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Preparation method of silica gel monolithic column

A silica monolithic column, silica gel technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problem of high difficulty in synthesis technology, and achieve the effect of good fracture shrinkage and control of fracture shrinkage

Active Publication Date: 2015-12-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high difficulty of its synthesis technology, only a few laboratories have mastered this technology

Method used

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  • Preparation method of silica gel monolithic column
  • Preparation method of silica gel monolithic column
  • Preparation method of silica gel monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A. In a three-necked flask equipped with a stirring device, the solid content is 44.77g of 25% silica gel, and 3.64g of analytically pure polyethylene glycol is added, and after stirring for 20min, it is completely dissolved to form a homogeneous solution, and then the device is placed in In an ice-water bath at a temperature of 0°C to 5°C, add distilled water dropwise to adjust the pH of the system to 9, continue stirring for 10 minutes, then add analytically pure methyl orthosilicate 3.1mL dropwise, stir for 15 minutes, and wait until it is completely in the system Install the tube after hydrolysis, and seal the two ends of the tube.

[0025] B. The monolithic column prepared in above A is placed in a 40°C water bath for sol-gel aging for 24 hours. After the column is gelled, the sealing films at both ends are removed, the column is placed in a larger petri dish, and 0.01mol / L, 0.1mol / L, 1mol / L ammonia water 200mL soaked for 3 hours each to prepare mesopores, then so...

Embodiment 2

[0028] A. In a three-necked flask equipped with a stirring device, the solid content is 25% silica gel 39.8g, and 3.64g of analytically pure polyethylene glycol is added, and after stirring for 20min, it is completely dissolved to form a homogeneous solution, and then the device is placed in In an ice-water bath at a temperature of 0°C to 5°C, add distilled water dropwise to adjust the pH of the system to 9. After continuing to stir for 10 minutes, add 6.2 mL of analytically pure methyl orthosilicate dropwise. After stirring for 15 minutes, wait until it is completely in the system. Install the tube after hydrolysis, and seal the two ends of the tube.

[0029] B. The monolithic column prepared in above A is placed in a 40°C water bath for sol-gel aging for 24 hours. After the column is gelled, the sealing films at both ends are removed, the column is placed in a larger petri dish, and 0.01mol / L, 0.1mol / L, 1mol / L ammonia water 200mL soaked for 3 hours each to prepare mesopores...

Embodiment 3

[0032] A. In a three-necked flask equipped with a stirring device, add 34.8 g of silica gel with a solid content of 25%, and add 3.64 g of analytically pure polyethylene glycol. After stirring for 20 minutes, wait for it to completely dissolve to form a homogeneous solution, and then place the device In an ice-water bath at a temperature of 0°C to 5°C, add distilled water dropwise to adjust the pH of the system to 9, continue stirring for 10 minutes, then add analytically pure methyl orthosilicate 9.3mL dropwise, stir for 15 minutes, and wait until it is in the system Fill the tube after complete hydrolysis, and seal the two ends of the tube.

[0033] B. The monolithic column prepared in above A is placed in a 40°C water bath for sol-gel aging for 24 hours. After the column is gelled, the sealing films at both ends are removed, the column is placed in a larger petri dish, and 0.01mol / L, 0.1mol / L, 1mol / L ammonia water 200mL soaked for 3 hours each to prepare mesopores, then so...

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Abstract

The invention discloses a preparation method of a silica gel monolithic column. In the invention, silicon dioxide hydrosol is employed as a silicon source, methyl silicate as a crosslinking agent and polyethylene glycol as a pore-forming agent, a sol-gel reaction is carried out under an alkaline environment. When the column is subjected to gelation, eluting the column with ammonia water, distilled water and N,N-dimethylformamide in different concentrations successively. The column is then dried in a vacuum drying box and is calcined in a muffle furnace. The silica gel monolithic column has a micron-scale framework, through-pores and nano-scale mesopores, wherein the through-pores enable the silica gel monolithic column to have strong permeability and is less in change of pressure drop with flow velocity. The mesopores provides a large specific surface area to the silica gel monolithic column, which is a pre-condition of ensuring high column efficiency. By means of adjustment of composition ratio of the reactants, the pore sizes of the through-pores and the mesopores can be controlled independently. The framework is 1-2 [mu]m is average size, the through-pores are 2-3 [mu]m is average size and the average size of the mesopores is 20 nm through a nitrogen desorption test. The silica gel monolithic column is higher than a packed column in pore volume and is beneficial to industrial development.

Description

technical field [0001] The present invention uses silica sol as a silicon source in an alkaline environment to prepare a monolithic column with micron-scale skeletons, through-holes and nano-scale mesopores. It has the advantages of saving raw materials, non-toxic and harmless, simple and fast. Background technique [0002] Since Russian botanist TSwett discovered chromatography in 1903, with the continuous development and progress of science, chromatography technology has developed rapidly in various scientific fields, and has been widely used in materials science, environmental science, life science, information science and other directions. As the core part of chromatographic technology, chromatographic columns are constantly developing in order to adapt to the advancement of science and technology. At present, the existing chromatographic technology can basically meet the requirements of various fields, but the special requirements of biochemical separation, the develop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22
Inventor 杨俊佼王伟伟
Owner BEIJING UNIV OF CHEM TECH
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