摘要
针对非光气氨基甲酸甲酯热解法制备4,4′-二苯甲烷二异氰酸酯(MDI)反应过程中异氰酸酯类产物无法定性、定量分析的技术难题,选用乙醇为衍生剂,利用高效液相色谱对中间产物4-(4′-苯氨基甲酸甲酯)苯甲烷异氰酸酯(MMI)及产物MDI的乙醇衍生物进行分析,成功建立了异氰酸酯类产物简单、快速、精确的高效液相色谱分析方法———乙醇衍生法。通过对产物进行熔点测定、元素分析、核磁共振氢谱、质谱等分析测试,证实分离所得样品即为高纯度的MMI及MDI乙醇衍生物。液相色谱条件为:流动相甲醇-水(体积比60∶40),流速1.2 mL/min,柱温30℃,紫外检测波长245 nm。在一定的质量浓度范围内,MMI及MDI乙醇衍生物纯品的线性相关系数均大于0.999 9,相对标准偏差均小于1.0%。
It was a big problem to qualitatively and quantitatively analyze the isocyanate products in the synthesis process of methylene-4,4′-di（phenylisocyanate）（MDI） by the non-phosgene route.A simple,rapid and accurate high performance liquid chromatographic method was established to qualitatively and quantitatively analyze the isocyanate products by means of analyzing their ethanol derivatives.Herein,the isocyanate products,the intermediate product methylene-4-（4′-methylphenyl-carbamate） phenylisocyanate（MMI） and the product MDI,were derived with ethanol.The derivative samples of MMI and MDI were separated with the chromatographic column,and analyzed and identified by melting point test,element analysis,1H nuclear magnetic resonance spectrometry and mass spectrometry.Results showed that the derivative samples were ethanol derivatives of MMI and MDI with high purity.Under the optimal conditions with mobile phase of methanol-water（60∶40,by volumn）,flow rate of 1.2 mL/min,temperature of 30 ℃,and detection wavelength of 245 nm,the calibration curves of MMI and MDI were linear in certain range with correlation coefficients more than 0.999 9.The relative standard deviations were less than 1.0%.The results indicated that the derivative method with ethanol was accurate.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第7期707-711,共5页
Journal of Instrumental Analysis
基金
国家科技支撑重大项目课题(2006BAC02A08)
中国科学院知识创新方向性项目课题(KGCX2-YW-215-2)
关键词
衍生法
高效液相色谱
4
4′-二苯甲烷二异氰酸酯
derivative method
high performance liquid chromatography
methylene-4
4′-di（phenylisocyanate）
