有机硅改性聚乙二醇型聚氨酯固相微萃取涂层的制备及其性能研究  

Preparation and property research of silicone modified polyethylene glycol polyurethane solid Phasemicroextraction coating

作　　者：邹慧敏[1] 申书昌[1] 

机构地区：[1]齐齐哈尔大学分析测试中心,黑龙江齐齐哈尔161006

出　　处：《齐齐哈尔大学学报（自然科学版）》2016年第1期51-55,59,共6页Journal of Qiqihar University(Natural Science Edition)

基　　金：黑龙江省自然科学基金资助项目(B201101)

摘　　要：以2,4-甲苯二异氰酸酯、聚乙二醇和羟基硅油作为原料合成了有机硅改性聚乙二醇型聚氨酯,将此聚合物涂于石英纤维表面,经高温缩合反应,制成固相微萃取头。用改装的5μL微量注射器为手柄,与萃取头合成为固相微萃取装置。通过红外光谱法、热重法、扫描电子显微镜对涂层的分子结构、热稳定性及表面结构进行了分析。结果表明合成的有机硅改性聚乙二醇型聚氨酯涂层的分解温度为290℃,其涂层的表面平整,直径均匀;共聚物涂在纤维丝表面的厚度约为10μm并且涂层截面的硅元素分布离散并且均匀。利用固相微萃取-气相色谱联用技术对水中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯进行分析测定,色谱峰面积与浓度呈现良好线性关系,4种物质的线性相关系数(R^2)分别为0.995 8,0.996 8,0.997 7和0.997 1,最低检测限分别为0.065,0.078,0.087和0.093 mg/L。Silicone modified polyethylene glycol polyurethane was synthesized using 2,4- toluene diisocyanate, polyethylene glycol and hydroxy silicone oil as raw materials, the polymer was coated on the surface of quartz fiber, the solid phase micro extraction was prepared by high temperature condensation reaction. A solid phase micro extraction device was made by combining a modified 5μL micro syringe as the handle with extraction head. The molecular structure, thermal stability and surface structure of the coating were analyzed by IR, TG, and SEM. The results showed that the decomposition temperature of the silicone modified polyurethane coating was 290℃, The surface of the coating was smooth, uniform diameter; The thickness of coated copolymer fibre surface was about 10 gm, the silicon element of coating cross section distributed discrete and uniform, dimethyl phthalate, diethyl phthalate, dibutyl phthalate and dioctyl phthalate was determined by Solid phase microextraction coupled with gas chromatography, the chromatographic peak area and concentration showed a good linear relationship, The linear correlation coefficient （R2） of the four species were 0.995 8, 0.9968, 0.997 7, 0.997 l respectively and the minimum detection limit were 0.065, 0.078, 0.087, 0.093mg/L. respectively

关 键 词：固相微萃取涂层 有机硅改性聚乙二醇型聚氨酯 固相微萃取-气相色谱联用 邻苯二甲酸酯 

分 类 号：TQ323.8[化学工程—合成树脂塑料工业]