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Preparation method of alkylated modified silica gel

A technology of alkylation modification and silica gel, which is applied in the direction of chemical instruments and methods, silicon oxide, silicon dioxide, etc., can solve the problems of volatile organic solvents, long consumption time, slow reaction rate, etc., and achieve low requirements, The effect of fast reaction speed and low modification cost

Pending Publication Date: 2019-12-13
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The heating and stirring method is relatively seldom used, but it overcomes the problem of complex experimental equipment in the heating and reflux method, but it also has obvious shortcomings, such as slow reaction rate, long time consumption, and large energy consumption. Although it overcomes the problem of complex equipment , but the organic solvent used in the reaction process is volatile under heating conditions, causing pollution
The use of distillation to prepare modified silica gel overcomes the pollution problem caused by the volatilization of organic solvents, but its disadvantages are also obvious, such as slow reaction speed, complex equipment, heating, and large energy consumption. (CN 109603736 A)

Method used

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  • Preparation method of alkylated modified silica gel
  • Preparation method of alkylated modified silica gel

Examples

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Effect test

Embodiment 1

[0027] A preparation method of modified silica gel, specifically comprising the following steps:

[0028] (1) Take 2.5g of silica gel particles (particle size: 150-200 mesh, about 90μm), put the silica gel in 10ml of hydrochloric acid solution (6mol / L), sonicate for 20min, filter, wash until neutral and dry at 60°C Dry for 3 hours.

[0029] (2) Add 4ml of dodecyltrimethoxysilane and 40ml of toluene in sequence in the flask, then place the silica gel prepared in step (1) in it, and put a balloon on the mouth of the flask to prevent water vapor from entering during the reaction. .

[0030] (3) Place the flask in step (2) in an ultrasonic oscillator for 15 minutes and take it out.

[0031] (4) The silica gel in step (3) is filtered and washed with toluene, methanol, and water several times, dried at 60° C. for 2 hours, and then taken out to obtain the modified silica gel material.

[0032] The prepared silica gel was characterized by elemental analysis, and the carbon content ...

Embodiment 2

[0039] A preparation method of modified silica gel, specifically comprising the following steps:

[0040] (1) Take 2g of silica gel particles (particle size is about 200 mesh, about 75μm-90μm), put the silica gel in 100ml of hydrochloric acid solution (2mol / L), ultrasonic for 10min, filter, wash until neutral and bake at 60°C Dry for 3 hours.

[0041] (2) Add 4ml of dodecyltrimethoxysilane and 20ml of toluene in sequence in the flask, then place the silica gel prepared in step (1) in it, and put a balloon on the mouth of the flask to prevent water vapor from entering during the reaction. .

[0042] (3) Place the flask in step (2) in an ultrasonic oscillator for 10 minutes and take it out.

[0043] (4) The silica gel in step (3) is filtered and washed with toluene, methanol, and water several times, dried at 60° C. for 2 hours, and then taken out to obtain the modified silica gel material.

Embodiment 3

[0045] A preparation method of modified silica gel, specifically comprising the following steps:

[0046](1) Take 2.2g of silica gel particles (particle size is about 150 mesh, about 90μm), put the silica gel in 10ml of hydrochloric acid solution (4mol / L), ultrasonic for 12min, filter, wash until neutral and dry at 50°C 2h.

[0047] (2) Add 4ml of dodecyltrimethoxysilane and 30ml of toluene in sequence in the flask, then place the silica gel prepared in step (1) in it, put a balloon on the mouth of the flask, and isolate water vapor from entering during the reaction. .

[0048] (3) Place the flask in step (2) in an ultrasonic oscillator for 15 minutes and take it out.

[0049] (4) The silica gel in step (3) is filtered and washed several times with toluene, methanol, and water, dried at 50° C. for 2 hours, and then taken out to obtain the modified silica gel material.

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Abstract

The invention relates to a preparation method of alkylated modified silica gel. A silanization reagent is taken as a silica gel modifier to carry out surface modification on silica gel under ultrasonic conditions to graft functional groups on the surface of the silica gel, so that the modified silica gel is prepared, wherein the silanization reagent is a methoxy silanization reagent containing C4-C30 alkyl groups. According to the method, the defects of long time consumption and high energy consumption in a silica gel modification method are overcome, and the problems of high energy consumption and low reaction speed caused by using a stirring reflux method are effectively avoided by using an ultrasonic method, so that time cost and expense in practical application are reduced, and the application prospect is wide.

Description

technical field [0001] The invention relates to the technical field of silica gel modification, in particular to a preparation method of alkylation modified silica gel. Background technique [0002] With the rapid development of life sciences, environmental sciences, and pharmaceuticals centered on human health and bioengineering, separation and analysis methods are being used more and more frequently, attracting people's attention. Solid phase extraction (i.e. SPE, the same below) column packing is the "heart" of separation analysis. Research in this area has been very active. At present, a variety of packing matrices have been developed, such as attapulgite, graphite, alumina, di Silicon oxide and other materials, but in all fillers, silica gel-based fillers have an irreplaceable role because of their good mechanical strength, porous structure, large specific surface area and thermal stability, but silica gel itself chooses Adsorption and adsorption capacity are poor, whi...

Claims

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Application Information

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IPC IPC(8): B01J20/30B01J20/10B01J20/22B01D15/08B01J19/10C01B33/14
CPCB01J20/103B01J20/22B01D15/08B01J19/10C01B33/14C01P2004/60C01P2002/82
Inventor 张洛宾许旭刘兆鑫
Owner SHANGHAI INST OF TECH