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以脂肪多胺四甲基乙二胺、五甲基二乙烯三胺、1,3-丙烷磺内酯为起始原料,经季铵化、酸化两步反应,合成了两种阳离子结构中具有双磺酸基官能团的Brφnsted酸功能化离子液体二(3-磺酸基)丁基四甲基乙二铵硫酸氢根盐、二(3-磺酸基)丁基五甲基乙二烯三铵硫酸氢根盐,离子液体的结构经红外光谱、核磁共振氢谱得到确认,以4-硝基苯胺为指示剂测定离子液体的Hammett酸函数,两种离子液体酸强度均高于硫酸。以合成的离子液体与1-丁基-3-甲基咪唑溴化物构成的二元离子液体体系为反应体系,应用于山梨醇与苯甲醛、对甲基苯甲醛、3,4-二甲基苯甲醛的缩合反应中,结果表明,当离子液体的摩尔分数为15%(以山梨醇计),n(山梨醇)∶n(醛)=1∶2.05,于70℃反应4 h时,反应即可在无溶剂均相反应条件下顺利完成,体系中加入水,目标化合物即可析出,分离产率77.6%~84.8%,产物熔距≤5℃,二元离子液体经旋蒸除水,乙醚洗涤、真空干燥后可循环使用,循环使用5次催化活性基本保持不变。
In the two-step reaction of quaternary ammonium and acidification, fatty polyamine tetramethylethylenediamine, pentamethyldiethylenetriamine and 1,3-propane sultone were used as starting materials to synthesize Brønsted acid functionalized ionic liquid bis (3-sulfonate) butyltetramethylethylammonium hydrogensulfate, bis (3-sulfonato) butylpentamethylpiperidine tris Ammonium bisulfate salt and ionic liquid were confirmed by IR and 1H NMR spectra. The Hammett acid function of ionic liquid was determined by 4-nitroaniline as indicator. The ionic strength of both ionic liquids were higher than that of sulfuric acid. The binary ionic liquid system composed of the synthesized ionic liquid and 1-butyl-3-methylimidazolium bromide is used as the reaction system and is used in the reaction system of sorbitol with benzaldehyde, p-methylbenzaldehyde, 3,4-dimethyl The results showed that when the mole fraction of ionic liquid was 15% (based on sorbitol), n (sorbitol): n (aldehyde) = 1: 2.05, reaction was carried out at 70 ℃ for 4 h, Can be successfully completed in the solvent-free homogeneous reaction conditions, the system was added water, the target compound can be precipitated, the separation yield of 77.6% to 84.8%, product melting ≤ 5 ℃, binary ionic liquid by rotary evaporation, Ether washing, vacuum drying can be recycled, recycling 5 times the catalytic activity remained unchanged.