Accelerated carbonation of ceramic materials. Application to bricks from Andalusian factories (Spain)

Depósito de investigación de la Universidad de Sevilla https://idus.us.es/ “This is an Accepted Manuscript of an article published by Elsevier in: CONSTRUCTION AND BUILDING MATERIALS on 2018, available at: https://doi.org/10.1016/j.conbuildmat.2018.05.285” 1 ACCELERATED CARBONATION OF 1 CERAMIC MATERIALS. APPLICATION TO 2 BRICKS FROM ANDALUSIAN FACTORIES 3 (SPAIN) 4 Domingo Martín*, Patricia Aparicio, Emilio Galán 5 Dpto. Cristalografía, Mineralogía y Química Agrícola, Facultad de Química, Universidad 6 de Sevilla, C/ Profesor García González, 1, Sevilla 41012, Spain. 7 8 KEYWORDS: Carbon capture, mineral carbonation, ceramic wastes. 9 10 ABSTRACT 11 This research explores the possibility of CO2 sequestration in ceramic building materials, 12 namely bricks. The bricks used are rich in calcium and magnesium. The reaction with 13 CO2 was carried out in sealed reactor with a 0.3 L volume in a CO2 atmosphere at 14 pressures of 10 bars. The solid-water ratio was 4:1, and the reaction time ranged from 24 15 hours to 30 days. The results show that the carbonation was proportional to the reaction 16 time. Those results open new future possibilities using brick waste to the capture of CO2 17 in ambient temperature and low pressure. 18 2 1. Introduction 19 The increase in average global temperatures since the mid-20th century may be ascribed 20 to the increased emission of anthropogenic greenhouse gases [1]. Generally, human 21 activities result in emissions of four long-lived greenhouse gases (GHGs): CO2, CH4, NO 22 and halocarbons. Of these, CO2 is the most important anthropogenic GHG, because it 23 has increased approximately 40% from the preindustrial era, as a consequence of fossil 24 fuel consumption and changes in soil use [2]. To avoid the potentially devastating 25 consequences of global warming and climate change, anthropogenic CO2 emissions into 26 the atmosphere should be reduced considerably. However, achieving such reductions 27 through reducing energy intensity or switching to less carbon intensive fuels, with parallel 28 increases in the use of renewable energies, seems to be unrealistic. Therefore, 29 technological proposals have been put forward for reducing emissions into the 30 atmosphere by means of carbon dioxide capture and storage (CCS). This strategy 31 involves the development of innovative, available and cost-effective technologies. 32 Storage of CO2 may be carried out through a number of mechanisms, including mineral 33 carbonation, oceanic storage, underground injection for enhanced fossil fuel recovery, 34 and injection into saline aquifers [1,3–10]. 35 Carbon dioxide sequestration by mineral carbonation mimics naturally occurring rock 36 weathering. In this natural process, CO2 and water play an important role in dissolving 37 unstable rock-forming minerals (i.e., K-feldspar, plagioclases, olivine, pyroxenes, and 38 others, depending on the rock composition), releasing alkali and alkaline-earths cations 39 and forming mostly phyllosilicates. 40 3 The mineral carbonation process as an alternative for CO2 reduction was originally 41 proposed by Seifritz [11]. The main advantage of this process is that the formed minerals 42 are similar to end products of geologic processes and are known to be stable over 43 geological time periods (millions of years). In addition, the reaction products can be 44 environmentally accepted. 45 The capture of CO2 follows the reaction: 46 MO+ CO2 ↔ MCO3 + heat 47 where M is a metallic element such as calcium, magnesium or iron. 48 There are many suitable magnesium or calcium silicates such as enstatite, anorthite, 49 diopside, talc, which are potential sources for both CaO and MgO. However, not all of 50 these silicates are abundant in the Earth’s surface, and direct carbonation is not easy 51 under low-pressure and low-temperature conditions. Experiments using reactors for the 52 carbonation of magnesium silicates (wollastonite and serpentine), via magnesium oxide 53 or magnesium hydroxide intermediates, have been carried out at temperatures and 54 pressures up to 600°C and 100 bars (allowing for both sub- and supercritical conditions 55 for CO2) [12–14], or under hydrothermal conditions, in the case of anorthite [15] and 56 several Ca and Mg-rich minerals [16,17]. However, these conditions are not very cost- 57 effective. 