Preparation and use of pore diameter controllable mesoporous silicon dioxide microsphere

A technology of mesoporous silica and silica gel microspheres, which is applied in the direction of silica, silica, etc., can solve problems such as application limitations, and achieve the effect of uniform particle size and easy preparation

Inactive Publication Date: 2009-04-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to solve this problem, three-stage polymers with a molecular weight of 2000 and above, such as Pluronic P123 (EO20-PO70-EO20), Pluronic F127 (EO106PO70EO106), etc., are currently used as templates to directly synthesize mesoporous materials with large pores. Non-ionic three-stage polymers play an important role in the preparation of large-diameter mesoporous silica spheres, but the particle size distribution of microspheres prepared with them is too wide, and their application in the field of chromatography is also limited to a certain extent.

Method used

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  • Preparation and use of pore diameter controllable mesoporous silicon dioxide microsphere
  • Preparation and use of pore diameter controllable mesoporous silicon dioxide microsphere
  • Preparation and use of pore diameter controllable mesoporous silicon dioxide microsphere

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Step (1) Add 10g of polyether amine with an average molecular weight of 4000, 1.1g of epichlorohydrin, and 25g of absolute ethanol in a 50ml round bottom flask, stir at room temperature for 12 to 24 hours, evaporate the solvent and excess Reactant.

[0044] Step (2) Dissolve the product obtained in step 1 in 25g of absolute ethanol, add 0.70g of trimethylamine alcohol solution, react at 80-85°C for 12-24 hours, evaporate the solvent under reduced pressure, and obtain a colorless or light yellow viscous The thick product is the new four-headed quaternary ammonium salt cationic surfactant 1.

Embodiment 2

[0046] In embodiment 1 step (1), the polyetheramine that 10g average molecular weight is 4000 is replaced by the polyetheramine that average molecular weight is 2000, and 1.1g epichlorohydrin is replaced by 0.55g epichlorohydrin, in embodiment 1 In step (2), the 0.70g trimethylammonium alcohol solution is replaced by 0.35g trimethylammonium alcohol solution, and other steps are all operated according to Example 1, and the obtained colorless or light yellow sticky substance is the surface of the new four-headed quaternary ammonium salt cation. active agent 2.

[0047] figure 1 It is a schematic diagram of the chemical structure of novel four-headed quaternary ammonium salt cationic surfactants 1 and 2.

[0048] (2) Preparation of mesoporous silica microspheres

Embodiment 3

[0050] Step (1) Add 0.50g of surfactant 1, 32g of anhydrous methanol, and 40g of deionized water into a 100ml round bottom flask and stir at 35°C for 20 minutes. After the solution is transparent, add 0.05ml of ammonia and 2.5g of normal Methyl silicate, stop stirring after the solution is turbid, let it stand for 3 hours, filter, wash with anhydrous methanol for 2 to 4 times, and dry at room temperature.

[0051] Step (2) Add 1 g of the obtained solid to 50 ml of deionized water, place it in an autoclave lined with polytetrafluoroethylene, let it stand at 55 ° C for 24 hours, filter it after cooling, and wash it with deionized water for 2 to 3 times , dried at room temperature, and then placed in a muffle furnace at 30-500°C for 2 hours, and then calcined at 500°C for 4 hours to obtain a white powder.

[0052] After scanning electron microscope analysis, the measured particle size is 1 μm. Use N 2 The adsorption and desorption instrument was used for analysis, and the avera...

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Abstract

The invention discloses a method for preparing a mesoporous silicon dioxide microsphere with controllable aperture. The method takes a novel tetra-quaternary ammonium salt cation surface active agent as a structure-directing agent and synthesizes the mesoporous silicon dioxide microsphere in an ethanol water system under the alkaline condition by a sol-gel method. The method has the advantages that the prepared silicon dioxide is micron spherical particles and has good monodispersion and large specific surface area; the mesoporous microsphere with large aperture can be prepared without an expanding agent; and the silicon dioxide microsphere prepared by the method has stable performance and is suitable for high-efficiency liquid-phase chromatographic separation and analysis.

Description

【Technical field】 [0001] The invention relates to the technical field of silicon dioxide, in particular to a preparation method and application of mesoporous silicon dioxide microspheres with controllable pore size. 【Background technique】 [0002] High-performance liquid chromatography is one of the most widely used analytical methods and separation methods in contemporary times, and is widely used in various departments of scientific research and various fields of social production. In the liquid chromatography system, the core that determines the analysis results and the degree of separation is the chromatographic column. Therefore, fillers, especially those based on silica gel, have always been an important topic of concern to chromatographic workers. Among the stationary phases of modern liquid chromatography, fillers based on silica microspheres account for about 80% of the entire application of high performance liquid chromatography. This is because silica microspher...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
Inventor 梁鑫淼李颖玉柯燕雄戴培春
Owner EAST CHINA UNIV OF SCI & TECH
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