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Preparation method and application of zero-valent iron/graphene 3D nano-microcapsules

A technology of nano-microcapsules and graphene, which is applied to the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of easy aggregation of particles, and achieve good dispersion, controllable size, and high magnetic saturation strength. Effect

Inactive Publication Date: 2016-08-10
CHONGQING TECH & BUSINESS UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method and application of zero-valent iron / graphene 3D nano-microcapsules, so as to solve the problem that the particles in the nano-microcapsules described in the background technology are easy to agglomerate

Method used

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  • Preparation method and application of zero-valent iron/graphene 3D nano-microcapsules

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Embodiment 1

[0056] S101: According to graphite powder, NaNO 3 and KMnO 4 The mass ratio of H is 2:1:6, H 2 SO 4 , deionized water and H 2 o 2 The volume ratio is 2:3:1 to prepare graphene oxide, specifically: at a concentration of 95% H 2 SO 4 Add graphite powder and NaNO 3 , and placed in an ice-bath environment, vigorously stirred and dispersed until the solution was dark green to obtain a mixed solution a, and the concentration of graphite powder in the mixed solution a was 0.1g / ml;

[0057] S102: Add KMnO to the mixed solution a 4 , stirred at 0°C for 2 hours, after no heat release, raised the temperature to 30°C and continued to stir for 30 minutes to obtain the mixed liquid b;

[0058] S103: Add deionized water to the mixed solution b, heat up to 95° C., stir for 30 minutes and react to obtain the mixed solution c;

[0059] S104: After stopping the heating, add H with a concentration of 30% into the mixed solution c 2 o 2 , stir and react;

[0060] S105: after the reacti...

Embodiment 2

[0068] S201: According to graphite powder, NaNO 3 and KMnO 4 The mass ratio of H is 2:1:6, H 2 SO 4 , deionized water and H 2 o 2 The volume ratio is 3:3:1 to prepare graphene oxide, specifically: at a concentration of 95% H 2 SO 4 Add graphite powder and NaNO 3 , and placed in an ice-bath environment, vigorously stirred and dispersed until the solution was dark green to obtain a mixed solution a, and the concentration of graphite powder in the mixed solution a was 0.15g / ml;

[0069] S202: Add KMnO to the mixed solution a 4 , stirred at 0°C for 2h, after no heat release, raised the temperature to 35°C and continued to stir for 30min to obtain the mixed solution b;

[0070] S203: adding deionized water to the mixed solution b, raising the temperature to 100° C., stirring for 30 minutes and reacting to obtain the mixed solution c;

[0071] S204: After stopping the heating, add H with a concentration of 30% into the mixed solution c 2 o 2 , stir and react;

[0072] S2...

Embodiment 3

[0080] S301: According to graphite powder, NaNO 3 and KMnO 4 The mass ratio of H is 2:1:6, H 2 SO 4 , deionized water and H 2 o 2The volume ratio is 3:3:1 to prepare graphene oxide, specifically: at a concentration of 95% H 2 SO 4 Add graphite powder and NaNO 3 , and placed in an ice-bath environment, vigorously stirred and dispersed until the solution was dark green to obtain a mixed solution a, and the concentration of graphite powder in the mixed solution a was 0.15g / ml;

[0081] S302: Add KMnO to the mixed solution a 4 , stirred at 0°C for 2h, after no heat release, raised the temperature to 40°C and continued to stir for 30min to obtain the mixed liquid b;

[0082] S303: Add deionized water to the mixed solution b, heat up to 98° C., stir for 30 minutes and react to obtain the mixed solution c;

[0083] S304: After stopping the heating, add H with a concentration of 30% into the mixed liquid c 2 o 2 , stir and react;

[0084] S305: after the reaction is comple...

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Abstract

The invention provides a preparation method of zero-valent iron / graphene 3D nano-microcapsules; the preparation method comprises the steps: firstly, respectively oxidating a graphite powder to obtain graphene oxide, and carrying out a hydrolysis reaction of a trivalent iron salt to obtain ferric oxyhydroxide; then treating graphene oxide and ferric oxyhydroxide by an aerosol method to obtain iron oxide / graphene 3D nano-microcapsules; and finally, carrying out high-temperature calcination on the iron oxide / graphene 3D nano-microcapsules in a hydrogen / argon environment to obtain the zero-valent iron / graphene 3D nano-microcapsules. Iron nanoparticles in the iron oxide / graphene 3D nano-microcapsules prepared by the method provided by the invention have good dispersity, are controllable in structure and size, can be stored for a long term and remain stable, and effectively avoid the defects that iron nanomaterials, especially nano zero-valent iron particles, are extremely unstable and are easily passivated and agglomerated. The zero-valent iron / graphene 3D nano-microcapsules prepared by the method can be used in the fields of dye decolorization, heavy metal adsorption and other pollution environmental remediation, as well as magnetic resonance imaging and other magnetic materials.

Description

technical field [0001] The invention relates to the technical field of graphene self-assembly, and more specifically, to a preparation method and application of a zero-valent iron / graphene 3D nanocapsule. Background technique [0002] Nano-sized zero-valent iron materials are cheap, easy to obtain, environmentally friendly, and have excellent catalytic performance and magnetic characteristics, and have received extensive attention in recent years. With the deepening of research, the following problems generally exist in the use of nano-zero-valent iron materials: 1) The particles are prone to deformation or even broken during the synthesis process, especially in high-temperature and high-pressure environments; Gravity, magnetism and other reasons are prone to agglomeration, so the dispersion is poor; 3) The resistance of the particles to changes in the external environment is weak, especially in environments such as strong acid and strong corrosion. At the same time, the par...

Claims

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Application Information

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IPC IPC(8): B01J13/02B22F9/22B22F1/02B01J23/745B01J20/30B01J20/20B01J20/28C02F1/28C02F101/20C02F101/30
CPCB01J13/02B01J20/02B01J20/20C02F1/281B01J20/28009B01J23/745B22F9/22C02F2101/308C02F2101/20C02F2101/36B22F1/16
Inventor 吕晓书张玉玲蒋光明张贤明
Owner CHONGQING TECH & BUSINESS UNIV
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