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Preparation of levulinic acid from hydrolysis of Salix psammophila catalyzed by acid and its separation and purification

GAO Xueyi,WU Yanwei,WANG Kebing   

  1. College of Science,Inner Mongolia Agricultural University,Huhhot 010018,Inner Mongolia,China
  • Online:2014-01-05 Published:2014-01-05

沙柳酸催化水解制备乙酰丙酸及分离提纯

高学艺,武彦伟,王克冰   

  1. 内蒙古农业大学理学院,内蒙古 呼和浩特010018

Abstract: Preparation of levulinic acid from hydrolysis of Salix psammophila catalyzed by sulfuric acid as catalyst was studied in this paper. The effects of catalyst concentration,reaction time,reaction temperature,liquid-solid ratio on the yield of levulinic acid were investigated. By orthogonal tests,the optimum hydrolysis reaction conditions were as follows:reaction temperature 200℃,reaction time 90 min,catalyst concentration 9%,liquid-solid ratio(mL∶g) 15∶1,the highest yield of levulinic acid was 18.80%,the order of the factors was obtained according to the degree to which they could affect hydrolysis reaction as follows:reaction time > catalytic concentration > reaction temperature > liquid-solid ratio. 335 weak basic anion-exchange resin was used for separation and purification of hydrolysis mixed solution,under the static conditions of adsorption temperature 35 ℃,amount of resin 15 g,eluent concentration (HCl) 0.5 mol/L,recovery of levulinic acid was 95.35%.

Key words: Salix psammophila, levulinic acid, anion-exchange resin, orthogonal tests, separation and purification

摘要: 以沙柳为原料,硫酸为催化剂,考察了催化剂浓度、反应时间、反应温度、液固比对沙柳水解制备乙酰丙酸得率的影响,通过正交实验方法得到最佳的水解反应条件为:反应温度200 ℃,反应时间90 min,催化剂质量分数9%,液固比(mL∶g)15∶1,乙酰丙酸的最高得率为18.80%;各因素对水解反应影响的大小顺序为:反应时间>催化剂浓度>反应温度>液固比。在静态条件下,用335弱碱性阴离子交换树脂对水解液进行分离提纯,在附吸温度为35 ℃、树脂投料量为15 g、盐酸洗脱剂浓度为0.5 mol/L时,乙酰丙酸的回收率为95.35%。

关键词: 沙柳, 乙酰丙酸, 阴离子交换树脂, 正交实验, 分离提纯

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