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”
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ACCELERATED CARBONATION OF
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CERAMIC MATERIALS. APPLICATION TO
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BRICKS FROM ANDALUSIAN FACTORIES
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(SPAIN)
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Domingo Ma ín*, Pa icia Apa icio, Emilio Galán
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Dp o. C is alog a ía, Mine alogía y Química Ag ícola, Facul ad de Química, Uni e sidad
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de Se illa, C/ P o eso Ga cía González, 1, Se illa 41012, Spain.
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KEYWORDS: Ca bon cap u e, mine al ca bona ion, ce amic was es.
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ABSTRACT
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This esea ch explo es he possibili y o CO2 seques a ion in ce amic building ma e ials,
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namely b icks. The b icks used a e ich in calcium and magnesium. The eac ion wi h
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CO2 was ca ied ou in sealed eac o wi h a 0.3 L olume in a CO2 a mosphe e a
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p essu es o 10 ba s. The solid-wa e a io was 4:1, and he eac ion ime anged om 24
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hou s o 30 days. The esul s show ha he ca bona ion was p opo ional o he eac ion
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ime. Those esul s open new u u e possibili ies using b ick was e o he cap u e o CO2
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in ambien empe a u e and low p essu e.
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1. In oduc ion
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The inc ease in a e age global empe a u es since he mid-20 h cen u y may be asc ibed
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o he inc eased emission o an h opogenic g eenhouse gases [1]. Gene ally, human
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ac i i ies esul in emissions o ou long-li ed g eenhouse gases (GHGs): CO2, CH4, NO
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and haloca bons. O hese, CO2 is he mos impo an an h opogenic GHG, because i
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has inc eased app oxima ely 40% om he p eindus ial e a, as a consequence o ossil
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uel consump ion and changes in soil use [2]. To a oid he po en ially de as a ing
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consequences o global wa ming and clima e change, an h opogenic CO2 emissions in o
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he a mosphe e should be educed conside ably. Howe e , achie ing such educ ions
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h ough educing ene gy in ensi y o swi ching o less ca bon in ensi e uels, wi h pa allel
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inc eases in he use o enewable ene gies, seems o be un ealis ic. The e o e,
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echnological p oposals ha e been pu o wa d o educing emissions in o he
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a mosphe e by means o ca bon dioxide cap u e and s o age (CCS). This s a egy
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in ol es he de elopmen o inno a i e, a ailable and cos -e ec i e echnologies.
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S o age o CO2 may be ca ied ou h ough a numbe o mechanisms, including mine al
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ca bona ion, oceanic s o age, unde g ound injec ion o enhanced ossil uel eco e y,
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and injec ion in o saline aqui e s [1,3–10].
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Ca bon dioxide seques a ion by mine al ca bona ion mimics na u ally occu ing ock
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wea he ing. In his na u al p ocess, CO2 and wa e play an impo an ole in dissol ing
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uns able ock- o ming mine als (i.e., K- eldspa , plagioclases, oli ine, py oxenes, and
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o he s, depending on he ock composi ion), eleasing alkali and alkaline-ea hs ca ions
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and o ming mos ly phyllosilica es.
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The mine al ca bona ion p ocess as an al e na i e o CO2 educ ion was o iginally
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p oposed by Sei i z [11]. The main ad an age o his p ocess is ha he o med mine als
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a e simila o end p oduc s o geologic p ocesses and a e known o be s able o e
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geological ime pe iods (millions o yea s). In addi ion, he eac ion p oduc s can be
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en i onmen ally accep ed.
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The cap u e o CO2 ollows he eac ion:
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MO+ CO2 ↔ MCO3 + hea
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whe e M is a me allic elemen such as calcium, magnesium o i on.
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The e a e many sui able magnesium o calcium silica es such as ens a i e, ano hi e,
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diopside, alc, which a e po en ial sou ces o bo h CaO and MgO. Howe e , no all o
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hese silica es a e abundan in he Ea h’s su ace, and di ec ca bona ion is no easy
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unde low-p essu e and low- empe a u e condi ions. Expe imen s using eac o s o he
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ca bona ion o magnesium silica es (wollas oni e and se pen ine), ia magnesium oxide
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o magnesium hyd oxide in e media es, ha e been ca ied ou a empe a u es and
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p essu es up o 600°C and 100 ba s (allowing o bo h sub- and supe c i ical condi ions
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o CO2) [12–14], o unde hyd o he mal condi ions, in he case o ano hi e [15] and
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se e al Ca and Mg- ich mine als [16,17]. Howe e , hese condi ions a e no e y cos -
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e ec i e.
