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Novel hybrid mesoporous silica gel chromatographic stationary phase and preparation method thereof

A technology of hybrid mesoporous silica gel and chromatographic stationary phase, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of spherical shape, rareness, constraints, etc., and achieve the effect of good separation performance

Inactive Publication Date: 2013-09-04
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, materials synthesized under acidic conditions are often difficult to obtain a good spherical shape. Although there are successful cases, they are rare.
Therefore, the application of this type of material in the field of chromatographic stationary phase is restricted.

Method used

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  • Novel hybrid mesoporous silica gel chromatographic stationary phase and preparation method thereof
  • Novel hybrid mesoporous silica gel chromatographic stationary phase and preparation method thereof
  • Novel hybrid mesoporous silica gel chromatographic stationary phase and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 0.858g (3mmol) of R-(+)-1,1'-binaphthyl-2,2'-diphenol to 60ml of dried methylene chloride, add 0.304g (3mmol) of triethylamine, and Under stirring, slowly add 0.742g (3mmol) isocyanatopropyltriethoxysilane (ICPTES) dropwise. After the dropwise addition, continue to stir at room temperature for 2h, evaporate the solvent and triethylamine in the reaction system to obtain colorless 0.96 g of transparent viscous product R-2-(3-triethoxysilyl)-propylcarbamoyloxy-2'-hydroxyl-1,1'-binaphthyl (M-binol).

Embodiment 2

[0018] Add 0.12g cetyltrimethylammonium bromide (CTAB), 0.696g triblock copolymer (P123) to a mixed solvent consisting of 8.7ml 2mol / L hydrochloric acid solution, 7.14ml ethanol and 58.0ml deionized water , stirred until completely dissolved, mixed 0.48g of homemade silicon source M-binol and 777ul 1,2-bistriethoxysilylethane (BTSE) evenly, then slowly added to the above mixed solution under vigorous stirring, at room temperature After stirring for 30 minutes, transfer it to a stainless steel polytetrafluoroethylene reactor, and let it stand at 100°C for 16 hours. Filter with suction, wash with deionized water until neutral, and dry under vacuum at 60°C overnight.

Embodiment 3

[0020] Add 0.12g cetyltrimethylammonium bromide (CTAB), 0.696g triblock copolymer (P123) to a mixed solvent consisting of 7.2ml 2mol / L hydrochloric acid solution, 7.14ml ethanol and 58.0ml deionized water , stirred until completely dissolved, mixed 0.48g of homemade silicon source M-binol and 777ul 1,2-bistriethoxysilylethane (BTSE) evenly, then slowly added to the above mixed solution under vigorous stirring, at room temperature After stirring for 30 minutes, transfer it to a stainless steel polytetrafluoroethylene reactor, and let it stand at 100°C for 16 hours. Filter with suction, wash with deionized water until neutral, and dry under vacuum at 60°C overnight.

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Abstract

The invention discloses a novel hybrid mesoporous silica gel chromatographic stationary phase and a preparation method thereof. Under the condition of a dual-template agent, an R-(+)-1,1'-binaphthyl -2,2'-diphenol group is introduced into the surface of hybrid mesoporous silica gel and firstly applied to the chromatographic stationary phase. After column-filling operation is carried out, five kinds of binaphthyl compounds are separated successfully; and the chromatographic peak is good in shape and can be separated rapidly. The method is simple in preparation process in which a cationic surfactant and a triblock copolymer are taken as the dual-template agent, the hybrid mesoporous silica gel chromatographic stationary phase is prepared by the copolycondensation of a binaphthol derivate silicon source with 1,2-bis-triethoxysilyl ethane (BTSE) under an acidic condition. The hybrid mesoporous silica gel chromatographic stationary phase has a neat spherical shape and is homogeneous in particle diameter distribution (3 to 10 microns) as well as uniform and adjustable in particle diameter. Thus, the chromatographic stationary phase disclosed by the invention can be applied widely.

Description

technical field [0001] The invention relates to the technical field of preparation and analysis of hybrid mesoporous silica gel, in particular to a novel hybrid mesoporous silica gel chromatographic stationary phase and a preparation method. Background technique [0002] Since the MCM41S series materials were reported in 1992, the development of ordered mesoporous materials has attracted more and more attention from researchers. This type of material uses a cationic surfactant as a template, and interacts electrostatically with the hydrolyzed silicon source precursor, which has a strong effect. Therefore, the formed material has an orderly pore structure, which can bring good permeability and large specific surface area. However, MCM41S series materials also have their own shortcomings, such as thin pore walls, and the mesoporous structure is easy to collapse after removing the template. In 1998, Zhao et al. (reference 1, ZhaoDY, HuoJL, StuckyGD, et al. Triblock copolymer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30
Inventor 狄斌钱洁
Owner CHINA PHARM UNIV
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