Preparation method of expandable graphite by optimizing proportional ratio of intercalation agent

A technology of expanded graphite and intercalation agent, which is applied in the field of expandable graphite preparation, can solve the problems of poor controllability of initial expansion temperature, low expansion performance of EG, low expansion volume, etc., and achieve good oxidation resistance and environmental stability, Effect of improving the initial expansion temperature and improving expansion performance

Inactive Publication Date: 2018-11-23
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, due to the low expansion volume of EG prepared by a single sulfuric acid intercalation agent, the mechanical strength of the carbon layer formed during combustion expansion will be significantly lower, which will affect the flame retardant effect.
Therefore, although EG has excellent flame retardant performance, the flame retardant performance is still obviously insufficient when used alone, and cannot effectively suppress the generation of molten droplets and smoke.
In order to solve the problem of low expansion performance of EG prepared by intercalation of sulfuric acid, poor controllability of initial expansion temperature, corrosion of substrate, and release of SO during combustion 2 Harmful gases and other issues, it is very important to study a preparation method of expandable graphite with an optimized ratio of intercalants

Method used

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  • Preparation method of expandable graphite by optimizing proportional ratio of intercalation agent

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Effect test

Embodiment 1

[0018] The present invention is a kind of preparation method of the expandable graphite that optimizes proportion intercalation agent, concrete steps are as follows:

[0019] 1) Take a clean 10mL pipette and a 300mL beaker. Pipette 4.6mL of distilled water into the beaker, measure 8.15mL of 98% sulfuric acid with a graduated cylinder, slowly pour into the beaker while stirring along the wall of the vessel, shake and shake well.

[0020] 2) Take by weighing 3g of the natural flake graphite that has passed through a 50 mesh sieve, and add the natural flake graphite in the beaker while stirring. After mixing evenly, under the condition of constant stirring, based on 3.00g graphite, according to the mass ratio C:KMnO 4 :H 2 SO 4 =1:0.23:5 Weigh and mix the medicines, and change FeCl in the range of 0.03~0.30g / g 3 ·6H 2 The mass ratio of O to C.

[0021] 3) Adjust the reaction tank to 40°C in advance. After the temperature reaches the requirement and is stable, place the beak...

Embodiment 2

[0026] The present invention is a kind of preparation method of the expandable graphite that optimizes proportion intercalation agent, concrete steps are as follows:

[0027] 1) Take a clean 10mL pipette and a 300mL beaker. Pipette 4.6mL of distilled water into the beaker, measure 8.15mL of 98% sulfuric acid with a graduated cylinder, slowly pour into the beaker while stirring along the wall of the vessel, shake and shake well.

[0028] 2) Take by weighing 3g of the natural flake graphite that has passed through a 50 mesh sieve, and add the natural flake graphite in the beaker while stirring. After mixing evenly, under the condition of constant stirring, based on 3.00g graphite, according to the mass ratio C:FeCl 3 ·6H 2 O:H 2 SO 4 =1:0.1:5 Weigh and mix medicines, and change KMnO in the range of 0.03~0.30g / g 4 Compared with the mass of C.

[0029] 3) Adjust the reaction tank to 40°C in advance. After the temperature reaches the requirement and is stable, place the beake...

Embodiment 3

[0034] The present invention is a kind of preparation method of the expandable graphite that optimizes proportion intercalation agent, concrete steps are as follows:

[0035] 1) Prepare 5 concentrations of sulfuric acid solution samples that are respectively 65%, 70%, 75%, 80%, and 85%.

[0036] 2) Take by weighing 3g of the natural flake graphite that has passed through a 50 mesh sieve, and add the natural flake graphite in the beaker while stirring. After mixing evenly, under the condition of keeping constant stirring, take 3.00g of natural flake graphite as the benchmark, according to the mass ratio of the medicine, it is C:KMnO 4 :FeCl 3 ·6H 2 O:H 2 SO 4 =1:0.23:0.1:5.0 Weigh the medicines and mix them separately. Five samples of sulfuric acid solution were mixed for five comparison experiments, and stirring should be continued while mixing to ensure sufficient reaction.

[0037]3) Adjust the reaction tank to 40°C in advance. After the temperature reaches the require...

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Abstract

The invention discloses a preparation method of expandable graphite by optimizing proportional ratio of an intercalation agent, and belongs to the field of preparation of expandable graphite. A trivalent iron salt with flame-resistant characteristic is used as an auxiliary intercalation agent, and is coupled with graphite through intercalation reaction, so as to prepare the composite expandable graphite. The proportional ratios of graphite material to oxidant and intercalation agent to auxiliary intercalation agent are optimized on the basis of multiple times of experiment; finally, the expandable graphite with initial expanding temperature of 160 DEG C and expanding volume of 578mL / g is prepared. Proofed by experiment, the preparation method has the advantages that by intercalating ferrictrichloride, one part of sulfuric acid is replaced, so that the content of sulfur is reduced; the expanding property of the product is improved, the initial expanding temperature is improved, the flame-retardant property and ductility of the expandable graphite are good, and the expandable graphite can be used as a flame-retardant material to be added into inflammable materials.

Description

technical field [0001] The invention belongs to the technical field of expandable graphite preparation, and in particular relates to a method for preparing expandable graphite with an optimized ratio of intercalation agent. Background technique [0002] Expandable graphite (EG) is a typical physical expansion flame retardant. It has the advantages of not falling down, strong instantaneous expansion force, and can extinguish the flame in a short time. It has become increasingly mature in modern innovative scientific research. Its application fields Very broad. The flame retardant mechanism of EG belongs to the solidified phase flame retardant mechanism, which is flame retardant by delaying or interrupting the production of flammable substances from solid substances. When EG is heated to a certain extent, it begins to expand, and the state of graphite after expansion changes from the original scale shape to the worm shape with very low density, thus forming a good thermal ins...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/22
CPCC01B32/22
Inventor 包红旭杨雨萌任逸轩张欣苏弘治张馨月李良玉吕志忠
Owner LIAONING UNIVERSITY
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