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Method for synthesizing carbon micron-spheres

A carbon sphere and micron technology, applied in the field of hollow or solid micron carbon spheres, can solve the problems of wide size distribution, difficult to accurately control physical parameters, and complicated operation.

Inactive Publication Date: 2010-11-03
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Among the above synthetic methods, although the size of the carbon spheres obtained by the self-assembly template method is very uniform, the method is cumbersome to operate and has many steps.
And this method needs to remove the inert carrier polystyrene, from the perspective of economic benefits, this method cannot be promoted on a large scale
The size distribution of carbon spheres prepared by the remaining methods is relatively wide. From the perspective of application, carbon spheres with non-uniform size distribution are limited in some applications, such as: drug release, catalyst carrier, etc.
The arc discharge method requires expensive devices, and the equipment investment is huge.
In addition, the above-mentioned synthetic methods are all batch operations. The disadvantage of batch reactions is that it is difficult to accurately control the physical parameters of the synthesis, such as stirring speed, temperature and time, etc., which leads to a certain degree of difference in the properties of each batch of products.

Method used

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  • Method for synthesizing carbon micron-spheres
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  • Method for synthesizing carbon micron-spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 1 g of furfuryl alcohol into 9 g of toluene, and stir evenly to obtain a 10% furfuryl alcohol solution. Next, add 10 g of concentrated sulfuric acid into water, stir and dissolve to obtain a 5 mol / L sulfuric acid solution. The furfuryl alcohol solution and the sulfuric acid solution were transported into a polyvinyl chloride capillary microreactor with a size of 0.5 mm by using two syringe pumps with a two-phase volume flow ratio of 80, wherein the inlet channel size of the furfuryl alcohol solution was 0.5 mm, and the sulfuric acid solution was The inlet channel size of the solution was 0.1 mm. The temperature of the oil bath for the pre-polymerization reaction was controlled to be 80°C, and the reaction time was 100s; the reaction was continued, the temperature was controlled to be 30°C, and the reaction time was 80h; the product was obtained. The reaction product was centrifuged, washed with absolute ethanol and n-hexane, baked in an oven at 30°C for 24 hours, a...

Embodiment 2-3

[0023] Embodiment 2-3 (oil phase kind)

[0024] Adopt the same method as Example 1 to carry out the test, but adopt different water-insoluble oil phases to prepare 10% furfuryl alcohol solution. The furfuryl alcohol solution was prepared with ethyl acetate and fatty acid methyl ester respectively, and the products obtained by the reaction were designated as samples A2 and A3, respectively. The average size of the obtained hollow carbon spheres was 210 and 208 μm, and the wall thickness was 20 and 18 μm, respectively, by scanning electron microscope characterization. It can be seen that under the same reaction conditions, changing the type of oil phase has no significant effect on the average size and wall thickness of the final hollow carbon spheres.

Embodiment 4-8

[0025] Embodiment 4-8 (kind and concentration of acid)

[0026] Experiments were carried out in the same manner as in Example 1, but with changes in the type and concentration of the acid catalyst. Prepare 8, 10, 8, 10, 18 mol / L aqueous acid catalyst solutions with acetic acid, hydrochloric acid, phosphoric acid, nitric acid and p-toluenesulfonic acid respectively, and the products obtained by the reaction are respectively designated as samples A4, A5, A6, A7 and A8. The average size of the hollow carbon spheres was 300, 400, 543, 354, and 376 μm, and the wall thicknesses were 15, 35, 55, 64, and 55 μm, respectively, by scanning electron microscopy. It can be seen that under the same reaction conditions, changing the type and concentration of the acid catalyst will lead to changes in the size and wall thickness of the prepared hollow carbon spheres.

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Abstract

The invention relates to a method for synthesizing carbon micron-spheres. The method comprises the following steps: dissolving furfuryl alcohol in a water-insoluble oil phase to prepare an oil phase solution; dissolving acid catalyst in water to prepare a water phase solution; delivering the oil phase solution and the water phase solution into a micro-reactor from the two inlets of the microstructure reactor to ensure that the furfuryl alcohol solution and the acid catalyst solution form water-in-oil two-phase droplet flow in the passage of the microstructure reactor; pre-polymerizing the formed droplet flow, keeping on reaction, and collecting reaction products; and centrifuging, cleaning, drying and heating the reaction products to obtain the carbon micron-spheres, wherein the carbon micron-spheres have narrower particle size distribution, and the average particle size is continuously adjustable between 150 and 600 mu m. The preparation process has simple operation, and the size and the wall thickness of the carbon-spheres can be adjusted conveniently.

Description

technical field [0001] The invention relates to a method for synthesizing micron carbon spheres, in particular to a new method for continuously preparing hollow or solid micron carbon spheres with uniform size in one step using a microstructure reactor, and belongs to the technical field of preparation methods of inorganic non-metallic materials. Background technique [0002] Carbon material is a material with high chemical stability, low density and good high temperature and heat resistance. At present, hollow carbon sphere materials can be used as drug release carriers, selective gas adsorbents, catalyst supports, lubricant materials, hydrogen storage materials, and electrode materials for lithium batteries, etc., so they have received great attention. [0003] At present, there are many methods for preparing hollow and solid carbon spheres, such as: self-assembly template method, vapor deposition, dielectric reduction, polymer pyrolysis, and arc discharge. CN 101177253A ...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 张利雄潘宜昌居敏花徐南平
Owner NANJING UNIV OF TECH
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