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Silica based material

A technology of silicon dioxide and base material, applied in the direction of silicon dioxide, silicon oxide, other chemical processes, etc., can solve problems such as low mechanical stability

Inactive Publication Date: 2011-05-11
AKZO NOBEL CHEM INT BV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mechanical stability of these two types of hybrid particles is much less than that of pure silica particles

Method used

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  • Silica based material
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] Embodiment 1 (preparation of organically modified silica-based material)

[0079] Add 21.50 mL of methyltrimethoxysilane to 300 mL of Milli-Q-water at room temperature. Add 30.00g of silicon dioxide particles (Kromasil) with an average particle size of 5 microns, an average pore diameter of 120 angstroms and a specific surface area of ​​320 square meters per gram. ), and heat the mixture to 95°C. This temperature was maintained for 3 hours. Then reduce the temperature to 80 °C and add 21 ml of 25% NH 3(aq) . This temperature was maintained for 2 hours. Afterwards, lower the temperature to room temperature and add 21 ml of 65% HNO 3(aq) . The mixture was heated to 95°C and maintained at this temperature for 88 hours, after which the mixture was filtered and washed with Milli-Q-water, tetrahydrofuran (THF) and acetone. Finally the material was dried at 90°C for 4 hours.

[0080] The carbon content was determined by elemental analysis to be 3.9% by weight.

Embodiment 2

[0081] Embodiment 2 (preparation of organically modified silica-based material)

[0082] 40.5 milliliters (33-36) of ethyltrimethoxysilane was added to 50 grams of silica particles (Kromasil 100 Angstroms) in 500 ml of Milli-Q-water. The mixture was heated to 98°C and maintained at this temperature for 16 hours. Cool the temperature below 40°C, filter and wash with Milli-Q-water and acetone. The material was dried at 90°C for 4 hours.

[0083] The carbon content was determined by elemental analysis to be 7.1% by weight.

Embodiment 3

[0084] Embodiment 3 (preparation of organically modified silica-based material)

[0085] The product of Example 2 was dispersed in Milli-Q-water, and the mixture was placed in an autoclave, the temperature was raised to 130° C. and maintained for 72 hours. The temperature was then cooled to below 40°C, filtered and washed with Milli-Q-water and acetone. The material was dried at 90°C for 4 hours.

[0086] The carbon content was determined by elemental analysis to be 7.1% by weight.

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Abstract

An organo-modified silica based material to be used for making a stationary phase for liquid chromatography comprising a part which is unmodified silica, and a part which is silica comprising organic groups bonded to the silica. A method for preparing an organo-modified silica based material comprising mixing in an aqueous medium a silica based material and an organosilane compound, and reacting the mixture. A stationary phase separation material prepared by functionalising the organo-modified silica based material is also disclosed.

Description

technical field [0001] The present invention relates to organomodified silica-based materials, and methods of preparing organomodified silica-based materials. The invention also relates to the use of organically modified silica-based materials for preparing stationary phase separation materials, methods for preparing stationary phase separation materials, stationary phase separation materials, and uses of stationary phase separation materials in chromatographic separation methods. Background technique [0002] Chromatographic stationary phase separation materials used in liquid chromatography are often based on porous supports on which silica has been functionalized in order to achieve the desired separation characteristics for some of the analytes to be separated. A common type of functionalization is the preparation of hydrophobic stationary phases, such as C18-phases, where octadecylsilane is often used as a functionalizing agent and reacts with silanol groups on porous s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/32B01J20/286B01J20/287
CPCB01J20/286B01J20/287B01J20/3242B01J20/3285B01J20/28061B01J20/3078B01J20/3227B01J20/3246B01J20/3257B01J20/3259B01J20/3261B01J2220/54B01J20/3092B01J2220/58B01J2220/82B01J20/28042B01J20/103B01J20/28083B01J20/28016B01J20/3204B01J20/32C01B33/12
Inventor J·艾克罗斯
Owner AKZO NOBEL CHEM INT BV