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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。
Ethanol was chosen as the derivatizing agent to decompose toluene dicarbamate into Toluene monoisocyanate (TMI), which is the intermediate of toluene diisocyanate (TDI) process, and the active group -NCO in TDI, Derivatives, by ethanol analysis of high performance liquid chromatography to achieve qualitative and quantitative analysis of TMI and TDI. High performance liquid chromatography conditions: mobile phase methanol - water (6: 4 by volume), flow rate 0.5mL / min, UV detection wavelength 254nm. The linear correlation coefficients of TDI and TMI ethanol derivatives were both greater than 0.999 and the relative standard deviations were all less than 1.0% at a certain concentration range. The method is accurate, simple and rapid, and can well meet the quantitative analysis of the reactants, intermediates and the target products in the toluene diisocyanate reaction system which is decomposed into tolylene dicarbamate and can also be used for the industrial production of toluene Isocyanate and toluene diisocyanate quantitative analysis.