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Ultra-high purity purifying technique for native graphite

A natural graphite, ultra-high-purity technology, applied in the field of ultra-high-purity purification process of natural flake graphite, can solve the problems of high cost, high cost, product loss, etc., achieve unstrict raw material requirements, reliable quality and performance, and reduce processing costs Effect

Active Publication Date: 2007-02-28
LUOYANG GUANQI INDAL & TRADE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In high-purity purification, high-temperature electrothermal method and alkaline purification with sodium hydroxide at a temperature of 700°C to 800°C are commonly used. The former uses the high-temperature resistance of graphite, puts it in an electric furnace, and heats it to 2500°C without air The ash in the graphite is volatilized above to produce more than 99.9% of high-purity graphite. This process is complex and requires the construction of a large-scale electric furnace. The power consumption is also quite large, and the inert gas needs to be continuously introduced, which is costly and especially important. When the purity of graphite reaches 99.93%, the purification limit has been reached, and the fixed carbon content cannot continue to increase
Alkaline purification using sodium hydroxide at a temperature of 700°C to 800°C, due to the reaction of impurities such as Si, Fe, Al, Ca, K, Na, Mg and other elements in graphite with sodium hydroxide at high temperature to form soluble Wash the water with a large amount of water to remove some water-insoluble substances. The reagents used in this method are strong alkali and strong acid corrosion. At the same time, the density of graphite is small and the floatability is good. It causes a large loss of products, and the increase of waste is not conducive to recycling, resulting in higher costs. At the same time, due to the defects of the process itself, the purity of natural graphite can only be purified to 98-99.8%.
In addition, the chlorination purification process of natural graphite disclosed in Chinese patent application number 94105051.3, this process is to adopt chlorine gas and bulk material layer infiltration or fluidization mode to carry out high-temperature chlorination under the action of catalyst and reducing agent in the reaction furnace. The process is complicated, and there are great potential safety hazards. The purity after treatment is only 98% to 99.9%. This process has not been industrialized, and no one in the industry uses it.
The carbon content of graphite used in the aerospace industry, the automotive industry, and the biotechnology industry must be high-purity graphite that must be above 99.9%, and some industries require that the carbon content must be above 99.99%. and defects, so that the carbon content can never reach 99.99%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 1.66 tons of Inner Mongolia 593 graphite + 1500 kg of water + 135 kg of concentrated sulfuric acid with a concentration of 96% into the reaction kettle 1 with a volume of 2000-3000 liters after anticorrosion treatment, stir evenly into a paste, react for 60 minutes, and dehydrate for 6 minutes , then add 120 kg of hydrochloric acid, react for 40 minutes, add 85 kg of water after dehydration, stir for 5 minutes, add 45 kg of hydrofluoric acid, stir for 6 minutes, react for 50 minutes, add water and stir for dehydration for 10 minutes, stop adding water and then dehydrate After 6 minutes, open the reaction kettle and discharge the material, pack into bags, and spin dry. The water content is 20%, and the carbon content is 97.5%. After melting in a container with a temperature of 560°C for 40 minutes, add 354 kg of caustic soda, stir once every 10 minutes, and stir for 3 minutes each time. After reacting for 66 minutes, put it in the kettle, discharge the material, and s...

Embodiment 2

[0026]Put 1.52 tons of Heilongjiang 890 graphite + 1395 kg of water + 163 kg of concentrated sulfuric acid into the reaction kettle 1 with a volume of 2000-3000 liters after anticorrosion treatment, stir evenly into a paste, react for 65 minutes, dehydrate for 6 minutes, and then add 138 hydrochloric acid React for 45 minutes, add 85 kg of water after dehydration, add 52 kg of hydrofluoric acid after stirring for 5 minutes, stir for 6 minutes, react for 50 minutes, add water and stir for dehydration for 10 minutes, stop adding water and dehydrate for 6 minutes, open the reactor once Gate discharge, bagging, drying, water content 22%, carbon content 96.8%. After melting in a container with a temperature of 680°C for 40 minutes, add 376 kg of caustic soda, stir once every 10 minutes, and stir for 3 minutes each time. After reacting for 66 minutes, put it in the kettle, discharge the material, and dry it to form a granular powder. Transport it to the reaction vessel by a slurry p...

Embodiment 3

[0028] Put 1.39 tons of Lingbao-185 graphite + 1268 kg of water + 176 kg of concentrated sulfuric acid into the reaction kettle 1 with a volume of 2000-3000 liters after anticorrosion treatment, stir evenly into a paste, react for 62 minutes, dehydrate for 6 minutes, and then add 156 kg of hydrochloric acid reacted for 43 minutes, then added 85 kg of water after dehydration, added 66 kg of hydrofluoric acid after stirring for 5 minutes, stirred for 6 minutes, reacted for 50 minutes, added water and stirred for 10 minutes, stopped adding water and then dehydrated for 6 minutes, and started the reaction The kettle is discharged from the gate, bagged, and dried, with a water content of 25% and a carbon content of 96.2%. After melting in a container with a temperature of 750°C for 40 minutes, add 331 kg of caustic soda, stir once every 10 minutes, and stir for 3 minutes each time. After reacting for 66 minutes, put it in the kettle, discharge the material, and dry it to form a gran...

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Abstract

The invention discloses a hyper-high purity extracting technology of natural graphite, which comprises the following steps: (1) putting natural graphite in the container to do oxidizing disposal with low-middle carbon content more than 98%; (2) fusing at high temperature; (3) inputting in the metal erosion-proof container; proceeding dealkalization; (4) deacidifying to wash to neutral; (5) proceeding electromagnetic black metal removing disposal in the floating pool; (6) heating in the autoclave from 118 deg, 206 deg and 220 deg separately; (7) using pure water to dispose; (8) dehydrating; (9) drying until the water content is less than 0.1%.

Description

technical field [0001] The invention relates to an ultra-high-purity purification method of natural graphite, in particular to an ultra-high-purity purification process of natural flake graphite. Background technique [0002] At present, the purification methods of natural graphite known at home and abroad are divided into low-purity purification and high-purity purification. In the industry, people usually refer to graphite with a carbon content of less than 94% as medium and low-carbon graphite, and refer to graphite with a carbon content of 94%. -99.8% is called high-carbon graphite; the carbon content of 99.9%-99.99% is called high-purity graphite, and the carbon content of more than 99.99% is called ultra-high-purity graphite. In high-purity purification, high-temperature electrothermal method and alkaline purification with sodium hydroxide at a temperature of 700°C to 800°C are commonly used. The former uses the high-temperature resistance of graphite, puts it in an el...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 侯玉奇侯旭异
Owner LUOYANG GUANQI INDAL & TRADE
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