Research Of Synthesis And Application Of 4-methyl-4'-vinyl Benzophenone

The present paper relates to the synthesization of polymeric photoinitiator 4-MVBP(4-methyl-4'-vinyl benzophenone).Detected the photopolymenzation performance by IR in the real time.And detected the remaining small molecule in special system by UV-Vis.First,raw material chlorobenzene is turned into p-chlorostyrene after acetylation,reduction and dehydration.Acetylation is performed at 40℃for 2.5h optimally while n(chlorobenzene):n(anhydrous aluminium chloride):n(acetyl chloride)=1.5:1.25:1.After the reaction,the superabundance chlorobenzene can be reused by anhydrous bitter salt dried.The way of reducting p-chloroacetophenone by aluminium isopropoxide is viable and more oecumenical.The reduction is performed for 6h at reflux temperature of isopropanol while the mole ratio of the synthesized p-chloroacetophenone and self-made aluminium isopropoxide is 1:1.2.The synthesized 1-(p-chlorophenyl)ethanol and potassium hydrogen sulfate are dehydrated into p-chlorostyrene at 220℃under vacuum.The overall yield is 68.2%with purification rate of 99.8%after rectification.The p-chlorostyrene as the raw material is turned into 4-methyl-4'-vinyl benzophenone after Grignard process and hydrolyzed with 4-methyl-benzonitrile.The conclusions were drawn as follows:in the Grignard process,n(Mg):n(Clst)=1.3:1,the temperature was 35℃,the time was 10h.The temperature of the reaction between Grignard reagent and 4-methyl-benzonitrile was 55℃,the time was 12h.The reaction final yield was 68.2%,and the purity of product can be 98.44%.The paper searched the solidified effect of the photoinitiator to the photopolymerization system,for example bisphenol-A epoxy diacrylate(6104),aliphatic polyurethane diacrylate(6105),polyether acrylate-epoxy acrylate(6106) and so on.We detected the change of maleimide groupes in the system by using IR in real time,then found out that the 10 has best effect.We can learn that at the same consistence of photoinitiator,according to the paint-film thicker,the solidified time become longer.And at the same thickness of paint film,according to the consistence of photoinitiator being higher,the solidified time become shorter.We detected the remaining small molecule in 6106 system which used 4-MVBP to solidify by UV-Vis.Then we found the remaining is less than the one using traditional photoinitiator BP.