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Optimized microwave-assisted functionalization and quantification of superficial amino groups on porous silicon nanostructured microparticles
Analytical Methods ( IF 2.7 ) Pub Date : 2020-12-29 , DOI: 10.1039/d0ay02083d Cándida Anahy Cisneros-Covarrubias 1, 2, 3, 4, 5 , Gabriela Palestino 1, 2, 3, 4, 5 , César F. A. Gómez-Durán 1, 2, 3, 4, 5 , Sergio Rosales-Mendoza 3, 4, 5, 6, 7 , María de Lourdes Betancourt-Mendiola 3, 4, 5, 6, 7
Analytical Methods ( IF 2.7 ) Pub Date : 2020-12-29 , DOI: 10.1039/d0ay02083d Cándida Anahy Cisneros-Covarrubias 1, 2, 3, 4, 5 , Gabriela Palestino 1, 2, 3, 4, 5 , César F. A. Gómez-Durán 1, 2, 3, 4, 5 , Sergio Rosales-Mendoza 3, 4, 5, 6, 7 , María de Lourdes Betancourt-Mendiola 3, 4, 5, 6, 7
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This work presents an optimized microwave (MW)-assisted method for the chemical functionalization of porous silicon particles (PSip). 3-(Aminopropyl)triethoxysilane (APTES) was grafted on previously stabilized PSip. The functionalization efficiency was studied and optimized in terms of reaction time (Rt) and reaction temperature (RT) using a central composite design (CCD). The effect of MW irradiation on the surface coverage was found to strongly depend on the PSip surface chemistry, Rt, RT, and percentage of APTES. Quantification of grafted amino groups was performed by the ninhydrin method (NHIM); confirming the results by thermogravimetric analysis (TGA). Reacting with 5% APTES solution at 95 °C for 26 min was the best functionalization conditions. The efficiency of PSip–APTES prepared under the optimized conditions was compared to those functionalized by the traditional method; MW irradiation increases by 39% the number of functional groups grafted onto the PSip surfaces with the additional benefit of having a drastic reduction in Rt.
中文翻译：
多孔硅纳米结构微粒的微波辅助功能化和表面氨基的优化定量
这项工作提出了一种优化的微波（MW）辅助方法，用于多孔硅颗粒（PSip）的化学功能化。将3-（氨基丙基）三乙氧基硅烷（APTES）接枝到先前稳定的PSip上。使用中央复合设计（CCD）研究并优化了反应时间（Rt）和反应温度（RT）的功能化效率。发现MW辐照对表面覆盖的影响在很大程度上取决于PSip表面化学性质，Rt，RT和APTES百分比。通过茚三酮方法（NHIM）进行接枝氨基的定量；通过热重分析（TGA）确认结果。与5％APTES溶液在95°C下反应26分钟是最佳的官能化条件。将在优化条件下制备的PSip-APTES的效率与通过传统方法功能化的PSip-APTES的效率进行了比较；MW辐射使接枝到PSip表面的官能团数量增加了39％，具有Rt大大降低的额外好处。
更新日期：2021-01-14
中文翻译：
多孔硅纳米结构微粒的微波辅助功能化和表面氨基的优化定量
这项工作提出了一种优化的微波（MW）辅助方法，用于多孔硅颗粒（PSip）的化学功能化。将3-（氨基丙基）三乙氧基硅烷（APTES）接枝到先前稳定的PSip上。使用中央复合设计（CCD）研究并优化了反应时间（Rt）和反应温度（RT）的功能化效率。发现MW辐照对表面覆盖的影响在很大程度上取决于PSip表面化学性质，Rt，RT和APTES百分比。通过茚三酮方法（NHIM）进行接枝氨基的定量；通过热重分析（TGA）确认结果。与5％APTES溶液在95°C下反应26分钟是最佳的官能化条件。将在优化条件下制备的PSip-APTES的效率与通过传统方法功能化的PSip-APTES的效率进行了比较；MW辐射使接枝到PSip表面的官能团数量增加了39％，具有Rt大大降低的额外好处。
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