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www.spm.com.cnSum160No.1ChemicalEngineer20091:2008-11-10:(1978-),,,,:1002-1124(2009)01-0061-04VCL/NVP,3,,(,266071):,N-(VCL)N-(NVP)N,N-(MBA),(DLS)(AFM):;1555,,(LCST)35;,:;;;:TQ316.3;TQ427.6:APreparationandcharacterizationofthermosensitivepoly(N-vinylcaprolactam-co-N-vinylpyrrolidone)microgelsthrowprecipitationpolymerizationLIGuo-ying,YAOHong-wei3,WUTu-ping,LIUYu-zhen(CollegeofChemicalEngineeringandEnvironment,QingdaoUniversity,Qingdao266071,China)Abstract:NewthermosensitivemicrogelparticlesproducedbyusingN-vinylcaprolactam(VCL),N-vi2nylpyrrolidone(NVP)andN,N-methylenebis(acrylamide)(MBA)throwprecipitationpolymerizationmeth2ods.VCLandNVParecomonomers,andMBAiscross-linker.AseriesofThermosensitivemicrogelswaspre2paredthrowchangethediveofcross-linker.Thesurfaceofthemicrogelparticleswerestudiedbyatomicforcemicroscope(AFM),andthetemperatureresponsivebehaviorswerecharacterizedbymeasuringthediameterofthemicrogelsbydynamiclightscattering(DLS)atdifferenttemperature.Theresultsmicrogelparticlesarespheresandrelatedtothesizedecreasedwithtemperatureincreaseintherange1555,thelowercriticalsolu2tiontemperature(LCST)around35,soitsatemperaturesensitivemicrogel.Thediveofcross-linkercannotchangeLCSTonlychangethesizeofmicrogelparticles.Keywords:precipitationpolymerization;temperaturesensitive;microgel;cross-linker,,,[1]N-(NIPAm)[2-4],:32(LCST),,,LCST,[5]LCST,LCSTN-(VCL),,[6,7]LCST32,,,11.1N-(VCL)(C.R.);N-(NVP);N,N-(MBA);(N-)(AIBA);©1994-2009ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:VCL/NVP20091HPPS2001HPPS(DLS);TG16A-WS;CSPM3000(AFM)1.2VCLNVP;MBA50,3,;1.30.9225gVCL0.1025gNVP0.0205gMBA95.00mLN2250mL,,N2701h,O2,0.025g5mL,N21h,7h,[8],MVN-10.04100.06600.08200.1025gMVN-2MVN-3MVN-4MVN-51.4,10000rmin-1,30min,3,1.5%1.4.131H2SO4-H2O28030min,NaOH10min,,10h,1.4.23mL,DLS,1555,,10min,3,22.111Fig.1Substancesusedformicrogelsynthsis1,VCLNVP,,MBAVCLNVP,,,,VCL,NVP,NVP,2.2,,AFM,23,,2MVN-2AFMFig.2AFMpethographofsampleMVN-22,4%,,300nm,,©1994-2009ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:VCL/NVP633MVN-4AFMFig.3AFMphotographofsampleMVN-43,8%,530nm,2,,,2.3(DLS),1555,,,,4abc4(a:MVN-1;b:MVN-3;c:MVN-5)Fig.4Etlectoftemperatureondiameterofminrogels4,z,,35,(LCST)35,,VCL,,,,2.49010,,,2%10%,,1,1MBATable1EflectofMBAonmicrogelsVCL/gNVP/gMBA/gMBA/%MVN-10.92250.10250.02052MVN-20.92250.10250.04104MVN-30.92250.10250.06606.5MVN-40.92250.10250.08208MVN-50.92250.10250.1025101,(DLS),5a.MVN-1;b.MVN-2;c.MVN-3;d.MVN-4;e.MVN-5525Fig.5Particlesizedistributionofmicrogelsat255,,0.12%10.0%,342.5nm870.4nm,,,,,©1994-2009ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.:VCL/NVP200913,N-(VCL)N-(NVP)N,N-(MBA);1555,(LCST)35,,;2%10%,[1],,.-pH[J].,2007,65(2):91-94.[2],.pH[J].,2006,23(7):20--22.[3]MKarg,IP-Santos,BRGonzalez,etal.Temperature,pH,andIonicStrengthInducedChangesoftheSwellingBehaviorofPNIPAM-Poly(allylaceticacid)CopolymerMicrogels[J].Langmuir,2008,24:6300-6306.[4]IM.Okhapkin,IR.Nasimova,EE.Makhaeva,etal.EffectofComplexationofMonomerUnitsonpH-andTemperature-Sen2sitivePropertiesofPoly(N-vinylcaprolactam-co-methacrylicacid)[J].Macromolecules,2003,36:8130-8138.[5]APich,SBhattacharya,YanLu,etal.Temperature-SensitiveHybridMicrogelswithMagneticProperties[J].Langmuir,2004,20:10706-10711.[6]VBoyko,SRichter,WBurchard,etal.ChainDynamicsinMi2crogels:Poly(N-vinylcaprolactam-co-N-vinylpyrrolidone)MicrogelsasExamples[J].Langmuir,2007,23:776-784.[7]AImaz,JForcada.N-Vinylcaprolactam-BasedMicrogels:EffectoftheConcentrationandTypeofCross-linker[J].Poly2merScience:PartA:PolymerChemistry,2008,2766-2775.[8]VBoyko,SRichter,IGrillo,etal.StructureofThermosensitivePoly(N-vinylcaprolactam-co-N-vinylpyrrolidone)Microgels[J].Macromolecules,2005,38:5266-5270.(60)7Table.7Paralleltestresults/g30.6030.6030.5930.4630.59/%99.0399.0398.9998.5798.993PVC:0.2g,1.02151,85min,60,,,,,,,,,[1],.[J].,1997,(11).[2],.[J].,2000,(04).[3].[J].,1994,15(11):34-36.[4],.[J].,1998,(04).[5],.50%[J].,1999,20(10):41.[6],.[J].,2000,(01):44-45;48.[7].[J].,1990,(04):28-29.[8].N,N-[J].,1995,(04)7-8.©1994-2009ChinaAcademicJournalElectronicPublishingHouse.Allrightsreserved.