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机构地区:[1]三明学院化学与生物工程系 [2]苏州大学材料与化学化工学部,苏州215021
出 处:《应用化学》2008年第11期1320-1323,共4页Chinese Journal of Applied Chemistry
基 金:福建省自然科学基金计划资助项目(E0610025)
摘 要:用pH值为3.5~4.0的冰乙酸水溶液将硅烷偶联剂配制成所需浓度的溶液,对多孔SiO2表面进行硅烷化处理,在过量的氢溴酸和-10~0℃低温作用下,合成了带溴端基的活性膜/多孔SiO2复合体。用X射线光电子能谱、扫描电子显微镜表征了硅烷化后的表面结构,用红外光谱表征了复合体表面的溴端基,用X光荧光光谱测量其表面的溴含量,通过冷水洗涤和热水煮沸考察水对含溴量的影响。结果表明,复合体表面含有稳定结合活性膜结构,并且能在其端基接上溴基团,最高含溴质量分数达0.34%。水对复合体表面端基溴的洗脱量较大,热水对于溴的洗脱率比冷水大。先水洗再溴化的试样要比先溴化再水洗的试样含溴量高。经30 min的冷水洗涤或热水煮沸后,前者的含溴质量分数降至0.15%和0.13%,后者的含溴质量分数降至0.09%和0.03%。Porous silica surface was treated with hydrobromic acid in excess at a low temperature of - 10-0 ℃, in a solution of silane coupling agent of pH 3.5 ~ 4. 0 adjusted with acetic acid, and bromine-containing active film/silica composites were prepared. The surface structure was characterized with X-ray photoelectron spectroscopy and scanning electron microscopy. The bromine at the surface of the composite was characterized with infrared spectrum. The bromine contents were measured with fluorescent X-ray spectroscopy after cold water or boiling water treatment, respectively. An active film with stable structure was formed on the surface of the silica composite, onto which bromine was grafted with a mass concentration as high as 0.34%. The bromine content at the surface of the composite was found to decrease after washing with water and hot water was more effective than cold water. In addition, the samples treated by water and then bromine showed higher bromine contents than the ones treated by bromine and then water. After the composites were washed for 30 min by cold water or boiling water, the bromine content of the former decreased to 0.15% and 0.13% respectively, and the bromine content of the latter decreased to 0.09% and 0.03%, respectively.
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