhr, H. (2015) Determination of Crystallization Kinetics and Size Distribution Parameters of Agglomerated Calcium Carbonate Nanoparticles during the Carbonation of a Suspension of Lime. Crystal Structure Theory and Applications, 4, 16-27. [2] Liao, P. and Hulburt, H. (1976) Agglomeration Process in Suspension Crystallization. Proceedings of 69th Annual Meeting American Institute of Chemical Engineers. [3] Tavare, N., Shah, M. and Garside, J. (1985) Crystallization and Agglomeration Kinetics of Nickel Ammonium-Sulfate in MSMPR Crystallizer. Powder Technology, 44, 13-18.
http://dx.doi.org/10.1016/0032-5910(85)85015-4 [4] Hounslow, M. (1990) Nucleation, Growth, and Aggregation Rates from Steady-State Experimental-Data. AIChE Jour- nal, 36, 1748-1752.
http://dx.doi.org/10.1002/aic.690361117 [5] Hostomsky, J. and Jones, A. (1991) Calcium-Carbonate Crystallization, Agglomeration and Form during Continuous Precipitation from Solution. Journal of Physics D—Applied Physics, 24, 165-170.
http://dx.doi.org/10.1088/0022-3727/24/2/012 [6] Rohani, S. and Chen, M. (1993) Aggregation and Precipitation Kinetics of Canola Protein by Isoelectric Precipitation. Canadian Journal of Chemical Engineering, 71, 689-698.
http://dx.doi.org/10.1002/cjce.5450710506 [7] Wojcik, J.A. and Jones, A.G. (1997) Experimental Investigation into Dynamics and Stability of Continuous MSMPR Agglomerative Precipitation of CaCO3 Crystals. Chemical Engineering Research & Design, 75, 113-118.
http://dx.doi.org/10.1205/026387697523516 [8] Li, T.S., Livk, I. and Ilievski, D. (2001) The Influence of Crystallizer Configuration on the Accuracy and Precision of Gibbsite Crystallization Kinetics Estimates. Chemical Engineering Science, 56, 2511-2519.
http://dx.doi.org/10.1016/S0009-2509(00)00451-6 [9] Georgieva, P., Meireles, M.J. and de Azevedo, S.F. (2003) Knowledge-Based Hybrid Modelling of a Batch Crystallization When Accounting for Nucleation, Growth and Agglomeration Phenomena. Chemical Engineering Science, 58, 3699-3713.
http://dx.doi.org/10.1016/S0009-2509(03)00260-4 [10] Zauner, R. and Jones, A.G. (2000) Determination of Nucleation, Growth, Agglomeration and Disruption Kinetics from Experimental Precipitation Data: The Calcium Oxalate System. Chemical Engineering Science, 55, 4219-4232.
http://dx.doi.org/10.1016/S0009-2509(00)00059-2 [11] Lallemand, S., Bertrand, M. and Plasari, E. (2012) Physical Simulation of Precipitation of Radioactive Element Oxalates by Using the Harmless Neodymium Oxalate for Studying the Agglomeration Phenomena. Journal of Crystal Growth, 342, 42-49.
http://dx.doi.org/10.1016/j.jcrysgro.2011.01.079 [12] Ilievski, D. and Livk, I. (2006) An Agglomeration Efficiency Model for Gibbsite Precipitation in a Turbulently Stirred Vessel. Chemical Engineering Science, 61, 2010-2022.
http://dx.doi.org/10.1016/j.ces.2005.10.051 [13] Lindenberg, C., Scholl, J., Vicum, L., Mazotti, M. and Brozio, J. (2008) L-Glutamic Acid Precipitation: Agglomeration Effects. Crystal Growth and Design, 8, 224-237.
http://dx.doi.org/10.1021/cg070161f [14] Hounslow, M.J., Ryall, R.L. and Marshall, V.R. (1988) A Discretized Population Balance for Nucleation, Growth, and Aggregation. AIChE Journal, 34, 1821-1832.
http://dx.doi.org/10.1002/aic.690341108 [15] Ilievski, D. and White, E. (1994) Agglomeration during Precipitation: Agglomeration Mechanism Identification for Al(OH)3 Crystals in Stirred Caustic Aluminate Solutions. Chemical Engineering Science, 49, 3227-3239.
http://dx.doi.org/10.1016/0009-2509(94)E0060-4 [16] Bramley, A.S., Hounslow, M.J. and Ryall, R.L. (1996) Aggregation during Precipitation from Solution: A Method for Extracting Rates from Experimental Data. Journal of Colloid and Interface Science, 183, 155-165.
http://dx.doi.org/10.1006/jcis.1996.0530 [17] Collier, A.P. and Hounslow, M.J. (1999) Growth and Aggregation Rates for Calcite and Calcium Oxalate Monohydrate. AIChE Journal, 45, 2298-2305.
http://dx.doi.org/10.1002/aic.690451105 [18] Tourbin, M. and Frances, C. (2008) Experimental Characterization and Population Balance Modelling of the Dense Silica Suspensions Aggregation Process. Chemical Engineering Science, 63, 5239-5251.
