Preparation of monolithic silica HPLC columns with truss-structured skeletons and embedded surfactant-templated mesopores

IF 2.3 4区材料科学 Q2 MATERIALS SCIENCE, CERAMICS Journal of Sol-Gel Science and Technology Pub Date : 2024-10-26 DOI:10.1007/s10971-024-06595-3

Takanori Detani, Kei Morisato, Masayoshi Ohira, Kazuki Nakanishi

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Abstract

Monolithic macro/mesoporous silica gels have been prepared via a sol-gel process using triblock copolymer Pluronic P123 (EO₂₀PO₇₀EO₂₀) as a structure-directing agent. In this synthesis, P123 not only induces phase separation to form macroporous structure but also acts as a supramolecular template to form mesopores with precisely controlled shape and size. Obtained was a monolithic silica composed of continuous truss-like columnar skeletons in which cylindrical mesopores are arranged in a 2D-hexagonal symmetry. These monolithic silica gels have extremely high porosity approaching 90% and exhibited high specific surface area and sharp pore size distribution as revealed by N₂ sorption measurements. Combinations of the initial composition and the post-gelation treatment on wet gels allowed the control of physical properties of meso- and macropore structures. The monolithic HPLC columns prepared using these silica gels surface-modified by ODS (octadecylsilyl) ligands gave as many as 140,000 theoretical plates/m for the separation of alkylbenzenes in a reversed-phase mode. Very weak dependence of height equivalent to theoretical plate, H, on the mobile phase velocity was also recognized in comparison with conventional particle-packed columns.

Graphical Abstract

SEM images of monolithic silica prepared with tetramethoxysilane (TMOS) and P123 composed of truss-structured continuous skeletons. The performance for HPLC separation medium was examined.

Abstract Image

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具有桁架骨架和嵌入表面活性剂模板介孔的整体硅胶高效液相色谱柱的制备

以三嵌段共聚物Pluronic P123 （EO20PO70EO20）为结构导向剂，采用溶胶-凝胶法制备了整体宏/介孔硅胶。在该合成中，P123不仅诱导相分离形成大孔结构，而且作为超分子模板形成具有精确控制形状和大小的介孔。获得的是由连续的桁架状柱状骨架组成的整体二氧化硅，其中圆柱形介孔以二维六边形对称排列。N2吸附测试结果表明，硅胶整体孔隙率高达90%，比表面积高，孔径分布明显。湿凝胶的初始组成和凝胶化后处理的组合可以控制介孔和大孔结构的物理性质。用ODS（十八烷基硅基）配体表面修饰的硅胶制备的整体高效液相色谱柱在反相模式下分离烷基苯的理论极板数高达14万/m。与传统的颗粒填充柱相比，还认识到与理论板等效高度H对流动相速度的依赖性非常弱。四甲基氧基硅烷（TMOS）和P123组成的桁架结构连续骨架制备的单片二氧化硅的sem图像。考察了其作为高效液相色谱分离介质的性能。

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来源期刊

Journal of Sol-Gel Science and Technology 工程技术-材料科学：硅酸盐

CiteScore

4.70

自引率

4.00%

发文量

280

审稿时长

2.1 months

期刊介绍： The primary objective of the Journal of Sol-Gel Science and Technology (JSST), the official journal of the International Sol-Gel Society, is to provide an international forum for the dissemination of scientific, technological, and general knowledge about materials processed by chemical nanotechnologies known as the "sol-gel" process. The materials of interest include gels, gel-derived glasses, ceramics in form of nano- and micro-powders, bulk, fibres, thin films and coatings as well as more recent materials such as hybrid organic-inorganic materials and composites. Such materials exhibit a wide range of optical, electronic, magnetic, chemical, environmental, and biomedical properties and functionalities. Methods for producing sol-gel-derived materials and the industrial uses of these materials are also of great interest.