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Preparation method for Fe3O4/GO magnetic composite material

A technology of magnetic composite materials and magnetic microspheres, applied in the direction of microsphere preparation, chemical instruments and methods, microcapsule preparations, etc., can solve problems such as difficult operation, and achieve mild conditions, good enrichment efficiency, and excellent enrichment capacity Effect

Inactive Publication Date: 2014-10-01
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when purely using GO as a solid-phase extraction adsorbent for the enrichment of trace organics in environmental water samples and biological samples, there are obvious shortcomings that are difficult to operate.

Method used

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  • Preparation method for Fe3O4/GO magnetic composite material
  • Preparation method for Fe3O4/GO magnetic composite material
  • Preparation method for Fe3O4/GO magnetic composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation of Fe 3 o 4 / GO-A

[0045] 20mg Fe 3 o 4 / SiO 2 / SH and 10mg GO were added to 60mL aqueous solution with pH 10.0, ultrasonically dispersed for 5min, then mechanically stirred at 60°C for 6h, then the reaction was stopped and the Fe 3 o 4 / GO was separated from the supernatant, washed 3 times with water and dried in vacuum to obtain a Fe 3 o 4 / GO magnetic composite material Fe 3 o 4 / GO-A.

[0046] Wherein the external magnet is to place a magnet outside the bottom of the beaker; the magnetic microspheres modified by thiol (Fe 3 o 4 / SiO 2 / SH) particle size is about 200nm.

Embodiment 2

[0048] Preparation of Fe 3 o 4 / GO-B

[0049] 20mg Fe 3 o 4 / SiO 2 / SH and 10mg GO were added to 60mL aqueous solution with pH 7.0, ultrasonically dispersed for 5min, then mechanically stirred at 90°C for 6h, then the reaction was stopped and the Fe 3 o 4 / GO was separated from the supernatant, washed 3 times with water and dried in vacuum to obtain another Fe 3 o 4 / GO magnetic composite material Fe 3 o 4 / GO-B.

[0050] Wherein the external magnet is to place a magnet outside the bottom of the beaker; the magnetic microspheres modified by thiol (Fe 3 o 4 / SiO 2 / SH) particle size is about 200nm.

[0051] The synthetic reaction schematic diagram of above-mentioned embodiment 1 and embodiment 2 sees figure 1 .

[0052] To the Fe obtained in above-mentioned embodiment 1 and embodiment 2 3 o 4 / GO magnetic composites were analyzed and tested, and their characterizations are as follows.

[0053] SEM analysis

[0054] Fe 3 o 4 / GO-A and Fe 3 o 4 / SEM images ...

Embodiment 3

[0067] Magnetic solid phase extraction of aromatic amines

[0068] First, weigh 10mg Fe 3 o 4 / GO was added to a 150mL water sample with a pH of 5.0, and the aromatic amine and Fe 3 o 4 / GO binding and capture to the solid surface. In order to capture the aromatic amine more completely, the mixture was first ultrasonicated for 2 min, and then placed in a water bath at 20°C for 15 min to equilibrate. Then a magnet is added to move the Fe 3 o 4 The / GO-arylamine complex was separated from the water sample, and the aromatic amine was desorbed with 2 mL of acetonitrile (1% NaOH).

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Abstract

The invention provides a preparation method for a ferroferric oxide / graphene oxide (Fe3O4 / GO) magnetic composite material. Go is bonded on the surface of a magnetic microsphere modified by sulfydryl through a click chemical synthesis method by using a lot of epoxy active groups contained on the surface of the GO. A preparation process comprises the following steps: adding the sulfydryl modified magnetic microsphere Fe3O4 / SiO2 / SH and the GO into a water solution with the pH (Potential of Hydrogen) of 6.5-10.0; carrying out ultrasonic dispersion, reacting at 60-100 DEG C and stirring; after reaction is completely stopped, applying a magnetic field to separate the Fe3O4 / GO from liquid; and finally, washing with the water, and drying in vacuum. The preparation method is simple and rapid and moderate in conditions; a lot of Fe3O4 / GO magnetic composite materials coated by the GO are successfully prepared. Particularly, the surface of Fe3O4 / GO-B of the Fe3O4 / GO magnetic composite material which is prepared when the pH of the water solution is 6.5-7.5 has a very thick graphene oxide coating and the enrichment capacity is better.

Description

technical field [0001] The present invention relates to graphene oxide (Graphene Oxide, GO), specifically graphene oxide magnetic composite material, more specifically Fe 3 o 4 / GO magnetic composite materials preparation method. Background technique [0002] Graphene oxide (Graphene Oxide, GO) is a product obtained by chemical oxidation and hydrolysis of reduced graphite powder. GO has the advantages of excellent electrical, mechanical and thermal conductivity, and there are a large number of hydroxyl, carboxyl, and epoxy active groups on its surface. [1,2] And other active groups, so it has good hydrophilicity, biocompatibility and easy chemical modification. GO can have strong π-π, hydrogen bonding and electrostatic interactions with trace analytes in environmental and biological samples, making it an ideal choice for solid-phase extraction materials [3-8] . However, when purely using GO as a solid-phase extraction adsorbent for the enrichment of trace organics in en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30B01J20/28B01J13/02
Inventor 卢昕刘晓菲陈丽红
Owner GUANGXI NORMAL UNIV
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