改性聚氨酯固相微萃取吸附材料的合成及光谱分析

The synthesis and spectral analysis of solid-phase microextraction adsorbent material with polyurethane modified

以羟基硅油、甲苯-2,4-二异氰酸酯(TDI)、聚己二酸乙二醇酯和1,6-己二醇为原料,以辛酸亚锡为催化剂,环己酮为溶剂,合成了有机硅-聚氨酯聚合物固相微萃取吸附材料。采用红外光谱法对聚合产物进行了结构表征。建立了分光光度法测定有机硅-聚氨酯共聚物中游离异氰酸酯基(NCO)含量的定量分析方法,吸光度与异氰酸基含量呈线性关系,相关系数为R2=0.9996。该方法相对标准偏差小于5%,回收率为99.4%～105%。考察了显色剂用量、体系的酸度、显色时间等因素对NCO测定结果的影响。

In this paper,silicone-polyuretheane copolymer was synthesized by toluene-2,4-discar-nate（TDI）,polyethylene glycol ester adipic acid,1,6-hexanediol and hydroxy silicone oil as raw materials,stannous octoate as catalyst and cyclohexanone as solvent.The structure of polymerization product was characterized by Infrared spectrum.Furthermore,the method of quantitative analysis of free isocyanate-group in the silicone-polyuretheane copolymer by spectrophotometry was found.Absorbency and the content of isocyanate-group in a linear relationship,the related coefficient R2=0.999 6.The relative standard deviation of this method less than 5% and coefficient of recovery was between 99.4% and 105.0%.Investigated visualization reagent dosage,acidity of the system,chromogenic time and other factors to the effet of the determination results of isocyanate-groups.