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

Depósi o de in es igación de la Uni e sidad de Se illa h ps://idus.us.es/ “This is an Accep ed Manusc ip o an a icle published by Else ie in: CONSTRUCTION AND BUILDING MATERIALS on 2018, a ailable a : h ps://doi.o g/10.1016/j.conbuildma .2018.05.285” 1 ACCELERATED CARBONATION OF 1 CERAMIC MATERIALS. APPLICATION TO 2 BRICKS FROM ANDALUSIAN FACTORIES 3 (SPAIN) 4 Domingo Ma ín*, Pa icia Apa icio, Emilio Galán 5 Dp o. C is alog a ía, Mine alogía y Química Ag ícola, Facul ad de Química, Uni e sidad 6 de Se illa, C/ P o eso Ga cía González, 1, Se illa 41012, Spain. 7 8 KEYWORDS: Ca bon cap u e, mine al ca bona ion, ce amic was es. 9 10 ABSTRACT 11 This esea ch explo es he possibili y o CO2 seques a ion in ce amic building ma e ials, 12 namely b icks. The b icks used a e ich in calcium and magnesium. The eac ion wi h 13 CO2 was ca ied ou in sealed eac o wi h a 0.3 L olume in a CO2 a mosphe e a 14 p essu es o 10 ba s. The solid-wa e a io was 4:1, and he eac ion ime anged om 24 15 hou s o 30 days. The esul s show ha he ca bona ion was p opo ional o he eac ion 16 ime. Those esul s open new u u e possibili ies using b ick was e o he cap u e o CO2 17 in ambien empe a u e and low p essu e. 18 2 1. In oduc ion 19 The inc ease in a e age global empe a u es since he mid-20 h cen u y may be asc ibed 20 o he inc eased emission o an h opogenic g eenhouse gases [1]. Gene ally, human 21 ac i i ies esul in emissions o ou long-li ed g eenhouse gases (GHGs): CO2, CH4, NO 22 and haloca bons. O hese, CO2 is he mos impo an an h opogenic GHG, because i 23 has inc eased app oxima ely 40% om he p eindus ial e a, as a consequence o ossil 24 uel consump ion and changes in soil use [2]. To a oid he po en ially de as a ing 25 consequences o global wa ming and clima e change, an h opogenic CO2 emissions in o 26 he a mosphe e should be educed conside ably. Howe e , achie ing such educ ions 27 h ough educing ene gy in ensi y o swi ching o less ca bon in ensi e uels, wi h pa allel 28 inc eases in he use o enewable ene gies, seems o be un ealis ic. The e o e, 29 echnological p oposals ha e been pu o wa d o educing emissions in o he 30 a mosphe e by means o ca bon dioxide cap u e and s o age (CCS). This s a egy 31 in ol es he de elopmen o inno a i e, a ailable and cos -e ec i e echnologies. 32 S o age o CO2 may be ca ied ou h ough a numbe o mechanisms, including mine al 33 ca bona ion, oceanic s o age, unde g ound injec ion o enhanced ossil uel eco e y, 34 and injec ion in o saline aqui e s [1,3–10]. 35 Ca bon dioxide seques a ion by mine al ca bona ion mimics na u ally occu ing ock 36 wea he ing. In his na u al p ocess, CO2 and wa e play an impo an ole in dissol ing 37 uns able ock- o ming mine als (i.e., K- eldspa , plagioclases, oli ine, py oxenes, and 38 o he s, depending on he ock composi ion), eleasing alkali and alkaline-ea hs ca ions 39 and o ming mos ly phyllosilica es. 40 3 The mine al ca bona ion p ocess as an al e na i e o CO2 educ ion was o iginally 41 p oposed by Sei i z [11]. The main ad an age o his p ocess is ha he o med mine als 42 a e simila o end p oduc s o geologic p ocesses and a e known o be s able o e 43 geological ime pe iods (millions o yea s). In addi ion, he eac ion p oduc s can be 44 en i onmen ally accep