CN111137882A - Method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite - Google Patents
Method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite Download PDFInfo
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Abstract
The invention discloses a method for treating natural crystalline flake graphite fine powder for preparing high-purity graphite, which comprises the following steps: (1) heating the fine graphite powder, and then quickly cooling; (2) repeating the operation of the step (1) for 5-20 times; (3) after each heating and cooling cycle, the graphite fine powder is subjected to ultrasonic vibration treatment. The method provides a graphite fine powder intermediate for a subsequent graphite purification process, so that the impurity removal effect of impurities is improved, the impurity removal time is shortened, the impurity removal efficiency is improved, and the impurity removal cost is reduced.
Description
Technical Field
The invention relates to the technical field of graphite purification, in particular to a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite.
Background
Natural graphite generally occurs as an ore such as graphite schist, graphite schist gneiss, graphite-containing schist, and metamorphic shale. The chemical component of graphite is carbon (C). Naturally produced graphite is rarely pure and often contains impurities, including SiO2，Al2O3，MgO，CaO，P2O5CuO, V2O5, H2O, S, FeO and H, N, CO2，CH4，NH3And the like. The technological properties and the use of graphite are mainly determined by the degree of crystallization, and natural graphite can be divided into two industrial types, namely crystalline graphite (flake graphite) and cryptocrystalline graphite (earthy graphite) according to the crystallization form of the graphite.
In crystalline (flake) graphite ore, the diameter of graphite crystal is larger than 1 μm, and the graphite crystal is flaky; the ore grade is low, but the selectivity is good; the graphite-associated minerals often include mica, feldspar, quartz, tremolite, diopside, garnet, a small amount of pyrite, calcite and the like, and the graphite-associated minerals also include rutile, vanadium and other useful components; the ore is in scaly, granite-scale or granular crystal-changing structure, sheet, flake or block structure. The mineral separation method of the graphite mineral separation production line comprises flotation, electric separation, gravity separation and the like, and the flotation method is most widely applied. The flake graphite has better floatability, so most of the flake graphite is separated by adopting a flotation method, in the use of a flotation reagent, kerosene or diesel oil is generally used as a collecting agent in China, No. two oil or novel flotation oil is used as a foaming agent, and through years of production practice, No. four oil is considered as an ideal graphite ore dressing foaming agent. In the flotation, in order to inhibit the minerals, water fluctuation, starch, dextrin, organic glue, cellulose and other agents can be used, for example, the pyrite content in the ore is higher, and lime and oxide can be added.
And removing impurities from the graphite subjected to flotation by adopting various purification technologies to obtain the high-purity graphite. Graphite with more than 99% of fixed carbon is called high-purity graphite. With the development of the material industry, the purity of the graphite becomes more and more severe, for example, the purity C of crystalline flake graphite is not less than 99.9%, the purity C of microcrystalline graphite is not less than 99%, and the graphite with certain particle size, particle size distribution and particle shape is high-purity graphite. By means of the characteristics of excellent electric and thermal conductivity, high-temperature thermal shock resistance, corrosion and radiation resistance, high strength, good toughness, self-lubrication, easy precision machining and the like, the high-purity graphite is widely applied to the fields of chemical engineering, aerospace, metallurgy, electronics, machinery, nuclear energy and the like, and has wide application space and bright application prospect in the fields of new technology, high technology and the like as a novel material.
The important position of graphite in national economy and basic public service type industries is increasing day by day, and the purity requirement of graphite in each industry is higher and higher, so that the development of graphite purification research is very important. At present, the method for preparing high-purity graphite at home and abroad mainly comprises two main types: chemical purification methods including flotation, alkaline-acid, hydrofluoric acid, and chlorination-roasting; the physical purification method mainly comprises a high-temperature purification method. The purification methods are all that the graphite fine powder obtained by floating the natural graphite is directly purified. But all have certain limitations. (1) The alkaline-acid method has been widely used in industrial production. The purification method has the advantages of low investment of one-time equipment, high product purity, simple process flow and conventional production equipment, and is the most widely applied method of the existing graphite purification method; however, the purification method requires a long time of high-temperature calcination and acid leaching, so that energy consumption is large, equipment corrosion is severe, and polluting acidic wastewater is generated. (2) The hydrofluoric acid method has better purification effect, and the industrial production is realized in Europe and America at the end of 20 th century. The method has high impurity removal efficiency and high product purity, does not influence the performance of the graphite product, and has low purification energy consumption; but hydrofluoric acid has serious influence on the environment, is toxic and highly corrosive, production equipment needs to have corrosion resistance, and production personnel need to adopt safety protection measures all the time, so the production cost is high and the recovery rate is low. Acidic waste water with strong toxicity and corrosiveness is generated in the purification process of the hydrofluoric acid method, and needs to be properly treated for discharge. (3) The chloridizing roasting method has low roasting temperature and low chlorine consumption, so the chloridizing roasting method has lower production cost, less production energy consumption and high product purity and recovery rate. However, chlorine gas has extremely bad influence on the environment, is toxic and strong in corrosivity, and needs strict sealing treatment in the production process in order to reduce pollution and reduce the corrosion rate of equipment; and the purification effect is limited, and the process stability is poor, so that the method is difficult to be applied to actual industrial production. (4) The high-temperature method has excellent purification effect, the content of impurities is lower than 0.005 percent, but the high-temperature roasting furnace needs to be separately designed and constructed, so the investment of disposable equipment is more, the production cost is high, and the production scale is limited. Because industries such as national defense, aerospace, superhard materials and the like urgently need a large amount of ultra-pure graphite, the industrial development of preparing ultra-pure graphite products by a high-temperature method is promoted to a certain extent.
