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1、浙江大學(xué)化工系碩士學(xué)位論文鄰甲酚醛環(huán)氧樹脂的制備與性能表征姓名:張學(xué)新申請學(xué)位級別:碩士專業(yè):化學(xué)工程指導(dǎo)教師:單國榮20090401浙江大學(xué)工程碩士學(xué)位論文摘要簡單介紹了國內(nèi)外環(huán)氧塑封料行業(yè)的發(fā)展歷史和目前的狀況以及環(huán)氧塑封料對鄰甲酚醛環(huán)氧樹脂的質(zhì)量指標(biāo)要求。詳細(xì)綜述了國內(nèi)外鄰甲酚醛環(huán)氧樹脂的研究動態(tài)和發(fā)展趨勢、生產(chǎn)現(xiàn)狀、制備方法及原理、性能的影響因素及其應(yīng)用情況。研究了制備鄰甲酚醛環(huán)氧樹脂的原理和制備方法、工藝流程、實驗裝置、中試裝置。對鄰甲酚醛樹脂、鄰甲酚醛環(huán)氧樹脂的反應(yīng)機理進行了探討,考察了制備過程中影響鄰甲酚醛樹脂、鄰甲酚醛環(huán)
2、氧樹脂性能的各個因素。對鄰甲酚醛環(huán)氧樹脂的性能進行了表征,制定了產(chǎn)品標(biāo)準(zhǔn).確定和優(yōu)化了工藝路線。以草酸、鹽酸為催化劑,醛/酚摩爾比在o.85~0.92,反應(yīng)溫度為98"C反應(yīng),時間為5小時,加堿中和催化劑,溶劑莘取,水洗等,合成出合適的鄰甲酚醛樹脂.以適量季銨鹽為催化劑,鄰甲酚醛樹脂于110"(2下與過量環(huán)氧氯丙烷先醚化,然后在60~70"C溫度及.82kPa真空條件下加堿閉環(huán)反應(yīng),堿的摩爾數(shù)為酚羥基當(dāng)量的1.05,再通過萃取、精制閉環(huán)、洗脫鹽等,合成出高品質(zhì)的鄰甲酚醛環(huán)氧樹脂。根據(jù)小試確定的工藝進行了中試,中試產(chǎn)品與國內(nèi)產(chǎn)品進行了比較
3、,中試產(chǎn)品送客戶試用,達到進口同類產(chǎn)品水平。關(guān)鍵詞:鄰甲酚醛環(huán)氧樹脂,制備,性能表征浙江大學(xué)工程碩士學(xué)位論文ABSTRACTThehistoryofthedevelopmentandcurrentsituationofmoldingcompoundanditstechnicalrequirementsforo—cresolformaldehydeepoxyresinwasbrieflyintroduced.Theresearchdynamicsanddevelopmenttrendsofo—cresolformaldehydeepoxy
4、resinanditsmanufacturestatus,preparationmethodsandprinciples,performancefactorsandapplicationwasreviewed.Thereactionprinciple,preparationmethods,process,experimentaldeviceandpilotplantdeviceofo-cresolformaldehydeepoxyresinwerestudiedinthispaper.Thereactionmechanismofo-cr
5、esolformaldehyderesinando-cresolformaldehydeepoxyresinwerediscussed.Thefactorsthathavingeffectsonthesynthesisofo-cresolformaldehyderesinando-cresolformaldehydeepoxyresinwereinvestigated.Thepropertiesofo-cresolformaldehydeepoxyresinwerecharacterized.Theproductstandardswer
6、esetup.Theprocessesofdeterminedandoptimizedaresummarizedasfollows.Oxalicacidandhydrochloricacidwereusedasthecatalyst.Themolarratioofformaldehydef0-cresolwas0.85~0.92.Thereactiontemperatureofo-cresolformaldehyderesinWas98C.Thereactiontimewas5hours.Addedsomecausticsodatone
7、utralizecatalyst.Theo-cresolformaldehyderesinWasextractedbysolventandwashedbywater.Thenthesuitableo-cresolformaldehyderesinWassynthesized.Highperformanceo—cresolformaldehydeepoxyresinWassynthesizedbyusingthecatalystmquaternaryammoniumsalt.Itunderwentetherizedreaction、析廿l
8、excessiveepicholohydrinunder110℃,reactedunder60~70.1Catvaccumof一82kPatoformepoxidestructure.Accordingto