ed. 45 The cap u e o CO2 ollows he eac ion: 46 MO+ CO2 ↔ MCO3 + hea 47 whe e M is a me allic elemen such as calcium, magnesium o i on. 48 The e a e many sui able magnesium o calcium silica es such as ens a i e, ano hi e, 49 diopside, alc, which a e po en ial sou ces o bo h CaO and MgO. Howe e , no all o 50 hese silica es a e abundan in he Ea h’s su ace, and di ec ca bona ion is no easy 51 unde low-p essu e and low- empe a u e condi ions. Expe imen s using eac o s o he 52 ca bona ion o magnesium silica es (wollas oni e and se pen ine), ia magnesium oxide 53 o magnesium hyd oxide in e media es, ha e been ca ied ou a empe a u es and 54 p essu es up o 600°C and 100 ba s (allowing o bo h sub- and supe c i ical condi ions 55 o CO2) [12–14], o unde hyd o he mal condi ions, in he case o ano hi e [15] and 56 se e al Ca and Mg- ich mine als [16,17]. Howe e , hese condi ions a e no e y cos - 57 e ec i e. 58 Acco ding o Fau h e al. [18], Lackne e al. [19] and Ze enho en e al. [20], 59 mine aliza ion o CO2 has bene i s, especially a loca ions whe e he isk o leakage is 60 conside ed unaccep able o whe e unde g ound s o age si es a e no a ailable while as 61 esou ces o sui able magnesium silica es exis . Wollas oni e is a a e mine al, and when 62 4 a wollas oni e deposi exis s, mining is p e e able because i is a e y impo an and 63 expensi e indus ial mine al. Se pen ine is mo e widely dis ibu ed, bu he main 64 se pen inized massi s a e loca ed in only some coun ies. Diopside, ano hi e and o he 65 Mg/Ca py oxenes and amphiboles a e ock- o ming mine als, bu hey do no occu as 66 mine al deposi s. 67 O he sou ces o Mg and Ca ha e been explo ed o po en ial ca bona ion, including Mg- 68 o Ca-con aining mine ailings and by-p oduc s o was es om indus y. This has included 69 in es iga ion o he ca bona ion o ly-ash [21], s eel making slag [22–25], asbes os- 70 mining ailings, elec ic a c u nace (EAF) dus , cemen -kiln dus , was e conc e e, and ai 71 pollu ion con ol (APC) esidues [9,26]. In addi ion, na u al ca bona ion in he o ma ion 72 o ca bona ed cemen sys ems has been well-known o many yea s. Alkaline ea h 73 hyd oxide cemen s and mo a s ha den slowly due o hei eac ion wi h a mosphe ic CO2. 74 O he well-known ca bona ion p ocesses occu in ce amic building ma e ials. These 75 ce amics a e ich in Ca/Mg silica es o med a high empe a u e du ing hea ing, in con ac 76 wi h a mosphe ic CO2 and humidi y such mine als can be ca bona ed [27]. Mo eo e , in 77 many low-quali y b icks he p esence o CaO is common, and ca bona ion is e y quick. 78 Fabb i e al. [27] p esen a e iew o he p esence o calci e on ce amic ma e ials, 79 indica ing ha he calci e can be o p ima y o seconda y o igin. P ima y calci e includes 80 he o ms o calci e ha a e p ese ed wi hou change du ing he ce amic i ing. 81 Seconda y calci e (an h opogenic calci e) includes all he o ms o calci e ha c ys allize 82 in he ce amics a e i ing, i espec i e o he ime, he cause, and he g ain size. 83 5 Taking in o accoun he easy ca bona ion o ce amic building ma e ials, his esea ch 84 aims o ca bona e b icks in he labo a o y, in o de o de elop a p ocedu e ha could be 85 indus ially p o i able. The main ca bona ion mechanisms we e s udied in he p esence 86 o wa e o simula e an accele a ed ca bona ion p ocess. 