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Preparation method of high flame retardant expansible graphite

An expanded graphite, high flame retardant technology, applied in fire-resistant coatings and other directions, can solve the problems of fly ash formation, limited flame retardant efficiency, environmental pollution, etc., and achieve further reduction of heat transfer, good flame retardant effect, and a wide range of applications. Effect

Active Publication Date: 2010-07-28
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]Expandable graphite mainly relies on the expansion insulation layer formed by its own volume expansion to delay or inhibit the combustion of polymers, and there is no or little interaction with the flame-retardant polymers Chemical action occurs, which is a typical condensed phase flame retardant mechanism; due to the weak adhesion between the expanded graphite, after the polymer matrix is ​​burned, the expanded graphite cannot form a solid expanded carbon layer. The expanded carbon layer on the surface may be destroyed under the action of the flame, forming fly ash, which leads to the loss of the thermal insulation expansion layer, and then causes the unburned polymer to be ignited, the flame continues to spread, and the flame retardant efficiency is limited. Combustible polymers often show a strong wick effect, which also weakens their flame retardancy to a certain extent.
Moreover, since the intercalation generally contains sulfur, it is easy to release harmful gases such as sulfur dioxide during the combustion process and pollute the environment, and it expands at a relatively low temperature. In many cases, it is difficult to match the processing temperature of the polymer material. Therefore, it can be The practical application of expanded graphite in the field of polymer flame retardancy is relatively limited

Method used

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  • Preparation method of high flame retardant expansible graphite
  • Preparation method of high flame retardant expansible graphite
  • Preparation method of high flame retardant expansible graphite

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The preparation method of highly flame-retardant expandable graphite is that fully dissolving 1.2 grams of potassium dichromate in a mixed solution of 65% concentrated nitric acid and 5 grams of 70% perchloric acid in a mass fraction of 15 grams to prepare a solution A; fully dissolve 5 grams of melamine and 0.3 grams of potassium dichromate in 30 milliliters of phosphoric acid with a mass fraction of 85%, to prepare solution B; then put 10 grams of 50 mesh flake graphite into solution A, at 35 ° C Stir for 60 minutes, after standing still for 0.5 hours, filter out the solution, put the product into solution B again, stir for 60 minutes at the same temperature, after standing still for 2 hours, filter and wash with water until PH=7; dry in an oven at 100 degrees After 6 hours, a sulfur-free high expansion rate expandable graphite product was obtained, which was expanded with a ceramic crucible in a 900-degree muffle furnace, and the expansion volume was 200ml / g.

Embodiment 2

[0025] The preparation method of highly flame-retardant expandable graphite is that fully dissolving 0.4 gram of potassium dichromate in 10 gram of mass fraction is the mixed solution of concentrated nitric acid of 65% and 3 gram of mass fraction of perchloric acid of 70%; The 2,4,6-triphenylamide-s-triazine obtained by the reaction of melamine and benzoyl chloride and 0.6 gram of potassium dichromate are fully dissolved in 20 milliliters of mass fraction in 85% phosphoric acid to prepare solution B; then Put 5 grams of 50-mesh flake graphite into solution A, stir at 45°C for 40 minutes, and after standing still for 2 hours, filter the solution, put the product into solution B again, stir for 60 minutes at the same temperature, and stand still for 4 hours. Filter and wash with water until PH = 6; dry in an oven at 120°C for 4 hours to obtain a sulfur-free high expansion rate expandable graphite product, which is expanded with a ceramic crucible in a 900°C muffle furnace, and th...

Embodiment 3

[0027] The preparation method of highly flame-retardant expandable graphite is that fully dissolving 0.5 gram of potassium dichromate in 10 gram of mass fraction is the concentrated nitric acid of 68% and 15 gram of mass fraction is the mixed solution of perchloric acid of 72%; The 2,4,6-tri-n-butyramide-s-triazine obtained by the reaction of melamine and n-butyryl chloride and 0.8 gram of potassium dichromate are fully dissolved in 30 milliliters of massfraction in 85% phosphoric acid to prepare solution B; then Put 7.5 grams of 100-mesh flake graphite into solution A, stir at 75°C for 45 minutes, and after standing still for 3 hours, filter the solution, put the product into solution B, stir at the same temperature for 30 minutes, and stand still for 6 hours , filtered and washed with water until PH = 7; dried in an oven at 100 degrees for 6 hours to obtain a sulfur-free high expansion rate expandable graphite product, expanded with a ceramic crucible in a muffle furnace at 9...

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Abstract

The invention relates to a preparation method of high flame retardant expansible graphite, which comprises the following steps: dissolving the graphite into a mixing solution of perchloric acid and concentrated nitric acid, wherein the dosage of the solution is 100-600% of the mass of the solution; oxidizing the graphite by using solid oxidant of which the dosage is 0.5-50% of the mass of the oxidant to obtain the primary expansible graphite, wherein the temperature of the expansible graphite is 20-80 DEG C, and the reaction time is 20-300min; dissolving tripolycyanamide or the derivants thereof and the solid oxidant into phosphoric acid of which the mass fraction is 85+ / -10% to form a phosphoric acid solution, wherein the dosage of the solid oxidant is 0.5-50% of the mass thereof, and the mass concentration of the tripolycyanamide or the derivants thereof of the formed phosphoric acid solution is 0.02-2g / ml; carrying out reaction of the primary expansible graphite and the phosphoric acid solution at the temperature of 20-80 DEG C for 20-300min to prepare the high flame retardant expansible graphite. The method has the advantages that the tripolycyanamide or the derivants thereof are inserted between the expansible graphite layers, thereby improving the expansibility, start expansion temperature and fire resistance of the expansible graphite, and can be widely used for the flame retardant of multiple materials such as plastic, rubber, paint, foam and the like.

Description

technical field [0001] The invention relates to a preparation method of a graphite material, in particular to a preparation method of a novel high flame-retardant expandable graphite. Background technique [0002] Expanded graphite, also known as graphite intercalation intercalation compound, is a new type of compound formed by intercalating heterogeneous atoms, molecules or ions between graphite layers by physical or chemical methods. Expanded graphite usually contains 90-98% carbon and is a black flake. It exhibits hundreds of times of volume expansion when subjected to high temperature, and the expanded product has excellent oxidation resistance and high temperature resistance. This feature makes it suitable for use in When a fire occurs, the flame of the flame-retardant polymer material will be smothered by the instantaneous increase in volume to achieve the purpose of flame retardancy and fire prevention. The flame-retardant polymer material has the advantages of non-t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C09K21/02
Inventor 李娟柯晨浩方科益顾群范欣愉严庆
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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