摘要
选用乙醇作为衍生剂,将甲苯二氨基甲酸甲酯分解制备甲苯二异氰酸酯(TDI)过程的中间产物甲苯单异氰酸酯(TMI)及最终产物TDI中的活泼基团-NCO进行封端保护,生成乙醇的衍生物,通过高效液相色谱对乙醇衍生物进行分析,实现了对TMI及TDI的定性及定量分析。高效液相色谱分析条件为:流动相甲醇-水(体积比6∶4),流速0.5mL/min,紫外光检测波长254nm。在一定的质量浓度范围内,TDI及TMI乙醇衍生物的线性相关系数均大于0.999,相对标准偏差均小于1.0%。本方法准确、简便、快速,能很好地满足甲苯二氨基甲酸甲酯分解合成甲苯二异氰酸酯反应系统中的反应物、中间产物以及目的产物的定量分析,也可用于工业TDI生产过程中甲苯单异氰酸酯及甲苯二异氰酸酯的定量分析。
In this paper, a simple and accurate high performance liquid chromatography （HPLC） analysis method for analyzing qualitatively and quantitatively the intermediate toluene mono-isocyanate （TMI） and desired product toluene diisocyanate （TDI） in the procedure of dimethyl toluene dicarbamate （TDC） decomposition to prepare TDI was established, in which the ethanol derivatives of TMI and TDI were determined. The optimal chromatography conditions are： methanol-water （6：4 by volume） as mobile phase, flow rate 0.5 mL/min, and detection wavelength 254 nrn. Under these conditions, the calibration curves of the ethanol derivatives of TD[ and TMI were all linear in certain range with correlation coefficients larger than 0. 999, the relative standard deviations were all less than 1.0%. The method can meet the requirements for the analysis of TDC, TMI and TDI in the reaction system of TDC decomposition to TDI, and also meet the analysis of TMI and TDI in the industrial process of synthesis TDI.
出处
《化学通报》
CAS
CSCD
北大核心
2013年第12期1120-1125,共6页
Chemistry
基金
国家自然科学基金项目(21236001)
河北省重大技术创新项目(12275603Z)
河北省自然科学基金项目(B2011202054)资助
关键词
乙醇衍生法
甲苯二异氰酸酯
甲苯二氨基甲酸甲酯
高效液相色谱
Ethanol derivative method, Toluene diisocyanate, Dimethyl Toluene dicarbamate, Highperformance liquid chromatography