87 88 2. Ma e ials and Me hods 89 Th ee b icks om di e en Andalusian (Sou h Spain) b ickwo ks we e chosen o 90 ca bona ion es s. The b ick MPC2 was a clinke b ick made in Bailen (Jaén), i ed a 91 1050°C. The b ick AUC1 was a pe o a ed b ick made in La Puebla de Cazalla (Se illa), 92 hea ed a 900°C and he b ick MSC1 was a hollow ce amic block om Jun (G anada), 93 hea ed a app oxima ely 800°C. The b icks we e g ound in a jaw c ushe and sie ed in 94 labo a o y. 95 The ca bona ion es s we e ca ied ou in a 0.3 L olume he me ic eac o om Pa 96 Ins umen . The ixed condi ions we e 10 ba s o CO2, 4:1 solid-wa e a io and oom 97 empe a u e. The a iable condi ions we e he eac ion ime (be ween 24 and 720 hou s) 98 and he pa icle size (> 4 mm, 2-4 mm, and 1-2 mm) (Table 1). These pa icle-size 99 ac ions we e selec ed because hey a e he mos ep esen a i e esul s o he c ushing 100 ea men . 101 102 Table 1. Expe imen al pa ame e alues du ing he ca bona ion eac ion es s. 103 6 A e inishing he ca bona ion es s, ea ed samples we e d ied a 70°C o 24 hou s, 104 powde ed, and sie ed a 100 µm o subsequen analysis. 105 The mine alogical composi ion o he un ea ed and ea ed samples was iden i ied by X- 106 ay di ac ion (XRD), using a B uke D8 Ad ance di ac ome e wi h s anda d 107 monoch oma ic CuKα adia ion ope a ing a 40 kV and 30 mA. Scanning was pe o med 108 wi h a 0.015º 2θ s ep size a 0.1 s pe s ep be ween 3-70°. Also, Rie eld e inemen was 109 ealized o de e mine he quan i a i e composi ion o un ea ed b icks, in his case, he 110 scanning was pe o med wi h a 0.010º 2θ s ep size a 0.5 s pe s ep be ween 3-120° and 111 adding zinci e as in e nal s anda d. 112 The majo elemen al composi ion exp essed in oxides was pe o med by X- ay 113 luo escence (XRF) wi h an au oma ed Panaly ical Axios model spec ome e . The 114 samples we e p epa ed o analysis as glass discs. 115 The ca bona ed con en o he aw and ca bona ed samples was de e mined by wo 116 di e en analy ical me hods: he mal decomposi ion (DTA-TG) and elemen al analysis. 117 DTA-TG analyses we e pe o med in a TG Ne zsch STA 409PC. Samples (app oxima ely 118 150 mg) we e hea ed in an aluminium oxide c ucible unde a ni ogen a mosphe e a 10°C 119 min-1 om oom empe a u e o 1200°C. Weigh loss was measu ed by TG in he ange 120 o 450-900°C ela i e o he o al ca bona ed decomposi ion. The elemen al ca bon 121 con en was also measu ed using an elemen al analyse , LECO CHNS 932, which 122 calcula es he ca bona ed a io. 123 Soluble Si, Ca and Mg ions o he o iginal and ea ed samples we e also de e mined. 124 The analysis was pe o med wi h simul aneous induc i ely-coupled plasma op ical 125 7 spec ome y (ICP-OES) analysis using a Ho iba Jobin Y on ULTIMA 2 model ins umen . 126 The samples we e p epa ed by mixing he solid powde samples wi h wa e and s i ing 127 o 24 h, a e wa ds isola ing he liquid phase by cen i uga ion and il e ed using a Nylon 128 0.22 µm sy inge il e . 129 The speci ic su ace a ea (BET) was measu ed wi h a Mic ome i ics Gemini 2360 130 ins umen using he abso p ion o N2 a liquid ni ogen empe a u e. P io o measu ing, 131 all he samples we e degassed a 80°C o 12 h and inally ou gassed o 10-3 To . 