无溶剂微波辐射下Bronsted酸性离子液体催化合成系列乳酸酯.pdf

石油化工
PETROCHEMICAL TECHNOLOGY
2010年第39卷第3期
无溶剂微波辐射下 Bronsted酸性离子液体
催化合成系列乳酸酯
李心忠,林棋
(闽江学院化学与化学工程系,福建福州350!08)
摘要:以N-甲某咪呼、此啶和苄基氯等为原料合成了4种B3r6 asked酸性离子液体一-1ー基-3-卬基咪唑硫酸氢盐、1-苄
基-3-基昧嘩磷酸狐盐、N-*基吡啶硫酸氢盐和N-菜甚吡啶磷酸二氧盐,它们溶于水、乙醇、不溶于乙醚、乙酸乙確等非
极性有机溶剂,甜度分州为2.630,6,430,2.750,6.370Pa?s(28),含水量(质量分数)分别为3.1%、,3.4%,3,5%,3.8%。以
这4利离子液体作为锉化剂和反应介质,考察了乳酸与直链脂醇、环已醇、苯甲醇在兀溶剂、徴波編射条們下的 Fischer酯化反
应、実验结果表明,当n(乳酸):n(嘛):n、离予液体)=1:1:0.5、反应时间20~35min、80~120℃时,酯化率为81.4%?
97.1%、乳酸酯的收率为74.3%~88.8%。离子液体经ザ生説水后可环使用,循环使3次后,催化活性基不保持不恋
关键词] Brinsted酸性离子液体催化剂;徽波射;无浴剂合成;乳酸;乳酸;醇
文章编号]1000-8144(2(010)03-0262-07
中图分类号:7TQ426.99
文献标识码」A
Solvent-free Synthesis of a Series of Lactates with
Novel Brinsted Acidic Tonic Liquids as Catalysts Under Microwave Irradiation
Li Xinzhong, Lin Qi
Department of Chemistry and Chemical Engineering, Minjiang University, Fuzhou Fujian 35010R, Chi
Abstract Four Bronsted acidic ionic liquids(BALS), namely 1-benzyl-3-methylimidazolium
hydrogen sulfate, 1-benzyl-3-methylimidazolium hydrogen phosphate, N-benzyl pyridinium hydrogen
sulfate and N-benzyl pyridinium hydrogen phosphate, were synthesized from N-methylimidazole
pyridine, benzyl chloride etc.. These BALLS are soluble in both water and alcohol but insoluble in
non-polar organic solvents such as cthyl ether and ethyl acetate. Their viscosities are 2,630, 6.430,
2. 750 and 6. 370 Pa s(28), respectively. And their water mass fractions are 3. 1%, 3.4%
3.5% and 3.8%, respectively. With the BAILS as reaction media and catalysts, Fischer esterifications
of lactic acid with straight chain aliphatic alcohols, cyclohexanol and benzyl alcohol with solvent-free
under microwave irradiation were studied. Under the conditions of n(lactic acid): n(alcohol)
BALLS) 1: 1: 0.5, reaction time 20-35 min, 80-120 t and microwave irradiation,
esterification rates and lactate yields in the Fischer esterification were 81.4%-97 I% and 74.3
88.8%o, respectively. The BALS could be recovered easily and recycled three times without any
significant loss in catalytic activity
Keywords Bronsted acidic ionic liquid catalyst microwave irradiation; solvent-free synthesis
lactate, lactic acid. alcohol
乳酸酯是一种州途广泛的精细化学品3,具、达到1.16Mr3,存在着一个巨大的需求市场。目
有溶解能力强、不挥发、无毒可生物降解等特点,可替前工业上乳酸酯的主要生产方法是以无机酸、固体
代近70%的石油基有机溶剂,同时它可作为香料、食
品、饮料的添加剂以及本氧丙酸类除草剂合成的中间「收稿目期】200-10-0:!修改稿日期1200-09
体;尤其是当前为应对日益枯竭的石油资源,由乳酸
L作者筒介李心忠(197ー),男、辽宁省沈開市人:博土?井帅,电
话13205900895、电郎BAI_Wl@63.com
酯脱氢制备闪烯酸鮨已成为一条替代石油路线的最[基金项目]」福建省自然科学基金资助项日(20R4);福建省教
佳途径4。预计我国2010年丙烯酸(酯)的需求最将育厅科研頭目(J1A09189):闽江学院科研局动项目(YKQ805)e