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Method for preparing micron SiO2 gas gel small ball

A micron-scale technology of airgel pellets, applied in chemical instruments and methods, silica, inorganic chemistry, etc., to achieve the effects of simplified operating conditions, easy control of conditions, and low price

Inactive Publication Date: 2006-01-04
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on making aerogels into micron-sized spheres suitable for chromatographic column packing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] First, select commercially available industrial silica sol as the silicon source, filter the silica sol with a filter screen to remove a small amount of suspended impurities in the commercially available silica sol, measure 45ml of the silica sol, and add 22.5 ml of silica sol under stirring conditions The nitric acid of ml6% (mass percentage composition), 75ml dehydrated alcohol, stop stirring, stand time 10min, obtain SiO 2 Alcohol sol.

[0017] Then, take 500ml of n-heptane, add 0.5g of Span 80, 0.05g of Tween 85, and 15ml of n-butanol, stir well, and then adjust the stirring speed to 700r·min -1 , take the above SiO 2 Add 100ml of alcohol sol into it to form a uniform milky white W / O emulsion. After stirring for 15 minutes, add 10ml of concentrated ammonia water and adjust the stirring speed to 500r·min -1 , stirred for another 30min, stopped stirring, separated the solid from the liquid, washed the resulting solid with acetone several times to obtain SiO 2 Gel p...

Embodiment 2

[0020] First, select commercially available industrial silica sol as the silicon source, filter the silica sol with a filter screen to remove a small amount of suspended impurities in the commercially available silica sol, measure 120ml of the silica sol, add 60ml1 % (mass percentage composition) of nitric acid, 24ml dehydrated alcohol, stop stirring, stand time 10min, obtain SiO 2 Alcohol sol. Then, take 500ml of n-hexane, add 2g of Span 80, 0.2g of Tween 85, and 20ml of n-hexanol, stir evenly, and then adjust the stirring speed to 500r·min -1 , take the above SiO 2 Add 200ml of alcohol sol to form a uniform milky white W / O emulsion. After stirring for 100min, add 10ml of concentrated ammonia water and adjust the stirring speed to 500r·min -1 , and then stirred for 60min, stopped stirring, separated the solid and liquid, washed the resulting solid with acetone several times to obtain SiO 2 gel balls.

[0021] The prepared SiO 2 The gel microspheres are first soaked and w...

Embodiment 3

[0023] First, select commercially available industrial silica sol as the silicon source, filter the silica sol with a filter screen to remove a small amount of suspended impurities in the commercially available silica sol, measure 30ml of the silica sol, add 60ml10 % (mass ratio) of nitric acid, 50ml dehydrated alcohol, stop stirring, stand time 10min, obtain SiO 2 Alcohol sol.

[0024] Then, take 500ml of n-heptane, add 5g of Span 80, 0.5g of Tween 85, and 50ml of n-butanol, stir well, and then adjust the stirring speed to 1300r·min -1 , take the above SiO 2Add 50ml of alcohol sol into it to form a uniform milky white W / O emulsion. After continuing to stir for 40min, add 10ml of concentrated ammonia water and adjust the stirring speed to 700r·min -1 , and then stirred for 15min, stopped stirring, separated the solid and liquid, washed the obtained solid several times with acetone, and obtained SiO 2 gel balls.

[0025] The prepared SiO 2 The gel microspheres are first so...

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PUM

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Abstract

The present invention relates to the process of preparing micron level SiO2 aerogel ball as the stuffing of chromatographic column for separating biological macromolecule. The process includes the following steps: preparing alcohol sol of SiO2 via mixing silicon gel and nitric acid in the volume ratio of 1 to 0.5-20, and adding anhydrous ethanol; mixing n-heptane, span-80, Tween-85 and n-butanol in certain volume proportion through stirring to obtain oil phase; adding the sol of SiO2 into the oil phase in certain volume ratio to form W / O emulsion; stirring, adding concentrated ammonia water to alkaline for depositing gel, further stirring, and liquid-solid separation to obtain SiO2 gel microballoon; washing with acetone and drying to obtain micron level SiO2 aerogel ball. The process has normal pressure, easy control, low cost, and other advantages.

Description

technical field [0001] A micron-sized SiO 2 The preparation method of the airgel pellet relates to a method for making the airgel into a micron-sized pellet as a chromatographic column filler that can satisfy the separation of biomacromolecules. Background technique [0002] Due to the wide application of high-performance liquid chromatography in life sciences and various requirements such as high-efficiency catalysis, the development of porous, especially mesoporous microspherical silica gel has attracted more and more attention. However, the control of the pore structure of this silica gel is a key issue. A rather difficult technique. At present, silica gel with an average pore diameter of 6-8nm is generally used in high performance liquid chromatography, but silica gel with this pore size cannot adapt to the characteristics of biological macromolecules, and silica gel with medium or large pores must be used (generally about 20nm or more) large)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/113C01B33/14C01B33/158
Inventor 甘礼华庞颖聪郝志显徐子颉陈龙武
Owner TONGJI UNIV
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