132 Mac o and mic o obse a ions we e ob ained by s e eomic oscope using a G eenough 133 Leica S8 APO equipped wi h a DC300 came a, and by scanning elec onic mic oscopy 134 (SEM) using a JEOL 6460 LV mic oscope and FEI Teneo, bo h equipped wi h ene gy 135 dispe si e spec ome e s (Ox o d Ins umen s INCA and EDAX, espec i ely). The 136 samples we e p epa ed wi h Au-spu e coa ing o imp o e he imagining o he samples. 137 Topog aphy measu emen s we e ca ied ou using a non-con ac 3D op ical p o ile 138 Senso a S-Neox. 139 140 3. Resul s and Discussion 141 Calcium oxide in he b icks anges om 15-24 w %, and magnesium oxide anges om 142 2-4 w % (Table 2). Such high Ca-ma e ials seem o be app op ia e o mine al 143 ca bona ion. 144 Table 2. Majo oxide composi ion (w %) by XRF o selec ed b icks. 145 146 8 The b icks a e composed o qua z and c is obali e (SiO2), diopside (CaMgSi2O6) and 147 mino o hoclase (KAlSi3O8). O he silica es we e also de ec ed, such as wollas oni e 148 (CaSiO3) in MPC2 and AUC1, ano hi e (CaAl2Si2O8) in MPC2, and gehleni e 149 (Ca2Al(AlSi)O7) in MSC1 (Table 3). Anhyd i e (CaSO4) was also iden i ied in AUC1 and 150 MSC1; in he la e sample, mica, and aces o calci e and hema i e we e also ound. This 151 mine alogy is consis en wi h he chemical analysis and he hea ing empe a u e o hese 152 ce amic ma e ials. 153 Table 3. Mine alogical composi ion (w %) o selec ed b icks. 154 Legend [28]: Q z: qua z; Anh: anhyd i e; Wo: wollas oni e; C s: c is obali e; O : 155 o hoclase; Ab: albi e; Di: diopside; An: ano hi e; Gh: gehleni e; Mca: mica; Cal: calci e; 156 Hem: hema i e; Amo ph: amo phous phase. 157 158 On he o he hand, mino ee Ca ions a e a ailable (100-800 mg/l) o p ecipi a e as 159 ca bona es du ing he eac ion wi h ca bonic acid ha is p oduced by he combina ion o 160 CO2 gas and humidi y. 161 The b icks we e g ound in a jaw c ushe and sie ed in labo a o y, ob aining he ollowing 162 a pa icle size dis ibu ion The ac ions > 4 mm, 2 - 4 mm and 1 - 2 mm ep esen mo e 163 han 80% o he samples (Table 4). The e o e, hose ac ions we e selec ed o 164 ca bona ed es s. 165 Table 4. G anulome ic ac ions o he c ushed samples (w %). 166 167 15 AUC1>MPC2>MSC1. These esul s ag ee easonably wi h he expe imen al ca bona ion 290 da a. 291 292 Table 5. Ca bona ion E iciency (C.E.) acco ding o S einou ’s equa ion and co ec ed. 293 294 Acco ding o he XRD da a, wollas oni e and/o anhyd i e s ill emain in he ea ed 295 ma e ial, which could con ibu e o an inc ease in he ca bona ion e iciency. 296 Ne e heless, se e al ac o s could p e en CO2 di usion in o he bulk o he sample 297 pa icles, such as he p esence o “ i eous” shee s, he illing o he po es wi h ca bona e 298 c ys als, o a dec ease in he CO2 p essu e and/o mois u e necessa y o he acidic 299 a ack. 300 301 4. Conclusions 302 The p esen s udy shows he possibili y o using ce amic cons uc ion was es o 303 ca bona ion unde su ace condi ions in a sho pe iod o ime. Speci ically, in his s udy 304 Ca- ich b icks we e success ul used as a aw ma e ial o di ec mine al ca bona ion. In 305 addi ion o he des uc ion o Ca-silica es, anhyd i es, which is occasionally p esen , may 306 also be a acked, and he Ca may be emo ed o a subsequen p ecipi a ion o 307 ca bona es. 308 16 The amoun o ca bona ion is p opo ional o he ime o eac ion ( he longe he ime, he 309 highe he cap u e e iciency), whe eas i does no seem o signi ican ly depend on he 310 pa icle size in he condi ions s udied. 