http://dx.doi.org/10.1016/j.ces.2008.06.028 [19] Lemanowicz, M., Al-Rashed, M.H., Gierczycki, A.T. and Kocurek, J. (2009) Application of the QMOM in Research on the Behavior of Solid-Liquid Suspensions. Chemical and Biochemical Engineering Quarterly, 23, 143-151. [20] Smoluchowski, M. (1917) Mathematical Theory of the Kinetics of the Coagulation of Colloidal Solutions. Zeitschrift für Physikalische Chemie, 19, 129-135. [21] Mumtaz, H.S., Hounslow, M.J., Seaton, N.A. and Paterson, W.R. (1997) Orthokinetic Aggregation during Precipitation. A Computational Model for Calcium Oxalate Monohydrate. Chemical Engineering Research and Design, 75, 152-159. [22] Hounslow, M., Mumtaz, H., Collier, A., Barrick, J. and Bramley, A. (2001) A Micro-Mechanical Model for the Rate of Aggregation during Precipitation from Solution. Chemical Engineering Science, 56, 2543-2552.
http://dx.doi.org/10.1016/S0009-2509(00)00436-X [23] Hollander, E.D., Derksen, J.J., Bruinsma, O.S.L., van den Akker, H.E.A. and van Rosmalen, G.M. (2001) A Numerical Study on the Coupling of Hydrodynamics and Orthokinetic Agglomeration. Chemical Engineering Science, 56, 2531- 2541.
http://dx.doi.org/10.1016/S0009-2509(00)00435-8 [24] Livk, I. and Ilievski, D. (2007) A Macroscopic Agglomeration Kernel Model for Gibbsite Precipitation in Turbulent and Laminar Flows. Chemical Engineering Science, 62, 3787-3797.
http://dx.doi.org/10.1016/j.ces.2007.03.030 [25] Schaer, E., Ravetti, R. and Plasari, E. (2001) Study of Silica Particles Aggregation in a Batch Agitated Vessel. Chemical Engineering and Processing, 40, 277-293.
http://dx.doi.org/10.1016/s0255-2701(00)00124-0 [26] Salvatori, F., Muhr, H. and Plasari, E. (2005) A New Solution for Closure Problem in Crystallization Modeling Using Moments Method. Powder Technology, 157, 27-32.
http://dx.doi.org/10.1016/j.powtec.2005.05.008
[1] Schnebelen, M., Ricaud, M., Jakob, A., Sy, D., Plasari, E. and Muhr, H. (2015) Determination of Crystallization Kinetics and Size Distribution Parameters of Agglomerated Calcium Carbonate Nanoparticles during the Carbonation of a Suspension of Lime. Crystal Structure Theory and Applications, 4, 16-27. [2] Liao, P. and Hulburt, H. (1976) Agglomeration Process in Suspension Crystallization. Proceedings of 69th Annual Meeting American Institute of Chemical Engineers. [3] Tavare, N., Shah, M. and Garside, J. (1985) Crystallization and Agglomeration Kinetics of Nickel Ammonium-Sulfate in MSMPR Crystallizer. Powder Technology, 44, 13-18.
http://dx.doi.org/10.1016/0032-5910(85)85015-4 [4] Hounslow, M. (1990) Nucleation, Growth, and Aggregation Rates from Steady-State Experimental-Data. AIChE Jour- nal, 36, 1748-1752.
http://dx.doi.org/10.1002/aic.690361117 [5] Hostomsky, J. and Jones, A. (1991) Calcium-Carbonate Crystallization, Agglomeration and Form during Continuous Precipitation from Solution. Journal of Physics D—Applied Physics, 24, 165-170.
http://dx.doi.org/10.1088/0022-3727/24/2/012 [6] Rohani, S. and Chen, M. (1993) Aggregation and Precipitation Kinetics of Canola Protein by Isoelectric Precipitation. Canadian Journal of Chemical Engineering, 71, 689-698.
http://dx.doi.org/10.1002/cjce.5450710506 [7] Wojcik, J.A. and Jones, A.G. (1997) Experimental Investigation into Dynamics and Stability of Continuous MSMPR Agglomerative Precipitation of CaCO3 Crystals. Chemical Engineering Research & Design, 75, 113-118.
http://dx.doi.org/10.1205/026387697523516 [8] Li, T.S., Livk, I. and Ilievski, D. (2001) The Influence of Crystallizer Configuration on the Accuracy and Precision of Gibbsite Crystallization Kinetics Estimates. Chemical Engineering Science, 56, 2511-2519.
http://dx.doi.org/10.1016/S0009-2509(00)00451-6 [9] Georgieva, P., Meireles, M.J. and de Azevedo, S.F. (2003) Knowledge-Based Hybrid Modelling of a Batch Crystallization When Accounting for Nucleation, Growth and Agglomeration Phenomena. Chemical Engineering Science, 58, 3699-3713.
