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Method for preparing high-purity silica packing through sol-gel process

A technology of chromatographic column packing and silica gel chromatographic column, which is applied in the field of preparation of high-purity silica gel, can solve the problems of unsuitability for high-purity products, long time, influence on product purity, etc., and achieve great application value, strong separation ability and monodispersity Good results

Inactive Publication Date: 2014-04-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method reflects the excellent characteristics of the sol-gel method, but the raw material silicate introduces a large number of heteroatoms, which has a great impact on the purity of the product and is not suitable for the preparation of high-purity products
In the report "A review on the synthesis, structure and applications in separation processes of mesoporous MSU-χsilica obtained with the two-step process" in "Elsevier [J], 2005 (8): 579-596", Prouzet et al. adopted Micron-sized mesoporous SiO obtained from cheap silica sol as silicon source 2 ball, but it is a two-step reaction, which takes a long time and takes 2 to 3 days

Method used

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  • Method for preparing high-purity silica packing through sol-gel process
  • Method for preparing high-purity silica packing through sol-gel process
  • Method for preparing high-purity silica packing through sol-gel process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 160mL of analytically pure ammonia water with a concentration of 25-28% in a 500mL three-necked bottle equipped with a reflux device, raise the temperature of the water bath to 70°C, and mechanically stir at a speed of 800rpm, add 16.0g of monocrystalline silicon powder (99.99%, 70μm), and continue to heat up When the temperature reaches 75°C, add 100 mL of ammonia water dropwise into the reaction vessel at a rate of 10 mL for half an hour. During the reaction process, ammonia gas was introduced to keep the pH value of the reaction solution not less than 11, and the reaction was terminated after 6 hours to obtain a silica hydrosol with a solid content of about 30.3%.

[0027]Take 5g of the silica aqueous sol prepared above in a beaker, add 0.1g of sodium dodecylbenzenesulfonate, oscillate ultrasonically for 15min, transfer to a three-necked flask equipped with a stirrer, thermometer and water separator, add 50mL For n-heptane, heat and stir, keep the temperature whe...

Embodiment 2

[0031] Add 160mL of analytically pure ammonia water with a concentration of 25-28% in a 500mL three-necked bottle equipped with a reflux device, raise the temperature of the water bath to 70°C, and mechanically stir at a speed of 900rpm, add 12.0g of monocrystalline silicon powder (99.99%, 70μm), and continue to heat up When the temperature reaches 80°C, add 140 mL of ammonia water to the reaction vessel at a rate of 10 mL for half an hour. Ammonia gas was introduced to keep the pH value of the reaction solution not less than 11, and the reaction was terminated after 7 hours to obtain a silica hydrosol whose solid content was determined to be about 31.2%.

[0032] Take 5g of the above-prepared silica aqueous sol in a beaker, add 0.3g of dedecyltrimethylammonium bromide, ultrasonically vibrate for 15min, transfer to a three-necked flask equipped with a stirrer, a thermometer and a water separator, add 70mL of n-heptane, heat and stir, keep the temperature when the temperature r...

Embodiment 3

[0036] Add 160mL of analytically pure ammonia water with a concentration of 25%-28% into a 500mL three-necked flask equipped with a reflux device, raise the temperature of the water bath to 70°C, and stir at a speed of 1000rpm, add 14.0g of monocrystalline silicon powder (99.99%, 60~100μm), When the temperature continued to rise to 90°C, 120 mL of ammonia water was added to the reaction vessel at a rate of 10 mL for half an hour. Ammonia gas was introduced to keep the pH value of the reaction solution not less than 11, and the reaction was terminated after 8 hours to obtain a silica hydrosol whose solid content was determined to be about 33.4%.

[0037] Take 5g of the above-prepared silica aqueous sol in a beaker, add 0.5g of polyglycol, ultrasonically vibrate for 15min, transfer to a three-necked flask equipped with a stirrer, a thermometer and a water separator, add 80mL of n-heptane, and heat Stir, keep the temperature when the temperature reaches 80°C, react until no water...

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Abstract

The invention discloses a method for preparing high-purity silica packing through a sol-gel process. The method is characterized in that monocrystalline silicon powder is taken as a silicon source, and under the catalysis of ammonia water, high-purity and monodispersed nanosilica hydrosol is firstly synthetized; and monodispersed microspheres are prepared through the sol-gel process, and the microspheres are subjected to thermal treatment, so that high-purity polyporous micron-size silica-based microspheres with the grain sizes of 2 to 10 um are finally obtained. According to the invention, the monocrystalline silicon powder is taken as the silicon source, and the ammonia water is taken as catalyst, so that such impurities as metal are prevented from mixing in, after the monodispersed microspheres are subjected to thermal treatment, the high-purity polyporous micron-size silica-based microspheres are obtained, have good monodispersity and uniformly-distributed surface pore structures, and can be used as silica packing directly without being processed in a grading manner.

Description

technical field [0001] The invention relates to a method for preparing high-purity silica gel, in particular to a method for preparing high-purity silica gel chromatographic column packing by a sol-gel method. Background technique [0002] Chromatography, as an efficient means of separation and analysis, is playing an increasingly important role in today's production, scientific research, detection, monitoring and other fields. Among them, chromatographic column packing is the key to the effective separation of complex components. Traditional silica-based chromatographic column packing contains a certain amount of metal impurities such as iron, aluminum, etc. These impurities will increase the surface activity of silica gel, and the acidity of residual silanol on the surface of the packing will increase, and the surface of silica gel will be negatively charged. Under normal separation conditions, the basic analyte is positively charged due to protonation, and its chromatogra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281C01B33/14
Inventor 杨俊佼彭秋瑾
Owner BEIJING UNIV OF CHEM TECH
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