Purification method of natural cryptocrystalline graphite

A technology of aphanitic graphite and a purification method, which is applied in the field of purification of natural aphanitic graphite as a raw material, can solve problems such as large energy consumption, strong corrosive pollution, and long purification process steps, so as to reduce energy loss and pollution degree of effect

Inactive Publication Date: 2015-04-08
林前锋
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, 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, The energy consumption 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
The content of graphite purified by alkali-acid method can reach more than 99%, but in the process of alkali calcination, high temperature sintering is required, energy consumption is large, equipment corrosion is serious, and purification process steps are long. Therefore, it is necessary to optimize process conditions, reduce energy loss, and minimize Reduce costs and improve efficiency
The carbon content of graphite purified by the two-step alkali-acid method is difficult to reach more than 99.90%. Even if the melting temperature is increased to 800 degrees, the carbon content can only be increased to 99.80%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 60g of carbon content 80%, aphanitic graphite with a particle size of 0.044mm is added to the reaction vessel, 100g of sodium hydroxide and 4g of additives are added (by 1.2g of sodium metaborate and 2.8g of sodium diisobutylnaphthalene sulfonate ), add tap water to form a 400ml solution, stir and mix well with a glass rod, place in an oil bath furnace, raise the temperature of the electric furnace to 150°C and stir for 2 hours, take it out, cool naturally to room temperature, separate the solution and graphite, wash the sample with water until When the pH value of the washing solution is 8, it precipitates; it is filtered, and then dried in a constant temperature blast drying oven for 2 hours. After drying the alkali-soluble sample, weigh 20g, add 40ml of 65% nitric acid and 15g of ammonium fluoride into the reaction vessel, and react at a temperature of 90°C for 2 hours. After the reaction, the solution and graphite are separated, and the graphite is washed with water ...

Embodiment 2

[0022] Add 40g of carbon content 80%, aphanitic graphite of 0.150mm in particle size into the reaction vessel, add 100g of sodium hydroxide and 2g of additives (by 0.4g of sodium metaborate and 1.6g of sodium diisobutylnaphthalene sulfonate ), add tap water to form a 450ml solution, stir and mix evenly with a glass rod, place in an oil bath furnace, raise the temperature of the electric furnace to 300°C and stir for 1.5 hours, take it out, cool naturally to room temperature, separate the solution and graphite, and wash the sample with water until When the pH value of the washing solution is 7, it precipitates; it is filtered, and then dried in a constant temperature blast drying oven for 2 hours. After drying the alkali-soluble sample, weigh 20g, add 50ml of 55% nitric acid and 20g of sodium fluoride into the reaction vessel, and react at a temperature of 60°C for 6 hours. After the reaction, the solution and graphite are separated, and the graphite is washed with water until t...

Embodiment 3

[0024] 70g of carbon content 85%, aphanitic graphite with a particle size of 0.120mm is added to the reaction vessel, 100g of sodium hydroxide and 8g of additives are added (by 2.4g of sodium metaborate and 5.6g of sodium diisobutylnaphthalene sulfonate composition), add tap water to make a 500ml solution, stir and mix well with a glass rod, place in an oil bath furnace, raise the temperature of the electric furnace to 200°C and stir for 2 hours, take it out, cool naturally to room temperature, separate the solution and graphite, wash the sample with water until When the pH value of the washing solution is 7, it precipitates; it is filtered, and then dried in a constant temperature blast drying oven for 2 hours. After drying the alkali-soluble sample, weigh 20g, add 50ml of 60% nitric acid and 16g of ammonium difluoride to the reaction vessel together, and react at a temperature of 80°C for 4 hours. After the reaction, the solution and graphite are separated, and the graphite i...

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Abstract

The invention provides a purification method of natural cryptocrystalline graphite. The method using natural cryptocrystalline graphite as a raw material comprises the following steps: adding a sodium hydroxide solid and an assistant to the raw material, adding water, heating, fully stirring the obtained solution for a reaction, separating the solution and graphite, washing, precipitating, filtering, and drying to prepare alkali washed graphite, wherein the assistant is composed of sodium metaborate and sodium diisobutyl naphthalene sulfonate; adding alkali washed graphite, a soluble fluoride salt and nitric acid into a reaction container, heating while carrying out a stirring and soaking reaction, and separating the obtained solution and graphite to prepare graphite; and washing acid-containing graphite, precipitating, filtering, and drying to prepare graphite with the carbon content of above 99.90%. The purification method has the advantages of low energy consumption, little environmental pollution and high purification efficiency.

Description

technical field [0001] The invention relates to a method for purifying natural graphite, in particular to a method for purifying natural aphanitic graphite as a raw material with little environmental pollution and low energy consumption. Background technique [0002] Microcrystalline graphite is an important raw material and additive in many industrial productions, and is also widely regarded as industrial monosodium glutamate. There are reserves of microcrystalline graphite in some countries and regions such as Asia, America, and Europe, and my country is the largest proven microcrystalline graphite reserve in Asia and even the world, and the reserves after repeated exploration are more than 34 million tons. In recent years, with the rapid development of electronic information industry, nuclear industry, national defense industry and automobile industry, the graphite market has also undergone tremendous changes. First of all, the market demand for "quantity" has increased,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 林前锋
Owner 林前锋
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