58 According to Fauth et al. [18], Lackner et al. [19] and Zevenhoven et al. [20], 59 mineralization of CO2 has benefits, especially at locations where the risk of leakage is 60 considered unacceptable or where underground storage sites are not available while vast 61 resources of suitable magnesium silicates exist. Wollastonite is a rare mineral, and when 62 4 a wollastonite deposit exists, mining is preferable because it is a very important and 63 expensive industrial mineral. Serpentine is more widely distributed, but the main 64 serpentinized massifs are located in only some countries. Diopside, anorthite and other 65 Mg/Ca pyroxenes and amphiboles are rock-forming minerals, but they do not occur as 66 mineral deposits. 67 Other sources of Mg and Ca have been explored for potential carbonation, including Mg- 68 or Ca-containing mine tailings and by-products or wastes from industry. This has included 69 investigation of the carbonation of fly-ash [21], steel making slag [22–25], asbestos- 70 mining tailings, electric arc furnace (EAF) dust, cement-kiln dust, waste concrete, and air 71 pollution control (APC) residues [9,26]. In addition, natural carbonation in the formation 72 of carbonated cement systems has been well-known for many years. Alkaline earth 73 hydroxide cements and mortars harden slowly due to their reaction with atmospheric CO2. 74 Other well-known carbonation processes occur in ceramic building materials. These 75 ceramics are rich in Ca/Mg silicates formed at high temperature during heating, in contact 76 with atmospheric CO2 and humidity such minerals can be carbonated [27]. Moreover, in 77 many low-quality bricks the presence of CaO is common, and carbonation is very quick. 78 Fabbri et al. [27] present a review of the presence of calcite on ceramic materials, 79 indicating that the calcite can be of primary or secondary origin. Primary calcite includes 80 the forms of calcite that are preserved without change during the ceramic firing. 81 Secondary calcite (anthropogenic calcite) includes all the forms of calcite that crystallize 82 in the ceramics after firing, irrespective of the time, the cause, and the grain size. 83 5 Taking into account the easy carbonation of ceramic building materials, this research 84 aims to carbonate bricks in the laboratory, in order to develop a procedure that could be 85 industrially profitable. The main carbonation mechanisms were studied in the presence 86 of water to simulate an accelerated carbonation process. 87 88 2. Materials and Methods 89 Three bricks from different Andalusian (South Spain) brickworks were chosen for 90 carbonation tests. The brick MPC2 was a clinker brick made in Bailen (Jaén), fired at 91 1050°C. The brick AUC1 was a perforated brick made in La Puebla de Cazalla (Sevilla), 92 heated at 900°C and the brick MSC1 was a hollow ceramic block from Jun (Granada), 93 heated at approximately 800°C. The bricks were ground in a jaw crusher and sieved in 94 laboratory. 95 The carbonation tests were carried out in a 0.3 L volume hermetic reactor from Parr 96 Instrument. The fixed conditions were 10 bars of CO2, 4:1 solid-water ratio and room 97 temperature. The variable conditions were the reaction time (between 24 and 720 hours) 98 and the particle size (> 4 mm, 2-4 mm, and 1-2 mm) (Table 1). These particle-size 99 fractions were selected because they are the most representative results of the crushing 100 treatment. 101 102 Table 1. Experimental parameter values during the carbonation reaction tests. 103 6 After finishing the carbonation tests, treated samples were dried at 70°C for 24 hours, 104 powdered, and sieved at 100 µm for subsequent analysis. 