CN115974070A - Alkaline-acid purification method of natural spherical graphite - Google Patents
Alkaline-acid purification method of natural spherical graphite Download PDFInfo
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- CN115974070A CN115974070A CN202211584383.2A CN202211584383A CN115974070A CN 115974070 A CN115974070 A CN 115974070A CN 202211584383 A CN202211584383 A CN 202211584383A CN 115974070 A CN115974070 A CN 115974070A
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Abstract
An alkaline-acid purification method of natural spherical graphite, which relates to the field of graphite processing. The alkali-acid method for purifying the natural spherical graphite comprises the steps of uniformly mixing a spherical graphite raw material with a sodium hydroxide solution under the vacuum degree of-0.05 to-0.10 MPa, and then pressurizing and stirring to obtain a mixed solution; filtering and roasting the mixed solution to obtain a roasted product; mixing the roasted product with water, ultrasonically discharging supernatant liquid until the roasted product is washed to be neutral; dehydrating the washed neutral roasted product, uniformly mixing the dehydrated product with acid liquor under the vacuum degree of-0.05 to-0.10 Mpa, and pressurizing and stirring to obtain spherical graphite after acid leaching; mixing the spherical graphite subjected to acid leaching with water, ultrasonically discharging supernatant liquid until the supernatant liquid is washed to be neutral, and obtaining the purified spherical graphite. The alkaline-acid purification method for natural spherical graphite can improve reaction efficiency and reduce purification cost under the condition of reducing the using amount of alkali and acid.
Description
Technical Field
The application relates to the field of graphite processing, in particular to an alkaline-acid purification method of natural spherical graphite.
Background
With the rapid development of new energy industry, particularly the electric automobile industry, the demand of the negative electrode material for the natural spherical graphite is rapidly increased. Common chemical purification methods for graphite include hydrofluoric acid and alkaline acid methods. Although the hydrofluoric acid method has good purification effect and simple process, F ions in the purified wastewater have great harm to the environment and are difficult to treat; the traditional alkaline-acid method for purifying graphite has low reaction efficiency and large energy consumption, the purity of the purified product is not high, and the fixed carbon content of the purified graphite is difficult to reach more than 99.90 percent.
Therefore, there is a need for a fluorine-free purification method of spherical graphite to reduce environmental pollution caused by purification.
Disclosure of Invention
The purpose of the application is to provide an alkaline-acid method for purifying natural spherical graphite, which can improve the reaction efficiency and reduce the purification cost under the condition of reducing the using amount of alkali and acid.
The embodiment of the application is realized as follows:
the application provides a method for purifying natural spherical graphite by an alkaline-acid method, which comprises the following steps:
uniformly mixing a spherical graphite raw material with a sodium hydroxide solution with the mass fraction of 30-50% under the vacuum degree of-0.05-0.10 MPa, and then stirring for 0.5-1 h at the temperature of 30-40 ℃ under the pressure condition of 0.03-0.08 MPa to obtain a mixed solution;
filtering the mixed solution to obtain a mixture, and roasting the mixture at 500-600 ℃ for 1-2 h to obtain a roasted product;
mixing the roasted product with water at 50-80 ℃, standing the mixture after ultrasonic treatment, discharging supernatant, and repeating the steps until the roasted product is washed to be neutral;
dehydrating the washed neutral roasted product to obtain a spherical graphite filter cake, uniformly mixing the spherical graphite filter cake with acid liquor under the vacuum degree of-0.05 to-0.10 Mpa, and stirring for 1 to 2 hours at the temperature of between 30 and 50 ℃ under the pressure condition of between 0.03 and 0.08Mpa to obtain acid-leached spherical graphite;
mixing the acid-leached spherical graphite with water at 50-80 ℃, standing after ultrasonic treatment, discharging supernatant, and repeating the steps until the spherical graphite is washed to be neutral to obtain the purified spherical graphite.
In some alternative embodiments, the mass ratio of the sodium hydroxide solution to the raw material for spherical graphite when mixed is 1.6 to 2:1.
in some optional embodiments, before the raw material of spherical graphite and the sodium hydroxide solution are mixed uniformly, the raw material of spherical graphite is maintained for 20-30 min under a vacuum degree of-0.05 to-0.10 MPa.
In some alternative embodiments, the frequency of sonication is 20 to 40kHz and the duration of sonication is 3 to 5min.
In some alternative embodiments, the acid solution is hydrochloric acid, nitric acid, or a mixture of hydrochloric acid and nitric acid, and the volume fraction of the acid solution is 15 to 20%.
In some alternative embodiments, the spherical graphite filter cake is maintained under a vacuum of-0.05 to-0.10 MPa for 20 to 30 minutes before the spherical graphite filter cake and the acid solution are mixed uniformly.
In some alternative embodiments, the acid solution and the spherical graphite filter cake are mixed in a mass ratio of 1 to 1.5:1.
in some alternative embodiments, after washing the roasted product out of the roasting container using boiling water, the roasted product is mixed with water of 50 to 80 ℃ for ultrasonic treatment and then left to stand.
In some alternative embodiments, the raw spheroidal graphite has a fixed carbon content of 93 to 98%.