http://dx.doi.org/10.1016/S0009-2509(03)00260-4 [10] Zauner, R. and Jones, A.G. (2000) Determination of Nucleation, Growth, Agglomeration and Disruption Kinetics from Experimental Precipitation Data: The Calcium Oxalate System. Chemical Engineering Science, 55, 4219-4232.
http://dx.doi.org/10.1016/S0009-2509(00)00059-2 [11] Lallemand, S., Bertrand, M. and Plasari, E. (2012) Physical Simulation of Precipitation of Radioactive Element Oxalates by Using the Harmless Neodymium Oxalate for Studying the Agglomeration Phenomena. Journal of Crystal Growth, 342, 42-49.
http://dx.doi.org/10.1016/j.jcrysgro.2011.01.079 [12] Ilievski, D. and Livk, I. (2006) An Agglomeration Efficiency Model for Gibbsite Precipitation in a Turbulently Stirred Vessel. Chemical Engineering Science, 61, 2010-2022.
http://dx.doi.org/10.1016/j.ces.2005.10.051 [13] Lindenberg, C., Scholl, J., Vicum, L., Mazotti, M. and Brozio, J. (2008) L-Glutamic Acid Precipitation: Agglomeration Effects. Crystal Growth and Design, 8, 224-237.
http://dx.doi.org/10.1021/cg070161f [14] Hounslow, M.J., Ryall, R.L. and Marshall, V.R. (1988) A Discretized Population Balance for Nucleation, Growth, and Aggregation. AIChE Journal, 34, 1821-1832.
http://dx.doi.org/10.1002/aic.690341108 [15] Ilievski, D. and White, E. (1994) Agglomeration during Precipitation: Agglomeration Mechanism Identification for Al(OH)3 Crystals in Stirred Caustic Aluminate Solutions. Chemical Engineering Science, 49, 3227-3239.
http://dx.doi.org/10.1016/0009-2509(94)E0060-4 [16] Bramley, A.S., Hounslow, M.J. and Ryall, R.L. (1996) Aggregation during Precipitation from Solution: A Method for Extracting Rates from Experimental Data. Journal of Colloid and Interface Science, 183, 155-165.
http://dx.doi.org/10.1006/jcis.1996.0530 [17] Collier, A.P. and Hounslow, M.J. (1999) Growth and Aggregation Rates for Calcite and Calcium Oxalate Monohydrate. AIChE Journal, 45, 2298-2305.
http://dx.doi.org/10.1002/aic.690451105 [18] Tourbin, M. and Frances, C. (2008) Experimental Characterization and Population Balance Modelling of the Dense Silica Suspensions Aggregation Process. Chemical Engineering Science, 63, 5239-5251.
http://dx.doi.org/10.1016/j.ces.2008.06.028 [19] Lemanowicz, M., Al-Rashed, M.H., Gierczycki, A.T. and Kocurek, J. (2009) Application of the QMOM in Research on the Behavior of Solid-Liquid Suspensions. Chemical and Biochemical Engineering Quarterly, 23, 143-151. [20] Smoluchowski, M. (1917) Mathematical Theory of the Kinetics of the Coagulation of Colloidal Solutions. Zeitschrift für Physikalische Chemie, 19, 129-135. [21] Mumtaz, H.S., Hounslow, M.J., Seaton, N.A. and Paterson, W.R. (1997) Orthokinetic Aggregation during Precipitation. A Computational Model for Calcium Oxalate Monohydrate. Chemical Engineering Research and Design, 75, 152-159. [22] Hounslow, M., Mumtaz, H., Collier, A., Barrick, J. and Bramley, A. (2001) A Micro-Mechanical Model for the Rate of Aggregation during Precipitation from Solution. Chemical Engineering Science, 56, 2543-2552.
http://dx.doi.org/10.1016/S0009-2509(00)00436-X [23] Hollander, E.D., Derksen, J.J., Bruinsma, O.S.L., van den Akker, H.E.A. and van Rosmalen, G.M. (2001) A Numerical Study on the Coupling of Hydrodynamics and Orthokinetic Agglomeration. Chemical Engineering Science, 56, 2531- 2541.
http://dx.doi.org/10.1016/S0009-2509(00)00435-8 [24] Livk, I. and Ilievski, D. (2007) A Macroscopic Agglomeration Kernel Model for Gibbsite Precipitation in Turbulent and Laminar Flows. Chemical Engineering Science, 62, 3787-3797.
http://dx.doi.org/10.1016/j.ces.2007.03.030 [25] Schaer, E., Ravetti, R. and Plasari, E. (2001) Study of Silica Particles Aggregation in a Batch Agitated Vessel. Chemical Engineering and Processing, 40, 277-293.
http://dx.doi.org/10.1016/s0255-2701(00)00124-0 [26] Salvatori, F., Muhr, H. and Plasari, E. (2005) A New Solution for Closure Problem in Crystallization Modeling Using Moments Method. Powder Technology, 157, 27-32.
http://dx.doi.org/10.1016/j.powtec.2005.05.008