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Method for preparing hollow carbon ball

A technology of hollow and carbon spheres, applied in the direction of carbon preparation/purification, etc., can solve problems such as simple, undiscovered process, and carbon sphere cracking, and achieve the effect of simple process route, overcoming complex process, and few process steps

Inactive Publication Date: 2014-06-25
CHANGZHOU ZHONGKE HAINA CARBON TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can synthesize hollow carbon spheres with good sphericity and controllable hollowness, the decomposition of polystyrene easily leads to the collapse of carbon spheres during the carbonization process.
In general, by tracking previous literature and patent reports, no method has been found that has a simple process and can be industrially prepared to produce hollow carbon spheres with good sphericity and controllable hollowness

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Prepare a 1% (mass ratio) polyvinyl alcohol aqueous solution at 25°C and stir evenly. Pour 100g of phenolic resin particles (particle size: 20 mesh; softening point: 90°C), 3g of hexamethylenetetramine and 500g of 1% (mass ratio) polyvinyl alcohol aqueous solution into the autoclave at the same time. In the autoclave, stir at a rate of 400 rpm and heat to 110° C. at a heating rate of 1° C. / min, and then keep the temperature for 0.5 hours. Cool naturally, filter, wash, and dry at 110°C. Put 100 g of hollow phenolic resin balls obtained above into a carbonization activation furnace, use nitrogen as a protective gas, heat up to 800 °C at a heating rate of 1 °C / min, and then heat it up to 800 °C at a constant temperature at 0.1 m 3 / h flow rate into the water vapor to activate the resin ball for 0.5 hours. Cool naturally to room temperature to get hollow carbon spheres, sphericity: 95%, hollowness: 85%, ball diameter: 1.5mm, specific surface area: 752m 2 / g.

Embodiment 2

[0019] Prepare a 3% (mass ratio) sodium dodecylsulfonate aqueous solution at 30°C and stir evenly. Pour 100g of phenolic resin particles (particle size: 30 mesh; softening point: 95°C), 5g of hexamethylenetetramine and 1000g of 3% (mass ratio) polyvinyl alcohol aqueous solution into the autoclave at the same time. In the autoclave, stir at a rate of 450 rpm and heat to 115° C. at a heating rate of 1.5° C. / min, and then keep the temperature for 1 hour. Cool naturally, filter, wash, and dry at 110°C. Put 100g of hollow phenolic resin balls obtained above into a carbonization activation furnace, use nitrogen as a protective gas, heat up to 810°C at a heating rate of 2°C / min, and then 3 / h flow rate into the water vapor to activate the resin ball for 3 hours. Cool naturally to room temperature to get hollow carbon spheres, sphericity: 95.5%, hollowness: 82%, ball diameter: 1.2mm, specific surface area: 784m 2 / g.

Embodiment 3

[0021] Prepare a 5% (mass ratio) aqueous solution of methyl pentanol at 35°C and stir evenly. Pour 100g of phenolic resin particles (particle size: 40 mesh; softening point: 80°C), 7g of NL curing agent and 800g, 5% (mass ratio) of polyvinyl alcohol aqueous solution into the autoclave at the same time. In the autoclave, stir at a rate of 380 rpm and heat to 110° C. at a heating rate of 0.5° C. / min, and then keep the temperature for 1.5 hours. Cool naturally, filter, wash, and dry at 110°C. Put 100 g of hollow phenolic resin balls obtained above into a carbonization activation furnace, use nitrogen as a protective gas, heat up to 820 °C at a heating rate of 2.5 °C / min, and then heat it at a constant temperature at 0.5 m 3 / h flow rate into the water vapor to activate the resin ball for 2 hours. Cool naturally to room temperature to get hollow carbon spheres, sphericity: 97%, hollowness: 76%, ball diameter: 0.9mm, specific surface area: 790m 2 / g.

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Abstract

The invention relates to a method for preparing carbon balls and in particular relates to a method for preparing a phenolic resin-based hollow carbon ball. The method comprises the following steps: simultaneously adding curing agent-free thermoplastic phenolic resin particles, a curing agent and an aqueous solution containing 1-10wt% of dispersing agent into an autoclave according to a mass ratio of 100:3-20:500-1500, heating to the temperature of 110-130 DEG C at a temperature rise rate of 0.5-5 DEG C / min while stirring; and keeping constant temperature for 0.5-3 hours; naturally cooling, filtering and drying to obtain the hollow phenolic resin ball; and finally, heating to the temperature of 800-1000 DEG C in a carbonization and activation furnace at a temperature rise rate of 0.5-5 DEG C / min by taking 100g of the hollow phenolic resin ball as reference, and keeping the constant temperature for 0.5-3 hours; and naturally cooling to obtain the hollow carbon ball. The hollow carbon ball prepared by the method is simple in process and high in yield and has high degree of sphericity and large sphere diameter, and the hollowness degree is easily regulated. The problems that the process is complex, the degree of sphericity is low, the hollowness degree is difficult to regulate and the like in the process of preparing the hollow carbon ball at present are solved, so that the hollow carbon ball is widely applied to the fields such as drug sustained release and catalyst carriers.

Description

technical field [0001] The invention relates to a method for preparing carbon spheres, in particular to a method for preparing phenolic resin-based hollow carbon spheres. Background technique [0002] Hollow carbon spheres have good thermal and chemical stability, light weight and good compression resistance, so they are widely used in slow-release materials, adsorption materials, lubricants, catalyst carriers, heat insulation materials and other fields. There are many methods for preparing hollow carbon spheres, such as metal reduction, supercritical, chemical vapor deposition, template and other methods. Its key technology is the control of sphericity and hollowness. Liu Boyang (patent publication number: CN1821068A) and others used ferrocene and ammonium chloride as raw materials, and prepared micron-sized hollow carbon spheres by chemical vapor deposition. Although this method can form hollow carbon spheres and is easy to industrialize, it is difficult to directly form...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 刘军张涛
Owner CHANGZHOU ZHONGKE HAINA CARBON TECH
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