concentrated inverse emulsion polymerization学术英语论文.docx
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concentrated inverse emulsion polymerization学术英语论文.docx
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concentratedinverseemulsionpolymerization学术英语论文
Abstract
Usingbutylmethacrylates(BMA)asmonomer,Span80asemulsifier,divinylbenzene(DVB)ascross-linkagent,ammoniumpersulfate(APS)/sodiumhydrogensulfite(SHS)asredoxinitiator,thehighoil-absorptionresinwassynthesizedbyconcentratedinverseemulsionpolymerization.Andtheeffectsofdifferentpolymerizationtechnologicalparameters,suchasinitiator,crosslinker,emulsifier,ontheoilabsorbencyofhighoil-absorptionresinswerediscussedindetail.Theresultindicatedthattheabsorptionoftheresinwasabout9.2(g/g)fortolueneand16.2(g/g)forchloroform.
Keywords:
concentratedinverseemulsionpolymerization;oilabsorptionresin;oilabsorptionrate
摘要
以甲基丙烯酸正丁酯为单体,二乙烯基苯为交联剂,Span80为乳化剂,过硫酸铵/亚硫酸氢钠为氧化还原引发剂,采用超浓反相乳液法合成了高吸油性树脂。
研究了引发剂用量,交联剂用量,乳化剂用量对树脂吸油性能的影响。
所制备的树脂可以吸收自身重9.2倍的甲苯、16.2倍的三氯甲烷。
关键字:
超浓反相乳液聚合;吸油性树脂;吸油速率
Contents
Abstractⅰ
AbstractinChineseⅱ
1Introduction1
2Experiment3
2.1Materials3
2.2Polymerization3
2.3Measurements3
2.3.1Oilabsorptiontest3
2.3.2Regenerationtest4
2.3.3Oilretention4
2.3.4Characterization4
3ResultsandDiscussion5
3.1Theeffectofcross-linkingamountontheoilabsorbency5
3.2Effectoftheamountoftheemulsifierontheoilabsorbency5
3.3Theeffectofinitiatoramountontheoilabsorbency6
3.4Oilabsorptionrateoftheresins7
3.5Relationofoilretentionratiowithtime8
3.6Oilabsorptionrepetitivecharacteristicofresins8
4Conclusions10
Bibliography11
1Introduction
Oilpollutionofmarineenvironmentsisbecomingaseriousissue.Withthegrowthoftheoff-shorepetroleumindustryandthenecessityofmarineoiltransportation.Variousmethodsforthetreatmentofspilledoilhavebeentried[1–5].Oneofthemethodstosolvethisproblemisbyusingoilabsorptiveresins,whichcancollectandremovetheoilspilledonwater,andsomehaveprovedtobehighlyefficient[6-7].
Highoil-absorptionresin,beingdifferentfromtraditionaloil-absorbingmaterials,isanewkindofself-swellingoil-absorbingmaterialwithmanyvirtuesofabsorbinglargequantityandvarietyofoils,onlyabsorbingoilfromoil/watermixtureandhighcapacityforoilretention,andhasapromisingfuture.Synthesisandapplicationsofhighoil-absorptionresinshaveveryimportantpracticalsignificanceforenvironmentprotection.
Acrylichasbeenwidelyusedasmonomerstopreparehighoil-absorbingresins.Copolymerizationofacryliccanbeapproachedbyvariousmethodssuchasemulsionpolymerizationandsuspensionpolymerization.However,theresinsobtainedbytheabovemethodsuniversallyhavesomedefectsofcompactstructure[8–10].Itisimportanttoselecta
suitabletechniqueandoptimizetheconditionsofpolymerizationforsynthesisofworkableacryliccopolymer.
Concentratedemulsionsaregel-likeemulsionsinwhichthevolumefractionofthedispersedphaseisgreaterthan0.74.Thedispersedphaseisintheformofsphericalorpolyhedralcellsseparatedbyacontinuous-phasenetworkofthinfilms.Concentratedemulsionshavethreeimportantcharacteristics:
[11-12]
(1)thereducedmonomermobilitybetweencells,becauseofthepresenceofareinforcedsurfactantlayer,cangenerateanearliergeleffect,whichleadstoadelayinthebimolecularterminationreactionand,therefore,ahighermolecularweight;
(2)theparticlesizecanbecontrolledeasilybytheselectionofasuitablesurfactanttypeandconcentration;and(3)apolymercontaininglittlewater,fromwhichpowderyresinsareeasilyformed,canbeobtainedthroughconcentratedemulsionpolymerization.
Incomparisonwiththefourmethodsoffree-radicalpolymerization(bulk,solvent,suspension,andemulsion),concentratedemulsionshavenotonlyapastelikeappearanceandahighsolidcontentbutalsoanucleationmechanismforthelatexparticle;themorphologyoflatexproductsisdifferentfromthatofconventionalemulsionpolymerization.Forthesereasons,concentratedemulsionpolymerizationdeservestobestudieddeeplyandwidely.Inthisessay,theinfluencesofemulsifiers,theamountofcross-linkagent,theamountofinitiatorontheabsorptionpropertiesoftheresinwereinvestigated.
2Experiment
2.1Materials
Butylmethacrylate(BMA)analyticalreagentgrade,TianjinKediReagent,wasusedasmonomer;Ammoniumpersulfate(APS)andsodiumhydrogensulfite(SHS)analyticalreagentgrade,TianjinFuchenReagents,wereusedasredoxinitiator;Span80analyticalreagentgrade,TianjinkemioReagent,wasusedasemulsifier;Divinylbenzene(DVB)chemicallypure,ShanghaReagent,wasusedascross-linkagent.
