硅胶表面季铵功能化接枝过程的^(29)Si CP/MS NMR和XPS法研究

Determination of Synthesis of Silica-Based Quaternary Ammonium Material Using ^(29)Si CP/MS NMR and XPS

本工作采用29Si CP/MS NMR和XPS测试方法对硅胶表面接枝季铵功能基团的过程和机理进行了分析。XPS光谱分析结果表明,硅基季铵化产品的XPS谱中含有Si、O、C、N元素,并出现了以R4N+形式存在的401.26eV结合能峰,表明硅胶表面已被季铵化。TGA-DTA分析其接枝率为0.46mmol/g,同时,本工作采用29Si CP/MS NMR法对接枝机理进行探索研究,得出了接枝的可能反应途径和产品分子结构。

The synthesis of silica-based quaternary ammonium material was investigated by using 29Si CP/MS NMR and XPS. The XPS wide scan spectra dominate by the C 1s and N 1s, except for Si 2s, 2p and O 1s, the N 1s core-level spectrum is curve-fitted with peak signals about 401.26 eV, attributable to the R4N＋, which indicates quaternary ammonium is bonded onto surface of silica gel. The grafting yield is about 0.46 mmol/g by TGA-DTA analysis. Forming mechanism of grafting was investigated by 29Si MAS/CP, the structural and reaction route were obtained.