CN111439750B - Preparation and purification method of high-purity graphite - Google Patents
Preparation and purification method of high-purity graphite Download PDFInfo
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- CN111439750B CN111439750B CN202010272885.6A CN202010272885A CN111439750B CN 111439750 B CN111439750 B CN 111439750B CN 202010272885 A CN202010272885 A CN 202010272885A CN 111439750 B CN111439750 B CN 111439750B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
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- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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Abstract
The invention relates to a preparation and purification method of high-purity graphite, wherein a graphite raw material is refined in an airflow vortex split refiner; graphite powder conveys materials to a cyclone separator through a spiral conveying rod, the diameter of the front end of the spiral conveying rod is smaller than that of the rear end of the spiral conveying rod, spiral threads on the front part of the spiral conveying rod are denser than those on the rear part of the spiral conveying rod, the internal temperature of a spiral conveying sleeve is controlled to be 300-shaped and 400 ℃, and a discharge nozzle on the front part of the spiral conveying sleeve is conical; carrying out filter pressing on the preliminarily classified fine graphite powder, adding water, carrying out filter pressing again, drying, and carrying out magnetic absorption to remove impurities; and refining the airflow vortex split refiner and grading the cyclone separator for many times. The yield of fine powder of the same grade of graphite powder produced by the process is improved by 10-20%, wherein the mass percentage of nitrogen and sulfur impurities is reduced by more than 60%.
Description
Technical Field
The invention relates to graphite powder, in particular to a preparation and purification method of high-purity graphite.
Background
Graphite is a high-energy crystalline carbon material, has high use value in high-function materials due to the characteristics of structure, electric conduction, heat conduction, smoothness, high temperature resistance, stable chemical function and the like, and is widely applied to the fields of metallurgy, machinery, environmental protection, chemical industry, fire resistance, electronics, medicine, military industry, aerospace and the like. Graphite is a good energy-saving and environment-friendly material, and with the development of modern scientific technology and industry, the application field of graphite is continuously widened, so that graphite becomes an important raw material of a novel composite material in the high-tech field, and has an important role in national economy. With the continuous development of new technology and new technology, the common high-purity graphite material cannot meet the requirements of many industries, the use characteristics and the comprehensive performance of the graphite material are determined by the purification quality of graphite, and the higher the purity of graphite is, the higher the application value is.
The natural graphite has carbon content of 85-95%, is called medium-high carbon crystalline flake graphite, and has main impurities including sulfur, nitrogen and oxides thereof, and metal bodies brought in the production process. The impurity removal process mainly removes these metal bodies and sulfur, nitrogen and oxides thereof.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for producing and purifying high-purity graphite.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the preparation and purification method of the high-purity graphite is characterized by comprising the following steps:
(1) refining the graphite raw material in an airflow vortex split refiner;
(2) graphite powder is conveyed to a cyclone separator through a spiral conveying rod, the diameter of the front end of the spiral conveying rod is smaller than that of the rear end of the spiral conveying rod, spiral grains in the front part of the spiral conveying rod are denser than those in the rear part of the spiral conveying rod, a spiral conveying sleeve outside the spiral conveying rod is matched with the spiral conveying rod, the spiral conveying rod is matched with an electric heating assembly, the temperature in the spiral conveying sleeve is controlled to be 300-plus 400 ℃, a discharge nozzle in the front part of the spiral conveying sleeve is conical, and the discharge nozzle pumps and conveys the graphite powder to the cyclone separator for primary classification through gas drainage; and after preliminary grading, the materials are subjected to preliminary magnetic metal impurity removal by a permanent magnet machine.
(3) Pickling the fine graphite powder subjected to preliminary impurity removal, performing filter pressing, adding water, performing filter pressing again, drying, and performing magnetic absorption to remove impurities;
(4) refining the graphite powder by the airflow vortex split refiner and grading by the cyclone separator for multiple times;
(5) removing impurities from the finally obtained graphite fine powder by magnetic absorption, and sieving.
The invention has the beneficial effects that:
(1) the internal temperature of the spiral conveying sleeve is controlled to be 300-400 ℃, the front part of the spiral conveying sleeve is provided with a conical discharge nozzle, the graphite powder is extruded by a spiral conveying rod in the spiral conveying sleeve, the air pressure of the graphite powder reaches 3-5MPa, and the graphite powder is extruded and expanded within the temperature range of 300-400 ℃, so that the graphite powder is fluffy and refined. The temperature of 300 ℃ and 400 ℃ can oxidize the nitrogen and the sulfur in the graphite into oxides, and the temperature range can not cause the oxidation and the combustion of the graphite.
