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Method for preparing low-sulfur expandable graphite from medium-low carbon fine flake graphite

A technology of expanded graphite and fine flakes is applied in the field of preparation of expanded graphite, which can solve the problems of long heating time and large power consumption.

Inactive Publication Date: 2016-12-07
黑龙江省宝泉岭农垦帝源矿业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, for the expansion of graphite, the traditional expansion method is to place it in a muffle furnace for expansion at 800 ° C to 1000 ° C, but this expansion method takes a long time to heat and consumes a lot of power during the expansion process

Method used

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  • Method for preparing low-sulfur expandable graphite from medium-low carbon fine flake graphite
  • Method for preparing low-sulfur expandable graphite from medium-low carbon fine flake graphite
  • Method for preparing low-sulfur expandable graphite from medium-low carbon fine flake graphite

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 10g of 80μm natural flake graphite with a fixed carbon content of 80% was placed in a 50ml beaker, 50ml of 60% sulfuric acid was added to stir, and then 2g of potassium permanganate was added to stir evenly, and then allowed to stand for 2h until the intercalation reaction was complete; add 100ml of Tap water, stir evenly, add 1.0ml of 30% hydrogen peroxide dropwise, and bubbles will appear. After the reaction is complete, heat the reaction solution to 50°C and stir for 30min; filter and wash to pH=7.0, put it in a 60°C oven to dry for 3 hours, take out, and measure the moisture content The mass fraction is 34%; the sample is transferred to a microwave atmosphere tube furnace, and 4000W microwave polymerization is set for 5s to obtain an expanded graphite product with an expansion ratio of 157ml / g.

Embodiment 2

[0026] 10g of 48μm natural flake graphite with a fixed carbon content of 70% was placed in a 50ml beaker, 60ml of 75% sulfuric acid was added to stir, and then 1.5g of potassium permanganate was added to stir evenly, and then let stand for 3 hours until the intercalation reaction was complete; 200ml tap water, stir evenly, add 6.0ml 3% hydrogen peroxide dropwise, bubbles are formed, when the reaction is complete, heat the reaction solution to 30 ° C, stir for 1 hour; filter and wash to PH = 7.0, put it in an 80 ° C oven to dry for 5 hours, take out, the water The mass fraction was determined to be 29%; the sample was transferred to a microwave atmosphere tube furnace, and 3000W microwave polymerization was set for 10s to obtain an expanded graphite product with an expansion rate of 80ml / g.

Embodiment 3

[0028] 10g of 75μm natural flake graphite with a fixed carbon content of 90% was placed in a 50ml beaker, 38ml of 85% sulfuric acid was added to stir, and then 1.2g of potassium permanganate was added to stir evenly, and then allowed to stand for 3 hours until the intercalation reaction was complete; 50ml tap water, stir evenly, add 1.0ml 15% hydrogen peroxide dropwise, bubbles are formed, when the reaction is complete, heat the reaction solution to 60 ° C, stir for 1 hour; filter and wash to PH = 7.0, put it in a 70 ° C oven to dry for 6 hours, take out, the water The mass fraction was determined to be 1.03%; the sample was transferred to a microwave atmosphere tube furnace, and 2000W microwave polymerization was set for 10s to obtain an expanded graphite product with an expansion rate of 200ml / g.

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Abstract

The invention relates to the field of preparation of expandable graphite, in particular to a method for preparing low-sulfur expandable graphite in the room temperature atmospheric environment by using low-concentration sulfuric acid as an intercalation reagent by a mild and easily-controlled chemical intercalation method in accordance with medium-low carbon fine flake graphite. The method is simple in equipment, safe, controllable, free from gas protection and special protection, and suitable for mass preparation of low-sulfur fine flake graphite expandable graphite with low cost. The method comprises the following steps of (1) adopting natural fine flake graphite as a raw material, wherein the percentage by mass of carbon is 50-90%, and the size of graphite is 45-180 <mu>m; (2) under the condition of room temperature, using potassium permanganate as an oxidant, adopting the sulfuric acid of which the percentage by mass is 30-85% as an intercalation agent, and performing effective intercalation on the graphite raw material under the condition of room temperature, wherein heating is not needed in the process, and after uniform stirring is performed, the process can be completed under the standing condition; and (3) adopting a microwave tube furnace for rapidly expanding the expandable graphite, and finally, obtaining a low-sulfur fine flake expandable graphite powder material with a high-expandable volume.

Description

Technical field: [0001] The invention relates to a preparation technology of expanded graphite, in particular to the mild preparation of low-sulfur expandable graphite by using medium-low carbon fine flake graphite and a low-concentration sulfuric acid solution at room temperature, and the preparation of high expansion ratio by utilizing the moisture control of expandable graphite and microwave expansion technology The method of low-sulfur expanded graphite is suitable for the macro-production of low-cost and high-expansion medium-low carbon fine flake expanded graphite. Background technique: [0002] With the continuous consumption of global non-renewable energy resources, the contradiction between energy supply and demand has become increasingly prominent, which intensifies the tension of the world order. Therefore, the effective use of existing energy and the development of new energy have received widespread attention from all countries. In recent years, with the wide a...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01P2002/72C01P2004/03
Inventor 王艺达阎兴斌杨娟李文博薛群基
Owner 黑龙江省宝泉岭农垦帝源矿业有限公司
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