3-甲基-2-氧代丁酸的分离提纯工艺研究

Study on the Processes of Separating and Purifying 3-Methyl-2-Oxobutanoic Acid

以3-甲基-2-氧代丁酸的收率及纯度为目标函数,对三种分离以3-甲基-2-氧代丁酰甲酯水解所得到的3-甲基-2-氧代丁酸的工艺进行了对比实验,确定了较为经济的分离工艺,采用单因素实验与正交试验优化了分离提纯的工艺条件,先将3-甲基-2-氧代丁酰甲酯在碱性条件下的水解液直接用盐酸酸化,选择合适的有机溶剂萃取,减压浓缩得到3-甲基-2-氧代丁酸粗品,将粗品再进行分子蒸馏精制,得到纯度不小于98%的精品3-甲基-2-氧代丁酸晶体(温度<10℃)。

The process optimizes the technique of separating and purifying with single factor experiments and orthogonal tests by taking the Recovery and rate of purity of 3-Methyl-2-Oxobutanoic Acid as its target function,and by comparing three techniques of separating 3-Methyl-2-Oxobutanoic Acid from the hydrolytic solution of 3-Methyl-2-Oxo-Butyryl ester.It first acidates the hydrolytic solution of 3-Methyl-2-Oxo-butyryl ester under alkaline condition with hydrochloric acid,then extracts proper organic solution,decompresses and concentrates that to get raw 3-Methyl-2-Oxobutanoic Acid,and finally get excellent 3-Methyl-2-Oxobutanoic Acid crystal with a rate of purity no less than 98% under the temperature of 10 ℃ by molecular distillation.