以离子液体为酸性催化剂,对天然产物大豆异黄酮糖苷在正丁醇溶剂中的醇解反应进行了研究。对离子液体的种类及用量、催化反应时间、温度等工艺条件进行了优化。确定最适宜的工艺条件是:采用[BIM]HSO4离子液体为催化剂,用量为0036g·mL^-1;反应温度为(104±1)℃,反应时间为100min。在此条件下,三种异黄酮糖苷的转化率均接近100%;另外,离子液体催化剂的稳定性测试结果表明,离子液体经3次循环使用,活性未见明显变化。采用浸渍法将离子液体固定化后用于催化醇解反应,结果表明,该固定化离子液体在首次使用时也具有较高催化活性,但稳定性差,难以重复使用,有必要进一步研究固定化离子液体的方法。
The alcoholysis of soybean isoflavones in the solvent of butanol using acidic ionic liquids as catalysts was studied. The effects of operation conditions, such as the kind and the amount of ionic liquid, reaction time, and reaction temperature were investigated. Results show that the optimal reaction conditions are: [BIM]HSO4 with amount of 0.036 g·mL^-1 as catalyst, reaction temperature (104±1)℃, reactS.on time 100 min. Under such optimized conditions, the conversions of the three kinds of isoflavon glycosides are all up to 100%; and the ionic liquid could be recycled at least three times without obvious deactivation. Additionally, the experiments of the ionic liquid immobilizing [BIM]HSO4 on silica support by impregnation method and using it to catalyze the soybean isoflavones alcoholysis were conducted. Results show that the immobilized ionic liquid exhibits good activity to alcoholysis reaction during the first use. However, the activity decreased seriously when being reused. Therefore, a further investigation on the immobilization method of ionic liquid is extremely needed.