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Preparation method for thermoplastic phenolic resin-based hollow carbon balls

A phenolic resin and thermoplastic technology, applied in the field of preparation of hollow carbon balls, can solve the problems of undiscovered process, cracking of carbon balls, simplicity, etc., and achieve the effects of simple process route, few process steps and high yield

Inactive Publication Date: 2012-08-15
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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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

[0016] 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

[0018] 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 100 g of the 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 heat it at a constant temperature at 0.3 m 3 / h flow rate into the water vapor to activate the resin ball for 3 hours. Cool naturally to room temperature to obtain hollow carbon spheres (sphericity: 95.5%, hollowness: 82%, ball diameter: 1.2mm, specific surface area: 784m 2 / g).

Embodiment 3

[0020] 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 of 5% (mass ratio) 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 obtain hollow carbon spheres (sphericity: 97%, hollowness: 76%, ball diameter: 0.9mm, specific surface area: 790m 2 / g).

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Abstract

The invention provides a preparation method for thermoplastic phenolic resin-based hollow carbon balls. The method comprises the following steps of: blending an aqueous solution containing 1-10 wt% dispersing agent at 20-50 DEG C; stirring phenolic resin, a curing agent and the aqueous solution of the dispersing agent in a mass ratio of 100:(3-20): (500-1500) in an autoclave, heating to 110-130 DEG C in the autoclave, insulating for 0.5 to 3 hours, and then cooling, filtering, and drying to obtain hollow phenolic resin balls; and heating the hollow phenolic resin balls to 800-1000 DEG C in a carbonization and activation furnace in the presence of nitrogen used as protective gas, keeping the temperature constant for 0.5-3 hours, activating the hollow phenolic resin balls at a vapour flow speed of 0.1-1.2 m<3> per hour for 100 g of the hollow phenolic resin balls during the constant-temperature section process, and cooling to obtain the hollow carbon balls. The preparation method for thermoplastic phenolic resin-based hollow carbon balls disclosed by the invention has the following advantages: the hollow carbon balls with ball diameter of 0.1-1.5 mm and the sphericity of 95%-99% are obtained; the volume production rate of a reaction kettle is high; and the hollowness degree of the carbon balls is controllable.

Description

technical field [0001] The invention belongs to the preparation of hollow carbon spheres, in particular to a preparation method of thermoplastic 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 to prepare 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: CN 1821068A) and others used ferrocene and ammonium chloride as raw materials to prepare 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 ...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 孙国华李开喜
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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