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Method for preparing sulphur-free expanded graphite by using middle-low carbon fine-scaled 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 large power consumption and long heating time.

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 sulphur-free expanded graphite by using middle-low carbon fine-scaled graphite
  • Method for preparing sulphur-free expanded graphite by using middle-low carbon fine-scaled graphite

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Place 10g of 80μm natural flake graphite with a fixed carbon content of 60% in a 250ml beaker, add 50ml of perchloric acid and stir, then add 2g of potassium permanganate and stir evenly, let stand for 2 hours until the intercalation reaction occurs completely; add 100ml Tap water, after stirring evenly, add 1.0ml of 30% hydrogen peroxide dropwise, bubbles are generated, after the reaction is complete, heat the reaction solution to 50°C, stir for 30min; filter and wash to PH = 7.0, put it in an oven at 60°C for 3h, take it out, and measure the water content The mass fraction is 34%; the sample is transferred to a microwave atmosphere tube furnace, and microwave polymerization is set at 4000W for 5s to obtain an expanded graphite product with an expansion rate of 73ml / g.

Embodiment 2

[0025] Place 10g of 80μm natural flake graphite with a fixed carbon content of 80% in a 50ml beaker, add 38ml of perchloric acid and stir, then add 1.5g of potassium permanganate and stir evenly, and let stand for 3 hours until the intercalation reaction occurs completely; add 200ml of tap water, stir evenly, add 5.0ml of 3% hydrogen peroxide dropwise, bubbles will appear, after the reaction is complete, heat the reaction solution to 30°C, stir for 1h; filter and wash to PH=7.0, put it in an oven at 80°C for 5h, take it out, The mass fraction was determined to be 29%; the sample was transferred to a microwave atmosphere tube furnace, and microwave polymerization was set at 3000 W for 10 s to obtain an expanded graphite product with an expansion rate of 155 ml / g.

Embodiment 3

[0027] Place 10g of 80μm natural flake graphite with a fixed carbon content of 90% in a 50ml beaker, add 30ml of perchloric acid and stir, then add 1.2g of potassium permanganate and stir evenly, and let stand for 3 hours until the intercalation reaction occurs completely; add 50ml of tap water, stir evenly, add 1.0ml of 15% hydrogen peroxide dropwise, bubbles are generated, after the reaction is complete, heat the reaction solution to 60°C, stir for 1h; filter and wash to PH=7.0, put it in an oven at 70°C for 7h, take out, and remove the water The mass fraction was determined to be 0.53%; the sample was transferred to a microwave atmosphere tube furnace, and microwave polymerization was set at 2000W for 10s to obtain an expanded graphite product with an expansion rate of 227ml / g.

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Abstract

The invention relates to the field of expandable graphite preparation. The method comprises the following steps: 1) employing natural fine-scaled graphite as a raw material, wherein the mass fraction of carbon content is 50-90% and the scale number is 45-180 [mu]m; 2) under room temperature condition, taking potassium permanganate as an oxidizing agent and perchloric acid as an intercalator, performing effective intercalation on the graphite raw material under room temperature condition, uniformly stirring the materials, and standing; and 3) employing a microwave tubular furnace, puffing the expandable graphite, and finally obtaining the sulphur-free expanded graphite powder material with high expansion capacity. By taking the fine-scaled graphite with middle-low carbon content as the raw material, a mild chemical intercalation method with easy control is employed, and the sulphur-free expanded graphite can be prepared by employing perchloric acid as the intercalator. The method has the advantages of simple equipment, safety and controllable performance, no requirement of gas protection and special protection, and is suitable for preparing the sulphur-free expanded graphite with low cost and large scale.

Description

Technical field: [0001] The invention relates to the preparation technology of expanded graphite, specifically the method of using medium and low carbon fine flake graphite to prepare sulfur-free expandable graphite gently at room temperature, and using microwave expansion technology to prepare sulfur-free expanded graphite with high expansion rate, which is suitable for low-cost and high-efficiency Macroscale preparation of low- and medium-carbon fine-scale exfoliated graphite with expansion ratio. Background technique: [0002] With the continuous consumption of non-renewable energy resources in the world, the contradiction between energy supply and demand has become increasingly prominent, thus exacerbating the tension in the world order. Therefore, the effective use of existing energy sources and the development of new energy sources have received widespread attention from all countries. In recent years, with the widespread application of carbon materials in the energy ...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01P2004/03
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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