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Preparation method of graphene covered silica gel

A technology of graphene wrapping and graphene, which is applied in chemical instruments and methods, silicon compounds, and other chemical processes, can solve the problems of long preparation cycle, low graphene bonding amount, and reduced adsorption amount, and achieve simple preparation methods Fast, high graphene content, good adsorption performance

Inactive Publication Date: 2013-01-30
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when pure graphene is directly used as SPE filler, the following problems will also be encountered: graphene will undergo irreversible agglomeration, resulting in a decrease in effective adsorption sites, which in turn will cause a decrease in adsorption capacity and difficulty in desorption; Loss in practical application, which will cause blockage of SPE cartridge and decrease of extraction efficiency
However, in the material prepared by the first method, a large number of adsorption sites of graphene will be occupied by silica gel, resulting in a decrease in the adsorption capacity; in the composite material prepared by the second method, graphene is wrapped on the surface of silica gel, which can effectively solve the problem. However, the method reported in the literature not only has a long preparation cycle, but also uses toxic substances such as hydrazine in the reduction process of graphene oxide, which is not conducive to human health and does not meet the development requirements of green chemistry.
More importantly, due to the harsh dehydration conditions during the reaction, the bonded amount of graphene in the final prepared material is low

Method used

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  • Preparation method of graphene covered silica gel
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  • Preparation method of graphene covered silica gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of graphene-coated silica gel

[0023] First prepare amino silica gel dispersion with a concentration of 7.0 g / mL and graphene oxide dispersion with a concentration of 2.0 g / mL, and then mix the two. After mixing, the concentrations of amino silica gel and graphene oxide are 3.5 g / mL and 1.0 g, respectively. / mL, stir the mixture for 2 h, put the mixture into the reaction kettle, react at 230 °C for 3 h, and use N,N-dimethylformamide to float the reaction product to remove the graphite not wrapped on the silica gel ene, to obtain graphene-wrapped silica gel D (such as figure 2 shown).

[0024] (2) Comparison of materials prepared by the present invention and materials prepared by prior art

[0025] In order to compare with the method of reducing graphene oxide-wrapped silica gel material in the prior art, free graphene oxide is removed before thermal reduction, only graphene oxide-wrapped silica gel is thermally reduced, and graphene-wrapped silica ge...

Embodiment 2

[0027] Preparation of graphene-coated silica gel

[0028] First prepare amino silica gel dispersion liquid with a concentration of 7.0 g / mL and graphene oxide dispersion liquid with a concentration of 1.0 g / mL, and then mix the two. The concentrations of amino silica gel and graphene oxide in the mixed liquid are 3.5 g / mL and 0.5 g / mL respectively. g / mL, stir the mixed solution for 2 h, put the mixed solution in a reaction kettle, react at 230 °C for 3 h, and use N,N-dimethylformamide to float the reaction product to remove the uncoated silica gel. Graphene, get graphene-coated silica gel.

Embodiment 3

[0030] Preparation of graphene-coated silica gel

[0031] Firstly, a dispersion of amino silica gel with a concentration of 7.0 g / mL and a dispersion of graphene oxide with a concentration of 5.0 g / mL were prepared, and then the two were mixed. After mixing, the concentrations of amino silica gel and graphene oxide were 3.5 g / mL and 2.5 g / mL, respectively, and the mixture was stirred for 1 h. The mixture was put into the reactor and reacted at 230 °C for 3 h. The reaction product is then floated with N,N-dimethylformamide to remove the graphene not wrapped on the silica gel to obtain the graphene-wrapped silica gel.

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Abstract

The invention discloses a preparation method of graphene covered silica gel. The method comprises the following steps of: firstly adsorbing graphene oxide on the surface of amino silica gel through an electrostatic adsorption effect; and then carrying out hydrothermal reduction treatment to obtain a material of the graphene covered silica gel. The material has a simple preparation method, is safe and environment-friendly, and has good reproducibility. The material obtained by the preparation method has high graphene content; the prepared graphene covered silica gel material is used as a filler of solid phase extraction (SPE) so as to have the higher adsorption amount when being compared with a document value; and the material is used for a desalting step of enriching peptide in a bovine serum albumin (BSA) enzymolysis solution and analyzing a matrix-assisted laser desorption / ionization time-of-flight mass spectrometry (MALDI-TOFMS), so as to obtain the better effect.

Description

technical field [0001] The invention relates to a preparation method of a graphene-wrapped silica gel material, which belongs to the sample pretreatment technology. Background technique [0002] Graphene is a two-dimensional substance with a hexagonal honeycomb structure composed of a single layer of carbon atoms. Since it was first experimentally prepared in 2004, it has attracted widespread attention from scientists all over the world. Graphene has a large theoretical specific surface area (2630 m 2 / g), so it can provide abundant adsorption sites; graphene is a substance rich in π-electron system, which can produce π-π interaction with substances containing benzene rings; graphene has excellent thermal and mechanical stability properties; graphene is cheap to produce. These advantages make graphene an ideal enrichment material in sample pretreatment. [0003] Solid phase extraction (SPE) has the advantages of high enrichment multiple, high recovery rate, less consumpti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10B01J20/30
Inventor 冯钰锜罗彦波朱钢添
Owner WUHAN UNIV
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