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Preparation method of hollow carbon nanospheres with MOFs (metal-organic frameworks) formed through limited-range growth inside

A technology of nanospheres and hollow carbon, which is applied in the direction of nanocarbon and nanotechnology, can solve the problems of MOFs materials without conductivity, material stability cannot be guaranteed, and limit the application of electrochemical fields, so as to achieve good shape control , material low toxicity, uniform size effect

Active Publication Date: 2017-12-29
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, MOFs materials are not conductive, which limits their application in the field of electrochemistry
The small size of MOFs materials makes it difficult to separate them from the reaction system
In addition, MOFs materials have poor stability in strong acid and strong alkaline solvents, which will cause the decomposition of MOFs. When used as adsorbents, catalysts, catalyst supports, drug sustained release carriers or lithium-ion battery electrode materials, the stability of the materials is improved. less than guaranteed

Method used

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  • Preparation method of hollow carbon nanospheres with MOFs (metal-organic frameworks) formed through limited-range growth inside
  • Preparation method of hollow carbon nanospheres with MOFs (metal-organic frameworks) formed through limited-range growth inside
  • Preparation method of hollow carbon nanospheres with MOFs (metal-organic frameworks) formed through limited-range growth inside

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Synthesis of mesoporous hollow carbon nanospheres:

[0037] Mix 75 ml of ethanol, 30 ml of deionized water and 3 ml of ammonia water, add 0.6 g of tetraethyl orthosilicate (TEOS) dropwise into the mixture at a constant speed, stir mechanically at room temperature, and react for 10 min to form SiO 2 nanospheres.

[0038] Next, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was carried out under mechanical stirring for 24 h at room temperature. The solid phase after centrifugal washing was dried at 60°C for 12 hours to form SiO 2 @resorcinol-formaldehyde resin.

[0039] The dried SiO 2 @Resorcinol-formaldehyde resin is calcined at a high temperature of 700°C for 5h under the protection of argon atmosphere, and the heating rate is 2°C / min to obtain SiO 2 @Cball.

[0040] Calcined SiO2 @C spheres were dispersed in 50 ml, 2 mol / L sodium hydroxide aqueous solution, etched at 60°C for 16 h, washed with water and e...

Embodiment 2

[0047] 1. Synthesis of mesoporous hollow carbon nanospheres:

[0048] Mix 75 ml of ethanol, 30 ml of deionized water and 3 ml of ammonia water, then slowly add 0.6 g of tetraethyl orthosilicate (TEOS) dropwise into the mixed solution at a uniform speed, stir mechanically at room temperature, and react for 10 min to form SiO 2 nanospheres.

[0049] Next, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was carried out under mechanical stirring for 24 h at room temperature. The solid phase after centrifugal washing was dried at 60°C for 12 hours to form SiO 2 @resorcinol-formaldehyde resin.

[0050] The dried SiO 2 @Resorcinol-formaldehyde resin is calcined at a high temperature of 700°C for 5h under the protection of argon atmosphere, and the heating rate is 2°C / min to obtain SiO 2 @Cball.

[0051] Calcined SiO 2 @C spheres were dispersed in 50 ml, 2 mol / L sodium hydroxide aqueous solution, etched at 60°C for 16 h, wa...

Embodiment 3

[0058] 1. Synthesis of mesoporous hollow carbon nanospheres:

[0059] Mix 75 ml of ethanol, 30 ml of deionized water and 3 ml of ammonia water, add 0.6 g of tetraethyl orthosilicate (TEOS) slowly and dropwise to the mixed solution at a uniform speed, stir mechanically at room temperature, and react for 10 min to form SiO 2 nanospheres.

[0060] Next, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was carried out under mechanical stirring for 24 h at room temperature. The solid phase after centrifugal washing was dried at 60°C for 12 hours to form SiO 2 @resorcinol-formaldehyde resin.

[0061] The dried SiO 2 @Resorcinol-formaldehyde resin is calcined at a high temperature of 700°C for 5h under the protection of argon atmosphere, and the heating rate is 2°C / min to obtain SiO 2 @Cball.

[0062] Calcined SiO 2 @C spheres were dispersed in 50 ml, 2mol / L aqueous hydroxide solution, etched at 60°C for 16 h, washed three t...

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Abstract

The invention discloses a preparation method of hollow carbon nanospheres with MOFs (metal-organic frameworks) formed through limited-range growth inside and belongs to the technical field of nanomaterial production. Tetraethyl orthosilicate, ethanol, deionized water, ammonium hydroxide, resorcinol and methanol are mixed for a reaction, SiO2@resorcinol-formaldehyde resin microspheres are obtained and calcined in argon, SiO2@C nanospheres with a core-shell structure are obtained and dispersed in a sodium hydroxide water solution to be etched, and mesoporous hollow carbon nanospheres are obtained; finally, the mesoporous hollow carbon nanospheres are dispersed in methanol, metallic nitrates and 2-methylimidazole are added for a reaction, and the hollow carbon nanospheres with MOFs formed through limited-range growth inside are obtained. Equipment used in the method is simple, the method is low in cost and simple in operation process, materials required in the reaction process are low in toxicity and harmless, the stoichiometric ratio of multi-component materials can be effectively controlled, and the obtained products are uniform in size, uniformly distributed and are good in morphological control.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial production, and in particular relates to a method for preparing hollow carbon sphere confined growth MOFs nanomaterials. Background technique [0002] Metal-organic frameworks (MOFs) are coordination polymers that have developed rapidly in the past decade. They refer to crystalline porous materials with periodic network structures formed by self-assembly of transition metal ions and organic ligands. It has the advantages of high porosity, low density, large specific surface area, regular pore channels, adjustable pore size, diversity of topology and tailorability, etc. It has a three-dimensional pore structure, generally with metal ions as connection points, supported by organic ligands. Constituting a 3D extension of space, it is another important new type of porous material besides zeolite and carbon nanotubes, which are widely used in catalysis, energy storage and separation. At present, ...

Claims

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Application Information

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IPC IPC(8): C08G83/00C01B32/15B82Y40/00
CPCB82Y40/00C01P2004/04C01P2004/62C01P2004/64C01P2006/16C08G83/008
Inventor 陈铭李文龙周克寒曹圣平张秀娥赵荣芳吴倩卉沈超
Owner YANGZHOU UNIV
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