(2) The venturi is formed at the discharge nozzle of the spiral conveying sleeve, the graphite is extruded in the spiral conveying sleeve, and then the graphite is diffused at the discharge nozzle to generate negative pressure, so that the graphite is further expanded under the negative pressure at the discharge nozzle, particles are loosened, and the pretreatment is performed for cyclone separation at the lower part.
(3) The yield of the fine powder of the same grade of the graphite powder produced by the process is improved by 30 percent, wherein the mass percentage content of nitrogen and sulfur impurities is reduced by more than 90 percent.
Drawings
Fig. 1 is a schematic view of a specific structure of the screw conveying rod of the present invention.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention and to clearly and unequivocally define the scope of the present invention.
The preparation and purification method of the high-purity graphite is characterized by comprising the following steps:
the first step is as follows: the graphite raw material is refined in an airflow vortex split refiner. The selected graphite raw material is graphite powder with the mass percentage content not lower than 90%, the graphite raw material is put into an airflow vortex split refiner for refining, the rotating speed is set to 2500-3000r/min, and the refining time is 30-60 s.
The second step is that: graphite powder conveys the materials to a cyclone separator through a spiral conveying rod. The structure of the specific spiral conveying rod is shown in the attached drawing 1 of the specification, the diameter of the front end of the spiral conveying rod is smaller than that of the rear end of the spiral conveying rod, spiral threads on the front portion of the spiral conveying rod are more compact than those on the rear portion of the spiral conveying rod, a spiral conveying sleeve 2 outside the spiral conveying rod 1 is matched with the spiral conveying rod 1, the spiral conveying rod is provided with an electric heating assembly, the electric heating assembly is an electric heating tile, and the electric heating tile 3 is arranged outside the spiral conveying sleeve. Controlling the internal temperature of the spiral conveying sleeve to be 300-400 ℃, wherein the front part of the spiral conveying sleeve is provided with a discharge nozzle 4 which is conical, and the discharge nozzle pumps and conveys the graphite powder to a cyclone separator for primary classification through a gas drainage tube; the graphite powder is extruded by the spiral conveying rod in the spiral conveying sleeve, the air pressure of the graphite powder reaches 3-5MPa, and the graphite powder is extruded and expanded within the temperature range of 300-400 ℃, so that the graphite powder is fluffy and refined. The temperature of 300 ℃ and 400 ℃ can oxidize the nitrogen and the sulfur in the graphite into oxides, and the temperature range can not cause the oxidation and the combustion of the graphite. The venturi is formed at the discharge nozzle of the spiral conveying sleeve, the graphite is extruded in the spiral conveying sleeve, and then the graphite is diffused at the discharge nozzle to generate negative pressure, so that the graphite is further expanded under the negative pressure at the discharge nozzle, particles are loosened, and the pretreatment is performed for cyclone separation at the lower part.
The discharge nozzle pumps and conveys the graphite powder to a cyclone separator for primary classification through gas drainage, and the particle size of the separated graphite powder is 2.5-80 mu m. The classified materials are subjected to permanent magnet to primarily remove materials containing obvious magnetic substances, so that high-quality graphite powder is provided for subsequent acid washing.
The third step: pickling graphite powder, filter-pressing with a plate-and-frame filter press, adding water, stirring, filter-pressing with a plate-and-frame filter press again, drying at 150 plus 200 ℃, magnetically attracting to remove impurities, and mixing again. The specific operation is as follows:
putting graphite into a dissolving tank, adding an eluent, wherein the eluent is a hydrochloric acid solution with the mass percentage of 20% -30%, and the mass fraction ratio of graphite powder to the eluent is 1: 2; the temperature of the dissolving tank is adjusted to be 100 ℃ and 120 ℃, and the reaction lasts 24 hours; then conveying the reacted graphite solution into a primary filter press for filter pressing; and washing and mixing the wet materials subjected to filter pressing with purified water, carrying out filter pressing again, conveying the graphite subjected to filter pressing to a flash evaporation dryer for scattering and drying, and carrying out magnetic absorption for removing impurities after drying.
