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Preparation method of high-flame-retardancy expandable graphite

An expanded graphite, high flame retardant technology, applied in the field of graphite material preparation, can solve the problems of damage to the expanded graphite layer, weak adhesion, limited flame retardant efficiency, etc. Effect

Inactive Publication Date: 2012-02-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, expandable graphite mainly relies on the expansion insulation layer formed by its own volume expansion to delay or inhibit the combustion of substances, and there is no or little chemical interaction with the flame retardant, which is a typical condensed phase flame retardant mechanism; expandable graphite The carbon layer formed after expansion has weak adhesion to each other. After being burned by the flame retardant matrix, a solid expanded carbon layer cannot be formed. Under the action of flame pressure or heat convection, the expanded graphite layer on the surface may be damaged. When it is destroyed, "fly ash" is formed, which leads to the loss of the thermal insulation expansion layer, and then causes the unburned substance to be ignited, and the flame continues to spread, so the flame retardant efficiency is limited
Moreover, expandable graphite often exhibits a strong "candle wick effect" when it is a flame-retardant polymer, which also weakens its flame-retardant ability to a certain extent.
Therefore, the practical application of expandable graphite in the field of flame retardancy is still relatively limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of ordinary expandable graphite is to dissolve 1 g of potassium dichromate in 25 ml of concentrated sulfuric acid with a mass fraction of 98%; then pour 10 g of 50 mesh natural flake graphite into it; stir and mix at 30°C. After standing and reacting for 30 minutes, suction filtration and water washing are repeated until the pH of the filtrate is 6-7; dried in an oven at 50°C for 24 hours to obtain ordinary expandable graphite products. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a resistance furnace at 950°C is 240 ml / g.

Embodiment 2

[0022] The preparation method of high flame-retardant expandable graphite is to dissolve 1 g of potassium dichromate in 25 ml of 98% concentrated sulfuric acid to prepare solution A; dissolve 15 g of guanidine carbonate in 30 ml of phosphoric acid, Prepare solution B; then pour 10 grams of 50 mesh natural flake graphite into solution A, stir and stand for reaction at 30°C for 30 minutes, suction filtration, repeated washing with water, and suction filtration until the pH of the filtrate is 4~ 5. Obtain primary expandable graphite; then put the primary expandable graphite into solution B, stir and stand for 80 minutes at 30°C, and then repeatedly filter and wash with water until the pH of the filtrate is 6-7; Dry it at 50°C for 24 hours to obtain high flame retardant expandable graphite. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a resistance furnace at 950°C is 256 ml / g.

Embodiment 3

[0024] The preparation method of high flame retardant expandable graphite is to dissolve 8 grams of potassium dichromate in 90 milliliters of 98% concentrated sulfuric acid to prepare solution A; dissolve 45 grams of guanidine carbonate in 90 milliliters of phosphoric acid, Prepare solution B; then pour 30 grams of 325 mesh natural flake graphite into solution A. After stirring and standing for 15 minutes at 30°C, suction filtration, repeated washing with water and suction filtration until the pH of the filtrate is 5.5~ 6.5, get the primary expandable graphite; then put the primary expandable graphite into solution B, stir and stand for 120 minutes at 30°C, then repeatedly filter and wash with water until the pH of the filtrate is 6-7; Dry at 40°C for 48 hours to obtain high flame retardant expandable graphite. According to the method specified in GB 10698-89 "Expandable Graphite", the expansion volume measured in a resistance furnace at 950°C is 55 ml / g.

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Abstract

The invention relates to a preparation method of high-flame-retardancy expandable graphite, which comprises the following steps: oxidizing graphite by using concentrated sulfuric acid / nitric acid mixture, nitric acid / phosphoric acid mixture, fuming nitric acid or concentrated sulfuric acid together with a solid strong oxidizer which accounts for 5-60 wt% of graphite, wherein the reaction temperature is 15-50 DEG C, and the reaction time is 10-100 minutes; after the reaction finishes, filtering, and washing with water until the pH value is 4-7, thereby obtaining the primary expandable graphite; and reacting the primary expandable graphite with guanidine salt solution at 20-80 DEG C for 20-200 minutes, carrying out repeated vacuum filtration, washing with water until the pH value is 6-7, and baking at 40-80 DEG C for 10-72 hours to obtain the high-flame-retardancy expandable graphite. The method provided by the invention intercalates guanidine salts into the interlayer of the expandable graphite, enhances the expansion ratio and flame retardancy, and can be widely used for flame retardancy for plastics, rubber, paint, foam and various other materials.

Description

Technical field [0001] The invention relates to a preparation method of graphite material, in particular to a preparation method of high flame retardant expandable graphite. Background technique [0002] Expandable graphite is a new type of compound with interlayer intercalation formed by natural flake graphite through oxidation intercalation reaction, inserting heterogeneous atoms, molecules or ions between graphite flake layers. When expandable graphite is subjected to high temperature, the interlayer material is rapidly vaporized by high heat, and the formed gas produces huge tension on the graphite sheets, which causes the expandable graphite to expand, and the expansion ratio is as high as tens to hundreds of times. The resulting carbon layer has excellent oxidation resistance and high temperature resistance, which can protect the substances under the carbon layer and achieve the purpose of flame retardancy and fire prevention. Compared with traditional flame retardants, ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C08K13/04C08K9/04C08K7/24C08K3/04C08L23/12
Inventor 刘定福
Owner SOUTH CHINA UNIV OF TECH
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