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Core-shell packing applied to liquid chromatography separation analysis and preparation method thereof

A liquid chromatography, separation and analysis technology, applied in the field of chemical analysis and separation, can solve the problems of small pore size, cumbersome operation, and many preparation steps of core-shell fillers, achieve narrow particle size distribution, reduce dead adsorption, and fast separation speed Effect

Active Publication Date: 2020-01-14
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The packing prepared by this method can withstand high temperature, but the core-shell packing has a smaller pore size
At present, there are other preparation methods that can prepare core-shell fillers with different specific surface areas and pore sizes, but in general, their preparation steps are many and the operation is cumbersome.

Method used

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  • Core-shell packing applied to liquid chromatography separation analysis and preparation method thereof
  • Core-shell packing applied to liquid chromatography separation analysis and preparation method thereof
  • Core-shell packing applied to liquid chromatography separation analysis and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method for a core-shell filler applied to liquid chromatography separation and analysis, comprising the following steps:

[0028] (1) Weigh 1g particle size as 1 ~5 The solid silicon spheres are uniformly dispersed in 50 mL of pure water, and the solid silicon spheres and pure water are fully stirred and mixed at room temperature at 15-25° C. to obtain a dispersion.

[0029] (2) Add 1 polydimethyldiallylammonium chloride to the dispersion liquid obtained in step (1) at room temperature at 15-25°C, and stir and mix with ultrasonic to obtain a white emulsion.

[0030] (3) Control the reaction temperature at 100°C, add 3mL of ammonia water to the white emulsion obtained in step (2), adjust the pH of the solution to 10, stir at 300-800r / min, and reflux for 24h.

[0031] (4) After the reaction is over, cool the reactant to room temperature at 15-25°C, centrifuge, wash with water, filter with suction, dry at low temperature (50-80°C), and then calcinate at 5...

Embodiment 2

[0034] A preparation method for a core-shell filler applied to liquid chromatography separation and analysis, comprising the following steps:

[0035] (1) Weigh 5g of particle size as 1 ~5 The solid silicon spheres are uniformly dispersed in 250 mL of pure water, and the solid silicon spheres and pure water are fully stirred and mixed under the condition of 15-25° C. to obtain a dispersion liquid.

[0036] (2) At 15-25°C, add 5-polydimethyldiallylammonium chloride to the dispersion liquid obtained in step (1), stir and mix with ultrasonic to obtain a white emulsion.

[0037] (3) Control the reaction temperature at 90°C, add 20mL ammonia water to the white emulsion obtained in step (2), adjust the pH of the solution to 10.69, stir at 300-800r / min, and reflux for 24h.

[0038] (4) After the reaction is completed, cool the reactant to 15-25°C, centrifuge, wash with water, suction filter, dry at low temperature (50-80°C), and then calcinate at 600°C for 6 hours; Drying at low...

Embodiment 3

[0041] A preparation method for a core-shell filler applied to liquid chromatography separation and analysis, comprising the following steps:

[0042] (1) Weigh 10g of particle size as 1 ~5 The solid silicon spheres are evenly dispersed in 500 mL of pure water, and the solid silicon spheres and pure water are fully stirred and mixed under the condition of 15-25° C. to obtain a dispersion liquid.

[0043] (2) At 15-25°C, add 10 polydimethyldiallylammonium chloride to the dispersion liquid obtained in step (1), stir and mix with ultrasonic to obtain a white emulsion.

[0044] (3) Control the reaction temperature at 80°C, add 75mL of ammonia water to the white emulsion obtained in step (2), adjust the pH of the solution to 12.33, stir at 300-800r / min, and reflux for 18h.

[0045] (4) After the reaction is completed, cool the reactant to 15-25°C, centrifuge, wash with water, suction filter, dry at low temperature (50-80°C), and then calcinate at 700°C for 6 hours; Drying at low...

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Abstract

The invention relates to a core-shell filling applied to liquid chromatogram separation analysis. The core-shell filling is formed by a solid core and a porous layer, the particle size is 1-5 microns, the specific surface area is 20m<2> / g-300m<2> / g, the aperture is 80-200 angstroms, and the shell thickness is 50nm-300nm. A preparation method of the core-shell filling comprises the following steps: (1) preparing dispersion liquid of solid silicon spheres and a reaction solvent; (2) adding a cationic polymer into the dispersion liquid, and carrying out ultrasonic stirring; (3) adding ammonia water to adjust the pH value under a temperature control condition, stirring at an intermediate speed, and carrying out reflex reaction; and (4) after the reaction, cooling to the room temperature, and carrying out centrifugation, washing, suction filtration, drying, calcination and diluted hydrochloric acid activation, so as to obtain the core-shell filling. The preparation is simple and convenient and can meet requirements of different separation modes, results are controllable, and the specific surface area, the shell thickness and the core-shell ratio can be adjusted. The core-shell filling prepared by virtue of the preparation method is narrow in particle size distribution, relatively large in aperture, intensively distributed, good in monodispersity, low in mass transfer resistance and operation pressure and high in separation speed and can be directly applied to liquid chromatogram analysis.

Description

technical field [0001] The invention relates to the technical field of chemical analysis and separation, and relates to the research and development of a new chromatographic column packing, in particular to a core-shell packing applied to liquid chromatography separation and analysis and a preparation method thereof. Background technique [0002] Chromatographic columns are the "heart" of separation and analysis instruments, so the research on chromatographic column packing has always been a hot spot in this field. Core-shell materials are composed of a solid core and a peripheral porous layer of a certain thickness. The use of core-shell materials as chromatographic column fillers for separation and analysis instruments can improve the shortcomings of existing chromatographic column fillers, such as low solid-phase mass transfer rate of fully porous particles, long sample diffusion time, increased peak broadening, and prolonged separation speed; improve existing chromatogra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/283B01J20/30B01J20/28
CPCB01J20/28021B01J20/28057B01J20/28059B01J20/2808B01J20/283B01J20/3078
Inventor 柯燕雄吴亚玲程玲平何云超何珊珊杜亚军陈龙
Owner EAST CHINA UNIV OF SCI & TECH
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