Preparation of low temperature expandable graphite

A technology of expanded graphite and low temperature, applied in the field of preparation of expandable graphite, can solve the problems of high expansion temperature and limit the application range of expandable graphite, and achieve the effects of high safety, low equipment requirements and strong operability

Inactive Publication Date: 2008-12-24
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, whether it is sulfur-containing, low-sulfur, or sulfur-free expandable graphite, its expansion temperature is high (generally graphite intercalation compounds begin to expand above 900°C), which limits the scope of expandable graphite applications (especially multi-band Smoke agent, intumescent flame retardant and fire extinguishing agent, etc., where the lower the expansion temperature, the better)

Method used

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  • Preparation of low temperature expandable graphite
  • Preparation of low temperature expandable graphite
  • Preparation of low temperature expandable graphite

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Take 3-25g of natural flake graphite, 3-30g of potassium permanganate, and 25-300ml of concentrated sulfuric acid. First add concentrated sulfuric acid into a three-necked flask, add natural flake graphite while stirring, slowly add potassium permanganate into the flask after stirring, control the temperature of the reaction solution at 30°C to 45°C, and oxidize for one hour. After the reaction, continuously add 100-800ml of deionized water into the flask, and control the temperature below 90°C. After keeping it for one hour, wash the reaction product until neutral, and finally use water exchange method to make water as the main intercalation agent , filtered, and baked at 50°C for 24 hours. The prepared expandable graphite begins to expand at 160°C, and the expansion volume at 200°C is 150ml / g (see the SEM image after it expands at 180°C figure 1 ).

Embodiment 2

[0029] Take 3-25g of natural flake graphite, 5-38g of potassium permanganate, 40-500ml of concentrated sulfuric acid, first add concentrated sulfuric acid into a three-necked flask, add natural flake graphite while stirring, and slowly add permanganate into the flask after stirring evenly Potassium, the temperature of the reaction solution is controlled at 30°C to 50°C, and the oxidation reaction takes two and a half hours. After the reaction is completed, continuously add 150 to 1200ml of deionized water into the flask, and keep the temperature below 90°C for two hours. , wash the reaction product to neutrality. Then, the concentrated sulfuric acid between graphite layers was replaced by water exchange method, water was used as the main intercalation agent, filtered, and baked at 90°C for 24 hours. The target object (expandable graphite) was obtained. It begins to expand at 160°C, and the expansion volume at 200°C is 200ml / g; the EDS energy spectrum test spectrum of the expa...

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Abstract

The invention relates to a preparation method of an expansible graphite (expansible graphite intercalation compound) which comprises the following steps: dipping a flake graphite in a solution mainly formed by oxidant and intercalation agent for intercalation reaction, replacing the intercalation compound between the graphite layers by water exchange method after filtration, drying the obtained solid formation to obtain target compounds. The invention has advantages of low energy consumption, environment friendly, and the prepared expansible graphite is capable of expansion at a low temperature.

Description

technical field [0001] The invention relates to a preparation method of expandable graphite (expandable graphite intercalation compound). Background technique [0002] Expandable graphite (expandable graphite intercalation compound) is an inorganic material with excellent performance. Due to the insertion of intercalation guests, the graphite host has many excellent properties such as heat resistance, corrosion resistance, softness, and conductivity. [0003] So far, the methods for preparing expandable graphite are mainly divided into two categories: chemical oxidation and electrochemical methods. Among them, the chemical oxidation method is currently the most widely used and relatively mature method. [0004] The chemical oxidation method refers to: immerse the flake graphite in a solution mainly composed of an oxidizing agent and an intercalation agent. Under the action of the oxidizing agent, the graphite is oxidized so that the neutral network planar macromolecules of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 马玉录谢林生汤先文卢亚云景军涛刘德礼
Owner EAST CHINA UNIV OF SCI & TECH
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