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Preparation method of hollow carbon nanospheres with internal confined growth MOFs

A nanosphere and hollow carbon technology, applied in nanocarbon, nanotechnology and other directions, can solve the problems of non-conductivity of MOFs materials, unguaranteed material stability, limited application in the field of electrochemistry, etc., and achieve good morphology control. , The effect of low toxicity of materials and uniform size

Active Publication Date: 2020-11-03
YANGZHOU UNIV
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  • 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 internal confined growth MOFs
  • Preparation method of hollow carbon nanospheres with internal confined growth MOFs
  • Preparation method of hollow carbon nanospheres with internal confined growth MOFs

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, add 0.6 g of tetraethylorthosilicate (TEOS) slowly and dropwise to the mixture at a uniform speed, stir mechanically at room temperature, and react for 10 min to form SiO 2 Nanosphere.

[0038] Then, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was mechanically stirred for 24 h at room temperature. After centrifugal washing, the solid phase 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 700℃ for 5h under the protection of argon atmosphere, heating rate is 2℃ / min, then SiO is obtained 2 @C球.

[0040] The calcined SiO 2 @C spheres are dispersed in 50 ml, 2 mol / L sodium hydroxide aqueous solution, etched at 60℃ for 16 h, after the reaction is over, washed with water and ethanol by centrifugation ...

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, and then add 0.6 g of tetraethyl orthosilicate (TEOS) slowly and uniformly into the mixed solution, stir mechanically at room temperature, and react for 10 min to form SiO 2 Nanosphere.

[0049] Then, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was mechanically stirred for 24 h at room temperature. After centrifugal washing, the solid phase is 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 700℃ for 5h under the protection of argon atmosphere, heating rate is 2℃ / min, then SiO is obtained 2 @C球.

[0051] The calcined SiO 2 @C spheres are dispersed in 50 ml, 2 mol / L sodium hydroxide aqueous solution, etched at 60°C for 16 h, after the reaction is over, washed with water and ethanol by centrif...

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, 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 Nanosphere.

[0060] Then, 1 ml of formaldehyde and 0.5 g of resorcinol were added to the above reaction system, and the reaction was mechanically stirred for 24 h at room temperature. After centrifugal washing, the solid phase is 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 700℃ for 5h under the protection of argon atmosphere, heating rate is 2℃ / min, then SiO is obtained 2 @C球.

[0062] The calcined SiO 2 @C spheres are dispersed in 50 ml, 2mol / L aqueous hydroxide solution, etched at 60℃ for 16 h, after the reaction is over, washed with water and ethanol by centrifugation t...

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Abstract

A method for preparing hollow carbon nanospheres with internal confinement growth of MOFs belongs to the field of nanomaterial production technology. Tetraethyl orthosilicate, ethanol, deionized water, ammonia water, resorcinol and formaldehyde are mixed and reacted to obtain SiO 2 @resorcinol‑formaldehyde resin microspheres, then calcined under argon to obtain SiO with core-shell structure 2 @C nanospheres are dispersed in sodium hydroxide aqueous solution and etched to obtain mesoporous hollow carbon nanospheres; finally, mesoporous hollow carbon nanospheres are dispersed in methanol, and metal nitrate and 2-methylimidazole are added for reaction. Hollow carbon nanospheres with internal confinement growth MOFs were obtained. The invention has simple equipment, low cost, simple operation process, low toxicity and harmless materials required in the reaction process, and can effectively control the stoichiometric ratio of multi-component materials, and the obtained products have uniform size, uniform distribution and good shape control .

Description

Technical field [0001] The invention belongs to the technical field of nano material production, and specifically relates to a preparation method of a hollow carbon sphere confined growth MOFs nano material. Background technique [0002] Metal organic framework compounds (MOFs) are a kind of 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 pores, adjustable pore size, and topological structure diversity and tailorability. It has a three-dimensional pore structure. Generally, metal ions are used as connection points and organic ligands support. Constructing a 3D extension of the space, it is another important new type of porous material besides zeolite and carbon nanotubes. It is widely used in catalysis, energy storage and sepa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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