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Acco ding o Fau h e al. [18], Lackne e al. [19] and Ze enho en e al. [20],
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mine aliza ion o CO2 has bene i s, especially a loca ions whe e he isk o leakage is
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conside ed unaccep able o whe e unde g ound s o age si es a e no a ailable while as
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esou ces o sui able magnesium silica es exis . Wollas oni e is a a e mine al, and when
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a wollas oni e deposi exis s, mining is p e e able because i is a e y impo an and
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expensi e indus ial mine al. Se pen ine is mo e widely dis ibu ed, bu he main
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se pen inized massi s a e loca ed in only some coun ies. Diopside, ano hi e and o he
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Mg/Ca py oxenes and amphiboles a e ock- o ming mine als, bu hey do no occu as
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mine al deposi s.
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O he sou ces o Mg and Ca ha e been explo ed o po en ial ca bona ion, including Mg-
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o Ca-con aining mine ailings and by-p oduc s o was es om indus y. This has included
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in es iga ion o he ca bona ion o ly-ash [21], s eel making slag [22–25], asbes os-
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mining ailings, elec ic a c u nace (EAF) dus , cemen -kiln dus , was e conc e e, and ai
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pollu ion con ol (APC) esidues [9,26]. In addi ion, na u al ca bona ion in he o ma ion
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o ca bona ed cemen sys ems has been well-known o many yea s. Alkaline ea h
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hyd oxide cemen s and mo a s ha den slowly due o hei eac ion wi h a mosphe ic CO2.
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O he well-known ca bona ion p ocesses occu in ce amic building ma e ials. These
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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
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wi h a mosphe ic CO2 and humidi y such mine als can be ca bona ed [27]. Mo eo e , in
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many low-quali y b icks he p esence o CaO is common, and ca bona ion is e y quick.
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Fabb i e al. [27] p esen a e iew o he p esence o calci e on ce amic ma e ials,
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indica ing ha he calci e can be o p ima y o seconda y o igin. P ima y calci e includes
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he o ms o calci e ha a e p ese ed wi hou change du ing he ce amic i ing.
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Seconda y calci e (an h opogenic calci e) includes all he o ms o calci e ha c ys allize
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in he ce amics a e i ing, i espec i e o he ime, he cause, and he g ain size.
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Taking in o accoun he easy ca bona ion o ce amic building ma e ials, his esea ch
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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
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indus ially p o i able. The main ca bona ion mechanisms we e s udied in he p esence
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o wa e o simula e an accele a ed ca bona ion p ocess.
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2. Ma e ials and Me hods
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Th ee b icks om di e en Andalusian (Sou h Spain) b ickwo ks we e chosen o
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ca bona ion es s. The b ick MPC2 was a clinke b ick made in Bailen (Jaén), i ed a
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1050°C. The b ick AUC1 was a pe o a ed b ick made in La Puebla de Cazalla (Se illa),
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hea ed a 900°C and he b ick MSC1 was a hollow ce amic block om Jun (G anada),
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hea ed a app oxima ely 800°C. The b icks we e g ound in a jaw c ushe and sie ed in
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labo a o y.
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The ca bona ion es s we e ca ied ou in a 0.3 L olume he me ic eac o om Pa
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Ins umen . The ixed condi ions we e 10 ba s o CO2, 4:1 solid-wa e a io and oom
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empe a u e. The a iable condi ions we e he eac ion ime (be ween 24 and 720 hou s)
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and he pa icle size (> 4 mm, 2-4 mm, and 1-2 mm) (Table 1). These pa icle-size
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ac ions we e selec ed because hey a e he mos ep esen a i e esul s o he c ushing
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ea men .
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Table 1. Expe imen al pa ame e alues du ing he ca bona ion eac ion es s.
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A e inishing he ca bona ion es s, ea ed samples we e d ied a 70°C o 24 hou s,
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powde ed, and sie ed a 100 µm o subsequen analysis.
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The mine alogical composi ion o he un ea ed and ea ed samples was iden i ied by X-
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ay di ac ion (XRD), using a B uke D8 Ad ance di ac ome e wi h s anda d
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monoch oma ic CuKα adia ion ope a ing a 40 kV and 30 mA. Scanning was pe o med
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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
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ealized o de e mine he quan i a i e composi ion o un ea ed b icks, in his case, he
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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
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adding zinci e as in e nal s anda d.
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The majo elemen al composi ion exp essed in oxides was pe o med by X- ay
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luo escence (XRF) wi h an au oma ed Panaly ical Axios model spec ome e . The
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samples we e p epa ed o analysis as glass discs.
