Preparation method of sulfur-free expansible graphite

A technology of expanded graphite and natural flake graphite, applied in the field of materials, can solve the problems of polluted environment, difficult operation, and high reaction temperature of the preparation process, and achieve the effects of high expansion volume, improved corrosion resistance, and good intercalation effect.

Active Publication Date: 2016-04-20
YANSHAN UNIV
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

However, the reaction temperature of the preparation process is high, it is not easy to operate, and the product has a high sulfur content, and a large amount of harmful gases such as sulfur dioxide will be released during the expansion process, which will pollute the environment. The expansion volume of the expanded graphite obtained is generally 200-300mL / g. not very good

Method used

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  • Preparation method of sulfur-free expansible graphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Mix 3g of natural flake graphite with a particle size of 32 mesh and a carbon content of 99.9% with 1.11g of potassium permanganate, then add 20.4mL of perchloric acid with a mass fraction of 70-72%, and keep stirring. After the reaction, soak in 50mL saturated dipotassium hydrogen phosphate solution at room temperature for 60min to carry out the second intercalation reaction; Dry for 24 hours to obtain sulfur-free expandable graphite; expand the prepared expandable graphite in a muffle furnace at 950°C for 10 seconds at high temperature to obtain expanded graphite with an expansion volume of 400mL / g.

[0016] The expansion volume test method of expanded graphite is determined by the method in "Expandable Graphite (GB / T10698-1989)": Weigh an appropriate amount of expandable graphite sample, accurate to 0.001g, and place it at a high temperature of 900-1000°C Put it into a quartz beaker that has been ignited in the furnace for 5 minutes, and immediately put it into a hig...

Embodiment 2

[0024] Mix 3g of natural flake graphite with a particle size of 32 mesh and a carbon content of 99.9% with 1.26g of potassium permanganate, then add 21.6mL of perchloric acid with a mass fraction of 70-72%, and keep stirring. After the reaction, soak in 50mL saturated dipotassium hydrogen phosphate solution at room temperature for 60min to carry out the second intercalation reaction; Dry for 24 hours to obtain sulfur-free expandable graphite; expand the prepared expandable graphite in a muffle furnace at 950°C for 10 seconds at high temperature to obtain expanded graphite with an expansion volume of 410mL / g.

[0025] Get 1g of the prepared expanded graphite to adsorb heavy oil, and the adsorption ratio is 95g / g.

Embodiment 3

[0027] Mix 3g of natural flake graphite with a particle size of 32 mesh and a carbon content of 99.9% with 1.2g of potassium permanganate, and then add 21mL of perchloric acid with a mass fraction of 70-72%, stirring continuously, at 22°C React for 65 minutes. After the reaction, soak in 50 mL of saturated dipotassium hydrogen phosphate solution at room temperature for 60 minutes to carry out the second intercalation reaction; Dry for 24 hours to obtain sulfur-free expandable graphite; expand the prepared expandable graphite in a muffle furnace at 950°C for 10 seconds at high temperature to obtain expanded graphite with an expansion volume of 430mL / g.

[0028] 1 g of the prepared expanded graphite was used to adsorb crude oil, and the oil absorption ratio was 114 g / g.

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Abstract

The invention provides a low-temperature preparation method of sulfur-free expansible graphite. The sulfur-free expansible graphite is prepared from, by mass, natural flake graphite, potassium permanganate and perchloric acid according to the ratio of 1:(0.37-0.42):(8.5-9.0). The method includes the steps of mixing natural flake graphite with potassium permanganate, adding perchloric acid, conducting unceasing stirring, making the mixture react for 60-70 min at the temperature of 20-25 DEG C, soaking the mixed solution and a dipotassium phosphate solution for 60 min at the room temperature according to the volume ratio of 1:(2.0-2.5) after the reaction ends, conducting the secondary intercalation reaction, conducting water washing till the pH value is 5-7, conducting suction filtration and dehydration, conducting drying at the temperature of 60 DEG C to prepare the sulfur-free expansible graphite, and obtaining the expansible graphite capable of adsorbing oil type pollutant by conducting expansion in a muffle furnace at the temperature of 950 DEG C. The method is free of high-temperature operation, safety and energy conservation are achieved, no sulfur dioxide pollutant is generated, industrialized production can be easily achieved, the expansion volume of expansible graphite reaches 400-430 mL / g, and the oil adsorption effect is good.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a preparation method of sulfur-free expandable graphite. technical background [0002] In recent years, the frequent occurrence of oil tanker accidents and the blind discharge of industrial oily sewage have caused serious pollution to the water environment. Therefore, the emergency response to marine oil spills has become a global hot issue. my country's natural flake graphite reserves are abundant, and expandable graphite can be obtained after intercalation oxidation treatment, and then expanded graphite can be obtained by high temperature treatment. The surface of expanded graphite is a non-polar aliphatic hydrocarbon group, and the inside is a micron-sized macroporous structure with a worm-like structure, so it is especially suitable for adsorbing organic macromolecules; It is especially suitable for the adsorption treatment of viscous oils. [0003] As early as the early ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2006/19Y02P20/10
Inventor 贺君李飞杨育林宋来洲杨红侠任小慧郑晓强
Owner YANSHAN UNIV
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