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Preparation method of oxidized-graphene-modified silica gel chromatography filling material

A technology of silica gel chromatography and graphene, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of uncontrollable graphene oxide content and achieve excellent chromatographic performance

Inactive Publication Date: 2015-05-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the graphene oxide content of the graphene oxide-modified silica gel chromatographic filler prepared by the prior art is uncontrollable, the embodiment of the present invention provides a preparation method of the graphene oxide-modified silica gel chromatography filler

Method used

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  • Preparation method of oxidized-graphene-modified silica gel chromatography filling material
  • Preparation method of oxidized-graphene-modified silica gel chromatography filling material
  • Preparation method of oxidized-graphene-modified silica gel chromatography filling material

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Preparation of Graphene Oxide Modified Silica Gel Chromatography Packing

[0055] Steps:

[0056] ① Put 10g of silica gel and 100mL of hydrochloric acid with a mass fraction of 37% into a reflux condensing device, heat and reflux at 110°C for 4h, then separate the silica gel, wash it with distilled water until neutral, and finally dry it in vacuum at 120°C for 6h to obtain the surface 10g of silica gel containing silanol;

[0057] ②Weigh 0.15g graphene oxide and add it into 100mL distilled water for 2h, centrifuge for 20min to obtain 1.5mg / mL yellowish-brown clear and transparent graphene oxide suspension;

[0058] ③Add 10g of silica gel pellets containing silanol on the surface prepared in step ① to 100g of the graphene oxide suspension prepared in step ②, sonicate for 20min, stir for 2h, wash with distilled water, and then vacuum dry at 60°C for 7h , to obtain micron-scale light gray GO / SiO 2 Small balls 10g;

[0059] ④The above-prepared GO / SiO 2 The pellets were...

Embodiment 2

[0062] Preparation of Graphene Oxide Modified Silica Gel Chromatography Packing

[0063] Steps:

[0064] ① Put 8g of silica gel and 80mL of hydrochloric acid with a mass fraction of 37% into a reflux condensing device, heat and reflux at 100°C for 5h, then separate the silica gel, wash it with distilled water until neutral, and finally dry it in vacuum at 120°C for 7h to obtain the surface Silica gel containing silanol 8g;

[0065] ② Weigh 0.08g graphene oxide and add it into 80mL distilled water for 2h, centrifuge for 20min to obtain 1mg / mL yellowish brown clear and transparent graphene oxide suspension;

[0066] ③ Add 8 g of silica gel pellets containing silanol produced in step ① to 80 g of the graphene oxide suspension prepared in step ②, sonicate for 25 minutes, stir for 3 hours, wash with distilled water, and then vacuum-dry at 70°C for 6 hours. Get micron-scale light gray GO / SiO 2 Small balls 8g;

[0067] ④The above-prepared GO / SiO 2 The microspheres were calcined ...

Embodiment 3

[0070] Preparation of Graphene Oxide Modified Silica Gel Chromatography Packing

[0071] Operation steps: ① Put 15g of silica gel and 150mL of hydrochloric acid with a mass fraction of 37% into a reflux condensing device, heat and reflux at 100°C for 5h, then separate the silica gel, wash it with water until neutral, and finally dry it in vacuum at 120°C for 7h. Obtain 15 g of silica gel containing silanol on the surface;

[0072] ② Weigh 0.15g of graphene oxide and add it to 150mL of distilled water, sonicate for 1.5h, and centrifuge for 20min to obtain a 1mg / mL yellow-brown, clear and transparent graphene oxide suspension;

[0073] ③Add 15g of silica gel pellets containing silanol on the surface prepared in step ① to 150g of the graphene oxide suspension prepared in step ②, stir for 4 hours after ultrasonication for 25 minutes, wash with distilled water, and then vacuum dry at 60°C for 8 hours , to obtain micron-scale light gray GO / SiO 2 Small balls 15g;

[0074] ④The abo...

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Abstract

The invention discloses a preparation method of an oxidized-graphene-modified silica gel chromatography filling material, and belongs to the field of silica gel chromatography filling materials. The preparation method comprises the following steps: adsorbing oxidized graphene to the surface of activated silica gel, and then carrying out a heat treatment under the protection of nitrogen gas so as to fixedly adhere the oxidized graphene to the silica gel surface. The content of the oxidized graphene on the surface of the silica gel chromatography filling material can be controlled by controlling the layers of oxidized graphene which is fixedly adhered to the silica gel surface. In the provided preparation method, the content of carbon on the surface of the silica gel chromatography filling material can be adjusted by controlling the content of oxidized graphene on the surface of the silica gel chromatography filling material so as to meet the application requirements of liquid chromatography, and finally an oxidized-graphene-modified silica gel chromatography filling material with an excellent chromatography performance is obtained.

Description

technical field [0001] The invention relates to the field of silica gel chromatography packing, in particular to a preparation method of graphene oxide modified silica gel chromatography packing. Background technique [0002] Graphene (graphene, abbreviated as G) is a two-dimensional graphite nanomaterial with a thickness of nanometer scale formed by stacking graphene with a single-layer carbon atom planar structure. The extreme case is single-layer graphene. Graphene oxide (graphene oxide, abbreviated as GO) is the oxide of graphene. There are many oxygen-containing groups (such as: C-O-C, C-OH, –-COOH, etc.) on the surface of graphene oxide, which can be easily bonded to the surface of the substrate through chemical reactions. Graphene oxide modified silica gel (GO / SiO 2 ) chromatographic packing is prepared by solidifying graphene oxide onto the surface of silica gel chromatographic packing through a one-step chemical reaction. [0003] At present, the preparation of g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286B01J2220/42B01J2220/4806B01J2220/54
Inventor 郑力军李忠兴李宪文郭方元杨海恩黎晓茸杨棠英谭俊领贾玉琴张涛刘笑春
Owner PETROCHINA CO LTD
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