A kind of preparation method of carbon hollow microspheres with asymmetric structure

An asymmetric structure, microsphere technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of low purity of carbon hollow spheres, less research on the mechanism of catalyst action, and increase the cost of carbon hollow spheres. And the effect of controllable hollow rate, rich pore size distribution, and large liquid storage capacity

Inactive Publication Date: 2017-03-01
SHANGHAI JIAOTONG UNIV +1
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Problems solved by technology

Since the synthesis of carbon hollow spheres by CVD method generally uses metal oxides as catalysts, but there are few studies on the mechanism of the catalyst, so a large number of by-products are often produced, and the purity of carbon hollow spheres is not high.
Carbon hollow spheres prepared by arc discharge method have high purity, such as Chinese invention patent CN1454839A (a method for preparing hollow carbon spheres by arc discharge method), but the high-voltage arc reaction chamber greatly increases the cost of carbon hollow spheres

Method used

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  • A kind of preparation method of carbon hollow microspheres with asymmetric structure
  • A kind of preparation method of carbon hollow microspheres with asymmetric structure
  • A kind of preparation method of carbon hollow microspheres with asymmetric structure

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preparation example Construction

[0027] A method for preparing carbon hollow microspheres with an asymmetric structure, using the following steps:

[0028] Step 1: Preparation of carbon hollow microsphere precursor slurry

[0029] The carbon hollow microsphere precursor slurry is prepared from a solute and a solvent. The polymer is first added to the solvent, and the slurry is fully stirred and dissolved for degassing, and finally a slurry suitable for the preparation of the carbon hollow microsphere precursor is obtained. The added polymer is any one of cellulose acetate, polysulfone, polyethersulfone or polyvinylidene fluoride, and the solvent is any one of N-methylpyrrolidone, acetone, acetylacetone or dimethylacetamide. The mass ratio of solute and solvent is 10-40:90-60.

[0030] Step 2: Preparation of carbon hollow microsphere precursor

[0031] Carbon hollow microsphere precursors in figure 1 Prepared in the peristaltic pump assisted coaxial microfluidic system shown, the structure of the peristalti...

Embodiment 1

[0037] Step 1: Add 8g of polyethersulfone to 90g of NMP, stir to dissolve and mix evenly, then age and degas to obtain a slurry.

[0038] Step 2: Use deionized water as the non-solvent. The inner tube 6 of the coaxial nozzle has a diameter of 0.15 mm and the outer tube 7 of the coaxial nozzle has a diameter of 0.5 mm. The distance between the coaxial nozzle 5 and the non-solvent tank 8 is set to 10 mm. First open the compressed nitrogen drive pressure system: compressed nitrogen cylinder 2, pressure reducing valve 10, precision pressure gauge 11, screw valve 12, rotameter 13 to deliver the driving pressure within 0.1MP, by adjusting the non-solvent pipeline The rotary valve and the peristaltic pump speed (0.5 rev / min) make the non-solvent in the non-solvent tank 3 smoothly drop out in droplet shape. Then pour the slurry prepared in step 1 into the slurry tank 1, open the screw valve 12 on the slurry pipeline, and adjust the rotameter to reach the driving pressure within the r...

Embodiment 2

[0041] Step 1: Add 28g of polyethersulfone into 60g of NMP, stir to dissolve, mix evenly, age and degas to obtain a slurry.

[0042] Step 2: Use deionized water as a non-solvent. Choose a coaxial nozzle with a diameter of 0.5 mm in the inner tube 6 of the coaxial nozzle and a diameter of 1.2 mm in the outer tube 7 of the coaxial nozzle. Set the coaxial nozzle 5 and the non-solvent tank 8. The distance between them is 50mm. First open the compressed nitrogen drive pressure system: compressed nitrogen cylinder 2, pressure reducing valve 10, precision pressure gauge 11, screw valve 12, rotameter 13 to deliver the driving pressure within 0.1MP, by adjusting the non-solvent pipeline The rotary valve and the peristaltic pump speed (0.5 rev / min) make the non-solvent in the non-solvent tank 3 smoothly drop out in droplet shape. Then pour the slurry prepared in step 1 into the slurry tank 1, open the screw valve 12 on the slurry pipeline, and adjust the rotameter to reach the driving ...

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Abstract

The invention relates to a preparation method of carbon hollow microspheres having a nonsymmetrical structure. The preparation method includes steps of preparation of a precursor slurry material, preparation of a precursor and carbonization sintering. In the method, by means of non-solvent-induced phase separation principle, dropped-off liquid drops of the precursor of the carbon hollow microspheres are collected to enable the outer surface of the dropped-off liquid drops are instantly subjected to phase-separation solidification, thereby effectively avoid deformation and refusion of the liquid drops, to obtain the precursor of the carbon hollow microspheres. The precursor then is subjected to room-temperature drying and carbonization sintering to finally obtain the carbon hollow microspheres. Compared with the prior art, the carbon hollow microspheres are good in degree of sphericity, are controllable in size and porosity, are free of consumption of large amount of energy resources and acid and alkali reagents, are simple in preparation process, and are easy to large-scale industrially produce.

Description

technical field [0001] The invention relates to a method for preparing carbon hollow microspheres, in particular to a method for preparing carbon hollow microspheres with an asymmetric structure. Background technique [0002] Carbon hollow sphere materials have large specific surface area, large pore volume, chemical inertness and excellent mechanical stability. These special properties determine their wide application in the fields of catalysis, adsorbents, electrode materials, capacitors, and energy storage materials. prospect. At present, the methods for preparing carbon hollow spheres are mainly: template method, vapor deposition method, arc discharge method, etc. The template method is the most widely used method for preparing hollow carbon spheres. The template method can be divided into hard template method and soft template method according to its material properties. The template method is the most widely used method for preparing carbon hollow spheres. The temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 郭芳威王国伟江志伟赵晓峰肖平
Owner SHANGHAI JIAOTONG UNIV
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