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1、湖南大學(xué)碩士學(xué)位論文水性光引發(fā)劑4-(2-羥乙氧基甲基)二苯甲酮合成研究姓名:臧陽(yáng)陵申請(qǐng)學(xué)位級(jí)別:碩士專業(yè):應(yīng)用化學(xué)指導(dǎo)教師:徐偉箭2002.6.18摘要水性光固化技術(shù)是一種環(huán)境友好的綠色技術(shù),隨著人們環(huán)保意識(shí)增強(qiáng),綠色環(huán)保產(chǎn)品水性光固化涂料近年來(lái)得到了蓬勃的發(fā)展,水性光引發(fā)劑的研究與開(kāi)發(fā)已成為熱門(mén)課題。本文合成了未見(jiàn)文獻(xiàn)報(bào)導(dǎo)的新型水性光引發(fā)劑4.(2.羥乙氧基甲基1二苯甲酮。由苯甲酰氯、甲苯、催化劑傅克反應(yīng)合成了中間體4.甲基二苯甲酮,進(jìn)行了條件試驗(yàn)、優(yōu)惠條件復(fù)證試驗(yàn),結(jié)果表明合成收率為58.6%,產(chǎn)品純度t>
2、99%,為工業(yè)化中試生產(chǎn)提供可靠實(shí)驗(yàn)數(shù)據(jù)。將4-甲基二苯甲釃溴化、重結(jié)晶,制各高純中間體4.溴甲基二苯甲酮,對(duì)其進(jìn)行了表征及定量分析,產(chǎn)品純度/>99%,收率>t48%。由甲醇鈉與7,Z醇脫甲醇制各乙二醇單鈉鹽。f由4-溴甲基二苯甲酮與L--醇單鈉鹽反應(yīng)合成了新化合物4.(2-羥乙氧基甲基’二苯甲酮,進(jìn)行了GC-MS。IR.’HNMR表征,確定了其結(jié)構(gòu),產(chǎn)品收率為78%(以4一溴甲基二苯甲酮計(jì)),純度≥95%。對(duì)新型水性光引發(fā)劑進(jìn)行了應(yīng)用試驗(yàn),結(jié)果表明,其光引發(fā)性能與二苯甲酮、1173及ciba2959進(jìn)行對(duì)比,
3、光固化速度略慢于BP,快于1173及ciba2959,揮發(fā)性氣昧與Ciba2959相當(dāng),明顯好于1173及BP?!?~本文的創(chuàng)新點(diǎn)在于首次臺(tái)成了未見(jiàn)文獻(xiàn)報(bào)導(dǎo)的新化合物4-(2.羥乙氧基甲基)二苯甲酮,并確定了其結(jié)構(gòu)。由于其具有光固化效率高、制成的光固化體系揮發(fā)性氣味小、開(kāi)發(fā)成本低,極具應(yīng)用開(kāi)發(fā)前景,對(duì)實(shí)現(xiàn)我國(guó)開(kāi)發(fā)出具有自主知識(shí)產(chǎn)權(quán)的水性光引發(fā)劑品種具有非常重要的意義。,關(guān)鍵詞:4-甲基二苯革酮,4.溴甲基二辜每酮,4.(2.羥乙氧基甲基)二苯甲酮,新化合物,水溶性光引發(fā)劑^qoAbstractWater—solu
4、bleUV-curedtechnologywasagreentechnologyofenvironment.Withtheenhancingofenvironmentprotectionconsciousness,inrecentyear,thegreenenvironmentalprotectionproduct———water—solubleUV-curedcoatinghadbeendevelopedvigorously,andtheresearchanddevelopmentofphotoinitiato
5、rshadbecomethehotsubject.Thenovelwater-solublephotoinitiator4-(2一hydroxyethoxymethyl)benzophenoneWassynthesizedinthispaper.Theintermediate4-MethylbenzophonewassynthesizedfrombenzoylchlorideandtoluenebyFrield—CraftreactionwithcatalystTheprocessconditionswgrete
6、stedandtheoptiufnprocessconditionsvc_ereretested.TheresultsindicatedthattheyieldWas78%andthepurityoftheproductupto99%.ItprovidedthereliabletechnicaldamfortheindustrialmiddletesLHighpurityintermediate4-BromomethylbenzophenoneWaspreparatedbybrominationof4-methy
7、lbenzophenone.ThesodiumethyleneglycolWaspreparatedbythereactionofethyleneglycolwithsodiummethan01.Thenewcompound4-(2-hydroxyethoxymethyl)benzophenonewassyhthesizedbythereactionof4-Bmmomethylbertzophenonewithsodiumethyleneglyc01.Theyieldwas78%,andthepurity.oft
8、henewproductWas95%.WeanalysizedtheGC·MS,IILNMRofthenewproductanddefineditsstructure.Weapplicatedthenewwater-solublephotoinitiatorsintheUV—curedcoating.Wecomparedthepropertiesofphotoinitia