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UtilizationofWasteMarblePowderinCementIndustryA.N.BdourandM.S.AlJuhani

UtilizationofWasteMarblePowderinCement
Industry
ByAhmedN.Bdour*andMohammadS.AlJuhani
December2011

1.AssociateProfessor,CivilEngineeringDepartment,Collegeof
Engineering,UniversityofTabuk,SaudiArabia*CorrespondingAuthor
2.Dean,CollegeofEngineering,UniversityofTabuk,SaudiArabia
Abstract
Presentlylargeamountsofslurryaregeneratedinmarblecuttingplantswith
aseriousconsequencesontheenvironmentandhumans.Thispaper
presentstestresultsshowingthefeasibilityofusingWasteMarblePowder
(WMP)incementindustryasasubstitutelimestone.Also,itdescribesthe
formulationofnewlimebased(CRII)cementitiousmaterialsderivedfrom
thusindustrialwastes.Powdermixtureswerepreparedandfiredatdifferent
temperatures.Forcomparison,similarformulationswerepreparedwithpre
treatedandcommerciallyavailablenaturalrawmaterialsandprocessedin
similarconditions.
Thecharacterizationincludedchemicalcomposition,determinedbyXray
fluorescence(XRF),thermalbehaviour(DTAandTGA)andparticlesize
distribution.Also,physicalparametersofmilledpowderssuchasthespecific
surfaceareaandthepercentofweightretainedinafixedsieve(75m)were
introduced.
TheCRIIclinkerwasfoundtocontaincommoncementitiousphases,such
asC3AandC3S,butfreelimeandcalciumaluminumoxidesulphatewere
alsoidentifiedbyhightemperatureXRDandNMR.Thelimebasedcement
obtainedfromwastesshowsastrongerhardeningcharacterthanthe
standardmaterial,whichtendstoshowdustingphenomenaduetothe
presenceofareasonableamountoffreelime.However,someimpurities
presentinthewastematerialsprogresstheoverallreactivityofthemixture.
CRIIbinderisparalleltootherconventionalbinderinthefieldofbuilding
constructionlikelime,cementandotheradmixturebutisdifferentfromthem
asitutilizesWMPasamajorcomponentwithotheringredients.Testresults
showthatthisWMPbasedcementiscapableofimprovinghardened
concreteperformanceupto16%,enhancingfreshconcretebehaviorand
canbeusedinarchitecturalconcretemixturescontainingwhitecement.CR
IIisanenvironmentfriendlyproduct,cheaperanditinvolvessmall
equipmentswithnoconvolutedtechnologiesanditrequiresverylowenergy
formanufacturing.
Keywords:WasteMarblePowder,Cement,Concrete,Limestone