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The ca bona ed con en o he aw and ca bona ed samples was de e mined by wo
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di e en analy ical me hods: he mal decomposi ion (DTA-TG) and elemen al analysis.
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DTA-TG analyses we e pe o med in a TG Ne zsch STA 409PC. Samples (app oxima ely
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150 mg) we e hea ed in an aluminium oxide c ucible unde a ni ogen a mosphe e a 10°C
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min-1 om oom empe a u e o 1200°C. Weigh loss was measu ed by TG in he ange
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o 450-900°C ela i e o he o al ca bona ed decomposi ion. The elemen al ca bon
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con en was also measu ed using an elemen al analyse , LECO CHNS 932, which
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calcula es he ca bona ed a io.
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Soluble Si, Ca and Mg ions o he o iginal and ea ed samples we e also de e mined.
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The analysis was pe o med wi h simul aneous induc i ely-coupled plasma op ical
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spec ome y (ICP-OES) analysis using a Ho iba Jobin Y on ULTIMA 2 model ins umen .
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The samples we e p epa ed by mixing he solid powde samples wi h wa e and s i ing
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o 24 h, a e wa ds isola ing he liquid phase by cen i uga ion and il e ed using a Nylon
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0.22 µm sy inge il e .
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The speci ic su ace a ea (BET) was measu ed wi h a Mic ome i ics Gemini 2360
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ins umen using he abso p ion o N2 a liquid ni ogen empe a u e. P io o measu ing,
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all he samples we e degassed a 80°C o 12 h and inally ou gassed o 10-3 To .
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Mac o and mic o obse a ions we e ob ained by s e eomic oscope using a G eenough
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Leica S8 APO equipped wi h a DC300 came a, and by scanning elec onic mic oscopy
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(SEM) using a JEOL 6460 LV mic oscope and FEI Teneo, bo h equipped wi h ene gy
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dispe si e spec ome e s (Ox o d Ins umen s INCA and EDAX, espec i ely). The
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samples we e p epa ed wi h Au-spu e coa ing o imp o e he imagining o he samples.
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Topog aphy measu emen s we e ca ied ou using a non-con ac 3D op ical p o ile
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Senso a S-Neox.
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3. Resul s and Discussion
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Calcium oxide in he b icks anges om 15-24 w %, and magnesium oxide anges om
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2-4 w % (Table 2). Such high Ca-ma e ials seem o be app op ia e o mine al
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ca bona ion.
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Table 2. Majo oxide composi ion (w %) by XRF o selec ed b icks.
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The b icks a e composed o qua z and c is obali e (SiO2), diopside (CaMgSi2O6) and
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mino o hoclase (KAlSi3O8). O he silica es we e also de ec ed, such as wollas oni e
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(CaSiO3) in MPC2 and AUC1, ano hi e (CaAl2Si2O8) in MPC2, and gehleni e
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(Ca2Al(AlSi)O7) in MSC1 (Table 3). Anhyd i e (CaSO4) was also iden i ied in AUC1 and
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MSC1; in he la e sample, mica, and aces o calci e and hema i e we e also ound. This
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mine alogy is consis en wi h he chemical analysis and he hea ing empe a u e o hese
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ce amic ma e ials.
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Table 3. Mine alogical composi ion (w %) o selec ed b icks.
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Legend [28]: Q z: qua z; Anh: anhyd i e; Wo: wollas oni e; C s: c is obali e; O :
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o hoclase; Ab: albi e; Di: diopside; An: ano hi e; Gh: gehleni e; Mca: mica; Cal: calci e;
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Hem: hema i e; Amo ph: amo phous phase.
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On he o he hand, mino ee Ca ions a e a ailable (100-800 mg/l) o p ecipi a e as
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ca bona es du ing he eac ion wi h ca bonic acid ha is p oduced by he combina ion o
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CO2 gas and humidi y.
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The b icks we e g ound in a jaw c ushe and sie ed in labo a o y, ob aining he ollowing
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a pa icle size dis ibu ion The ac ions > 4 mm, 2 - 4 mm and 1 - 2 mm ep esen mo e
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han 80% o he samples (Table 4). The e o e, hose ac ions we e selec ed o
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ca bona ed es s.
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Table 4. G anulome ic ac ions o he c ushed samples (w %).
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AUC1>MPC2>MSC1. These esul s ag ee easonably wi h he expe imen al ca bona ion
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da a.
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Table 5. Ca bona ion E iciency (C.E.) acco ding o S einou ’s equa ion and co ec ed.
