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建立利用大孔吸附树脂吸附法结合氯仿溶解法分离混合二元酸中丁二酸、戊二酸和己二酸的方法并使其分别达到一定的纯度和收率。首先利用LC-ESI-MS方法测定了混合二元酸中丁二酸、戊二酸和己二酸含量,然后通过对3种大孔吸附树脂AB-8、NKA-Ⅱ和D-380吸附性能的综合比较,筛选出AB-8大孔吸附树脂作为吸附剂,以水、10%、30%和95%乙醇水溶液作为洗脱剂对混合二元酸进行初步的分离,得到A、B、C和D4个分离部位,再利用氯仿对二元酸溶解度的不同,将该4个分离部位在55℃水浴恒温分别用氯仿进行溶解、过滤,通过LC-ESI-MS方法测定确定相应部位的组成情况后进行适当合并,最终达到将混合二元酸分离的目的。丁二酸纯度:70.3%,收率:92.7%;戊二酸纯度:94.1%,收率89.2%;己二酸纯度:90.7%,收率:88.7%。
A method for separating succinic acid, glutaric acid and adipic acid from mixed dibasic acids by using macroporous adsorption resin adsorption method and chloroform dissolution method was established and their purity and yield were respectively achieved. The contents of succinic acid, glutaric acid and adipic acid in the mixed dibasic acids were determined by LC-ESI-MS. The adsorption capacity of three macroporous resins AB-8, NKA-Ⅱ and D-380 Through comprehensive comparison, the AB-8 macroporous adsorption resin was screened as the adsorbent. The mixed dibasic acids were separated by water, 10%, 30% and 95% ethanol as eluents to get A, B, C and D4 separated parts, and then the use of chloroform on the different solubility of dibasic acid, the four parts were heated at 55 ℃ water bath was dissolved in chloroform, respectively, filtered, determined by LC-ESI-MS method to determine the composition of the corresponding parts of the situation The appropriate merger, and ultimately achieve the purpose of separation of mixed dibasic acid. Succinic acid purity: 70.3%, yield: 92.7%; glutaric acid purity: 94.1%, yield 89.2%; adipic acid purity: 90.7%, yield: 88.7%.