单分散介孔二氧化硅微球的制备

Synthesis of monodisperse mesoporous silica microsphere

在Stober方法基础上制备了单分散二氧化硅微球,系统研究了反应条件对成球粒径以及单分散性的影响。通过多种测试手段,发现随着正硅酸乙酯和氨水浓度的提高,成球的粒径逐渐增大;而温度的提高会促使氨水挥发而使得成球的粒径降低;反应时间在反应初期对成球粒径的影响很大,然后逐渐趋于平缓。经对煅烧前后产物的小角X射线衍射对比分析,发现煅烧后产物的峰强度增加,并且重叠峰向右漂移,指示表面活性剂分子从孔中移除并发生了孔径收缩现象,同时发现不同反应条件对产物的织构性质有一定的影响。研究了相关的反应机理,认为在碱性条件下二氧化硅微球由正硅酸乙酯的水解和缩聚两步过程完成的,该方法为制备单分散介孔二氧化硅微球提供了一种简单有效的并且可重复的路径,从而可能用于大批量生产。

Modified Stober method was used to prepare monodisperse mesoporous silica microsphere by two-step reaction including hydrolysis and condensation of tetraethyl orthosilicate（TEOS）with ammonia as catalyst.Effects of the reaction parameters on the size and mono-disperse of the microsphere were discussed based on many characterization tests.Results showed： the microsphere size increased with the increment of ammonia and TEOS concentrations while decreased at higher temperature due to the evaporation of ammonia;effects of the reaction time on the particle distribution existed mainly in the initial stage,then got smooth gradually.The comparison of small angle X ray analysis suggested that peak intensity of silica microsphere increased and the overlapping peaks drifted rightward after calcination,indicating that the surfactant molecules were removed from the hole and the aperture shrank at the same time.In addition,the texture of the product was affected by reaction conditions to some extent.The mechanism study revealed the formation of silica microsphere was achieved through TEOS hydrolysis and polycondensation two steps successively.This is a simple,effective and repeatable method,which may be used for mass production,for the preparation of mono-dispersed mesoporous silica microspheres.