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Acco ding o he XRD da a, wollas oni e and/o anhyd i e s ill emain in he ea ed
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ma e ial, which could con ibu e o an inc ease in he ca bona ion e iciency.
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Ne e heless, se e al ac o s could p e en CO2 di usion in o he bulk o he sample
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pa icles, such as he p esence o “ i eous” shee s, he illing o he po es wi h ca bona e
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c ys als, o a dec ease in he CO2 p essu e and/o mois u e necessa y o he acidic
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a ack.
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4. Conclusions
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The p esen s udy shows he possibili y o using ce amic cons uc ion was es o
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ca bona ion unde su ace condi ions in a sho pe iod o ime. Speci ically, in his s udy
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Ca- ich b icks we e success ul used as a aw ma e ial o di ec mine al ca bona ion. In
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addi ion o he des uc ion o Ca-silica es, anhyd i es, which is occasionally p esen , may
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also be a acked, and he Ca may be emo ed o a subsequen p ecipi a ion o
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ca bona es.
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The amoun o ca bona ion is p opo ional o he ime o eac ion ( he longe he ime, he
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highe he cap u e e iciency), whe eas i does no seem o signi ican ly depend on he
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pa icle size in he condi ions s udied.
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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
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we e o med in he po es o he ce amic pieces. In addi ion, some physical adso p ion
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was also obse ed.
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An accep able ca bona ion and/o CO2 cap u e le els ha e been achie ed unde
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a ou able condi ions o low p essu e and empe a u e, wi h low ene gy cos s and
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he e o e en i onmen al p o ec ion.
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These esul s open he possibili y o u u e s udies on using exhaus ed qua ies illed
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wi h b ick was es, which could be di ec ly ca bona ed by injec ing CO2 “in si u”.
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AUTHOR INFORMATION
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Co esponding Au ho
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Domingo Ma ín, dm[email p o ec ed], ORCID Id: o cid.o g/0000-0003-3725-6598
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Au ho s
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Domingo Ma ín, dm[email p o ec ed], ORCID Id: o cid.o g/0000-0003-3725-6598
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Pa icia Apa icio, papa [email protected], ORCID Id: o cid.o g/0000-0001-5307-1433
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Emilio Galán, [email p o ec ed], ORCID Id: o cid.o g/0000-0002-8466-5047
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P esen Add esses
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Depa amen o C is alog a ía, Mine alogía y Química Ag ícola, Facul ad de Química,
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Uni e sidad de Se illa, Calle P o eso Ga cía González, 1, Se illa 41012, Spain
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Au ho Con ibu ions
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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
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app o al o he inal e sion o he manusc ip . All au ho s con ibu ed equally.
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Funding Sou ces
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This esea ch was unded by he Jun a de Andalucía (Conseje ía de Economía y
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Conocimien o) (P12-RNM-568 MO p ojec ).
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Acknowledgmen
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This esea ch was unded by he Jun a de Andalucía (Conseje ía de Economía y
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Conocimien o) (P12-RNM-568 MO p ojec ) and he con ac o Domingo Ma ín g an ed
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by he V Plan P opio de In es igación de la Uni e sidad de Se illa. XRD, XRF, ICP-OES,
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C-elemen al and SEM analysis we e pe o med using he acili ies o he Gene al
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Resea ch Cen e a he Uni e si y o Se ille (CITIUS).
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ABBREVIATIONS
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APC, ai pollu ion con ol; BET, B unaue , Emme and Telle speci ic su ace; C.E.,
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ca bona ion e iciency; CCS, ca bon cap u e and s o age; DTA-TG, simul aneous
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he mog a ime ic and di e en ial he mal analysis; E.C., expe imen al cap u e; EAF,
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elec ic a c u nace; GHG, g eenhouse gases; ICP-OES, induc i ely coupled plasma
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op ical emission spec ome y; LOI, loss on igni ion pe o med; SEM, scanning elec on
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mic oscope; T.C., heo e ical cap u e; XRD, X- ay di ac ion; XRF, X- ay luo escence.
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Lis o ables and igu es:
480
Table 1. Expe imen al pa ame e alues du ing he ca bona ion eac ion es s.
481
Table 2. Majo oxide composi ion (w %) by XRF o selec ed b icks.
482
Table 3. Mine alogical composi ion (w %) o selec ed b icks.
483
Table 4. G anulome ic ac ions o he c ushed samples (w %).
484
Table 5. Ca bona ion E iciency (C.E.) acco ding o S enoi ’s equa ion and co ec ed.
485
486
Figu e 1. 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