Preparation method of magnetic graphene ternary composites based on click chemistry

A technology of magnetic graphene and composite materials, applied in the field of graphene, which can solve the problems of difficult solid-liquid phase separation, irregular shape, and uneven particle size, and achieve regular shape, uniform particle size, and good dispersion Effect

Inactive Publication Date: 2017-03-01
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yang et al. used surface click functional modification to attack the epoxy groups on the surface of graphene oxide with amino-containing ionic liquid (IL-NH2), and realized the covalent bond functionalization of graphene oxide through affinity ring-opening reaction. Modification, although the graphene prepared by this method overcomes its solubility problem in water and organic media, there are still deficiencies such as solid-liquid phase separation difficulties in the sample processing process (H.Yang, C.Shan, F .Li, et al., Covalent functionalization of polydispersechemically-converted graphene sheets with amine-terminated ionic liquid, Chem.Commun.2009, 3880-3882.)
Yang et al. used edge click functional modification, and the magnetic nano-Fe 3 o 4 The introduction of graphene oxide through non-covalent bonding has prepared a magnetic graphene oxide binary composite material with good solid-liquid separation performance under the action of an external magnetic field. The reaction temperature and the pH of the reaction system are demanding, and the obtained nano-Fe 3 o 4 The particle size is not uniform, the shape is irregular, and its repeatability needs to be further improved (X.Yang, C.Chen, J.Li, et al., Graphene oxide and reduced grapheme oxide-iron oxide hybrid materials for the removal of organic and inorganic pollutants , RSC Adv.2012, 2, 8821.)

Method used

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  • Preparation method of magnetic graphene ternary composites based on click chemistry
  • Preparation method of magnetic graphene ternary composites based on click chemistry
  • Preparation method of magnetic graphene ternary composites based on click chemistry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Magnetic Fe 3 o 4 preparation of

[0023] 1.0g FeCl 3 ·6H 2 O was added to 20mL of ethylene glycol, ultrasonically dispersed at 50°C for 0.5h until the solution was clear; then 3.0g of anhydrous sodium acetate was added, ultrasonically dispersed at 50°C for 0.5h, and then the mixed solution was added to a polytetrafluoroethylene autoclave Reaction at 200°C for 6h. Cool to room temperature, magnetically separate, wash several times with ultrapure water to pH 7.0, then wash several times with ethanol, and vacuum dry at 60°C for 6 hours to obtain magnetic Fe 3 o 4 . Produced Fe 3 o 4 The TEM image of figure 1 As shown, Fe prepared by traditional solvothermal method 3 o 4 The particle size is 300-500nm.

Embodiment 2

[0024] Embodiment 2: magnetic nanometer Fe 3 o 4

[0025] 1.0g FeCl 3 ·6H 2 Add O to 20mL of ethylene glycol, ultrasonically disperse at 50°C for 0.5h until the solution is clear; then add 3.0g of anhydrous sodium acetate, ultrasonically disperse at 50°C for 0.5h, then add 0.4g of sodium hydroxide and 10.0mL of ethylenediamine , ultrasonically disperse at 50°C for 0.5h until the solution is clear; then add the mixed solution into a polytetrafluoroethylene autoclave and react at 200°C for 6h. Cool to room temperature, magnetically separate, wash several times with ultrapure water until the pH is 7.0, then wash several times with ethanol, and vacuum dry at 60°C for 6 hours to obtain magnetic nano-Fe 3 o 4 . The prepared magnetic nano-Fe 3 o 4 The scanning electron microscope image of figure 2 As shown, the Fe prepared by the modified solvothermal method 3 o 4 The particle size is 50-60nm, with regular shape, uniform particle size and good dispersion.

Embodiment 3

[0026] Example 3: Preparation of Amino-modified Magnetic Graphene Ternary Composite Material

[0027] 1.0g FeCl 3 ·6H 2Add O to 20mL of ethylene glycol, ultrasonically disperse at 50°C for 0.5h until the solution is clear; then add 3.0g of anhydrous sodium acetate, ultrasonically disperse at 50°C for 0.5h, then add 0.4g of sodium hydroxide and 10.0mL of ethylenediamine , ultrasonically disperse at 50°C for 0.5h until the solution is clear; add 50mg of carboxylated graphene, ultrasonically disperse at 50°C for 1h, then add the mixed solution into a polytetrafluoroethylene autoclave at 200°C for 6h. Cool to room temperature, magnetically separate, wash several times with ultrapure water until the pH is 7.0, then wash several times with ethanol, and dry in vacuum at 60°C for 6 hours to obtain an amino-modified magnetic graphene ternary composite. The scanning electron microscope picture of the above-mentioned amino modified magnetic graphene ternary composite material is as fol...

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Abstract

The invention relates to a preparation method of a magnetic graphene ternary composite material based on click chemistry. The preparation method comprises the following steps: adding 1.0-5.0 g of trivalent ferric salt to 10-50 ml of reactive solvent, and carrying out ultrasonic dispersion until a solution is clear; then adding 1.0-5.0 g of a stabilizer, carrying out ultrasonic dispersion for 0.1-0.5 h at the temperature of 50-60 DEG C, then adding 0.2-1.0 g of strong alkaline reagent and 5-20.0 mL of amine functional reagent, and carrying out ultrasonic dispersion until the solution is clear; adding 50-100 mg of graphene, carrying out ultrasonic dispersion for 0.3-1 h at the temperature of 50-60 DEG C, and then adding the mixed solution in a polytetrafluoroethylene high-pressure autoclave for reacting for 4-10 h; cooling to room temperature, carrying out magnetic separation, washing with ultrapure water for several times until the pH is 7.0, then washing with ethyl alcohol for several times, and drying to obtain the amino-modified magnetic graphene ternary composite material. The preparation method is simple in technology, controllable in functional group proportion, high in repeatability and the like, the prepared amino-modified magnetic graphene ternary composite material has the advantages of high magnetism, multiple functions and the like, and the prepared amino-modified magnetic graphene ternary composite material is relatively higher in application value and wide in application prospect.

Description

technical field [0001] The invention relates to the field of graphene, in particular to a method for preparing a magnetic graphene ternary composite material based on click chemistry. Background technique [0002] In 2004, graphene (Graphene Oxide, GO) was prepared by Geim and Novoselov, two Russian-born scientists at the University of Manchester, UK, through the tape stripping method. Graphene has excellent electrical, mechanical and thermal conductivity, and there are a large number of Active groups such as carboxyl, hydroxyl, and epoxy groups make it have good hydrophilicity, biocompatibility and easy chemical modification. Graphene, as an emerging carbon nanomaterial, has great potential application value in the pretreatment of sample analysis. Under normal circumstances, graphene is prone to irreversible aggregation and precipitation in water and organic media, which greatly limits the application of graphene. In view of this, the functional modification of graphene i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 赵永纲潘胜东陈晓红金米聪
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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