Novel hydrophilic alkyl bonded silica gel filler preparation method

A technology of bonding silica gel and hydrophilic alkanes, which is applied in the field of liquid chromatography packing preparation, can solve the problems of a large amount of organic solvent consumption, tedious derivation preparation process, etc., and achieve the effect of reducing the amount of solvent

Inactive Publication Date: 2018-12-28
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the shortcomings of this type of packing are: cumbersome derivatization preparation process and a large amount of organic solvent consumption

Method used

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  • Novel hydrophilic alkyl bonded silica gel filler preparation method
  • Novel hydrophilic alkyl bonded silica gel filler preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A. Covalent bonding of octyldimethylsilane to silica gel In an inert atmosphere, take 100 g of silica gel (Fuji silica gel, diameter 10 μm, specific surface area 350 m 2 / g) was mixed with 20 mL of pyridine in 400 mL of benzene, preheated to 100 °C, azeotroped for 6 h and then removed to obtain a silica gel suspension; 21.7 g of octyldimethylchlorosilane was weighed and dissolved in 50 mL Add dropwise silica gel suspension to toluene, ensure that the dropping is completed within 1 hour, and heat to reflux after dropping for 24 hours; B. Covalent bonding of octamethylcyclotetrasiloxane and silica gel Into the reaction solution prepared in step A, 32 g of octamethylcyclotetrasiloxane was added at one time, and the reaction was refluxed for 48 hours; C. Iodotrimethylsilane shields the silanol groups, weighs 28g of iodotrimethylsilane and dissolves it in 50 mL of benzene, drops it into the mixed solution prepared in step B, and adds it for 2 hours, and refluxes it for 12 ho...

Embodiment 2

[0030] A. Covalent bonding of octadecyldimethylsilane to silica gel In an inert atmosphere, take 50 g of silica gel (Daiso silica gel, diameter 10 μm, specific surface area 450 m 2 / g) mixed with 11mL pyridine in 200 mL xylene, preheated to 100 °C, azeotroped for 6 h, and then removed the water to obtain a silica gel suspension; weigh 24g octadecyldimethylsilane and dissolve it in 25mL toluene Add the silica gel suspension dropwise to ensure that the dripping is completed within 0.5h, and then heat to reflux after the dripping, and keep for 24h;

[0031] B. Covalent Bonding of Hexamethylcyclotrisiloxane to Silica Gel

[0032] Into the reaction solution prepared in step A, 15 g of hexamethylcyclotrisiloxane was added at one time, and the reaction was refluxed for 24 hours;

[0033] C. Hexamethyldisilazane masking of silanol

[0034] Weigh 15g of hexamethyldisilazane and dissolve it in 25mL of benzene, drop into the mixed solution prepared in step B for 1 h, and reflux for 2...

Embodiment 3

[0036] A. Covalent bonding of butyldimethylsilane to silica gel In an inert atmosphere, take 250 g of silica gel (Fuji silica gel, 10 μm in diameter, 350 m 2 / g) mixed with 55mL pyridine in 1.0L toluene, preheated to 100 °C, azeotroped for 6 h, and then removed water to obtain a silica gel suspension; weigh 53g butyldimethylsilane and dissolve it in 120mL benzene, drop Add the silica gel suspension, ensure that the dripping is completed within 2 hours, and heat to reflux after the dripping, and keep for 24 hours;

[0037] B. Covalent Bonding of Decamethylcyclopentasiloxane to Silica Gel

[0038] Into the reaction solution prepared in step A, 97 g of decamethylcyclopentasiloxane was added at one time, and the reaction was refluxed for 48 hours;

[0039] C. Trimethylchlorosilane masking silanol

[0040] Weigh 40g of trimethylchlorosilane and dissolve it in 25 mL of benzene, drop into the mixed solution prepared in step B, the dropwise addition time is 1 h, and reflux for 24...

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Abstract

The invention discloses a novel hydrophilic alkyl bonded silica gel filler preparation method. The method comprises the steps that alkylchlorosilane is used as silica gel to introduce bonded alkyl, polymethylcyclopolysiloxane is supported on the silica gel, finally, a conventional micromolecule endcapping agent is used for masking residual silicon hydroxyl, and the hydrophilic alkyl bonded silicagel filler is obtained; due to the fact that for the prepared chromatographic filler, the preparation technology adopts a one-pot multi-step reaction, multiple times of filtering and drying are avoided, and the solvent dosage is reduced; the filler contains rich silyl ether bonds, it can be ensured that the filler can be fully infiltrated in water, and the method is more suitable for separation ofmacromolecules such as polypeptide and protein.

Description

technical field [0001] The invention belongs to the field of liquid chromatography filler preparation, and in particular relates to a preparation method of a hydrophilic alkyl-bonded silica gel filler without polar groups. Background technique [0002] Alkyl bonded silica gel is widely used in reversed-phase chromatography packing due to its excellent chemical inertness and stability, and convenient and mature preparation process. For non-polar lipophilic analytes, conventional alkyl-bonded silica gel has excellent performance; when the analyte is strongly polar or even hydrophilic, the retention capacity of this type of packing cannot meet the existing needs. In actual operation, the retention capacity of this type of packing is often improved by reducing the proportion of the organic phase in the mobile phase. Even so, this type of packing cannot be used for separation and analysis in a pure water environment because they cannot be wetted by water. Therefore, The developm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/287B01D15/32
CPCB01D15/325B01J20/287
Inventor 张明亮韩海峰范大双张大兵
Owner JIANGSU HANBON SCI & TECH CO
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