摘要
本文采用膦腈碱P2为催化剂对乙酸乙烯酯和蔗糖的酯交换反应进行研究。通过正交试验的方法,以多酯酯化率为优化目标,得到最佳反应条件:反应温度353K(80℃),n(蔗糖):n(醋酸乙烯酯)=1∶10,n(催化剂)∶n(蔗糖)=0.15∶1反应时间为10h。其多酯酯化率可达77.09%,八酯酯化率达40%。通过TLC、HPLC-MS-MS对其进行定性定量分析,柱色谱分离得到蔗糖八乙酯,并通过红外光谱和NMR确定蔗糖八乙酯结构,经柱色谱分离得到蔗糖八乙酯的含量与HPLC-MS-MS分析结果基本一致。因此,用HPLC-MS-MS检测方法可简单、快速测定蔗糖酯。
The transesterification of vinyl acetate with sucrose was studied using phosphazene base P2 as catalyst.The optimum reaction conditions were obtained through orthogonal experiment with the esterification rate of polyesters as the objective.The reaction temperature was 353K (80 ℃),n (sucrose)∶n (vinyl acetate)= 1∶10,n (catalyst)∶n (sucrose)= 0.15∶1,and the reaction time was 10 h.The structure of sucrose octaethyl ester was determined by infrared spectroscopy and NMR.The content of sucrose octaethyl ester obtained by column chromatography was consistent with the results of HPLC-MS-MS analysis. HPLC-MS-MS analysis can be used to determine sucrose esters easily and efficiently.
作者
李文娟
万洪维
吴世新
杜广芬
代斌
郭旭虹
Li Wenjuan;Wan Hongwei;Wu Shixin;Du Guangfen;Dai Bin;Guo Xuhong(School of Chemistry and Chemical Engineering/Key Laboratory for Green Processing of Chemical Engineering of Xinjiang Bingtuan/Key Laboratory of Materials-Oriented Chemical Engineering of Xinjiang Uygur Autonomous Region,Shihezi University,Shihezi,Xinjiang 832003,China)
出处
《石河子大学学报(自然科学版)》
CAS
北大核心
2019年第1期60-66,2,共7页
Journal of Shihezi University(Natural Science)
基金
石河子大学应用基础研究青年项目(2015ZRKXYQ03)