Introduction
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Environmentalconstraints,increasingindustrialactivityandrisingcostsofnaturalmineral
resources,haveforcedthetransformingindustrytoreviewthelogisticsofrawmaterialssupply
(Saaketal.,1999).Worldwide,therehasbeenanincreasedinterestinresourcerecovery,
recyclingandresourceconservationaskeyparametersforanysustainabledevelopment
plans(Mileticetal.,2003).
Wastemarblepowderisgeneratedasabyproductduringcuttingofmarble.Thewasteis
approximatelyintherangeof20%ofthetotalmarblehandled.Theamountofwastemarble
powdergeneratedatthestudysiteeveryyearisverysubstantialbeingintherangeof250
400tones.Themarblecuttingplantsaredumpingthepowderinanynearbypitorvacant
spaces,neartheirunitalthoughnotifiedareashavebeenmarkedfordumping.Thisleadsto
seriousenvironmentalanddustpollutionandoccupationofvastareaoflandespeciallyafter
thepowderdriesup(asshowninFigure1).Thisalsomayleadstocontaminationofthe
undergroundwaterreserves(Brancoetal.,2004Vijayalakshmietal.,2001).
Traditionally,WMPproductsaredisposedofassoilconditionersorlandfill.However,there
mightbereusingorrecyclingalternativesthatshouldbeinvestigatedandeventually
implemented.ThankstoCivilEngineeringresearch,numeroususesofwastemarblepowder
havebeenintroduced,includinguseintilesmanufacturing,concretemixes,subgradefill,and
modifiedbinder(Huseyinetal.,2010Nunesetal.,2009Akbulutetal.,2007andBacheH.,
1981).OfourparticularinterestistheuseofWMPincementindustryasasubstituteof
limestonefortheproductionofclinker.
Whilemarbleblocksarecutbygangsaws,waterisusedasacoolant.Thebladethicknessof
thesawsisabout5mmandnormallytheblocksarecutin20mmthicksheets.Therefore,out
ofevery25mmthicknessofmarbleblock,5mmareconvertedintopowderwhilecutting.This
powderflowsalongwiththewaterasmarblepowder.Thus,nearly20%ofthetotalweightof
themarbleprocessedresultsintoWMP.TheproducedWMPhasnearly35%45%water
content.Thetotalwastegenerationfromminingtofinishedproductisabout50%ofmineral
mined.
Ingeneral,theclinkeristhe
Figure1WMPpitsatalocalcompanysite
maincomponentofcement,and
isobtainedbyfiringthe
appropriatemixtureofraw
materialsatabout1500C.
CommonphasesinPortland
cementclinkersare:alite
(3CaOSiO2,C3S),belite
(2CaOSiO2,C2S),tricalcium
aluminate(3CaOAl2O3,C3A),
andtetracalciumaluminate
ferrite(4CaOAl2O3.Fe2O3,
C4AF)(Giacomoetal.,2010)..
Beliteorsulphobelitebased
cementscontainthephases
belite(C2S)andtetracalcium
trialuminatesulphate(C4A3S)astheirmainconstituents(Bonavettietal.,2003).Theydonot
containaliteortricalciumaluminate,butmaycontainvariableamountsofcalciumaluminate
ferrite.Theyalsocontaincalciumsulphate(CS)inamountshigherthannormalinPortland
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cement(Hoetal.,2001Noguchietal.,1999).Onetypicalcompositionconsistsof:C2S40%
C4A3S32%C4AF20%CS8%.Sulphobelitecementsmayperformeitherasnon
expansivehighearlystrengthcements,orasexpansivecements,dependingontheproportion
oftheindividualphasesintheclinkerandtheamountofintergroundcalciumsulphate
(Bonavettietal.,2003).Twomainadvantagesaregenerallyattributedtothesetypesof
cements,namely:(i)energysavingsuponfiring(maximumclinkeringtemperatureis1350C
(ii)lowervolumeofCO2emissions.
Freecalciumoxideinsmallamounts(usuallybelow1%ofweight)isaregularconstituentof
Portlandclinker,butlargeramountsmaybepresentifthemaximumtemperatureinthe
productionoftheclinkeristoolow,theburningtimeistooshort,ortheCaOcontentintheraw
materialexceedstheacceptablerange(limesaturationfactor>100).Largeamountsmay
causeexpansion,strengthlossandcrackingofthehardenedpaste,duetoadelayed
hydrationoffreecalciumoxidetocalciumhydroxide,whichtakesplacetopochemicallyandis
associatedwithanincreaseinvolume(Giacomoetal.,2010).Thus,excessiveamountsof
freecalciumoxideinclinkermustbeavoided.However,oldcementshavelimeand/or
pozzolansasmainhardeningphasesandtheirdurabilityiseasilyprovedinseveralhistorical
monumentsandcommonbuildings.Itisthenobviousthantheporousstructureofthose
mechanicallyweakstructuresaccommodateslargerdimensionalchangeswithoutserious
damage(Giacomoetal.,2010).

