聚氨酯固化剂中游离HDI气相色谱分析.pdfVIP

全国中文核心期刊 中国科技核心期刊 聚氨酯固化剂中游离HDI 气相色谱分析 张鑫芳，张心亚，何勇，陈焕钦 （华南理工大学化学与化工学院，广东 广州 510640） 摘要：以DB1701P 毛细管柱为分析柱，十四烷为内标物，建立了一套用于聚氨酯固化剂中游离六亚甲基二异氰酸酯（HDI）检测 的气相色谱条件。通过对进样温度、气化室程序升温进行选择，分别对低浓度游离HDI 样品（已知样品N75）和高浓度游离HDI 样品 （实验室制HDI 缩二脲未知样）进行分析。实验结果得到已知样品变异系数为6.48% ，未知样品变异系数为1.77%；同时对合成反应 过程中的高游离HDI 的检测也有很好的准确度和重现性。表明该方法既适用于检测聚氨酯固化剂产品中的低浓度（0.1%～2.0%）游 离HDI 含量，也适用于跟踪反应过程中高浓度（30%～90%）游离HDI 含量变化，对于确定合成反应的终点和检测HDI 缩二脲产品性 能具有重要意义。 关键词：聚氨酯；异氰酸酯；游离HDI ；气相色谱分析 中图分类号：TQ016.1 文献标识码：A 文章编号：1001-702X （2011）10-0040-05 Determination of free HDI content in polyurethane curing agent by gas chromatography ZHANG Xinfang ，ZHANG Xinya ，HE Yong ，CHEN Huanqin （School of Chemistry and Chemical Engineering ，South China University of Technology ，Guangzhou 510640 ，Guangdong，China） Abstract ：A method to determine unreacted hexamethylene diisocyanate （HDI） content in polyurethane curing agent was established by gas chromatography with DB1701P capillary column and tetradecane as the internal standard. Through the choice of the injection temperature and vaporizer temperature program ，HDI samples in low concentration range （with known sample N75）and HDI samples in high concentration range （unknown sample prepared in lab with HDI biuret）were analyzed. The coefficients of variation of the known sample and unknown sample were 6.48% and 1.77% ，respectively ；and detection of high free HDI during the synthesis reaction also had good accuracy and reproducibility. The experimental results show this method can not only determine the content of free HDI with low concentration （0.1%～2.0%）in the polyurethane curing agent ，but also track the content variation