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Preparation method of monodisperse aperture-adjustable full-porous silicon dioxide chromatographic microspheres

A silicon dioxide, monodisperse technology, applied in the direction of silicon dioxide, silicon oxide, chemical instruments and methods, etc., can solve problems such as difficulty in obtaining spherical silica gel stationary phase, affecting separation effect, difficult pore size, etc.

Active Publication Date: 2021-05-28
XIAMEN CHROMATOGRAPHIC ANALYSIS INSTR CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, due to the characteristics of sol-gel, the silica gel packing used today has a wide particle size distribution. Even if time-consuming and labor-intensive sieving technology is used in the later stage, it is difficult to obtain a monodisperse spherical silica gel stationary phase; secondly, it is difficult to control the size of the pores. Flexible control to obtain the required pore size; large-scale preparation of packing usually uses silicate as the silicon source, which inevitably leads to metal ions on the packing, which affects the final separation effect
The emergence of the above-mentioned problems restricts the further development of chromatographic packing materials, and ultimately limits the separation effect of chromatography.

Method used

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  • Preparation method of monodisperse aperture-adjustable full-porous silicon dioxide chromatographic microspheres
  • Preparation method of monodisperse aperture-adjustable full-porous silicon dioxide chromatographic microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0029]In a 25mL single-necked flask, add 1.8mL ammonia water, 3.25mL EtOH, 4.95mL water, 0.153g dodecylamine and 0.153g dodecylamine polyoxyethylene ether, stir and mix at a stirring speed of 1100rpm, then add the previously mixed 0.9mL TEOS and 9.1mL EtOH were quickly poured into the reaction flask. After stirring and reacting at a stirring speed of 1100rpm for 1min, lower the rotating speed to 360rpm, and stir and react at room temperature for 2h; filter the reaction solution, wash with water, wash with alcohol, and dry, take 50mg of washed seed microspheres, and add them to 330mL In the reaction solution, wherein the concentration of ammonia water is 3.5mol / L, the concentration of water is 10mol / L, and the rest are all ethanol, and 3.212g dodecylamine and 3.212g dodecylamine polyoxyethylene ether are added therein, and the stirring speed is 1500rpm Mix the reactants evenly, and slowly inject 100mL of 0.03mol / L TEOS solution (solvent is ethanol) into the reaction system for ...

Embodiment 2

[0032] In a 25mL single-necked flask, add 1.8mL ammonia water, 1.00mL EtOH, 7.10mL water, 0.153g dodecylamine and 0.153g dodecylamine polyoxyethylene ether, stir and mix at a stirring speed of 1100rpm, then add the previously mixed 0.9mL TEOS and 9.1mL EtOH were quickly poured into the reaction flask. After stirring and reacting for 1min at a stirring speed of 1100rpm, reduce the rotating speed to 360rpm, and stir and react at room temperature for 2h, filter the reaction solution, wash with water, wash with alcohol, and dry, take 50mg of the washed seed microspheres and add them to 330mL In the reaction solution, wherein the concentration of ammonia water is 3.5mol / L, the concentration of water is 10mol / L, and the rest are all ethanol, and 3.212g dodecylamine and 3.212g dodecylamine polyoxyethylene ether are added therein, and the stirring speed is 1500rpm Mix the reactants evenly, and slowly inject 100mL of 0.03mol / L TEOS solution (solvent is ethanol) into the reaction system...

Embodiment 3

[0034] Similar to Example 1, the difference is that in the template-guided seed growth step, the volume ratio of ethanol / water in the solvent system of water and ethanol is 1:1, and the template agent adopts polyethylene oxide-polypropylene oxide- Polyethylene oxide triblock copolymer. In the seed growing step, the concentration of TEOS in the TEOS solution is 0.03 mol / L, the concentration of the ammonia water is 1 mol / L; the stirring speed of high-speed stirring is 1800 rpm. The temperature of hydrothermal hole expansion is 100°C, and the time of hydrothermal hole expansion can be 96h. The temperature of constant temperature calcination is 500° C. for 7 hours, and the atmosphere is oxygen. The temperature of lye reaming is 90℃, and the time of lye reaming can be 60h.

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Abstract

The invention discloses a preparation method of monodisperse aperture-adjustable full-porous silicon dioxide chromatographic microspheres, and relates to a preparation process of a silica gel stationary phase in chromatographic separation. Two major aspects of the appearance and the particle size of the microspheres and the control of the pore size and the pore size distribution are separated and regulated one by one, so that the defect that the two problems are simultaneously solved by seeking a one-pot method in a traditional mode is overcome; and the preparation method of the monodisperse pore-size-adjustable full-porous silicon dioxide chromatographic microspheres which are full-porous, adjustable in pore size and free of metal is provided. The method mainly comprises the steps of template-guided seed synthesis, seed growth, template agent chambering, calcination curing, alkali liquor chambering and the like. The prepared silicon dioxide microspheres are excellent in sphericity and monodispersity and controllable in particle size, the pore size regulation and control method is simple, the pore size distribution range is narrow, no metal element residues exist, and expansibility and replicability are achieved. As the used reagents do not contain inorganic salt, the purity of the microspheres is high, and the method is particularly suitable for high performance liquid chromatography separation and analysis.

Description

technical field [0001] The invention relates to a preparation process of silica gel stationary phase used in chromatographic separation, in particular to a method for preparing monodisperse fully porous silica chromatographic microspheres with adjustable apertures. Background technique [0002] As an important separation and analysis tool, chromatography technology has been widely used in many fields such as food, biology, medicine and environment, and has become one of the indispensable tools. The chromatographic separation has been shortened from more than an hour at the beginning to a few minutes or even a minute today. The significant shortening of the separation time and the rapid improvement of the separation efficiency are not only due to the development of chromatographic instrument technology, but also mainly due to the chromatographic packing material. impetus for development. [0003] The ideal chromatographic packing generally meets the following requirements: 1...

Claims

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Application Information

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IPC IPC(8): C01B33/18
CPCC01B33/186C01P2004/61C01P2004/32C01P2006/16C01P2004/03
Inventor 张博曾巨星
Owner XIAMEN CHROMATOGRAPHIC ANALYSIS INSTR CO LTD
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