In summary, the existing purification processes and methods remove impurities by acid-base liquid, gas or high temperature. The impurities are removed by changing the external reaction environment and volatilizing the liquid or gas capable of reacting with the impurities or the impurities. But the embedding relation between the target mineral graphite and the gangue mineral in the graphite ore is complicated. Meanwhile, impurities with smaller particle sizes exist in the graphite in the form of inclusions, and the particle size of the graphite concentrate subjected to flotation is larger than the sizes of the inclusions, so that more impurity inclusions still exist in the graphite concentrate. Even with the above process, it is difficult to completely remove fine inclusion impurities. Primarily because these inclusions are difficult to fully contact and react with the above-mentioned liquid and gaseous tissues. Thus, all the purification methods described above have limitations.
The graphite concentrate after flotation is subjected to grinding and concentration for different times. Generally, the monomer dissociation rate of graphite minerals increases as the fineness of grinding decreases, but complete monomer dissociation is difficult even after many times of fine grinding as the fineness decreases. Meanwhile, as the graphite ore contains a certain amount of muscovite, and the muscovite has better floating performance, even if the inhibition is strengthened in the flotation process, part of the muscovite still enters the final graphite fine powder. Because the particle size of the graphite fine powder after flotation is larger than the size of the inclusion of the impurities, if the graphite fine powder is not pretreated, the good impurity removal effect can not be obtained even if the impurity removal process is utilized. The traditional graphite purification process is to directly contact graphite concentrate with acid solution or alkali solution (alkali melt) or gas to generate chemical reaction to remove impurities, and the graphite concentrate is not treated at all, so that the direct impurity removal effect is not ideal, and most inclusion impurities are not contacted with an impurity removal medium.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite, which provides a graphite fine powder intermediate for a subsequent graphite purification process, thereby improving the impurity removal effect of impurities, shortening the impurity removal time, improving the impurity removal efficiency and reducing the impurity removal cost.
The invention is realized by the following technical scheme:
a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite comprises the following steps:
(1) heating the fine graphite powder, and then quickly cooling;
(2) repeating the operation of the step (1) for 5-20 times;
(3) after each heating and cooling cycle, the graphite fine powder is subjected to ultrasonic vibration treatment.
According to the invention, the graphite fine powder subjected to flotation is repeatedly heated and then rapidly cooled, the volume of impurities such as mica embedded in the graphite crystal can be changed due to different linear expansion coefficients of the impurities such as mica and the graphite, and the interface of the impurities such as mica and the graphite crystal in contact can fall off due to repeated expansion and contraction.
After several cycles of repeated expansion and rapid cooling, a gap is generated between the embedded inclusion in the graphite crystal and the graphite crystal, the two is separated even after ultrasonic vibration treatment, so that the monomer dissociation rate of the graphite crystal is improved, the graphite crystal is cracked due to the volume expansion of the inclusion, more inclusions are exposed, more contact areas and contact probabilities are provided for subsequent purification, the reaction contact area is effectively increased for the subsequent purification process, the impurity removal time is greatly shortened, the production efficiency is improved, and the production energy consumption is also reduced.
Because the mosaic relation between the impurity inclusion and the graphite crystal is changed, the purification process can be more sufficient and thorough, so that the impurity content of the purified graphite can be greatly reduced, and the purity of the graphite can be further improved.
Wherein, in the step (1), the graphite heating adopts electromagnetic induction heating or microwave vibration heating.
Further, the electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 300 MHZ-300 GHZ.
Further, in the step (1), air quenching is adopted as a cooling mode, the cooling temperature is 0-5 ℃, and the time required for reducing the temperature of the fine graphite powder from 450 ℃ to 0-5 ℃ is 10-15 min.
