采用正硅酸乙脂(TEOS)为硅源,以十六烷基三甲基溴化铵(CTAB)为结构模板剂,用三甲氧基苯基硅烷(TMPS)作偶联剂,在碱性介质中合成苯基修饰MCM-41(Phenyl-MCM-41),对比研究了合成方法和脱模方式。结果表明,在分步合成法中,采用酸萃取脱模方式不仅可除去表面活性剂模板剂,而且MCM-41表面的Si-OH反应活性较高,有利于提高键合量;室温条件下,采用TEOS和TMPS共水解缩聚一步直接合成Phenyl-MCM-41,可进一步提高有机键合量,且高键合量的介孔复合体具有高的热稳定性和很强的疏水性。以Phenyl-MCM-41作为固相微萃取(SPME)的吸附涂层材料,与HPLC联用,考察了对水样中邻苯二甲酸酯的吸附分离性质及其在黄河水样中的分析应用,该法具有操作简单、吸附速度快、线性范围宽和灵敏度高的特点。
This paper describes a lab-scale experiment on synthesis of phenyl functionalized MCM-41 ( Phenyl-MCM-41) in an alkaline medium, which is related to tetraethyl orthosilicate ( TEOS) used as a silica source, trimethoxyphenylsiliane ( TMPS) as a silanized reagent in the presence of cetyltrimethylammonium bromide (CTAB). Method of step -by -step synthesis of Phenyl-MCM-41 is compared with that of template removal and it has been found that acid extraction is not only able to remove the template but promotes in...