4/27/2017 Physicochemicalanalysisofflexiblepolyurethanefoamscontainingcommercialcalciumcarbonate

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SabrinaSeSant'AnnaIDenilsonArlindodeSouzaIDanielle CurriculumScienTI
MarquesdeAraujoICornliodeFreitasCarvalhoIIMariaIrene Automatictranslation
YoshidaI,*
Indicators
I DepartmentofChemistry,UFMG,Av.AntnioCarlos,6627,Pampulha,
Relatedlinks
31270901BeloHorizonteMG,Brazil
II DepartmentofChemistry,CampusUniversitrio,UFOP,Morrodo Share
Cruzeiro,35400000OuroPretoMG,Brazil
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ABSTRACT

Calciumcarbonate(CaCO3)isafilleroftenutilizedbytheBrazilianmattressfactoriesintheproductionof
polyurethanefoams.Thefillerallowsthesubstitutionofpartofthepolymericagents,conferringdimensional
stabilityandhardnesstothefoams.However,inagreementwithexperimentaldata,itisobservedthatthe
excessofcommercialCaCO3utilizedinindustrycausestheincreaseofhysteresis,possiblycausingpermanent
deformationsanddamagingthequalityofthefinalproduct.Inthepresentwork,thephysicochemicalanalyses
oftheflexiblepolyurethanefoamswithdifferentcontentsofCaCO3wereperformed.Thefoamsaresubmitted
tothemorphological,mechanicalandpositronanalysestoverifythealterationsprovokedbytheprogressive
introductionofthisfiller.

Keywords:polyurethane,foam,calciumcarbonate

1.Introduction

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Theversatilityofpolyurethanechemistrypermitstheproductionofagreatvarietyofmaterialssuchdepending
ontheinitialingredientsusedinthesynthesis1.Flexiblepolyurethanefoamsareoneofthemostimportant
classesofcellularplasticandcanbeappliedinthefabricationofawiderangeofmaterialsfordifferentuses
suchasfoammattresses,pillows,furniture,cushioningmaterialsforautomobiles,packing,recreation,shoes,
etc.2.

Ingeneral,industriesthatproduceflexiblepolyurethanefoamsusefillerstomodifythematerial'spropertiesin
someway,suchas:dimensionalstability,retractionfromthemoldanddensity34.Whenaddingafillertoa
polymertoformaconjugatedbiphasicmaterial,thetensionappliedtothepolymericmatrixwillbetransferred
inparttothedispersephase,thefiller,sinceitpresentspropertiessuperiortothepurepolymer 5.Efficient
reinforcementisachievedbyinteractionsoftheconstituentsofthebiphasicmaterial 67viamechanismsof
adhesion,whichcouldbe:adsorption,electrostaticattraction,chemicalbondingandmechanicaladhesion.

Chemicalbondingisthemostefficientformofadhesionandoccurswiththeapplicationofcouplingagentson
thesurfaceofthefiller,whichservesasabridgebetweenthepolymerandthereinforcement.Inmechanical
adhesion,thepolymerfillsinthegroovesofthefillerthisadhesiontendstobelowunlessthereisalarge
numberofrecessesonthesurfaceofthefiller 8.

Inprincipleanymaterialcanbeusedasafiller.However,someaspectsmustbeconsideredwhenselectingthe
materialforthispurpose.Theseinclude:size9,inthattheparticlesmustbesmallandabletoeasilydispersein
thepolymermatrixchemicalpurity,toavoidundesiredreactionsandabrasiveness,whichcancauseexcessive
deteriorationtothemixingequipmentandincreasecosts8.

Amongtheinorganicmaterialsutilizedasfiller,notableonesinclude:calciumcarbonate,aluminumhydroxide,
silica,titaniumdioxideandtalc6.Someoftheorganicmaterialsmorecommonlyusedarecarbonblack10and
naturalfibers1112.

Inflexiblepolyurethanefoams,thefillerspromoteanincreaseindensityandresistancetocompression.
However,theyreducetheresiliencyandcontributetotheincreaseinpermanentdeformation.Inaddition,
propertiessuchastearstrength,forexample,aresignificantlyaffectedbytheintroductionoffiller 13.
Accordingly,itisnecessarytoknowtheenduseofthematerialinordertousethecorrectconcentrationinthe
polymermatrix,obtainingaproductofreliablequality.

Inspiteofthepolyurethaneindustrywidelyusingcalciumcarbonateasafiller,generallythequantityusedis
definedrandomly.Commercialcalciumcarbonatehaslargeuseinthisindustriesbecauseitslowercost,non
toxicity,nonabrasivenessandfacilitatepigmentation.InthebusinessesvisitedintheregionofBeloHorizonte,
nodatawasavailableontheinfluenceofthisfilleronthefoam,norwasthereanymethodologytodefinethe
idealquantityofcalciumcarbonatethatshouldbeaddedwithoutcausingdamagetothemechanicalproperties
ofthefinalproduct.

