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Preparation method of expansible graphite with flame retardant property

A technology of expanded graphite and flame retardant properties, which is applied in the field of preparation of expandable graphite, can solve the problems of high flame retardant expandable graphite, etc., and achieve the effect of low burning rate and low heat release rate

Inactive Publication Date: 2015-01-07
无锡市新颖密封材料厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chemical oxidation is currently the main method for preparing expandable graphite. Sulfuric acid, nitric acid, phosphoric acid, etc. are mostly used as intercalation agents. In recent years, in order to reduce the sulfur content of expanded graphite, the preparation of low-sulfur or sulfur-free expandable graphite has gained relatively Pay more attention, but there is no report on high flame retardant expandable graphite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for preparing expandable graphite with flame-retardant properties includes the following steps:

[0024] Step A. Dissolve ammonium polyphosphate and potassium dichromate in an amount of 50% of the mass of said ammonium polyphosphate in phosphoric acid with a mass fraction of 75% to form phosphoric acid with a mass concentration of ammonium polyphosphate of 2g / ml Solution; The degree of polymerization of the ammonium polyphosphate is 100-1000.

[0025] Step B. Using a mixed solution of sulfuric acid and nitric acid or a concentrated sulfuric acid solution, take 15% of the graphite mass of potassium dichromate graphite oxide, the temperature of the expanded graphite is 50°C, and the reaction time is 300 minutes to obtain primary expandable graphite ; The mass ratio of graphite and concentrated sulfuric acid is 1:5. The mass ratio of sulfuric acid to nitric acid in the mixed solution of sulfuric acid and nitric acid is 1:3. The graphite is natural flake graphite with...

Embodiment 2

[0029] A method for preparing expandable graphite with flame-retardant properties includes the following steps:

[0030] Step A. Dissolve ammonium polyphosphate and potassium dichromate in an amount of 30% of the mass of the ammonium polyphosphate in phosphoric acid with a mass fraction of 75% to form a ammonium polyphosphate with a mass concentration of 0.1 g / ml Phosphoric acid solution; the degree of polymerization of the ammonium polyphosphate is 100-1000.

[0031] Step B. Using a mixed solution of sulfuric acid and nitric acid or a concentrated sulfuric acid solution, take potassium dichromate graphite oxide in an amount of 10% of the graphite mass, the temperature of the expanded graphite is 55°C, and the reaction time is 200 minutes to obtain primary expandable graphite ; The mass ratio of graphite and concentrated sulfuric acid is 1:8. The mass ratio of sulfuric acid to nitric acid in the mixed solution of sulfuric acid and nitric acid is 1:4. The graphite is artificial or...

Embodiment 3

[0035] A method for preparing expandable graphite with flame-retardant properties includes the following steps:

[0036] Step A. Dissolve ammonium polyphosphate and potassium dichromate in an amount of 40% of the mass of said ammonium polyphosphate in phosphoric acid with a mass fraction of 75% to form phosphoric acid with a mass concentration of ammonium polyphosphate of 1g / ml Solution; The degree of polymerization of the ammonium polyphosphate is 100-1000.

[0037] Step B. Using a mixed solution of sulfuric acid and nitric acid or a concentrated sulfuric acid solution, take potassium dichromate graphite oxide in an amount of 10% of the graphite mass, the temperature of the expanded graphite is 60°C, and the reaction time is 200 minutes to obtain primary expandable graphite ; The mass ratio of graphite and concentrated sulfuric acid is 1:10. The mass ratio of sulfuric acid to nitric acid in the mixed solution of sulfuric acid and nitric acid is 1:5. The graphite is artificial or...

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Abstract

The invention discloses a preparation method of expansible graphite with a flame retardant property. The preparation method comprises the following steps: dissolving ammonium polyphosphate and potassium dichromate accounting for 20%-50% of the mass of the ammonium polyphosphate in a phosphoric acid having the mass fraction of 75% to form a phosphoric acid solution in which the concentration of the ammonium polyphosphate is 0.02g / ml-2g / ml; taking a mixed solution of sulfuric acid and nitric acid or a concentrated sulfuric acid solution and oxidizing graphite by use of potassium dichromate accounting for 10-20% of the mass of the graphite to obtain a primary expansible graphite; reacting the phosphoric acid solution with the primary expansible graphite at a temperature in the range of 70-80 DEG C, after the reaction is finished, filtering and washing with water until the pH is in the range of 6-7, and drying at 100 DEG C for 6-12 hours to obtain the expansible graphite with the flame retardant property. The preparation method of the expansible graphite with a flame retardant property is characterized in that a phosphorous compound is inserted between the layers of the graphite so that the adhesion of the prepared expansible graphite with the high flame retardant property to each other can be improved so that a better flame retardant effect can be achieved, in addition to a relatively high expansion volume of the expansible graphite.

Description

technical field [0001] The invention belongs to the technical field of preparation of expanded graphite materials, and in particular relates to a preparation method of expandable graphite with flame-retardant properties. Background technique [0002] Due to the interaction between the carbon atomic layer and the intercalation layer atoms, the expandable graphite has a series of new properties, especially when the expandable graphite is subjected to high temperature, it shows a volume expansion of hundreds of times, which makes it suitable for fire. When the flame is suffocated by the instantaneous increase in volume, the purpose of flame retardancy and fire prevention is achieved. Expandable graphite with sulfuric acid as an intercalation agent is a commercial product widely used at present. The flame-retardant polymer material has the advantages of non-toxicity, low smoke, low burning rate, and low heat release rate when burning. The development trend of combustible materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 陆峰
Owner 无锡市新颖密封材料厂
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