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Method for preparing coating type cellulose derivative chiral monolithic column

A cellulose derivative and coating technology is applied in the field of preparation of a coated cellulose derivative chiral monolithic column, which can solve the problems of limited rapid separation, large column pressure drop, and difficulty in entering polysaccharide derivatives.

Inactive Publication Date: 2011-05-11
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polysaccharide chiral stationary phase is mainly to bond or coat amylose, cellulose derivatives, and modified cyclodextrin on the silica gel carrier, and pack it into a column for high-pressure liquid chromatography separation. The finer the particle size, the higher the column efficiency of the chromatographic column, but the greater the column pressure drop, which has become a bottleneck restricting rapid separation; in addition, the traditional silica gel carrier has too small pore size, and it is difficult for polysaccharide derivatives with large molecular weight to enter Silica gel channels, not conducive to chiral recognition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Preparation of silica gel monolithic column: add a certain amount of distilled water, nitric acid, tetraethyl orthosilicate (TEOS) and polyethylene glycol (PEG) in the suction filter bottle, and make the ratio of the amount of the four substances, H 2 O: HNO 3 :TEOS:PEG=15.7:0.25:1:6.9×10 -4 , stirred in an ice-water bath for 1 h. The obtained sol was slowly poured into a molding mold, and placed in a constant temperature water bath at 40°C for 36 hours of reaction. Take out the silica gel column, soak it in 0.01M ammonia water, hydrothermally treat it for 4 hours, dry it at 70°C for 12 hours, and then bake it in a box-type resistance furnace at 1°C min -1 The temperature was raised to 550° C. at a constant temperature for 4 hours to prepare a monolithic column of double-hole silica gel.

[0013] Preparation of cellulose derivative chiral compound: Take 0.28g of microcrystalline cellulose, add 42.8ml of anhydrous pyridine, stir, reflux at 90°C for 12h, then add 0.96m...

Embodiment 2

[0017] Preparation of silica gel monolithic column: add a certain amount of distilled water, nitric acid, tetraethyl orthosilicate (TEOS) and polyethylene glycol (PEG) in the suction filter bottle, and make the ratio of the amount of the four substances, H 2 O: HNO 3 :TEOS:PEG=15.7:0.25:1:6.9×10 -4 , stirred in an ice-water bath for 1 h. The obtained sol was slowly poured into a forming mold, and the stomach was reacted in a constant temperature water bath at 40°C for 24 hours. Take out the silica gel column, soak it in 0.05M ammonia water, hydrothermally treat it for 4h, dry it at 60°C for 20h, and then bake it in a box-type resistance furnace at 1°C min -1 The temperature was raised to 550° C. at a constant temperature for 4 hours to prepare a monolithic column of double-hole silica gel.

[0018] Preparation of cellulose derivative chiral compound: Take 0.30g of microcrystalline cellulose, add 45ml of anhydrous pyridine, stir, reflux at 90°C for 12h, then add 1.3ml of 3,5...

Embodiment 3

[0022] Preparation of silica gel monolithic column: In a beaker, add 50 mL of acetic acid aqueous solution with a pH of 5.0, then add 6.0 g of polyethylene glycol, stir, add 35 mL of tetramethoxysilane, and stir at 0°C for 10 min. The resulting mixture was poured into a molding mold, placed in a water bath at 40°C, and aged for 24 hours after reaching the gel point to obtain a wet silica gel column. Soak the silica gel column after demoulding and rinsing in 0.1mol / L ammonia water, hydrothermally treat it for 6h, then place it in a constant temperature box, dry it at 80°C for 10h, and then bake it in a box-type resistance furnace at 1°C min -1 The temperature was raised to 550° C. at a constant temperature for 4 hours to prepare a monolithic column of double-hole silica gel.

[0023] Preparation of cellulose derivative chiral compound: Take 0.30g of microcrystalline cellulose, add 45ml of anhydrous pyridine, stir, reflux at 90°C for 12h, then add 1.3ml of 3,5-dimethylphenylisoc...

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Abstract

The invention provides a method for preparing a coating type cellulose derivative chiral monolithic column. Alkoxy silane is used as a silicon source, polyethylene glycol is used as a macroporous template agent, and ammonia water is used as a mesoporous template agent. The method comprises the following steps of: preparing a diplopore silica gel monolithic column by an improved sol-gel process through demolding, washing, drying and calcining; stirring microcrystalline cellulose and anhydrous pyridine, and reflowing; adding 3,5-dimethyl phenyl isocyanate; reflowing, stirring, filtering, washing, and drying in vacuum to obtain a cellulose derivative chiral compound; dissolving the cellulose derivative chiral compound in an organic solvent; washing the silica gel monolithic column by using the obtained solution; and washing, performing suction filtration, drying and coating to obtain the coating type cellulose derivative chiral monolithic column.

Description

technical field [0001] The invention relates to a preparation method of a coated cellulose derivative chiral monolithic column. Background technique [0002] There are enantiomeric differences in the environmental behavior of chiral pollutants, and the hazards posed by different enantiomers to human health and ecological security are also very different. Therefore, the environmental behavior of chiral organochlorine pesticides, Potential toxicity and ecological effects are more scientific. [0003] Studies have shown that the chiral stationary phase of carbamate derivatives in polysaccharide chiral stationary phases has good chiral recognition ability and is suitable for the preparation and separation of enantiomers, especially the 3,5 -Dimethylphenylcarbamate chiral stationary phase, which shows good chiral recognition performance for various types of chiral compounds. The polysaccharide chiral stationary phase is mainly to bond or coat amylose, cellulose derivatives, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30
Inventor 马小东万伟郭洪雯陈建宏代历杨五林
Owner NANKAI UNIV