Thustheproposalofthepresentworkwastoanalyzethemorphologicalandmechanicalbehaviorwhenvarious
concentrationsofcommercialcalciumcarbonatewereintroducedintothepolymermatrix,usingscanning
electronmicroscopy(SEM),energydispersiveXrayspectroscopy(EDS)microanalysis,compressivestrength
testsinaccordancewiththeISO3386Part1standard14,thermalanalysis(TGA/DTA)andpositronannihilation
lifetimespectroscopy.Inparticular,thepositronannihilationtechniqueisrevealingitselftobeapromisingtool
tostudythepropertiesofthefreevolumeholesinanondestructiveform.

2.Experimental
2.1.Rawmaterials

Therawmaterialsemployedwerethefollowing:PolyetherpolyolVoranol4730NandTDIVoranateT80(Dow
Chemical)thesiliconesurfactantPDMS/POE(GeneralElectric)amineAricatAA805(Arinos)andstannous
dioctoateII(MiracemaNuodex)wereusedascatalystsinthepolymerizationandexpansionreactions1516
distilledwaterandcommercialcalciumcarbonateobtainedfromthemattressmanufacturingindustriesinthe
regionofBeloHorizonte.Theisocyanateindexusedwas132.AFisatommodel710shaftstirringdevice(power:
25W,rotation:25200rpm)wasusedforstirring.Table1showstheformulationsemployedinthiswork.

2.2.Preparationofflexiblefoams

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Polyolandthefillerwereplacedinaplasticreceptacle,andthemixturewasstirreduntilcomplete
homogenization.Next,theamine,surfactantandwaterwereadded.Themixturewassubmittedtomechanical
stirringforoneminute.Shortlyafterthecatalystwasaddedandthemixturewasstirredagainfor30seconds.
Afterintroducingtheisocyanate,themixturewassubmittedtosixsecondsofstirringandthenpouredintoa
cubicalcardboardbox(7x7x7cm).Thefoamswerelefttocurefortreedays.

2.3.Flexiblefoamsanalyses

Fortheinstrumentalanalyses,thefollowinginstrumentswereused:SEMJeolJSM840

Microanalysis(EDS)Jeol8900electronprobemicroanalyzermechanicalanalysisLloydLR5Kthermal
analysisNetzschSTA409EPpositronannihilationsprectroscopyAfastfastcoincidencespectrometerfrom
Ortec.

SEM:Thesampleswerecutintolittlepieces(0.5x0.5x0.5cm)usingscissors.Nexttheywerecoveredwitha
finelayerofgold.Thesampleswereanalyzedundermagnificationsof50,150and500x.

EDS:Thesamplesofcalciumcarbonatewerecoveredwithafinelayerofcarbonandanalyzedunderan
acceleratingvoltageof15kVandacurrentof20nA.

Mechanicalanalysis:Thespecimenstaken,5.0cmfromtheedge,weresubmittedtofourcompression
decompressioncyclesat70%oftheiroriginalheightandavelocityof100mm/mininaccordancewiththeISO
3386Part1standard.Duringthefourthcyclethehysteresiswasobtained17.

Thermogravimetricanalysis(TGA):TheTGA/DTGcurveswereperformedinthetemperaturerangeof25950
C,withsamplesofapproximately12mgpackedinaluminacrucible,anddynamicairatmosphere(100mL/min
gasflow).

Positronannihilationlifetimespectroscopy(PALS):Forthismeasurement,anelectronicdevicecalledafast
fastcoincidencecircuititwasusedandconsistingbasically,oftwogammadetectors,twoconstantfraction
differentialdiscriminators(CFDD)andatimetoamplitudeconverter(TAC)wasused.Themeasurementofthe
foamssampleswereperformedwith 22Napositronsourceinsandwichconfiguration.ThecalibrationofMCAwas
50ps/channelandthetimeresolutionofthepositronlifetimespectrometermeasuredforrayof 60Cowas260
ps.TheanalysesbyPALSwereperformedonfoamsgroundinliquidnitrogen.Thelifetimespectrawere
satisfactorilyresolvedinthreecomponentsutilizingthePOSITRONFITEXTENDEDprogramandsupplyingthe
valuesforintensities(Ii)andmeanlifetime(ti).Thesubscriptsi=1,2,3refertotheparapositronium(pPs),
freepositronandorthopositronium(oPs)species,respectively1819.

3.ResultsandDiscussion
3.1.Analysisofcommercialcalciumcarbonate

Whenafillerisintroducedintoapolymericmaterial,theidealisthatithasregulargranulometryandthatits
particlesaresufficientlysmalltoenablegooddistributioninthematrix7.Figure1presentsthescanningelectron
microscopyofcommercialcalciumcarbonateatamagnificationof500x.