Further, in the step (3), the frequency of ultrasonic vibration treatment is 300 MHZ-300 GHZ, and the ultrasonic vibration treatment time is 30 min-45 min.
Further, in the step (1), the temperature of the graphite fine powder is raised to 400-450 ℃, and the temperature raising process is carried out at normal temperature and normal pressure.
Or, in the step (1), the temperature of the graphite fine powder is raised to 450-1000 ℃, and the temperature raising process is carried out under the protection of inert gas.
An application of the refined powder of natural crystalline flake graphite for preparing high-purity graphite in purifying graphite.
The present invention utilizes the difference in linear expansion coefficient between graphite and impurities such as mica, for example: the linear expansion coefficient of mica is 19.8-19.9 x 10-6/° c (20 ℃ to 500 ℃); the linear expansion coefficient of quartz is 7.10 to 12.22 x 10 in parallel direction-6V deg.C and vertical direction 13.24 to 20.91 x 10-6/° c (20 ℃ to 500 ℃); expansion coefficient of feldspar type impurities (potassium feldspar and albite about 8.5 to 12.5 x 10)-6/° c)) 20 ℃ to 500 ℃; and the linear expansion coefficient of the graphite is 2.85 to 3.70 x 10 in the parallel direction-6V deg.C and vertical direction 2.94 to 3.50 x 10-6The repeated expansion and contraction of graphite and impurities at 20-400 ℃ can cause the contact interface of impurities such as mica and the like and graphite crystals to fall off, so that the mosaic relation between the impurity inclusion in the fine graphite powder and the graphite crystals is changed.
The method for treating the graphite fine powder does not need to specially design and build a high-temperature furnace, has simple equipment and less one-time investment, and in addition, has low heating temperature, lower energy consumption and lower production cost.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite, the graphite fine powder subjected to flotation is repeatedly heated and then rapidly cooled, the volume of impurities such as mica and the like embedded in the graphite crystal can be changed due to the fact that the impurities such as mica are different from the linear expansion coefficient of the graphite, the repeated expansion and contraction can cause the contact interface of the impurities such as mica and the like and the graphite crystal to fall off, and meanwhile, the linear expansion coefficient of the impurities such as mica and the like is larger and the volume expansion is larger than the volume change of the graphite crystal, so that the effect of force can be exerted on the graphite crystal after the volume expansion, even the graphite crystal can be cracked, the impurities such as a wrapping body and the like can be in direct contact with the outside, and the embedding rule of the impurities in the graphite crystal is effectively changed;
2. according to the method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite, after repeated expansion and rapid cooling for a plurality of cycles, gaps are formed between the embedded inclusion in the graphite crystal and the graphite crystal, and the embedded inclusion and the graphite crystal are even separated after ultrasonic vibration processing, so that the monomer dissociation rate of the graphite crystal is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
As shown in fig. 1, the method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite of the present invention specifically comprises the following steps:
1) heating the fine graphite powder to 400-450 ℃ at normal temperature and normal pressure, and then quenching the fine graphite powder to 0-5 ℃ in air;
2) repeating the operation of the step 1) for 5-20 times;
3) after each heating and cooling period, carrying out ultrasonic vibration treatment on the graphite fine powder, wherein the frequency of the ultrasonic vibration treatment is 300 MHZ-300 GHZ, and the time of the ultrasonic vibration treatment is 30 min-45 min.
Wherein, in the step (1), the graphite heating adopts electromagnetic induction heating or microwave vibration heating. The electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 300 MHZ-300 GHZ.
The time for reducing the temperature of the graphite fine powder from 450 ℃ to 0-5 ℃ is 10-15 min.
Example 2
The invention relates to a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite, which specifically comprises the following steps:
1) heating the fine graphite powder to 450 ℃ at normal temperature and normal pressure, and then quenching the fine graphite powder to 0 ℃ in air;
2) repeating the operation of the step 1) for 10 times;
3) after each heating and cooling period, the graphite fine powder is subjected to ultrasonic vibration treatment, wherein the frequency of the ultrasonic vibration treatment is 10GHZ, and the ultrasonic vibration treatment time is 30min 1.
Wherein, in the step (1), the graphite heating adopts electromagnetic induction heating or microwave vibration heating. The electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 10 GHZ.
The time for reducing the temperature of the fine graphite powder from 450 ℃ to 0 ℃ is 10 min.
Example 3
The invention relates to a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite, which specifically comprises the following steps:
1) under the protection of inert gas, heating the fine graphite powder to 700 ℃, and then quenching the inert gas to 2 ℃;
2) repeating the operation of the step 1) for 6 times;
3) after each heating and cooling period, carrying out ultrasonic vibration treatment on the graphite fine powder, wherein the frequency of the ultrasonic vibration treatment is 10GHZ, and the ultrasonic vibration treatment time is 30 min.
