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Method for preparing metallic cladding expansion graphite

A technology of expanded graphite and metal, which is applied in the field of graphite material preparation, can solve the problems of high energy consumption, harsh heat treatment atmosphere, strong toxicity of chlorine gas, etc., and achieve the effects of friendly process environment, high chemical stability and structural stability

Active Publication Date: 2012-08-15
HUNAN SHINZOOM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the traditional process, anhydrous chloride-graphite intercalation compounds of Fe, Co, Ni and other metals can be prepared by solid phase method, and then decomposed to prepare graphite intercalation compounds of Fe, Co, Ni and other metals. However, using This method will produce highly toxic chlorine gas, and the energy consumption is high, the heat treatment atmosphere is harsh, and the reaction cycle is long. More importantly, during the volatilization process of chlorine gas, metal elements will also come out of the graphite interlayer with it, resulting in the loss of metal elements. The amount of intercalation is difficult to control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A method for preparing metallic iron intercalated expanded graphite, the steps are as follows:

[0016] (1) First mix 1000Kg graphite and 462g perchloric acid powder uniformly, then add it to 1200mL glacial acetic acid under rapid stirring, continue stirring for 30min, transfer to a ball mill mixer, stir at 3000rpm for 3h, and then under 1800W power After 72 hours of ultrasonic treatment, the expandable graphite is obtained by centrifugation, and then the obtained expandable graphite is heat-treated at 900°C for 1 min in an air atmosphere to prepare the expanded graphite;

[0017] (2) At 60℃, mix 250g of anhydrous ferric chloride with 1000mL of molten n-triacontane to obtain an anhydrous ferric chloride suspension solution, add expanded graphite to the ferric chloride suspension, stir well, and then Let it stand for 1 hour, then transfer it into a tube furnace to isolate the air and heat it to 600°C, keep it for 48 hours, and then cool it to obtain iron-intercalated expanded...

Embodiment 2

[0019] A method for preparing metallic nickel intercalated expanded graphite, the steps are as follows:

[0020] (1) Mix 1000Kg graphite and 387g perchloric acid powder uniformly, then add it to 1200mL glacial acetic acid under rapid stirring, continue stirring for 30min, transfer to a ball mill mixer, stir at 5000rpm for 3h, and then sonicate under 1500W power After 72 hours of treatment, the expandable graphite is obtained by centrifugation, and then the obtained expandable graphite is heat-treated at 1000° C. for 2 minutes in an air atmosphere to prepare the expanded graphite.

[0021] (2) Mix 200 g of anhydrous nickel chloride with 1000 mL of molten n-octadecane at a temperature of 80°C to obtain a suspension of anhydrous nickel chloride. Add expanded graphite to the nickel chloride suspension and stir evenly. Then it was allowed to stand for 2h, then transferred to a tube furnace to isolate air and heat to 500°C, keep it for 20h, and obtain nickel intercalated expanded graphit...

Embodiment 3

[0023] A method for preparing metallic cobalt intercalated expanded graphite, the steps are as follows:

[0024] (1) Mix 1000Kg graphite and 80g perchloric acid powder uniformly, then add it to 1200mL glacial acetic acid under rapid stirring, continue stirring for 10min, transfer to a ball mill mixer, stir at 3500rpm for 3h, and then sonicate under 1800W power After 72 hours of treatment, the expandable graphite is obtained by centrifugation, and then the obtained expandable graphite is heat-treated at 1100°C for 2 minutes in an air atmosphere to prepare the expanded graphite;

[0025] (2) At 45℃, mix 150g of anhydrous cobalt chloride with 1000mL of paraffin oil to obtain an anhydrous cobalt chloride suspension solution, add expanded graphite to the cobalt chloride suspension, stir well, and then stand for 1h , Transferred to a tube furnace, isolated from air, heated to 700°C, kept for 36 hours, and cooled to obtain cobalt intercalated expanded graphite.

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PUM

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Abstract

The invention provides a method for preparing metallic cladding expansion graphite by means of liquid phase technology. The method includes the steps: synthesizing raw graphite into expansion graphite; uniformly mixing anhydrous metal salt with liquid aprotic organic matters at the temperature of 20-100 DEG C to obtain anhydrous metal salt organic suspending liquid; uniformly stirring the expansion graphite with the anhydrous metal salt organic suspending liquid prior to standing for 0-4h; preserving heat for 12-48h at the temperature of 400-700 DEG C in an air isolating manner; and cooling the expansion graphite to obtain the metallic cladding expansion graphite. By the aid of the method, high embedding quantity of metallic elements can be ensured, so that the relative content of metallics in the metallic cladding expansion graphite can be precisely controlled. Compared with a traditional method for preparing metallic cladding expansion graphite by means of solid phase technology, the method is higher in operability, environment-friendly and low in energy consumption.

Description

Technical field [0001] The invention relates to a preparation method of graphite material, in particular to a preparation method of metal intercalation expanded graphite. Background technique [0002] Metal elements such as Fe, Co, and Ni are commonly used catalysts for preparing carbon nanotubes by vapor phase chemical deposition. The requirements are that the metal particles cannot be oxidized and the particle size should be small enough. However, nano-scale metal particles have high activity and are easy to Oxidized by air, it is not conducive to storage. Inserting these metal catalysts between the graphite layers can not only ensure the nanometer size of the metal particles, but also is not easy to oxidize and deteriorate. [0003] In the traditional process, the anhydrous chloride-graphite intercalation compound of Fe, Co, Ni and other metals can be prepared by solid phase method, and then the graphite intercalation compound of Fe, Co, Ni and other metals can be prepared by d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J23/755B01J23/75B01J37/00
Inventor 石磊皮涛黄越华胡孔明蔡宁熊文权朱进
Owner HUNAN SHINZOOM TECH
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