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Itwasobservedthatthecalciumcarbonatepresentedirregular,heterogeneousandcoarsegranulometry.The
calciumcarbonate,usedinthepresentwork,showedalargepolydispersioningranulometricanalysiswith
sievesofdefinedparticlesizes.Theparticlesizevariedbetween100and+250mesh.Thisfillerisusedinthe
mattressindustrywithoutanypretreatmentbecauseitisaresiduegeneratedinthefabricationoflimeandsold
tothemanufacturersatreducedprices.

ThecalciumcarbonatewasalsosubmittedtoaqualitativeXrayenergydispersivespectrum(EDS,Figure2),
whereitwaspossibletodetectthevariouselementsofitsconstitution.Itisworthnotingthattoimprovethe
foamquality,granulometryaside,theidealistoutilizeachemicallypurematerialthatdoesnotcontain
substancesthatcouldreactwiththematrix8.

3.2.Analysisofflexiblefoams

Figure3presentstheSEManalysisoftheflexiblepolyurethanefoamscontaining21%ofcalciumcarbonate.
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Itisobservedthatthecalciumcarbonateaddedisagglomeratedinsomepointsinthepolymermatrixandnot
evenlydistributedhomogenously,asisrequiredtopromoteanefficientreinforcement5,20.Eventhoughtheuse
ofexcessivequantitiesoffillercausesenrichment,italsoisresponsiblefordamagetothematrix(Figure4)21,
causingthefoamtoloseitscharacteristicpolyhedralmorphology.Thearrowsshowtheworseningmorphology
ashigherconcentrationsareadded.

Alowinteractionofthefillerusedandthepolymericmatrixwasfurtherverifiedbymicroscopy(Figure5),
whichprobablycontributedtothedeformationsseenearlier(Figure4).

Figure6illustratesthethermogravimetric/derivativethermogravimetric(TGA/DTG)curvesofthesynthesized
polyurethanefoamandofthecommercialcalciumcarbonatefiller.Thepolyurethanefoampresentstypical
decompositionintwostagesbetween200and600C,generatingafinalresidueof1.73%.Thecommercial
calciumcarbonatedecomposesinthetemperaturerange550760C,losingCO2andgeneratingCaOwithafinal

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residueof~65.6%.Thishighvalueoftheresiduemeansthatthecommercialcalciumcarbonate,probably,
containsinertcompoundslikeCaO,SiO2,Al 2O3,etc,asshowintheEDSanalysis.

3.3.Mechanicalanalysis

Inthemechanicalanalyses,theflexiblefoamsweresubmittedtofourcompressiondecompressioncycleswith
theobjectiveofevaluatingthehysteresiswithincreasingcarbonateconcentration14.Inflexiblefoams,
hysteresis2223isrelatedtothelossoftheenergyofthesystemwhenitissubmittedtoacompression
decompressioncycle.Hysteresisisaveryimportantpropertyforevaluatingthequalityoffoams.Itisrelatedto
thelossofenergycausedbytheirreversibleslippageofthepolymerchainsinthecompressiondecompression
cycleduringuseofthefoam.Thegreaterthehysteresis,thegreaterthesusceptibilityofthematerialtosuffer
irreversibledeformations13.Asflexiblefoamsaresubmittedtocyclesofcompressionanddecompressionin
dailyuse,principallywhenusedinupholsteryandmattresses,themeasureofhysteresispredictspossible
deformationsthatwillinfluencethequalityoftheflexiblefoam2.Figure7presentsthehysteresisvaluesofthe
foamsincompressiondecompressiontestsasafunctionofincreasingfillerconcentration.

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Itwasobservedthatincreasingthequantityofcalciumcarbonateinthematrixalsoincreasedthehysteresis
values,signifyingthatthesystemwaslosingitsabilitytoreturntotheoriginalshape.Thereforeitwas
concludedthattheprogressiveadditionoffillerreducedthefoamqualitysincetheincreasedlossofenergy
duringthecompressiondecompressionledtodeformationofthematrix.Itisworthemphasizingthe
progressiveincreaseinhysteresisvaluesasafunctionofthequantityoffiller.Hysteresisisalsorelatedtothe
distributionofthefillerinthefoams.Thecarbonateisafillerthatpresentsalargesurfaceenergyand
interactionbetweentheparticles,tendingtoformagglomeratesinthematrix24.Inthismanner,theforcesare
notequallydistributedduringthecompressiondecompression,whichisalsoresponsibleforthedeformation
exhibitedbythefoams.

