乙酰丙酸的清洁合成及络合萃取法分离制备

Clean synthesis of levulinic acid and its separation based on complexometric extraction

以Fe3+改性的ZSM-5X分子筛作催化剂,高温条件下利用生物质酶解糖液清洁合成平台化合物——乙酰丙酸,并以乙酰丙酸的产率为指标,应用响应面分析方法研究最佳的合成条件。以三辛胺(TOA)为萃取剂,正丁醇、磷酸三丁酯、仲辛醇等为溶剂进行萃取、水相反萃取、分离乙酰丙酸。合成实验结果表明,在催化剂质量为5 g,温度为200℃,反应时间为3.7 h条件下,乙酰丙酸的最大产率为42.76%。优化后的萃取条件为:选择V(正丁醇)/V(三辛胺)为99/1或V(磷酸三丁酯)/V(三辛胺)为99.5/0.5的萃取体系络合萃取乙酰丙酸,再用水相反萃取,可达到较好的分离效果。

Levulinic acid is cleanly synthesized via high temperature degradation of glucose in enzymatic hydrolysate using Fe3 ~ modified zeolite molecular sieve ZSM-SX as catalyst. The operation conditions for clean synthesis and separation of levulinic acid are optimized. The results show that when the dosage of catalyst is 5 g, reaction temperature is 200~C and reaction time is 3.7 hours ,the highest yield of levulinie acid is 42.76% （mass fraction）. The high efficiency and high selectivity for separating levulinie acid can be achieved by using extraction separation technique based on reversible chemical complexation under the following conditions：99：1 volumetric ratio of N-butyl alcohol and trioctylamine and 99. 5： O. 5 volumetric ratio of tributyl phosphate and trioctvlamine.