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Graphite purification method

A graphite purification and purification method technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of high impurity removal efficiency, large energy consumption, serious equipment corrosion, etc., achieve good purification effect and wide application , The effect of simple process

Inactive Publication Date: 2018-08-03
赵文渊
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The flotation method has the lowest cost, the least energy consumption and reagent consumption, but it is difficult to obtain graphite with a carbon content of more than 95%; the removal efficiency of the hydrofluoric acid method and the hydrofluoric acid-salt (sulfur) acid method is high and the energy It is also relatively low, but the scope of application of this method is limited due to the high toxicity and strong corrosiveness of hydrofluoric acid, which pollutes the environment
Alkaline-acid purification requires high-temperature sintering during the alkali calcination process, high energy consumption, serious equipment corrosion, long purification process steps, and poor purification effect on low-grade aphanitic graphite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In this example, the aphanitic graphite in Chenzhou, Hunan, with a content of 72.83% is used as a raw material, and 20 g of aphanitic graphite in Chenzhou, Hunan is weighed, and it is ultrafinely pulverized to 45 μm, so that the gangue and aphanitic graphite in the raw ore A certain degree of dissociation is obtained; then use 16g of sodium hydroxide, add 60mL of water, add flux agent sodium metaborate 1g, and react in a reaction kettle at 180°C for 2h; wash the product after alkali fusion with water until the pH is 7.5-7.8, and add 500mL volume Dilute sulfuric acid with a concentration of 2%, stir well, let it settle for 1 hour, take out the upper layer liquid, add 250mL of dilute sulfuric acid with a volume concentration of 2%, wash the acid-washed ore sample until neutral, filter, and dry to obtain 14.35g of product with a grade of 99.21%.

Embodiment 2

[0027] In this embodiment, the aphanitic graphite in Chenzhou, Hunan, with a content of 68.34% is used as a raw material, and 10 g of aphanitic graphite in Chenzhou, Hunan is weighed, and it is ultrafinely pulverized to 40 μm, so that the gangue and aphanitic graphite in the raw ore A certain degree of dissociation is obtained; then use 10g of sodium hydroxide, add 20mL of water, add flux agent sodium metaborate 0.8g, and react in the reaction kettle at 180°C for 3h; wash the product after alkali fusion until the pH is 7.5-7.8, and add 200mL Dilute sulfuric acid with a volume concentration of 3%, stir well, let it settle for 1 hour, take out the upper layer liquid, add 100mL of dilute sulfuric acid with a volume concentration of 3%, wash the mineral sample after pickling until neutral, filter, and dry. 6.89 g of product with a grade of 99.85% were obtained.

Embodiment 3

[0029] In this embodiment, the aphanitic graphite in Chenzhou, Hunan, with a content of 65.25% is used as a raw material, and 25 g of aphanitic graphite in Chenzhou, Hunan is weighed, and it is ultrafinely crushed to 38 μm, so that the gangue and aphanitic graphite in the raw ore A certain degree of dissociation is obtained; then use 35g of sodium hydroxide, add 40mL of water, add 2g of flux lithium metaborate, and react in a reaction kettle at 210°C for 3h; wash the product after alkali fusion with water until the pH is 7.5-7.8, and add 500mL of volume Dilute sulfuric acid with a concentration of 5%, stir well, let it settle for 1 hour, take out the upper layer liquid, add 250mL of dilute sulfuric acid with a volume concentration of 5%, wash the acid-washed ore sample until neutral, filter, and dry to obtain 15.87g of product with a grade of 99.74%.

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PUM

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Abstract

The invention discloses a graphite purification method which comprises the following steps: 1) with low-grade cryptocrystalline graphite of which the cryptocrystalline graphite content is 65-73% as araw material, performing superfine crushing treatment till the particle size of the ore sample is 45 [mu]m or less; 2) putting the cryptocrystalline graphite subjected to superfine crushing treatmentin the step 1) into a reaction kettle, adding sodium hydroxide, sodium metaborate and water, performing a reaction for 2-3 hours at 150-260 DEG C, and performing alkali fusion treatment; and 3) performing acid soaking on the cryptocrystalline graphite after alkali fusion in the step 2), namely washing the cryptocrystalline graphite after alkali fusion in the step 2) with water till the pH value is7.5-7.8, adding an acid for a first time, uniformly stirring, and leaving to stand and settling down for 1-1.5 hours, wherein the volume concentration of the acid is 2-5%. According to the method, the low-grade cryptocrystalline graphite of which the cryptocrystalline graphite content is 65-73% as the raw material, through processes of superfine crushing and alkali fusion-acid soaking in the reaction kettle, high-grade cryptocrystalline graphite of which the cryptocrystalline graphite content is greater than or equal to 99.0% is prepared, and the cryptocrystalline graphite can be relatively wide in application range.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a graphite purification method. Background technique [0002] At present, many of the purification of aphanitic graphite still refer to the purification technology of natural flake graphite. Common purification methods include: (1) flotation method; (2) alkali-acid two-step method; (3) hydrofluoric acid method; (4) ) hydrofluoric acid-salt (sulfur) acid method, etc. The flotation method has the lowest cost, the least energy consumption and reagent consumption, but it is difficult to obtain graphite with a carbon content of more than 95%; the removal efficiency of hydrofluoric acid method and hydrofluoric acid-salt (sulfur) acid method is high, and energy It is also relatively low, but the scope of application of this method is limited due to the high toxicity and strong corrosiveness of hydrofluoric acid that pollutes the environment. Alkali-acid purificat...

Claims

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Application Information

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IPC IPC(8): C01B32/215
CPCC01B32/215
Inventor 赵文渊
Owner 赵文渊
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