Study On A Process For Synthesis Of α-Hydroxy Carbonyls Photoinitiator

The photoinitiator which is an importang kind of fine chemical, can be widely a pplied in UV curings chemistry. Synthetic technology of 1-hydroxy-cyclohexyl-phenyl ketone and 2-hydroxy-2-methyl-l-phenyl-propan-1-one was studied in this dissertation. The mechanism was discussed, the final product was analyzed by GC-MS, IR and N MR.The intermediate cyclohexyl phenyl ketone and a-methylpropiophenon were synthe sized using cyclohexane carbonyl chloride and isobutyryl chloride by the reaction of F rield-Crafts reaction. The optimum reaction conditions were as follows:Frield-Crafts re action temperature was 5-8℃. n(cyclohexane carbonyl chloride):n(aluminum trichloride) =1:1.2, n(cyclohexane carbonyl chloride):n(benzene)=1:6, reaction time was 4h. The yi eld of cyclohexyl phenyl ketone was 91% and the purity was 99%. Temperature was 15℃. n(isobutyryl chloride):n(aluminum trichloride)=1:1.2, n(isobutyryl chloride):n(benz ene)=1:3, reaction time was 5h, the yield of a-methylpropiophenon was 87% and the purity was 99%.The photoinitiator 1-hydroxy-cyclohexyl-phenyl-ketone and 2-hydroxy-2-methyl-1-p henyl-propan-1-one was prepared from cyclohexyl phenyl ketone and a-methylpropioph enon. a-Hydroxylating with potassium hydroxide in the presence of phase transfer cata lyst and carbon tetrachloride. a-Hydroxylating optimum reaction conditions were as fol lows:reaction temperature was 70℃, n(cyclohexyl phenyl ketone):n(potassium hydroxi de)=1:8, n(cyclohexyl phenyl ketone):n(carbon tetrachloride)=1:2, the reaction time was 6h. The yield of 1-hydroxy-cyclohexyl-phenyl-ketone was 96% and the purity was 99 %. Reaction temperature was 70℃. n(a-methylpropiophenon):n(potassium hydroxide)=1: 8, n(a-methylpropiophenon):n(carbon tetrachloride)=1:2, the reaction time was 6h. The yield of 2-hydroxy-2-methyl-l-phenyl-propan-l-one was 84% with the purity of 99%.