{"title":"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","authors":"Takanori Detani, Kei Morisato, Masayoshi Ohira, Kazuki Nakanishi","doi":"10.1007/s10971-024-06595-3","DOIUrl":null,"url":null,"abstract":"<div><p>Monolithic macro/mesoporous silica gels have been prepared via a sol-gel process using triblock copolymer Pluronic P123 (EO<sub>20</sub>PO<sub>70</sub>EO<sub>20</sub>) 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 N<sub>2</sub> 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, <i>H,</i> on the mobile phase velocity was also recognized in comparison with conventional particle-packed columns.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><img></picture></div><div><p>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.</p></div></div></figure></div></div>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":"113 1","pages":"63 - 69"},"PeriodicalIF":2.3000,"publicationDate":"2024-10-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10971-024-06595-3.pdf","citationCount":"0","resultStr":"{\"title\":\"Preparation of monolithic silica HPLC columns with truss-structured skeletons and embedded surfactant-templated mesopores\",\"authors\":\"Takanori Detani, Kei Morisato, Masayoshi Ohira, Kazuki Nakanishi\",\"doi\":\"10.1007/s10971-024-06595-3\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>Monolithic macro/mesoporous silica gels have been prepared via a sol-gel process using triblock copolymer Pluronic P123 (EO<sub>20</sub>PO<sub>70</sub>EO<sub>20</sub>) 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 N<sub>2</sub> 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, <i>H,</i> on the mobile phase velocity was also recognized in comparison with conventional particle-packed columns.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><img></picture></div><div><p>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.</p></div></div></figure></div></div>\",\"PeriodicalId\":664,\"journal\":{\"name\":\"Journal of Sol-Gel Science and Technology\",\"volume\":\"113 1\",\"pages\":\"63 - 69\"},\"PeriodicalIF\":2.3000,\"publicationDate\":\"2024-10-26\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://link.springer.com/content/pdf/10.1007/s10971-024-06595-3.pdf\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Sol-Gel Science and Technology\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://link.springer.com/article/10.1007/s10971-024-06595-3\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"MATERIALS SCIENCE, CERAMICS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Sol-Gel Science and Technology","FirstCategoryId":"88","ListUrlMain":"https://link.springer.com/article/10.1007/s10971-024-06595-3","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"MATERIALS SCIENCE, CERAMICS","Score":null,"Total":0}
Preparation of monolithic silica HPLC columns with truss-structured skeletons and embedded surfactant-templated mesopores
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.
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.
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