The fourth step: refining the fine graphite powder subjected to preliminary classification by an airflow vortex split refiner and classifying by a cyclone separator for multiple times; refining in a secondary airflow vortex split refiner at the rotating speed of 2500-; the particle size of the graphite powder separated by the cyclone separator is 2-60 mu m. Refining in a third airflow vortex split refiner at the rotating speed of 2500-; the particle size of the graphite powder separated by the cyclone separator is 1.5-40 μm.
The fifth step: and finally, carrying out double adsorption and impurity removal on the obtained graphite fine powder by an electromagnet and a permanent magnet, and then carrying out 325-mesh sieving treatment.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, that the preferred embodiments of the present invention are described above and the present invention is not limited to the preferred embodiments, and that various changes and modifications may be made without departing from the spirit and scope of the present invention and these changes and modifications are within the scope of the invention as claimed.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. The preparation and purification method of the high-purity graphite is characterized by comprising the following steps:
(1) refining the graphite raw material in an airflow vortex split refiner;
(2) graphite powder is conveyed to a cyclone separator through a spiral conveying rod, the diameter of the front end of the spiral conveying rod is smaller than that of the rear end of the spiral conveying rod, spiral grains in the front part of the spiral conveying rod are denser than those in the rear part of the spiral conveying rod, a spiral conveying sleeve outside the spiral conveying rod is matched with the spiral conveying rod, the spiral conveying rod is matched with an electric heating assembly, the temperature in the spiral conveying sleeve is controlled to be 300-plus 400 ℃, a discharge nozzle in the front part of the spiral conveying sleeve is conical, and the discharge nozzle pumps and conveys the graphite powder to the cyclone separator for primary classification through gas drainage; after preliminary grading, the materials are subjected to preliminary magnetic metal impurity removal by a permanent magnet machine;
(3) pickling the fine graphite powder subjected to preliminary impurity removal, performing filter pressing, adding water, performing filter pressing again, drying, and performing magnetic absorption to remove impurities;
(4) refining the graphite powder by the airflow vortex split refiner and grading by the cyclone separator for multiple times;
(5) removing impurities from the finally obtained graphite fine powder by magnetic absorption, and sieving.
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| CN113998696B (en) * | 2021-12-10 | 2023-09-26 | 营口博田材料科技有限公司 | Impurity removing method for high-purity graphite |
| CN115924907B (en) * | 2022-12-21 | 2023-07-14 | 江苏金亚隆科技有限公司 | Physical purification process of graphite raw material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850964A (en) * | 2009-11-27 | 2010-10-06 | 洛阳市冠奇工贸有限责任公司 | Spherical graphite with median diameter of 17 to 30 mu m and preparation method thereof |
| CN102241322A (en) * | 2010-05-11 | 2011-11-16 | 江苏清溢环保设备有限公司 | Spiral medicine addition device |
| CN204096503U (en) * | 2014-08-14 | 2015-01-14 | 湖南超牌科技有限公司 | Powder conveying apparatus |
| CN104437771A (en) * | 2014-12-04 | 2015-03-25 | 山东双轮股份有限公司 | Crushing press used in kitchen |
| CN105346952A (en) * | 2015-11-02 | 2016-02-24 | 湖南顶立科技有限公司 | Continuous type graphite purification equipment and continuous type graphite purification material conveying device |
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- 2020-04-09 CN CN202010272885.6A patent/CN111439750B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101850964A (en) * | 2009-11-27 | 2010-10-06 | 洛阳市冠奇工贸有限责任公司 | Spherical graphite with median diameter of 17 to 30 mu m and preparation method thereof |
| CN102241322A (en) * | 2010-05-11 | 2011-11-16 | 江苏清溢环保设备有限公司 | Spiral medicine addition device |
| CN204096503U (en) * | 2014-08-14 | 2015-01-14 | 湖南超牌科技有限公司 | Powder conveying apparatus |
| CN104437771A (en) * | 2014-12-04 | 2015-03-25 | 山东双轮股份有限公司 | Crushing press used in kitchen |
| CN105346952A (en) * | 2015-11-02 | 2016-02-24 | 湖南顶立科技有限公司 | Continuous type graphite purification equipment and continuous type graphite purification material conveying device |
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