柠檬酸酐的合成与表征  

Synthesis and characterization of citric acid anhydride

作　　者：金柱[1] 张军[1] 杨效益[1] 杨秀全[1] 周媛[1] 

机构地区：[1]中国日用化学工业研究院,山西太原030001

出　　处：《日用化学工业》2016年第4期212-215,共4页China Surfactant Detergent & Cosmetics

基　　金："十二五"国家科技支撑计划资助项目(2014BAE03B03);山西省青年科技研究基金资助项目(2014021015-6);"伽蓝"研究基金资助项目(JL005)

摘　　要：以无水柠檬酸和乙酸酐为原料合成柠檬酸酐,通过单因素试验利用滴定法考察投料摩尔比、反应温度以及溶剂用量对反应转化率和收率的影响。结果表明:反应温度为52℃,n(乙酸酐)∶n(无水柠檬酸)=1.2∶1,n(乙酸)∶n(无水柠檬酸)=1.0∶1,反应时间为1.5 h时,柠檬酸酐收率达88.8%。利用红外光谱、核磁共振氢谱和质谱表征了合成产物,证明其为五元环状柠檬酸酐。Citric acid anhydride was prepared in laboratory with anhydrous citric acid and acetic anhydride as starting materials. Effects of mole ratio of the reactants,reaction temperature and dosage of solvent on the conversion and the yield were investigated with titration method via single factor tests. Results indicated that the yield of citric acid anhydride is 88. 8% at the suitable conditions as reaction temperature 52 ℃,reaction time 1. 5 h,n（ acetic anhydride） ∶ n（ citric acid） = 1. 2 ∶ 1 and n（ acetic acid） ∶ n（ citric acid） = 1. 0 ∶ 1.Chemical structure of the product was characterized by FT- IR,1H NMR and MS,and the results of characterization showed that the product is a five member cyclo- anhydride.

关 键 词：柠檬酸酐 合成 滴定法 

分 类 号：TQ423[化学工程]