Wherein, in the step (1), the graphite heating adopts electromagnetic induction heating or microwave vibration heating. The electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 10 GHZ.
The time for reducing the temperature of the fine graphite powder from 700 ℃ to 2 ℃ is 10 min.
Example 4
The invention relates to a method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite, which specifically comprises the following steps:
1) heating the fine graphite powder to 450 ℃ at normal temperature and normal pressure, and then quenching the fine graphite powder to 0 ℃ in air;
2) repeating the operation of the step 1) for 2 times;
3) after each heating and cooling period, the graphite fine powder is subjected to ultrasonic vibration treatment, wherein the frequency of the ultrasonic vibration treatment is 10GHZ, and the ultrasonic vibration treatment time is 30min 1.
Wherein, in the step (1), the graphite heating adopts electromagnetic induction heating or microwave vibration heating. The electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 10 GHZ.
The time for reducing the temperature of the fine graphite powder from 450 ℃ to 0 ℃ is 10 min.
This example differs from example 2 in that: the repetition times of step 1) are different.
Example 5
A graphite powder purification process comprises the following steps:
(1) preparing solid sodium hydroxide into a solution with the concentration of 40 percent;
(2) mixing sodium hydroxide and graphite fine powder according to the weight ratio of 1:0.7, uniformly stirring, and melting at 500 ℃ for 1.5 hours;
(3) then cooling to below 100 ℃, washing, and then adding hydrochloric acid for acid leaching, wherein the addition amount of the hydrochloric acid is 30-40% of the graphite fine powder;
(4) and washing the obtained product with clear water to neutrality after acid leaching, and then carrying out solid-liquid separation and drying to obtain the high-carbon graphite product.
Taking quantitative fine graphite powder, dividing into 5 parts, wherein the numbers are 1, 2, 3, 4 and 5, the fine graphite powder with the number 1 is not subjected to any treatment, the fine graphite powder with the number 2 is directly purified by the purification process of the example 5 without being subjected to treatment, and the fine graphite powder with the numbers 2, 3 and 4 is respectively subjected to the processes of the examples 2, 3 and 4 and then purified by the purification process of the example 5. Then, the chemical components of the refined graphite powder, the chemical components of the directly purified refined graphite powder and the chemical components of the activated refined graphite powder are analyzed by an X-ray fluorescence spectrometer (XRF), and the comparison results are shown in the following table.
From the above table detection results, it can be seen that the purity of the graphite obtained by purifying the graphite fine powder after the process treatment of the embodiments 2 and 3 is significantly higher than that of the graphite directly purified without the activation treatment, and is also significantly higher than that of the graphite purified after the process treatment of the embodiment 4.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for processing natural crystalline flake graphite fine powder for preparing high-purity graphite is characterized by comprising the following steps:
(1) heating the fine graphite powder, and then quickly cooling;
(2) repeating the operation of the step (1) for 5-20 times;
(3) after each heating and cooling cycle, the graphite fine powder is subjected to ultrasonic vibration treatment.
2. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite according to claim 1, wherein in the step (1), the graphite is heated by electromagnetic induction heating or microwave vibration heating.
3. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite according to claim 2, wherein the electromagnetic induction heating mode is high-frequency heating; the microwave heating working frequency is 300 MHZ-300 GHZ.
4. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite according to claim 1, wherein in the step (1), the cooling mode adopts air quenching, the cooling temperature is 0-5 ℃, and the time required for reducing the temperature of the graphite fine powder from 450 ℃ to 5 ℃ is 10-15 min.
5. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite as claimed in claim 1, wherein in the step (3), the frequency of the ultrasonic vibration treatment is 300 MHZ-300 GHZ, and the time of the ultrasonic vibration treatment is 30 min-45 min.
6. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite according to claim 1, wherein the temperature of the graphite fine powder in the step (1) is 400 to 450 ℃, and the temperature rise process is carried out at normal temperature and normal pressure.
7. The method for processing the natural crystalline flake graphite fine powder for preparing the high-purity graphite according to claim 1, wherein the temperature of the graphite fine powder in the step (1) is 450-1000 ℃, and the temperature rise is carried out under the protection of inert gas.
8. Use of the fine powder of natural crystalline flake graphite for the preparation of high purity graphite according to any one of claims 1 to 7 in the purification of graphite.
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| CN114634179A (en) * | 2022-03-25 | 2022-06-17 | 矿冶科技集团有限公司 | Pretreatment equipment and method before grinding of graphite ore |
| CN114890415A (en) * | 2022-05-25 | 2022-08-12 | 福建邵武科踏高纯石墨有限公司 | Preparation method of fine flake high-purity expanded graphite |
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