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分析测试,20091225,19(6):56~59CHINAELASTOMERICS:20090624:(1983),,,,,GPC(SSBR)崔英,胡才仲,宋同江,史工昌,怀惠珍,龚光碧(,730060):采用凝胶渗透色谱(GPC)对溶聚丁苯橡胶(SSBR)合成过程中的反应试剂与阴离子聚合的反应条件进行选择;标定了GPC的校正曲线并确定了GPC的测试条件,得出避免SSBR样品过载的经验公式在此基础上采用GPC谱图及数据确定了结构调节剂十二烷基苯磺酸钠(SDBS)的用量反应溶剂偶联剂反应温度及反应时间结果表明,当n(SDBS)/n(Li)=0.3时,环己烷作为溶剂,SiCl4作为偶联剂,在60下反应1h,制备的SSBR具有优异的物理机械性能:凝胶渗透色谱;溶聚丁苯橡胶;阴离子聚合:TQ333.1:A:10053174(2009)06005604(GPC),,GPC,GPC(SSBR),SSBR1GPCGPC(M),,ViscotekTDA302(,10),,t,lgM,(1):lgM=-0.003333t2+0.113333t+4.20004(1)GPC,,(THF)1.0mL/min,30(,0.1mL)GPC,,GPC,80%~90%,,,,[1~3]1SSBR/(gL-1)1SSBR1,0.25~1.5g/L,,,Moore[4],SSBR:[]V0.1(2):[],mL/g;,g/mL;V,mL22.1,,GPC,,GPC,GPC1n(SDBS)/n(Li)SSBR1,n(SDBS)/n(Li),(MnMw),(Mw/Mn)SDBS,n(SDBS)/n(Li),SDBS,1n(SDBS)/n(Li)SSBRn(SDBS)/n(Li)MnMwMw/MnMnMwMw/MnMnMwMw/Mn0.31867093637721.9484373484973831.1371587811689011.0640.52609093453881.3245811946268631.0792210032450331.1090.72041772660441.3035200575877171.1301913202044241.0682,SDBS,,/mL2n(SDBS)/n(Li)SSBR12,n(SDBS)/n(Li)=0.3,SSBR,SSBR,n(SDBS)/n(Li)=0.32n(SDBS)/n(Li)SSBRn(SDBS)/n(Li)0.30.50.7/%51.333.839.42.2SSBR,3SSBR3SSBRMnMwMw/MnMnMwMw/MnMnMwMw/Mn1713792249691.3133150923537711.1231343311415781.0542674653426641.2815774046098981.0562510352719161.08376986877631.1401416011460651.03263202692681.0961199601457321.2152327342438651.0481043551135421.0883,,,,,SSBR,,,,3SSBR576,.GPC(SSBR)(1HNMR)43,,17.01%,52.18%4,,,1h100%,,,1h2.3SSBR,SiCl4SnCl4,5GPC5,,,SiCl467%,SnCl458%,,SnCl4SiCl4:C!SiC!SnSiCl4SSBR2.4,,58194SSBR4SSBR/MnMwMw/Mn50100000869311451741.67601000001069471593511.49701000001569141898651.21801000001936972072551.074,60,SSBR,,603SSBRSSBR:[1]RosaGarcaLopera,IsabelIrurzun,ConcepcinAbad,etal.Fractalcalibrationinsize-exclusionchromatography[J].JournalofChromatographyA,2003,996(1):33~43.[2]Tsai,YWu.GPCobservationsofbranchingeffectsinanionicpolymerizationofmethylmethacrylate:Apreliminarystudy[J].JournalofAppliedPolymerScience,2009,111(4):2099~2103.[3]YoungSDoh,SerjiNAmirkhanian,KwangWKim.AnalysisofunbalancedbinderoxidationlevelinrecycledasphaltmixtureusingGPC[J].ConstructionandBuildingMaterials,2008,22(6):1253~1260.[4]JCMoore,KHAltgelt,YLSegal,etal.Gelpermeationchromatography[M].NewYork:MarcelDekkerInc,1971.137~138.ApplicationofGPCinthepreparationofSSBRCUIYing,HUCaizhong,SONGTongjiang,SHIGongchang,HUAIHuizhen,GONGGuangbi(LanzhouPetrochemicalResearchCenter,PetroChina,Lanzhou730060,China)Abstract:GPC(GelPermeationChromatography)isanewtypeliquidchromatography.Theconstituentsareseperatedaccordingtothesizeofmolecularvolume,andnowGPChasbecomeanimportantseperationmethodinchemistryfield.GPCwasusedtodeterminethereactionreagentandthereactionconditionsofanionicpolymerizationinthepreparationofsolutionpolymerizedstyrenebutadienerubber(SSBR)inthispaper.ThecorrectioncurvewascalibratedandthetestconditionsofGPCweredetermined.AlsotheempiricalformulatoaviodoverloadofSSBRwasobtainedinthispaper.Andonthebaseofthat,thespectrasanddataofGPCwereusedtodeterminetheamountofSDBS(sodiumdodecylbenzenesulfonate),reactionreagent,couplingagent,reactiontemperatureandreactiontimeoftheanionicpolymerization.TheresultsshowedthatSSBRwithexcellentmechanicalpropertiescanbeobtaindat60for1hourincyclohexane,theratioofSDBS/Liis0.3andthecouplerisSiCl4.Keywords:gelpermeationchromatography(GPC);solutionpolymerizedstyrenebutadienerubber(SSBR);anionicpolymerization596,.GPC(SSBR)