Anotherimportantparameterobtainedinthemechanicalanalyseswasthecompressionforcedeflectionat40%
compression,wherethefoamsweresubmittedtothecompressionnecessarytocauseadeformationof40%of
theoriginalsize.Thisparameterquantifiesthecompressionthataflexiblefoamsupportswithoutasignificant
lossinitsmorphology.ThehighertheCFD40value,themoredifficultthecompressionbecomesbecausethe
foamisharderandthereforehasagreaterdimensionalstability.Figure8showsthegraphobtainedofCFD40
asafunctionoffillerconcentrationforfoamswithcalciumcarbonate.

Itwasobservedthattheincreaseinfillerconcentrationincreasedthefoam'shardness,improvingthe
dimensionalstability.However,thefoammusthaveanequilibriumbetweentheCFD40andhysteresisinspite
oftheresultingimproveddimensionalstabilityofthefoam,theincreaseoffillerfavoreddeformationsthatlead
toadeclineinthequalityofthematerial.

3.4.Positronannihilationlifetimespectroscopy(PALS)

Polymerscienceusesthefreevolumeconcepttorationalizemanypropertiesatthemicroscopicstructurallevel,
alsorelatingthemtomacroscopicproperties.Onevaluablemethodforstudyingholeswithsubnanometersizes
ispositronannihilationlifetimespectroscopy(PALS)itcanalsobeusedtodeterminethesizedistributionofthe

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holesaswellasthefreevolumefractions.Insidepolymermatrices,thermalizedpositronscanform
positroniums(Ps)thatwillthenbeconfinedtofreevolumeholes.Themainannihilationmechanismofthe
orthopositronium(oPsthelonglivedtripletstateofpositronium)isthepickoffannihilationbyelectronsof
thehostmedium.Theannihilationparametersdependonthephysicochemicalproperties.Thelifetimeand
intensityoftheoPscanthenyieldtheholesizeanddensity2526.

Inthepresentwork,PALSwasutilizedtoconfirmthatthecalciumcarbonateadheresinamechanicalwayto
thepolymermatrix,nothavingsignificantinteractionsbetweenthetwomaterials.Forthis,twoparameters
wereanalyzed:I3and3.TheparameterI3givestheprobabilityoforthopositroniumformationandisrelated
totheconcentrationofholespresentinthematerial.Theparametert3evaluatesthedimensionsoftheempty
spacesinthebiphasicmaterialitsvariationsuggestssignificantinteractionsbetweentheconstituentmaterials.

BasedonthegraphofthevariationofI3(%)asafunctionofcalciumcarbonateconcentrationinthepolymer
matrix(Figure9a),alineartrendwasseenthatistypicalofmaterialsthathavetheircomponentslinkedby
simplemechanicaladhesion19.Thisverificationshowedthatthesystempresentstwophases,signifiedbythe
presenceofemptyspacescreatedintheinterfacesofthepolyurethane/CaCO3composite.

Itwasstillobservedthatforthepurecomponents,thereisasignificantdifferencethatreferstothepositronium
formation.Thepurepolyurethaneshowedsignificant(~28%)positroniumformation,whiletheCaCO3(1.9%)
waswithintheexperimentalerroranddidnotformpositronium.Suchaparameter,therefore,issensitiveto
thepossibleinteractionsbetweenthetwocomponents.

Figure9bdisplaysthegraphof3asafunctionoftheconcentrationofcalciumcarbonateinthepolymermatrix.
Atallconcentrationsitwasobservedthatthecarbonatedidnotcauseasignificantvariationin3,which
suggeststhatthecarbonateisonlyadheringtothematrixbysimplemechanicaladhesion.Suchaparameter,
I3,thereforeissensitivetothepossibleinteractionsbetweenthetwocomponents.

4.Conclusions
Thecalciumcarbonateandthepolymermatrixpresentalowinteractionthatisproportionaltomechanical
adhesion,asverifiedbyPALSanalysis.

Thecarbonatedidnotdispersewellinthematrixsinceithasvariableparticlesizeandpresentsinteractions
thattendtoformagglomerates,makingitsothatthereisnotadistributionofforcebetweenthecarbonateand
thematrixduringtheutilizationoftheflexiblefoam.

Althoughtheflexiblepolyurethanefoamfactoriesusecalciumcarbonateasafiller,theintroductionofhigh
quantitiescorroborateswiththeincreaseinhysteresisvalues,leadingtoalossinquality.

Acknowledgements
TheauthorsaregratefultoCNPqforfinancialsupportandProf.Dr.JosCaetanoMachadoforthepositron
annihilationanalyses.

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Received:May28,2008
Revised:December19,2008

*email:mirene@ufmg.br

Allthecontentsofthisjournal,exceptwhereotherwisenoted,islicensedunderaCreativeCommonsAttributionLicense

UFSCarDep.deEngenhariadeMateriais
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