EnvironmentalProblemsAttributedtoWasteMarblePowder
TheWMPimposesseriousthreatstoecosystem,physical,chemicalandbiological
componentsofenvironment.Problemsencounteredare:
Itadverselyaffectstheproductivityoflandduetodecreasedporosity,waterabsorption,
waterpercolationetc.
Whendried,itbecomesairborneandcausesevereairpollution.Introduces
occupationalhealthproblems,italsoaffectsmachineryandinstrumentsinstalledin
industrialareas(Hwangetal.,2008).
Affectingqualityofwaterduringrainyseason,andreducingstoragecapacitiesand
damagingaquaticlife.
Itadverselyaffectsocialandindustrialactivitiesofpeoplesincetheheapsofpowder
remainscatteredallroundthecountryareaneyesoreandspoilaestheticsofentire
region(MunozMontanoetal.,2003).
Itisthereforeasocialandlegalresponsibilityofgovernmentandindustrytosolvetheproblem
ofWMPpollution(Corinaldesietal.,1998).Assuch,developmentofcountryisonlypossible
bysustainablebalancedindustrialization.Recently,therapidsocial,economical,and
environmentalchangesinJordanstressedhumansocietywithunprecedentedchallenges.
Thus,newapproachesthatconsiderindustrialwastesasalternativerawmaterialsbecomes
interesting,bothtechnicallyandeconomically,forawiderangeofapplications.Ofour
particularinterestistheuseofWMPincementindustryasasubstituteoflimestoneforthe
productionofclinker.

Objectives
BecauseoftheenvironmentalthreatsassociatedwiththeWMP,theirproperdisposalhas
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attractedalotofattentionoftheenvironmentalistsinthelastyears.Inordertoproperly
disposeofthesehundredstothousandsoftonnesofpowder,theuseofinnovativetechniques
torecyclethemisimportant.Withouttheproperdisposalofthispowdermaterial,theresulting
stockpileswouldcausemajorhealthrisksforthepublicandtheenvironment(Accharetal.,
2006).
Thispaperproposesagainfulutilizationofwastemarblepowderasapartsubstituteof
limestoneinacementplant.Bearinginmindtherecentrapideconomicalgrowthand
developmentsintheconstructionsectorinJordan.Inparticular,cementfabricationinvolvesa
hugeconsumptionofnaturalrawmaterials(e.g.limestoneandclay).Ofourparticularinterest
istheuseofwastemarblepowderincementindustryasasubstituteoflimestoneforthe
productionofclinker.
Thisresearchdescribesattemptstodefinethecompositionsofwastebasedmixturesandthe
correspondingprocessingconditionssuitabletotheproductionpowderbasedcements.Also,
thisstudyassessesthepropertiesofthefinalproductafterincorporatingwastemarble
powder.Ultimately,asanoutcomeofthisproject,theincorporationofwastemarblepowderin
cementindustrycouldleadtoaviable,environmentallyfriendlymaterialwithattractive
properties.

