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1、12羅翠銳等:低分子量水溶性酚醛樹脂的合成及表征絕緣材料2010,43(3)低分子量水溶性酚醛樹脂的合成及表征1a1a21b1a1a1a羅翠銳,翁凌,吳化軍,李子帙,王鳳春,朱興松,劉立柱(1.哈爾濱理工大學a.材料科學與工程學院;b.應用科學學院,哈爾濱150040;2.嘉興市清河高力絕緣有限公司,浙江嘉興314031)摘要:以Ba(OH)28H2O為催化劑,在苯酚與甲醛摩爾比為12的條件下,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樹脂。使用C_NMR對產(chǎn)物結構進行表征,通過GPC、DSC測量最終產(chǎn)物的分子量2+及分布和
2、熱行為。結果表明:在Ba催化作用下的羥甲基化反應中,苯酚的鄰位活性更高。合成的水溶性酚醛樹脂是聚合度為2~4的聚合體的混合物,這些聚合體以鄰-對位和對-對位方式連接形成亞甲基橋,有大量的高鄰位取代羥甲基苯酚,樹脂多分散指數(shù)為1.17,分子量分布較窄,DSC譜圖分別在144~168和186~199出現(xiàn)兩個獨立的放熱峰,樹脂通過兩步反應實現(xiàn)最終固化。關鍵詞:酚醛樹脂;分子結構;分子量分布;固化行為中圖分類號:TM215.1;TQ0631.6文獻標志碼:A文章編號: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前言會價值。水溶
