Utilizat ion of the cem en t indu stry CO 2 in the p rod uction of calcium carbonate nan op articles throu gh p recipitation p rocess intensifj cation on a packed bed reactor F . Liendo, F .A. Deorsola, S. Bensaid, G. Saracco Department of Applied Science and T echnology, Politecnico di T orino, T orino, Italy Heraklion, Greece, 28 th June 2019
ReCode: Concept overview 2 • Recycling Carbon dioxide in the cement industry to produce added-value additives • Development of a demo plant to showcase CO 2 circular economy • 13 European partners www.recodeh2020.eu Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Introduction 3 ⎼ Aim of the work: recovery of CO 2 from cement fmue gases through carbonation route for obtaining Calcium Carbonate Nanoparticles (CCNPs) ⎼ Optimization of intensifjed process for enhanced CO 2 conversion CaCO 3 and CCNP features particles Non toxicity T unable size and PROPERTIES Porosity Biocompatibili morphology ty Material Food APPLICATIONS Biomedical s fjller industry Boyjoo, Yash and K. Pareek, Vishnu and Liu, Jian, 2014. Synthesis of micro and nano-sized calcium carbonate particles and their applications J. Mater. Chem. A Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
CaCO 3 formation 4 Precipitation method Classical CaCO 3 precipitation mechanism Polymorphic abundance (%) Change in Polymorphic abundance 100% 80% Pre nucleation Nucleation Post Nucleation 60% • Calcium and • Homogeneou • Growth carbonate s nucleation 40% ions in • Heterogeneo • Aggregation 20% solution us nucleation and • Metastabile agglomeratio • Clusters of 0% ACC Vaterite clusters n critical size Time (min) Calcite • Particle size Pure & Appl. Chem., Vol. 69, No. 5, pp 921-928, 1997. Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Main synthesis methods 5 CaCO 3 synthesis Other Biomimetic CO 2 bubbling synthesis synthesis methods Microwave Precipitation Reverse No additives and method emulsion ultrasound Atomized (a) the spontaneous precipitation method, With No additives microemulsi (b) the slow carbonation method, (c) the additives on reverse (W/O) emulsion method and (d) the CO2 bubbling method. The biomimetic method is represented by (a), (b) and (c). With Spray drying additives Boyjoo, Yash and K. Pareek, Vishnu and Liu, Jian, 2014. Synthesis of micro and nano-sized calcium carbonate particles and their applications J. Mater. Chem. A Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Experimental procedure 6 CaCO 3 Particles CaCO 3 characterizati particles Drying on separation precipitation by overnight • Particle size • Vacuum carbonation at 90 °C distribution Filtration with process • Polymorphism Membrane Filter (Pore • Morphology diameter 0.45 µm) Solution Equilibria Byprodu ct of Byprodu other ct of processe other processe s s Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Bubbling reactor experimental 7 setup Bubbling reactor parameters Length [mm] 200 Bubbling Diameter [mm] 100 Reactor (BR) Sparger level 30 [mm] Stirrer length 30 [mm] Both experimental setup were tested varying the operating conditions, such as fmowrates and initial concentrations, in order to obtain as small as possible particles. Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Packed bed reactor experimental setup 8 Packed bed reactor parameters Length [mm] 370 Crystallization Inner Diameter 10 Zone [mm] Stabilization Zone Packing Surface 2500 Area [m 2 /m 3 ] ε [m 3 /m 3 ] 0.62 Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
CaCO 3 particles 9 characterization + isopropanol Particle size distribution Ultrasound bath analysis (15 min) Malvern zetasizer Zeiss Merlin FE-SEM for morphologic analysis Xpert PRO (PANalytical) for XRD analysis Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Bubbling reactor performance 10 Optimal operating conditions (BR) Gas fmowrate (mL/min) 250 Liquid fmowrate (mL/min) -- Initial CaO concentration 0.015 (mol/L) Initial pH 12.45 Synthesis time (min) 1.5 200 nm 200 nm Calcium conversion 83% CO 2 conversion 40% Absorption rate Precipitation rate Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Process intensifjcation 11 CO 2 • Maximize the efgectiveness of intra- and intermolecular events • Give each molecule the same processing experience which results in products with uniform Magnetic stirrer properties Mass transfer • Optimize the driving forces at every scale and maximize the Intensified precipitation specifjc surface area process Precipitation • Maximize the synergetic efgects kinetics from partial processes which Tian Y, Demirel SE, Hasan MMF, Pistikopoulos EN, Chemical Engineering and Processing - Process Intensifjcation enable multitasking (2018) Bao-Chang Sun, Xue-Mei Wang, Jian-Ming Chen, Guang-Wen Chu, Jian-Feng Chen, Lei Shao 2011, Chemical Utilization of the cement industry CO 2 in the production of Engineering Journal, p. 731–736. calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Packed bed reactor 12 performance Optimal operating conditions (BR) Gas fmowrate (mL/min) 571 Liquid fmowrate (mL/min) 108 Initial CaO concentration 0.015 (mol/L) Initial pH 12.45 Synthesis time (min) 2 Calcium conversion 95% CO 2 conversion 21% Absorption rate Precipitation rate Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Reactors comparison 13 200 nm Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
Conclusions 14 ⎼ CO 2 was successfully recovered into Calcium Carbonate Nanoparticles by a carbonation route ⎼ The process was intensifjed by employing a Packed Bed Reactor ⎼ The intensifjcation allowed to ⎼ maximize the efgectiveness of intra- and intermolecular events ⎼ give each molecule the same processing experience ⎼ optimize the driving forces at every scale ⎼ By this way, growth and agglomeration were controlled and nanosized calcite CaCO 3 particles with narrow PSD were produced, with increased calcium and CO 2 conversion Utilization of the cement industry CO 2 in the production of calcium carbonate nanoparticles through precipitation process intensifjcation on a packed bed reactor
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