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1、12罗翠锐等:低分子量水溶性酚醛树脂的合成及表征绝缘材料2010,43(3)低分子量水溶性酚醛树脂的合成及表征1a1a21b1a1a1a罗翠锐,翁凌,吴化军,李子帙,王凤春,朱兴松,刘立柱(1.哈尔滨理工大学a.材料科学与工程学院;b.应用科学学院,哈尔滨150040;2.嘉兴市清河高力绝缘有限公司,浙江嘉兴314031)摘要:以Ba(OH)28H2O为催化剂,在苯酚与甲醛摩尔比为12的条件下,采用一次逐步加入甲醛的方式合13成了低分子量水溶性酚醛树脂。使用C_NMR对产物结构进行表征,通过GPC、DSC测量最终产物的分子量2+及分布和
2、热行为。结果表明:在Ba催化作用下的羟甲基化反应中,苯酚的邻位活性更高。合成的水溶性酚醛树脂是聚合度为2~4的聚合体的混合物,这些聚合体以邻-对位和对-对位方式连接形成亚甲基桥,有大量的高邻位取代羟甲基苯酚,树脂多分散指数为1.17,分子量分布较窄,DSC谱图分别在144~168和186~199出现两个独立的放热峰,树脂通过两步反应实现最终固化。关键词:酚醛树脂;分子结构;分子量分布;固化行为中图分类号:TM215.1;TQ0631.6文献标志码:A文章编号:1009-9239(2010)03-0012-04SynthesisandChar
3、acterizionofWater-solubleLow-molecular-weightPhenol-formaldehydeResolResin1a1a21bLUOCui-rui,WENLing,WUHua-jun,LIZi-zhi,1a1a1aWANGFeng-chun,ZHUXing-song,LIULi-zhu(a.CollegeofMaterialsScienceandEngineering;b.CollegeofAppliedScience,1.HarbinUniversityofScienceandTechnology,Ha
4、rbin150040,China;2.JiaxingQingheGaoliInsulatingMaterialCo.,Ltd,Jiaxing314031,China)Abstract:Awater_solublelow_molecular_weightphenol_formaldehyderesolresinwassynthesizedwithamolarratioof1:2betweenthecatalystBa(OH)28H2Oandagradualadditionofformalinina13oneprocessstep.Thest
5、ructuralchangeoftheresinwasdeterminedbyCnuclearmagneticresonance(NMR);Gelpermeationchromatography(GPC)wasusedinthedeterminationofaveragemolarmasses;andthethermalbehavioroftheresolsolutionwasstudiedusingdifferentialscanningcalorimetry(DSC).Inthestudy,ahigherreactivityoffre
6、eorthositestowardthemethylolgroupsofthephenolicunitswasobserved;theproductisamixtureconsistingofpolymerswithpolymerizationdegreefrom2to4,inwhichthephenolicringwaslinkedviamethyleneinortho-paraandpara_parapositions.Inthemixture,manyphenolicringssubstitutedbyhydroxymethylsa
7、torthopositionswereobserved.Thepolydispersityoftheresinis1.17withnarrowmolecularweightdistribution.Twowell_separatedcuringsignalswereobservedintheexothermsoftheresolresinat144~168and186~199,respectively;andtheresinwascuredviatwo_stepreactions.Keywords:phenol_formaldehydere
8、solresin;moleculorstructure;molecularweightanditsdistribution;curingbehavior[1]1前言会价值。水溶
