浙江化工
浙江化工
절강화공
ZHEJIANG CHEMICAL INDUSTRY
2014年
11期
22-25
,共4页
离子液体%甲基丙烯醛%Mannich反应
離子液體%甲基丙烯醛%Mannich反應
리자액체%갑기병희철%Mannich반응
ionic liquid%methacrolein%Mannich reaction
合成了1-甲基咪唑醋酸([Mim]Ac)质子型离子液体,对其进行了1H NMR和IR表征。以[Mim]Ac为催化剂,甲醛、丙醛、二乙胺为原料,通过Mannich反应制备了甲基丙烯醛。考察了原料投料比、[Mim]Ac用量、Mannich反应温度和反应时间等因素对甲基丙烯醛收率的影响。研究结果表明,当甲醛、丙醛和二乙胺的摩尔比为1.1:1.0:1.0,[Mim]Ac用量(物质的量)为丙醛的10.0%,Mannich反应温度为45℃,反应时间为50 min,分解反应温度为75℃,甲基丙烯醛的收率为95.3%,并对产物进行了1H NMR表征。同时,对[Mim]Ac质子型离子液体催化Mannich反应的机理进行了初步研究。
閤成瞭1-甲基咪唑醋痠([Mim]Ac)質子型離子液體,對其進行瞭1H NMR和IR錶徵。以[Mim]Ac為催化劑,甲醛、丙醛、二乙胺為原料,通過Mannich反應製備瞭甲基丙烯醛。攷察瞭原料投料比、[Mim]Ac用量、Mannich反應溫度和反應時間等因素對甲基丙烯醛收率的影響。研究結果錶明,噹甲醛、丙醛和二乙胺的摩爾比為1.1:1.0:1.0,[Mim]Ac用量(物質的量)為丙醛的10.0%,Mannich反應溫度為45℃,反應時間為50 min,分解反應溫度為75℃,甲基丙烯醛的收率為95.3%,併對產物進行瞭1H NMR錶徵。同時,對[Mim]Ac質子型離子液體催化Mannich反應的機理進行瞭初步研究。
합성료1-갑기미서작산([Mim]Ac)질자형리자액체,대기진행료1H NMR화IR표정。이[Mim]Ac위최화제,갑철、병철、이을알위원료,통과Mannich반응제비료갑기병희철。고찰료원료투료비、[Mim]Ac용량、Mannich반응온도화반응시간등인소대갑기병희철수솔적영향。연구결과표명,당갑철、병철화이을알적마이비위1.1:1.0:1.0,[Mim]Ac용량(물질적량)위병철적10.0%,Mannich반응온도위45℃,반응시간위50 min,분해반응온도위75℃,갑기병희철적수솔위95.3%,병대산물진행료1H NMR표정。동시,대[Mim]Ac질자형리자액체최화Mannich반응적궤리진행료초보연구。
1-Methylimidazolium acetate ([Mim]Ac) protic ionic liquid was prepared, and its structure was confirmed by 1H NMR and IR. Methacrolein was prepared through Mannich reaction of formaldehyde, propionaldehyde, and diethyl amine with [Mim]Ac as the catalyst. The influences of molar ratio of reactants, amount of catalyst, Mannich reaction temperature and reaction time were investigated. The proper reaction conditions were as follows: the molar ratio of formaldehyde to propionaldehyde to diethyl amine was 1.1:1.0:1.0, amount of [Mim]Ac was 10.0% (relative to propionaldehyde), Mannich reaction temperature was 45 ℃, reaction time was 50 min, decomposition temperature was 75 ℃, the yield of methacrolein was 95.3%. The structure of methacrolein was confirmed by 1H NMR. A preliminary study was carried out on the Mannich reaction mechanism catalyzed by [Mim]Ac.