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机构地区:[1]湖北师范学院化学与环境工程系生化分析技术湖北省重点实验室,湖北黄石435002
出 处:《化学反应工程与工艺》2007年第4期343-347,共5页Chemical Reaction Engineering and Technology
基 金:湖北省自然科学基金项目(2005ABA053)
摘 要:以MCM-41分子筛负载磷钨钼杂多酸H_3PW_6Mo_6O_(40)为催化剂,以不同的酮或醛(乙酰乙酸乙酯、环己酮、丁酮、苯甲醛和正丁醛)和二元醇(乙二醇、1,2-丙二醇)为原料,合成不同的缩醛(酮)化合物(2-甲基-2-乙氧羰甲基-1,3-二氧环戊烷、2,4-二甲基-2-乙氧羰甲基-1,3-二氧环戊烷、环己酮乙二醇缩酮、环己酮1,2-丙二醇缩酮、丁酮乙二醇缩酮、丁酮1,2-丙二醇缩酮、2-苯基-1,3-二氧环戊烷、4-甲基-2-苯基- 1,3-二氧环戊烷、2-丙基-1,3-二氧环戊烷和4-甲基-2-丙基-1,3-二氧环戊烷),考察了醛或酮与二元醇摩尔比、催化剂用量和反应时间对缩醛(酮)收率的影响。结果表明,较合适的反应条件为醛或酮与二元醇摩尔比为1:1.5,催化剂的用量为反应物料总质量的0.2%,反应时间45min。在此条件下,缩醛(酮)的收率为46.8%~88.5%。A new environmental friendly catalyst H3PW6 Mo6 O40/MCM-41 was prepared. Different acetals and ketals (2-methyl-2-ethoxycarbonylmethyl-1,3-dioxolane, 2,4-dimethyl-2-ethoxycarbonyl- methyl-1, 3-dioxolane, cyclohexanone ethylene ketal, cyclohexanone 1,2-propanediol ketal, butanone ethylene ketal, butanone 1,2-propanediol ketal, 2-phenyl-1, 3-dioxolane, 4-methyl-2-phenyl-1,3-dioxolane, 2-propyl-1,3-dioxolane, 4-methyl-2-propyl-1,3-dioxolane) were synthesized with different ketone or aldehyde and dihydric alcohols over H3PW6Mo6O40/MCM-41 catalyst. Effects of the molar ratio of ketone or aldehyde to dihydric alcohols, H3 PW6 Mo6 O40/MCM-41 catalyst dosage and reaction time on the yield of acetals and ketals were discussed. The results showed that the appropriate conditions were the molar ratio of ketone or aldehyde to dihydric alcohols 1 : 1.5, the mass ratio of the catalyst to the reactant 0.2% and reaction time 45 rain. Under the conditions, the yield of acetals and ketals was 46.8%-88.5%.
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