Approach(Methodology)
Forthepurposeofthisresearch,severalWMPspecimenswereprepared.Therawmaterial
wasprovidedbyalocalcompany,andthenthesematerialsweremilledandsievedthrough75
msievesize.Afterthat,rigorousanalyseswerecarriedoutattheCivilEngineering
LaboratoriesandtheCentreforEnvironmentalStudiesattheHashemiteUniversity.
Thecharacterizationincludedchemicalcomposition,determinedbyXrayfluorescence(XRF,
PhilipsX'UNIQUEII),thermalbehaviour(DTAandTGA,Setaram)andparticlesize
distribution(Coulter)inalcohol.Also,physicalparametersofmilledpowders(about2hina
ringsmill+porcelainjar)suchasthespecificsurfacearea(SSA,byBET)andthepercentof
weightretainedinafixedsieve(75m)weredetermined(Ahn2004Singhetal.,2001).
Forcomparison,andtoclarifytheeffectofminorcomponents,presentintheWMPmaterials,
onthefinalproductproperties,similarcompositionswerealsopreparedwithcommercialhigh
puritygraderawmaterials,M1calciteareusedasstandardsamples.
Inordertopreparethecorrespondingcement(CM)carbonate(11%)andcalciumsulphate
(6%hemihydrate)isaddedtotheclinkerbeforemilling.Sincetheavailableamountof
materialissmall,settingcharacteristicsoftheoptimizedformulations(water/cement
ratio=0.45)isinferredfromtemperaturemeasurementsofthefreshpastes.Sampleshave
beenplacedinaspecialthermalinsulatingboxinordertoassurealmostadiabaticconditions.
Temperaturesarecontinuouslymeasuredthroughtheinsertionofathermocoupleinthepaste
(Giacomoetal.,2010).
XrayPhotoelectronSpectroscopy(XPS)wasusedtocharacterizetheoutermostatomic
layersonthesurfaceofcementformulationsagedfor1and2months.Eachsamplewas
groundinanagatepestleandmortartoexposefreshsurfacesforanalysis.Thepowder
obtainedwascompressedintoholes10mmindiameterand0.5mmdeepmachinedintoa
coppersampleholder.
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ThepreparedsampleswereimmediatelytransferredintotheXPSsampleintroduction
chambertominimizetheeffectsofsurfacecontaminationandreaction.Anareaof
approximately4mm4mmonthecompressedpowdersurfacewasanalyzedusinga
ThermoVGScientificEscascopespectrometerwithanAlK(1486eV)Xraysource,operated
at280W(14kV,20mA).Widescansurveyspectrawereobtainedbetween0and900eV
bindingenergy(BE)withastepsizeof1.0eV.
Theevolutionofcompressivestrengthwithcuringtimeisalsomonitoredonsmalltestbars
(~221410mm)castfromthecementpastesintoironmoulds.Phasesformeduponcuring
aredeterminedbyXRD(RigakuGeigerflexD/maxSeries,CuKat40kVand50mA)andby
DTA.Finally,characterizationtechniqueswereusedtoassessmicrostructuraland
compositionalchallengesoftheagedcements(Nunoetal,2007).TheseincludedRaman
spectroscopy,XrayPhotoelectronSpectroscopy(XPS),andFocusedIonBeamimaging
(FIB).

ResultsandConclusions

Figure2Locationinthecompositiondiagramofthe
SiO2Al2O3CaOternarysystem,ofthewastemarble
powderandthecompositionsinvestigated(CRII/CRIIP)

CharacterizationofClinkers
Figure2showsthelocationofthe
formulationsintheternarydiagramSA
C.Theresultingloosepowderswere
calcinedatselectedtemperatures(10
C/minheatingrate,1hsoaking)and
namedasCRII.Thestandardclinkers
(herebydistinguishedbyaCRIIP)were
preparedinasimilarmanner,butusing
theCalcitecM1calcitecommercial
reagents.
Chemicalandphysicalparametersof
milledWMPandparticlesizedistribution
areshownTable1,Table2,andTable
3,respectively.
Table1ChemicalAnalysisofWaste
MarblePowder
N
1.
2.
3.
4.
5.
6.
7.
8.

TestCarriedOut
Lossonignition
Silica
Alumina
IronOxide
Lime
Magnesia
Soda
Potash

TestValue%
39.66
1.58
0.99
0.22
54.17
3.87
<.015
<.015

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Table2PhysicalPropertiesof
WasteMarblePowder
Property
BulkDensity(gm/cc)
SpecificGravity
Particlesize

Result
1.251.65
2.752.98
<343.2

Table3ParticleSizeDistributionof
WasteMarblePowder
ParticleSize(mm) %FinerbyVolume
345.1
100
195.0205.8
90
133140
80
82.096.7
70
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55.562.51
38.545.1
23.928.1
14.2417.2
4.97.15
1.331.89
0.421

Figure3comparestheverycomplex
powderXRDpatternsofCRIIandCRII
Pclinkers.TermssuchasW(W+G)
meanthatpeakiscommontoboth
phases.CRIIPcontainstheexpected
hydraulicphases(C2S,C3SandC3A),
whileCRIIcontains,inadditiontoC2S
andGehlenite,C12A7andcalcium
aluminumoxidesulphate.