105 The mineralogical composition of the untreated and treated samples was identified by X- 106 ray diffraction (XRD), using a Bruker D8 Advance diffractometer with standard 107 monochromatic CuKα radiation operating at 40 kV and 30 mA. Scanning was performed 108 with a 0.015º 2θ step size at 0.1 s per step between 3-70°. Also, Rietveld refinement was 109 realized to determine the quantitative composition of untreated bricks, in this case, the 110 scanning was performed with a 0.010º 2θ step size at 0.5 s per step between 3-120° and 111 adding zincite as internal standard. 112 The major elemental composition expressed in oxides was performed by X-ray 113 fluorescence (XRF) with an automated Panalytical Axios model spectrometer. The 114 samples were prepared for analysis as glass discs. 115 The carbonated content of the raw and carbonated samples was determined by two 116 different analytical methods: thermal decomposition (DTA-TG) and elemental analysis. 117 DTA-TG analyses were performed in a TG Netzsch STA 409PC. Samples (approximately 118 150 mg) were heated in an aluminium oxide crucible under a nitrogen atmosphere at 10°C 119 min-1 from room temperature to 1200°C. Weight loss was measured by TG in the range 120 of 450-900°C relative to the total carbonated decomposition. The elemental carbon 121 content was also measured using an elemental analyser, LECO CHNS 932, which 122 calculates the carbonated ratio. 123 Soluble Si, Ca and Mg ions of the original and treated samples were also determined. 124 The analysis was performed with simultaneous inductively-coupled plasma optical 125 7 spectrometry (ICP-OES) analysis using a Horiba Jobin Yvon ULTIMA 2 model instrument. 126 The samples were prepared by mixing the solid powder samples with water and stirring 127 for 24 h, afterwards isolating the liquid phase by centrifugation and filtered using a Nylon 128 0.22 µm syringe filter. 129 The specific surface area (BET) was measured with a Micromeritics Gemini 2360 130 instrument using the absorption of N2 at liquid nitrogen temperature. Prior to measuring, 131 all the samples were degassed at 80°C for 12 h and finally outgassed to 10-3 Torr. 132 Macro and micro observations were obtained by stereomicroscope using a Greenough 133 Leica S8 APO equipped with a DC300 camera, and by scanning electronic microscopy 134 (SEM) using a JEOL 6460 LV microscope and FEI Teneo, both equipped with energy 135 dispersive spectrometers (Oxford Instruments INCA and EDAX, respectively). The 136 samples were prepared with Au-sputter coating for improve the imagining of the samples. 137 Topography measurements were carried out using a non-contact 3D optical profiler 138 Sensofar S-Neox. 139 140 3. Results and Discussion 141 Calcium oxide in the bricks ranges from 15-24 wt%, and magnesium oxide ranges from 142 2-4 wt% (Table 2). Such high Ca-materials seem to be appropriate for mineral 143 carbonation. 144 Table 2. Major oxide composition (wt%) by XRF of selected bricks. 145 146 8 The bricks are composed of quartz and cristobalite (SiO2), diopside (CaMgSi2O6) and 147 minor orthoclase (KAlSi3O8). Other silicates were also detected, such as wollastonite 148 (CaSiO3) in MPC2 and AUC1, anorthite (CaAl2Si2O8) in MPC2, and gehlenite 149 (Ca2Al(AlSi)O7) in MSC1 (Table 3). Anhydrite (CaSO4) was also identified in AUC1 and 150 MSC1; in the latter sample, mica, and traces of calcite and hematite were also found. This 151 mineralogy is consistent with the chemical analysis and the heating temperature of these 152 ceramic materials. 153 Table 3. Mineralogical composition (wt%) of selected bricks. 154 Legend [28]: Qtz: quartz; Anh: anhydrite; Wo: wollastonite; Crs: cristobalite; Or: 155 orthoclase; Ab: albite; Di: diopside; An: anorthite; Gh: gehlenite; Mca: mica; Cal: calcite; 156 Hem: hematite; Amorph: amorphous phase. 157 158 On the other hand, minor free Ca ions are available (100-800 mg/l) to precipitate as 159 carbonates during the reaction with carbonic acid that is produced by the combination of 160 CO2 gas and humidity. 161 The bricks were ground in a jaw crusher and sieved in laboratory, obtaining the following 162 a particle size distribution The fractions > 4 mm, 2 - 4 mm and 1 - 2 mm represent more 163 than 80% of the samples (Table 4). Therefore, those fractions were selected for 164 carbonated tests. 