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Chiral core-shell chromatography stationary phase and preparation method

A core-shell type, core-shell technology, applied in the field of chiral core-shell liquid chromatography filler and its preparation, can solve the problems of small specific surface area, low content of chiral selector, etc., and achieve high permeability and fast analysis speed , not easy to lose the effect

Inactive Publication Date: 2014-11-12
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few studies on chiral core-shell chromatographic packing, and there is no commercial chiral core-shell chromatographic packing.
Compared with fully porous materials, core-shell materials have a small specific surface area due to the existence of a non-porous core, and traditional bonding or coating methods will lead to the problem of low chiral selector content

Method used

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  • Chiral core-shell chromatography stationary phase and preparation method
  • Chiral core-shell chromatography stationary phase and preparation method
  • Chiral core-shell chromatography stationary phase and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Under nitrogen protection, in a 250mL two-necked flask, add 0.38g trans-(1R,2R)-cyclohexanediamine (DACH), 100mL anhydrous CH 2 Cl 2 , slowly drop 1.73g isocyanate propyltriethoxysilane (ICPTES) into the above reaction solution with a syringe, react at room temperature for 2h, and distill CH under reduced pressure 2 Cl 2 , to obtain a solid product. Then the resulting solid was washed with anhydrous n-hexane, filtered, and the excess ICPTES was removed together with the filtrate, and the filter cake was vacuum-dried to obtain chiral cyclohexanediamine disiloxane: N, N'-di-[(triethoxy Silyl)propyl]-trans-(1R,2R)-bis-(ureide)-cyclohexane (DACH-BS) as a white solid.

[0021] (2) Mix ammonia water, ethanol and deionized water at a volume ratio of 200:56:80 to make liquid A, add 2ml liquid A + 1ml tetraethyl orthosilicate (TEOS) to a 50ml round-bottomed flask, and place in an ice-water bath Stir for 5 minutes, and add liquid A and TEOS dropwise at room temperature wi...

Embodiment 2

[0025] (1) Under nitrogen protection, in a 250mL two-necked flask, add 0.38g trans-(1R,2R)-cyclohexanediamine (DACH), 100mL anhydrous CH 2 Cl 2 , slowly drop 1.73g isocyanate propyltriethoxysilane (ICPTES) into the above reaction solution with a syringe, react at room temperature for 2h, and distill CH under reduced pressure 2 Cl 2 , to obtain a solid product. Then the resulting solid was washed with anhydrous n-hexane, filtered, and the excess ICPTES was removed together with the filtrate, and the filter cake was vacuum-dried to obtain chiral cyclohexanediamine disiloxane: N, N'-di-[(triethoxy Silyl)propyl]-(1R,2R)-bis-(ureide)-cyclohexane (DACH-BS) as a white solid.

[0026] (2) Mix ammonia water, ethanol and deionized water at a volume ratio of 200:60:100 to prepare liquid A, mix and stir liquid A with tetraethyl orthosilicate at a volume ratio of 2:1 in an ice bath for 1.5 h, The obtained product was washed with deionized water and ethanol until neutral, and dried at 8...

Embodiment 3

[0030] figure 1 It is the scanning electron micrograph of the chiral cyclohexanediamine core-shell chromatographic filler in Example 1

[0031] figure 2 It is the transmission electron microscope figure of the chiral cyclohexanediamine core-shell chromatographic filler in Example 1

[0032] image 3 It is the chiral cyclohexanediamine core-shell chromatographic packing material of the present invention to separate (A) R / S-1,1'-binaphthalene-2,2'-diphenol, (B)R / S under normal phase system - Chromatogram of 6,6'-dibromo-1,1'-binaphthyl-2,2'-diol.

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Abstract

The invention discloses a chiral core-shell chromatography stationary phase. The inner layer is nonporous silica gel which is coated with a hybrid mesoporous silica gel shell layer containing a chiral diaminocyclohexane group. Meanwhile, the invention also discloses a preparation method of the above chiral core-shell liquid chromatography packing. The hybrid mesoporous silica gel has characteristics of high permeability and uniform distribution of organo-functional groups, and the core-shell packing has advantages of high column efficiency and fast analysis speed. By combining the characteristics of the hybrid mesoporous silica gel and the advantages of the core-shell packing, a novel chromatography stationary phase packing is formed.

Description

technical field [0001] The invention relates to the technical field of porous material preparation and analytical chemistry, in particular to a chiral core-shell liquid chromatography filler and a preparation method thereof. Background technique [0002] Hybrid ordered mesoporous silica refers to the silicon ester [(OR) 3 SiR'Si(OR) 3 ] As one of the silicon sources, ordered mesoporous silica gel containing organic groups in the skeleton is directly prepared after hydrolysis polymerization. Hybrid silica gel has a large specific surface area, regularly arranged pores, narrow pore size distribution, and has better hydrothermal stability, mechanical stability and chemical stability. In recent years, chiral hybrid mesoporous silica has shown excellent prospects in the application of chromatographic separation of chiral compounds. However, the characteristics of high organic functional group loading and large specific surface area of ​​hybrid mesoporous silica make the adsorp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30
Inventor 狄斌吴夏冰尤淋君杜迎翔
Owner CHINA PHARM UNIV
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