腰果酚二胺基苯并噁嗪树脂的制备及性能分析-preparation and performance analysis of cardanol diamine benzoxazine resin.docxVIP

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腰果酚二胺基苯并噁嗪树脂的制备及性能分析-preparation and performance analysis of cardanol diamine benzoxazine resin.docx

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腰果酚二胺基苯并噁嗪树脂的制备及性能分析-preparation and performance analysis of cardanol diamine benzoxazine resin

AbstractCardanolisakindofphenoliccompound,itnotonlyisnaturalbutalsohasvarietyexcellentproperties.Itcanbeusedinplaceoftraditionalphenol.Inthispaper,cardanolwasusedtosynthesizecardanol-basedaromaticdiaminebenzoxazineresin(PCBOZ),thenstudiedandimproveditsproperties.Usingunsaturatedcardanol、4,4’-diaminodiphenylmethaneandformaldehydetosynthesizecardanol-basedaromaticdiaminebenzoxazine(CBOZ)bysolventmethod.AndthemonomerCBOZwascharacterizedbyFTIRand1HNMR.ThesynthesisprocrssofCBOZwasoptimizedbysinglefactorexperiments,gottheoptimumconditions:reactiontemperatureis100℃,reactiontimeis4h,theamountofsolvent(toluene)is30ml/0.2molcardanol,n(4,4’–diaminodiphenylmethane):n(cardanol):n(formaldehyde)is1:2:4.5.Onthisreactioncondition,theyieldofCBOZis91.3%.StudiedthemonomerCBOZ’scuringbehaviorandkineticsbynon-isothermalDSCtestmethod.Thecuringkineticsfactorswerecalculated:activationenergyE=93.71kJ/mol,thepre-exponentialfactorA=6.51×108,thereactionordern=0.91.ThecuringprocesstemperatureofCBOZwasdeterminedby(T-β)extrapolationmethod:initialcuringtemperature(Ti)is221℃,thermostaticcuringtemperature(Tp)is234℃,after-treatmenttemperature(Tf)is248℃.CuringthemonomerCBOZandepoxyresinE-44/CBOZbytemperature-programmedmethodrespectivelytosynthesizebenzoxazineresinPCBOZandblendingresinPCBOZ-E.ComparingtheFTIRspectrasofthemonomerCBOZandthecuredresindeterminedthatthemonomerCBOZhadbeensuccessfulonring-openingpolymerization.StudiedthecuringexothermicpeakenthalpyofPCBOZandPCBOZ-EwerebyDSCtestmethod,thedegreeofcuringaboutPCBOZis100%,andthedegreeofcuringaboutPCBOZ-Eis100%whenthecontentofepoxyresinE-44wasnomorethan50%.Thecross-sectionsofPCBOZandPCBOZ-EwereinvestigatedbySEM.Thecross-sectionsdidn’texistbubbles,PCBOZwasbrittleIIfracture,PCBOZ-Ewasductilefracture.ThethermalstabilitiesofPCBOZandPCBOZ-EwerestudiedbyTGtest.Theinitialdecompositiontemperature(T0%)ofcardanol-basedbenzoxazineresinPCBOZwas260.1℃,whichwas30℃higherthanthatofphenol-basedbenzoxazineresinPBOZ(T0%=233.2℃).ThenblendingresinPCBOZ-Ewassuperiorinhea