165 Table 4. Granulometric fractions of the crushed samples (wt%). 166 167 15 AUC1>MPC2>MSC1. These results agree reasonably with the experimental carbonation 290 data. 291 292 Table 5. Carbonation Efficiency (C.E.) according to Steinour’s equation and corrected. 293 294 According to the XRD data, wollastonite and/or anhydrite still remain in the treated 295 material, which could contribute to an increase in the carbonation efficiency. 296 Nevertheless, several factors could prevent CO2 diffusion into the bulk of the sample 297 particles, such as the presence of “vitreous” sheets, the filling of the pores with carbonate 298 crystals, or a decrease in the CO2 pressure and/or moisture necessary for the acidic 299 attack. 300 301 4. Conclusions 302 The present study shows the possibility of using ceramic construction wastes for 303 carbonation under surface conditions in a short period of time. Specifically, in this study 304 Ca-rich bricks were successful used as a raw material for direct mineral carbonation. In 305 addition to the destruction of Ca-silicates, anhydrites, which is occasionally present, may 306 also be attacked, and the Ca may be removed for a subsequent precipitation of 307 carbonates. 308 16 The amount of carbonation is proportional to the time of reaction (the longer the time, the 309 higher the capture efficiency), whereas it does not seem to significantly depend on the 310 particle size in the conditions studied. 311 Precipitated calcite layers were observed on the brick surface and new crystal growths 312 were formed in the pores of the ceramic pieces. In addition, some physical adsorption 313 was also observed. 314 An acceptable carbonation and/or CO2 capture levels have been achieved under 315 favourable conditions of low pressure and temperature, with low energy costs and 316 therefore environmental protection. 317 These results open the possibility for future studies on using exhausted quarries filled 318 with brick wastes, which could be directly carbonated by injecting CO2 “in situ”. 319 320 321 AUTHOR INFORMATION 322 Corresponding Author 323 Domingo Martín, dm[email protected], ORCID Id: orcid.org/0000-0003-3725-6598 324 Authors 325 Domingo Martín, dm[email protected], ORCID Id: orcid.org/0000-0003-3725-6598 326 Patricia Aparicio, [email protected], ORCID Id: orcid.org/0000-0001-5307-1433 327 Emilio Galán, [email protected], ORCID Id: orcid.org/0000-0002-8466-5047 328 329 330 17 Present Addresses 331 Departamento Cristalografía, Mineralogía y Química Agrícola, Facultad de Química, 332 Universidad de Sevilla, Calle Profesor García González, 1, Sevilla 41012, Spain 333 Author Contributions 334 The manuscript was written through contributions of all authors. All authors have given 335 approval to the final version of the manuscript. All authors contributed equally. 336 Funding Sources 337 This research was funded by the Junta de Andalucía (Consejería de Economía y 338 Conocimiento) (P12-RNM-568 MO project). 339 340 Acknowledgment 341 This research was funded by the Junta de Andalucía (Consejería de Economía y 342 Conocimiento) (P12-RNM-568 MO project) and the contract of Domingo Martín granted 343 by the V Plan Propio de Investigación de la Universidad de Sevilla. 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Mineralogical composition (wt%) of selected bricks. 483 Table 4. Granulometric fractions of the crushed samples (wt%). 484 Table 5. Carbonation Efficiency (C.E.) according to Stenoir’s equation and corrected. 485 486 Figure 1. Mineralogical evolution of MPC2 after 720 hours of reaction, with three particle 487 sizes. a) MPC2 with significant detail, b) AUC1 with significant detail, and c) MSC1. 488 Figure 2. a) Soluble Ca, Mg, and Si ions measured in untreated and treated MPC2 after 489 240 and 720 hours of reaction; b) Soluble Ca (divided by 10), Mg, and Si ions measured 490 in untreated and treated AUC1 after 240 and 720 hours of reaction; c) Soluble Ca (/10), 491 Mg (/10), and Si ions measured in untreated and treated MSC1 after 240 and 720 hours 492 of reaction. 493