摘要
将纳米Al2O3粉体经一定浓度的KF浸泡活化后制成纳米固体碱KF/Al2O3,将其用于催化合成氰乙基丙二酸二乙酯的Michael加成反应以考察其活性.分析了纳米固体碱制备过程及Michael加成反应过程中各因素的影响,研究结果表明,较好的制备条件是:负载46.5％KF/Al2O3;浸渍温度:65℃;浸渍溶剂:乙醇;表面活性剂:PEG6000和PEG400按摩尔比1:1混合使用;煅烧温度:400℃,此时获得的KF/Al2O3活性最高.当催化剂用量以F-计为0.03mol,反应原料丙二酸二乙酯与丙稀腈之比为3:1,反应时间为2 h,加成反应的转化率最高.
Nano solid base KF/A12O3 has been prepared by immersing nana γ-Al2O3 powder into KF solution and activating it. Its activity has been examined by acting as a catalyst to synthesize which is a Michael addition reaction. The effects of varied factors on catalyst preparation and Michael addition reaction have been analyzed by uniform design. The results of test show that the better reaction conditions are : 15mmol KF loading on 1g A12O3, immersing time: 3 h, immersing temperature: 65 ℃, surface active agent: PEG, calcining temperature: 400 ℃ , immersing solvent: ethanol. The size of nano solid base KF/Al2O3 attained under these conditions is less than 30 nm and the catalytic activity is the best. When the amount of catalyst is 0.03 mol (based on F-) and the molar ratio of acrylon to malonic ester is 1:3, the yield of Michael addition reaction was over 88% after 3 hours.
出处
《山东大学学报（理学版）》
CAS
CSCD
北大核心
2004年第3期88-91,共4页
Journal of Shandong University(Natural Science)
基金
江苏省自然科学基金资助项目(KB2003086)