2.2Polymerization
BMAwascarriedoutin150-mlroundbottomflask.Atypicalprocedurewasasfollows:
therequiredamountsofSpan80andDVBwereputintothereactionsystem.ThesystemwaschargedwithN2for20minsandwassealedunderN2.Then32-mldeionizedwaterwasinjectedintothereactionsystem.Afterthat,ammoniumpersulfate(APS)/sodiumhydrogensulfite(SHS)wereinjectedintothereactionsystem.Theflaskwaswhollyimmersedinawaterbathheldat40℃byathermostattostartthepolymerization.Thereactionwascarriedoutunderstirring.Thereactiontimewas3h.Thepolymerwasdriedinvacuumfor24hata35℃.AlloftheingredientsusedaresummarizedinTable1.
Table1.StandardrecipefortheconcentratedinverseemulsionpolymerizationofBMA
Ingredient
Dosage
BMA
7ml
DVB
0.6ml
Span80
0.501g
H2O
32ml
(NH4)2S4O8
0.161g
NaHSO3
0.235g
2.3Measurements
2.3.1Oilabsorptiontest(goil/gsample)
Theoilabsorbency(W)wasdeterminedbytheweighingmethod.Aquantityof0.1~0.2gofdriedsampleweightedbeforehandwasputintoafilterbagandimmersedintolueneatroomtemperature.Aftergiventimeperiods(24hisneededforfulloilabsorbency),thefilterbagwiththesamplewasliftedfromtheoilanddrainedfor1min.Thenthesamplewasimmediatelytakenoutandweighed.Theoilabsorbencywascalculatedbythefollowingformula:
W1=(G2-G1)/G1
whereG1istheweightofresinsbeforeoilabsorptionandG2istheweightofresinsafteroilabsorption.
Forthestudyofoilabsorptionrateoftheresins,theabovemeasurementsarerepeatedfromtimetotime.
2.3.2Regenerationtest
Oil-absorbedsamplesweredriedinvacuumfor24h.Usingtheabovemeasurementstestsoilabsorbencyatfivetimes.
2.3.3Oilretention
Theresinsafteroilabsorptionwereputindryingovenfor5hat50℃,andthenweighted.
2.3.4Characterization
TheparticlemorphologyoftheBMApolymerwasobservedwithscanningelectronmicroscopy(SEM;JSM-5610LV).Thesamplesweresputter-coatedwithAufilmbeforetheexaminationandthevoltageis20kV.
3ResultsandDiscussion
3.1Theeffectofcross-linkingamountontheoilabsorbency
Theoil-absorbingprocessofhighoil-absorptionresins,aslowdegreeofpolymer,wasswellingprocess.Asevidence,notonlythesortsofcrosslinkercanaffecttheinterstitialspacestructuresoftheresins,butalsotheamountofcrosslinkercandirectlyinfluencetheparticlemorphologyandthedegreeofcrosslinkingoftheresins.Figure1illustratedtherelationshipbetweenoilabsorbencyandtheamountofDVB.AsshowninFig.1,therewasamaximumpoint.WhentheamountofDVBwassmallerthanthatatthemaximumpoint,theoilabsorbencyincreasedwithincreasingDVB.However,theoilabsorbencydecreasedwithincreasingDVBwhenthemountofDVBwaslargerthanthatatthemaximumpoint.
Fig.1Theeffectofcross-linkingamountontheoilabsorbency
Itiswellknownthatanincreaseintheamountofacrosslinkercausesthedensernetworkofthepolymer.AddinglessamountofDVB,thedegreeofcrosslinkingoftheresinswaslower,thetridimensionalnetworkwasnotsatisfying.Theresinsweresolubleinoilandtheviscosityoftheproductincreased.Theresinswhichhaveabsorbedoilcannotrecover.Iftheamountofcrosslinkerwastoogreat,thecrosslinkerdegreeincreasedandthenetworkspaceintheresinsdecreased.Asaresult,theoilabsorbencyreduced.Theresinshadthebestoilabsorptivitywhentheinterstitialspaceisatitsoptimumvalue.Figure.1showsthatthisoccursat8.8.
3.2Effectoftheamountoftheemulsifierontheoilabsorbency
Inconcentratedinverseemulsionpolymerization,althoughemulsifiersdonotdirectlytakepartinthereaction,theyhavereducinginterfacetension,emulsification,anddispersingeffects.Themaindifferencewithaconventionalemulsionpolymerizationisthatapartofemulsifierispresentatthemonomer/waterinterfaceandnotonlyatthepolymerparticle/waterinterface.Anotherpointisthat,inmostcases,theamountoftheemulsifierisverylow,sothattheparticlesformedbytheemulsionprocessarenotstableenoughandeasilycoalescetogivemuchlargerprimaryparticles.
Fig.2TheeffectofSpan80concentrationontheoilabsorbency
TheeffectoftheamountoftheemulsifierbasedontheoilabsorbencywasshowninFig.2.Whenconcentrationemulsifierislow,theoilabsorbencyincreased.Becausetheprimaryparticlesformedwithagglomeratesoflatexparticlesweremorestablebecauseofthecolloidprotectionbehavioroftheemulsifier,theoilabsorbencyincreased.WithincreasingSpan80concentration,thecolloidprotectionbehaviorwasmoreprominent,andthepolymerizationproceededstably;then,theprimaryparticlesexistedmorestably,andmorelargeparticleswereformed.Asaresult,theoilabsorbencydecreased.
3.3Theeffectofinitiatoramountontheoilabsorbency
BMApolymerasshort-chainhighoil-absorptionresinswerepreparedbyconcentratedinverseemulsionpolymerization,withtheformationofradicalsinwaterphase,andtheradicalswer
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