六亚甲基-1,6-二氨基甲酸酯热解产物的HPLC分析  

HPLC analysis of pyrolysis products of Hexamethylene-1,6-butylcarbamate

作　　者：刘喆[1,2] 王庆印[2] 姚洁[2] 陈学君[2] 张华[2] 胡静[2] 王公应[2] 

机构地区：[1]中国科学院大学,北京100049 [2]中国科学院成都有机化学研究所,四川成都610041

出　　处：《化学研究与应用》2016年第5期623-628,共6页Chemical Research and Application

基　　金：中国科学院"西部之光"人才培养计划-西部博士项目(20130910)资助

摘　　要：建立了六亚甲基-1,6-二氨基甲酸酯热分解产物的HPLC分析方法。以N-甲基苯胺为衍生剂;采用Waters Xbridge C18(4.6 mm×150 mm,5μm)色谱柱,以V_(乙腈)∶V_水=4∶6为流动相,流速1.0 m L·min^(-1);柱温40℃;检测波长205 nm;进样体积10μL。在此条件下,HDI衍生物、六亚甲基-6-氨基甲酸丁酯-1-异氰酸酯(HDUI)衍生物和六亚甲基-1,6-二氨基甲酸丁酯(HDU-B)分离度良好,在测定范围内具有良好的线性关系(r>0.999)、准确性、精密度和重复性。该法可用于热解氨基甲酸酯合成HDI过程中原料HDU-B、热解产物HDUI和HDI的含量分析,操作简单快速。A method for determinating the content ofpyrolysis products of Hexamethylene-1,6-butylcarbamateby HPLC was estab-lished. A derived method,which applied N-methyl aniline as the derivative,and Waters-Xbridge C18(4. 6mm×150mm,5μm)col-umn was used in this study. The mobile phase was a two mixture phase consist of acetonitrile and water(4:6). The flow rate was set as 1. 0 mL·min-1 ,the column temperature was 40 ℃,the detection wavelength was 205nm and the injection volume was 10 μL. This method exhibited good linearity(correlation coefficients r>0. 999)in the detection range,excellent precision and high stability. With the desirable specificity,sensitivity and repeatability,this method can be used to determine the content of HDU-B,hexamethyl-ene-6-carbamic acid butyl ester-1-isocyanate( HDUI) and HDI.

关 键 词：六亚甲基-1 6-二异氰酸酯 衍生 HPLC 

分 类 号：O657.7[理学—分析化学]