311 P ecipi a ed calci e laye s we e obse ed on he b ick su ace and new c ys al g ow hs 312 we e o med in he po es o he ce amic pieces. In addi ion, some physical adso p ion 313 was also obse ed. 314 An accep able ca bona ion and/o CO2 cap u e le els ha e been achie ed unde 315 a ou able condi ions o low p essu e and empe a u e, wi h low ene gy cos s and 316 he e o e en i onmen al p o ec ion. 317 These esul s open he possibili y o u u e s udies on using exhaus ed qua ies illed 318 wi h b ick was es, which could be di ec ly ca bona ed by injec ing CO2 “in si u”. 319 320 321 AUTHOR INFORMATION 322 Co esponding Au ho 323 Domingo Ma ín, dm[email p o ec ed], ORCID Id: o cid.o g/0000-0003-3725-6598 324 Au ho s 325 Domingo Ma ín, dm[email p o ec ed], ORCID Id: o cid.o g/0000-0003-3725-6598 326 Pa icia Apa icio, papa [email protected], ORCID Id: o cid.o g/0000-0001-5307-1433 327 Emilio Galán, [email p o ec ed], ORCID Id: o cid.o g/0000-0002-8466-5047 328 329 330 17 P esen Add esses 331 Depa amen o C is alog a ía, Mine alogía y Química Ag ícola, Facul ad de Química, 332 Uni e sidad de Se illa, Calle P o eso Ga cía González, 1, Se illa 41012, Spain 333 Au ho Con ibu ions 334 The manusc ip was w i en h ough con ibu ions o all au ho s. All au ho s ha e gi en 335 app o al o he inal e sion o he manusc ip . All au ho s con ibu ed equally. 336 Funding Sou ces 337 This esea ch was unded by he Jun a de Andalucía (Conseje ía de Economía y 338 Conocimien o) (P12-RNM-568 MO p ojec ). 339 340 Acknowledgmen 341 This esea ch was unded by he Jun a de Andalucía (Conseje ía de Economía y 342 Conocimien o) (P12-RNM-568 MO p ojec ) and he con ac o Domingo Ma ín g an ed 343 by he V Plan P opio de In es igación de la Uni e sidad de Se illa. XRD, XRF, ICP-OES, 344 C-elemen al and SEM analysis we e pe o med using he acili ies o he Gene al 345 Resea ch Cen e a he Uni e si y o Se ille (CITIUS). 346 347 ABBREVIATIONS 348 APC, ai pollu ion con ol; BET, B unaue , Emme and Telle speci ic su ace; C.E., 349 ca bona ion e iciency; CCS, ca bon cap u e and s o age; DTA-TG, simul aneous 350 he mog a ime ic and di e en ial he mal analysis; E.C., expe imen al cap u e; EAF, 351 18 elec ic a c u nace; GHG, g eenhouse gases; ICP-OES, induc i ely coupled plasma 352 op ical emission spec ome y; LOI, loss on igni ion pe o med; SEM, scanning elec on 353 mic oscope; T.C., heo e ical cap u e; XRD, X- ay di ac ion; XRF, X- ay luo escence. 354 355 Re e ences 356 [1] IPCC, B. Me z, O. Da idson, H. De Coninck, M. Loos, L. Meye , IPCC, IPCC special 357 epo on ca bon dioxide cap u e and s o age, In e go e nmen al Panel on Clima e 358 Change, Gene a (Swi ze land). Wo king G oup III, 2005. 359 [2] IPCC, 2013: Summa y o Policymake s., in: Clim. 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Mine alogical e olu ion o MPC2 a e 720 hou s o eac ion, wi h h ee pa icle 487 sizes. a) MPC2 wi h signi ican de ail, b) AUC1 wi h signi ican de ail, and c) MSC1. 488 Figu e 2. a) Soluble Ca, Mg, and Si ions measu ed in un ea ed and ea ed MPC2 a e 489 240 and 720 hou s o eac ion; b) Soluble Ca (di ided by 10), Mg, and Si ions measu ed 490 in un ea ed and ea ed AUC1 a e 240 and 720 hou s o eac ion; c) Soluble Ca (/10), 491 Mg (/10), and Si ions measu ed in un ea ed and ea ed MSC1 a e 240 and 720 hou s 492 o eac ion. 493