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Hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and preparation method thereof

A hybrid mesoporous and silica gel technology, applied in chemical/physical processes, ion exchange, ion exchange treatment devices, etc., to achieve the effect of reducing column pressure, good water resistance, and reducing column pressure

Inactive Publication Date: 2011-08-10
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are two main defects in commercially available amino chromatography columns: the proportion of water phase in the mobile phase should not be higher than 25% and the pH range should be 2-8

Method used

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  • Hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and preparation method thereof
  • Hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and preparation method thereof
  • Hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Synthesis of Aminopropyl Hybrid Ordered Mesoporous Silica Gel

[0042] At room temperature, weigh 1.23g of N-trimethyloctadecylammonium chloride and place it in a 100ml round bottom flask, add deionized water 24.0ml, methanol 19.1ml and sodium hydroxide solution (0.66M, 14.0ml) successively, continuously Stir vigorously to make it evenly mixed to obtain a clear and transparent solution. Under vigorous stirring, 1.50ml of 1,2-bis(triethoxysilyl)ethane and 0.35ml of aminopropyltriethoxysilane were added rapidly, and the stirring was continued for 5 hours at room temperature, and then the reaction solution was transferred to poly Stand still at 90°C for 21 hours in a PTFE reaction kettle, filter, wash thoroughly with deionized water, and dry at 90°C under normal pressure for 10 hours to obtain aminopropyl hybrid silica gel, which has a spherical shape with uniform particle size, see figure 1 and figure 2 . Its transmission electron microscope picture is shown in imag...

Embodiment 2

[0044] Synthesis of Aminopropyl Hybrid Ordered Mesoporous Silica Gel

[0045] At about 25°C at room temperature, weigh 1.47g of N-trimethyloctadecylammonium chloride and place it in a 100ml round-bottomed flask, add 28.8ml of deionized water, 22.8ml of methanol and sodium hydroxide solution (0.66M, 17.0 ml) Stir vigorously continuously to make it evenly mixed to obtain a clear and transparent solution. Under vigorous stirring, 1,2-bis(triethoxysilyl)ethane (1.44ml) and 0.66ml of aminopropyltriethoxysilane were added rapidly, and stirring was continued for 4 hours at room temperature, and then the reaction solution was transferred Put it in a polytetrafluoro reactor at 120°C for 16 hours, filter, wash thoroughly with deionized water, and dry at 90°C under normal pressure for 10 hours to obtain aminopropyl hybrid silica gel, which has a spherical shape with uniform particle size.

Embodiment 3

[0047] Solvent extraction to remove templating agent

[0048] Weigh 0.5 g of the spherical aminopropyl hybrid ordered mesoporous silica gel crude product synthesized in Example 2 and suspend in 150 ml of acidic ethanol (200 ml of absolute ethanol contains 3 ml of 36% concentrated hydrochloric acid), stir and react at room temperature for 10 hours, filter , fully washed with absolute ethanol, and dried under normal pressure at 90°C; this operation was repeated once to obtain aminopropyl hybrid ordered mesoporous silica gel.

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Abstract

The invention relates to the chemical technical field of mesoporous material preparation and analysis, in particular to a hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing and a preparation method thereof. The hybrid ordered mesoporous silica gel chromatograph stationary-phase stuffing is characterized in that: hydroxyl connected with silicon atoms on the original hybrid ordered mesoporous silica gel is substituted by aminopropyl. The stuffing has regular and smooth spherical appearance; frameworks of the silicon gel are doped with ethylene radical which has weak hydrophobicity, therefore, the stuffing can not generate silicon gel dissolution phenomenon when being used in flow phase with high aqueous phase proportion and can bear larger pH range (1-11); furthermore, mesoporous pore paths are distributed sequentially, therefore, the mass transfer can be accelerated, and the column pressure is reduced; and the invention is suitable for fast segregation analysis under high aqueous phase proportion.

Description

technical field [0001] The invention relates to the technical field of porous material preparation and analytical chemistry, in particular to a hybrid ordered mesoporous silica gel, which can be used as a chromatographic stationary phase filler. 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. Compared with ordered mesoporous silica gel, hybrid silica gel not only has high specific surface area, regularly arranged pores, narrow pore size distribution, but also has better hydrothermal stability, mechanical stability and chemical stability, and the preparation method It is simple and highly controllable, and shows excellent prospects in the application of chromatographic separation. [0003] Commercial chromatographic column fillers are basically prepared ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26B01D15/08C08G77/18C08J9/26
Inventor 狄斌李纯
Owner CHINA PHARM UNIV
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