三氯化铁催化山梨糖醇醚化反应的研究

Study on Etherification of Sorbitol Catalyzed by Ferric Chloride

以山梨糖醇为原料,六水合三氯化铁(FeCl_(3)·6H_(2)O)为催化剂,采用跟踪测定产物羟值的办法,研究了山梨糖醇醚化反应的失水规律。考察了制备方法、FeCl_(3)·6H_(2)O的用量以及反应温度对山梨糖醇醚化反应的影响,并采用傅里叶变换红外光谱法(FTIR)和气-质联用(GC-MS)技术,对山梨糖醇醚化产物的结构进行了分析。结果表明,FeCl_(3)·6H_(2)O对山梨糖醇的醚化失水反应具有良好的催化效果,当添加量为0.6%~0.8%、反应温度为140~150℃、真空度在-0.1MPa左右、反应时间为2~3h时,可将醚化产物的羟值控制在1300~1360 mgKOH·g-1范围内。

Applied sorbitol as raw material,ferric chloride(FeCl_(3)·6H_(2)O)as a catalyst,the method of tracking the hydroxyl value of the product was used to study the etherification performance of D-sorbitol.The influences of the reaction system environment,the concentration of the catalyst,and the reaction temperature on the hydroxyl value of sorbitol were investigated.In addition,the sorbitol and etherification products were analyzed by Fourier transform infrared spectroscopy(FTIR)and gas chromatography-mass spectrometer(GC-MS).The experimental results showed that the hydroxyl value of sorbitol could be controlled at range of 1300~1360 mgKOH/g after 2~3h reaction when the amount of FeCl_(3)·6H_(2)O was 0.6%~0.8%of the system,the reaction temperature was kept 140~150℃,and the generated water was removed in a timely manner to maintain a degree of vacuum of the system at−0.1MPa.