60
50
40
30
20
10
0.00

Figure3XRDofCRIIandCRIIPclinkers:W(C2Sin
CRIIandC2SinCRII)W(W+G)F(calciumsulpho
aluminate)F(W+F),M(mayenite,C12A7)U(alite
C3S:M1JCPDS130272eM3JCPDS420551),
U*(U+W),T(C3A:JCPDS381429)T*(T+U)

Thisdifferenceiscertainlyduetoa
sluggishtendencytoequilibriuminthe
solidstateandthepresenceofother
minorconstituentsinthepowder
materials.ThislimebasedCRIIclinker
predictablycontainsahigheramountof
sulphurbutlessthan0.2%weightof
Na2O+K2O.Therelativelylowamountof
alkalismightcontributetothelowstability
ofthehightemperatureC2Spolymorphs(alpha),whilethehighamountofsulphur(N2wt.%as
SO3)ledtotheformationofcalciumaluminateoxidesulphate.Thosephasesarewellknown
bytheirexpansivecharacteristicsandmightberesponsiblefortheobserveddustingtendency
ofCRIIsamples.NMRtechniquehasalsobeenusedtoclarifythestructureofcementitious
phases,mostlyafterhydration.CommonphasesinPortlandtypecementclinkers(C2S,C3S,
C3A,andC4AF)werepreparedwithpurechemicalreagentsandcharacterized,tobeusedas
references,aimingataneasiercharacterizationoftheactualcomplexclinkers.
Figure4comparesthe29SiMASNMRspectraofthe
CRIIandCRIIPclinkers.Twomajorpeaksbetween
65and75ppmcanbeobserved.Suchchemical
shiftscorrespondtoQ0orQ1monosilicates,totally
depolymerisedtetrahedral.TheC2Spolymorph(peak
at71.3ppm)andtheC3Sphase(peakat73.5ppm)
arepresentinbothCRIIandCRIIP,butthelater
seemstobeabettercrystallizedmaterial(sharper
resonances)andcontainahigheramountofC2S
(higherpeakarea).IntheWMPbasedclinker,the
peaksat67.4and69.5ppmareattributedtoQ0and
Q1sitesincrystallinesilicates,alsopresumedinthe
broadshoulderbetween67and69ppmintheC1
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Figure429SiMASNMRspectra
oftheCRIIandCRIIPclinkers

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spectrum.InCRII,theclearpresenceofC2S(peakat
73.7ppm)mayalsocontributetodustingbehaviorof
thispowderwhenexposedtoambientconditions.The
delayinthesettingprocessdisplayedbytheCRII
clinkermayalsobeexplainedbyitslowerC2Scontent.
The27AlMASNMRspectrumoftheCRIIclinker
(Figure5)showsapeakat67.7ppmwhich,usingthe
XRDinformation,canbeattributedtoC12A7.Besides
C12A7,thespectrumoftheCRIIPsampleexhibits
extrapeaks,attributedtoC3A(peakat54.0ppm)and
probablehydrates(peakatca.17ppm).Duetolowiron
oxidecontentintherawmaterials,itisnotsurprising
thatthepresenceofC4AFwasnotdetectedinCRII
(AkbulutandGure,2007).
Tosummarize,Table4givesmainidentifiedphasesin
theclinkersbythetwotechniques.

