The highly efficient separation of product mixtures in chemical synthesis is increasingly crucial for realizing sustainable chemical processes. Here, we report that large-volume monolithic silica with a well-defined cocontinuous porous structure brings significant benefits to liquid chromatography, satisfying both the enhanced efficiency and remarkable reduction of chromatographic wastes of solvent and solid separation media. Reusability of the monolithic silica column has been demonstrated by regeneration with an acid-flow washing, in which the cocontinuous porous structure of monolithic silica is well retained even in aqua regia in the regeneration process. The resolution of separation is comparable to preparative high-performance liquid chromatography, and the extremely low column back-pressure is suitable for open and flash columns. Moreover, a good correlation of the retention with conventional thin-layer chromatography and the high loading capacity up to 10 wt % are advantageous in overloading purification. Improved productivity with the large-volume monolithic silica has been confirmed in the practical purification of a low-solubility compound, 9-[4-(4,6-diphenyl-1,3,5-triazin-2-yl)phenyl]-N,N,N′,N′-tetraphenyl-9H-carbazole-3,6-diamine (DACT-II), for a highly efficient organic light-emitting diode. Reduction of solvent and solid consumption by 60 and 90%, respectively, with increased purities in each step of the total synthesis of DACT-II, has been demonstrated in comparison with purification with standard silica particles.

中文翻译：

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通过可重复使用的大体积整体硅胶柱显着减少液相色谱中的废物

化学合成中产品混合物的高效分离对于实现可持续化学过程越来越重要。在这里，我们报告说，具有明确的共连续多孔结构的大体积整体二氧化硅给液相色谱带来了显着的好处，既提高了效率，又显着减少了溶剂和固体分离介质的色谱废物。通过酸流洗涤再生，证明了整体式二氧化硅柱的可重复使用性，其中即使在再生过程中的王水中，整体式二氧化硅的共连续多孔结构也得到了很好的保留。分离分辨率可与制备型高效液相色谱相媲美，极低的柱背压适用于开放柱和闪蒸柱。此外，与传统薄层色谱保留的良好相关性和高达10 wt%的高负载容量有利于超载纯化。在低溶解度化合物 9-[4-(4,6-二苯基-1,3,5-三嗪-2-基)苯基]-的实际纯化中证实了大体积整体式二氧化硅提高了生产率N , N , N ', N '-四苯基-9 H-咔唑-3,6-二胺（DACT-II），用于高效有机发光二极管。与使用标准二氧化硅颗粒进行纯化相比，已证明在 DACT-II 全合成的每个步骤中，溶剂和固体消耗分别减少了 60% 和 90%，并且纯度增加。