Figure527AlMASNMRspectra
oftheCRIIandCRIIPclinkers

Table4Summaryofmaindetectedphasesonclinkers
byusingdistincttechniques
Clinker XRD
CRII

NMR
C2SC12A7C2AScalcium C2SC2SC3S
C12A7C2AS
aluminumoxidesulphate

CRII C SC SC A
2
3
4
P

C2SC3SC3AC
SHCAH

BehaviorofCements
Table5showssomecharacteristicsofCMIIandCMIIPcements.Figure6showsthe
evolutionoftheircompressivestrengthwithcuringtime.Thesevaluesaremuchlowerthan
thosereportedforPortlandcement(about10%after7daysofcuring),meaningthatthe
hardeningprocessismuchslower.However,longtermresistanceismorecomparable.For
example,samplescuredfor3monthsshowcompressivestrengthofabout32MPa.
Table5Initialsettingtimeandmechanicalstrength
developmentuponcuringofcements
Property
Initialsettingtime(min)
Compressivestrength7days(MPa)
Compressivestrength28days(MPa)
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CMII CMIIP
628 347
3.58
3.79

Figure6Evolutionofthecompressive
strengthofcementswithcuringtime,
CMIIandCMIIPformulations

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Comprehensivecharacterizationofthe28dayaged
sampleswasconductedbydifferenttechniques.Using
DTA,decompositionreactions(between110and350
C)ofCAHandCSHhydratesseemtobe
strongerinCMIIP,revealingtheirpresenceinhigher
amounts.Theabsenceorsmallexpressionofsuchkind
ofpeaksinCMIIcementiscompatiblewithitsweak
hydrauliccharacter.

Conclusions
Inconclusion,theWMPbasedclinkerswerefoundtocontaintheexpectedcementitious
phasesandagoodagreementwasobtainedbetweenthecharacterizationstechniquesused.
Inparticular,thedustingphenomenaobservedinCRIIclinkerswasexplainedbythe
formationofcalciumaluminumoxidesulphateandalsobythepresenceofC2S.
Onitsstandardcountersample(CRIIP)theC2Sisstabilizedinstead.Sincethetotal
amountofalkalisinCRIIPisevenlower,thenonoccurrenceofexpansive(dusting)reactions
inthismaterialmeansthatthelackofthosemineralizingagentsisnotthecontrollingfactorof
theunwantedphenomenon.Sothatsulphurcontentshouldbethedeterminingfactor,inducing
theformationofdetectedexpansivesulphurcontainingphases.
TheWMPbasedcementobtainedfromwastesshowsastrongerhardeningcharacterthanthe
standardmaterial,whichtendstoshowdustingphenomenaduetothepresenceofa
reasonableamountoffreelime(astheresultofitsexpansivereactionwithambientmoisture).
Somefluxingimpurities(e.g.alkalis)presentinthewastematerialsimprovetheoverall
reactivityofthemixture.
Thisnewlydevelopbinderisparalleltootherconventionalbinderinthefieldofbuilding
constructionlikeLime,cementandotheradmixturebutisdifferentfromthemasitutilizes
WMPwithotheringredients.TestresultsshowthatthisWMPbasedcementiscapableof
improvinghardenedconcreteperformanceupto16%,enhancingfreshconcretebehaviorand
canbeusedinarchitecturalconcretemixturescontainingwhitecement.Thenewbinderis
environmentfriendly,cheaperincostfromtheotherconventionalmaterialalsoitinvolves
smallequipmentwithnocomplicatedtechnologiesandrequiresverylowenergyfor
manufacturing.
Acknowledgements
Theauthorswouldliketothanktheanonymousrefereeswhosecommentshavehelpedto
improvethequalityofthismanuscript.ThestaffoftheCivilEngineeringLaboratoriesandthe
CentreforEnvironmentalStudiesattheHashemiteUniversityandtheUniversityofTabukfor
theirassistanceandsupportduringthecourseofthisresearch.Also,theHigherCouncilof
ScienceandTechnology(HCST),fortheirgenerousfinancialsupport.
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