The beneficial effect of this application is: the alkaline-acid purification method of the natural spherical graphite comprises the following steps: uniformly mixing a spherical graphite raw material with a sodium hydroxide solution with the mass fraction of 30-50% under the vacuum degree of-0.05-0.10 MPa, and then stirring for 0.5-1 h at the temperature of 30-40 ℃ under the pressure condition of 0.03-0.08 MPa to obtain a mixed solution; filtering the mixed solution to obtain a mixture, and roasting the mixture at 500-600 ℃ for 1-2 h to obtain a roasted product; mixing the roasted product with water, performing ultrasonic treatment, standing, discharging supernatant, and repeating the steps until the roasted product is washed to be neutral; dehydrating the washed neutral roasted product to obtain a spherical graphite filter cake, uniformly mixing the spherical graphite filter cake with acid liquor under the vacuum degree of-0.05 to-0.10 Mpa, and stirring for 1-2 h at the temperature of 30-50 ℃ under the pressure condition of 0.03-0.08 Mpa to obtain acid-leached spherical graphite; mixing the acid-leached spherical graphite with water at 50-80 ℃, standing after ultrasonic treatment, discharging supernatant, and repeating the steps until the spherical graphite is washed to be neutral to obtain the purified spherical graphite. The alkaline-acid purification method for natural spherical graphite can improve reaction efficiency and purify spherical graphite with the fixed carbon content of 93-98% to more than 99.95% under the condition of reducing the using amount of alkali and acid, and effectively reduces the extraction cost.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
Fig. 1 is a schematic flow chart of a method for purifying natural spherical graphite by an alkaline-acid method according to an embodiment of the present disclosure.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. Thus, the following detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The characteristics and properties of the method for purifying natural spherical graphite by the alkaline-acid method of the present application will be described in further detail with reference to examples.
Example 1
The embodiment of the application provides a method for purifying natural spherical graphite by an alkaline-acid method, which comprises the following steps:
step one, preparing a 30% sodium hydroxide solution from 12g of sodium hydroxide and 28mL of water, and placing the solution into a sample injection bottle for later use;
secondly, pressurizing and alkaline leaching by taking the northeast China spherical graphite with the fixed carbon content of 95.45 percent as a raw material; weighing 10g of Asclepias spherical graphite, putting the 10g of Asclepias spherical graphite into a reaction kettle, vacuumizing the reaction kettle, maintaining the vacuum degree of-0.05 MPa for 20min, pumping the sodium hydroxide solution in the sampling bottle into the reaction kettle by utilizing negative pressure, uniformly stirring, closing a valve of the sampling bottle, applying pressure to the inside of the reaction kettle, wherein the pressure is 0.05MPa, heating the reaction kettle by using a water bath, and uniformly stirring the solution in the reaction kettle for 30min at the water bath temperature of 30 ℃ to obtain a mixed solution.
And step three, carrying out suction filtration on the mixed solution obtained in the step two, carrying out suction filtration on the mixed solution to a non-flowing state, and then transferring the mixed solution into a reaction container to obtain a mixture, wherein 10mL of 30% sodium hydroxide solution is obtained and can be used for subsequent purification.
Step four, roasting the mixture obtained in the step three through suction filtration for 1 hour at the temperature of 500 ℃, and washing the roasted spherical graphite out of a roasting container by using boiling water; mixing hot water with the roasted spherical graphite at 60 ℃ for ultrasonic treatment with the ultrasonic frequency of 30kHz and the ultrasonic time of 4min, standing, discharging supernatant, and repeating the steps until the roasted spherical graphite is washed to be neutral.
Step five, carrying out suction filtration and dehydration on the spherical graphite washed to be neutral in the step four to obtain a spherical graphite filter cake, adding the spherical graphite filter cake into a reaction kettle, opening a vacuum pump to carry out vacuum pumping, keeping the vacuum degree at-0.05 Mpa for 20min, then closing a valve of the vacuum pump, opening a valve of a sample feeding bottle, and enabling hydrochloric acid with the volume fraction of 15% and placed in the sample feeding bottle in advance to flow into the reaction kettle as acid liquor through pressure difference, wherein the liquid-solid ratio of the hydrochloric acid to the spherical graphite filter cake is 1.2: closing a valve of a sample injection bottle, uniformly mixing and stirring acid liquor and graphite, opening a valve of a vacuum pump for pressurizing, wherein the pressure is 0.05MPa, uniformly stirring for 2 hours in a water bath at 40 ℃ to obtain spherical graphite after acid leaching, mixing 60 ℃ hot water with the spherical graphite after acid leaching for ultrasonic treatment, wherein the ultrasonic frequency is 30kHz, the ultrasonic time is 3min, standing to discharge supernatant, repeating the steps until the spherical graphite after acid leaching is washed to be neutral, and then performing suction filtration and drying to finally obtain 8.4g of high-grade spherical graphite with the fixed carbon content of 99.96%.
Example 2
The embodiment of the application provides an alkaline-acid method for purifying natural spherical graphite, which comprises the following steps:
step one, preparing sodium hydroxide solution with the mass fraction of 50% by taking 20g of sodium hydroxide and 20mL of water, and putting the sodium hydroxide solution into a sample injection bottle for later use;
step two, performing pressurized alkaline leaching by taking Jilin spherical graphite with the fixed carbon content of 96.45 percent as a raw material; weighing 10g of northwest spherical graphite, putting the northwest spherical graphite into a reaction kettle, vacuumizing the reaction kettle, maintaining the vacuum degree at-0.08 MPa for 30min, pumping the sodium hydroxide solution in the sample injection bottle into the reaction kettle by utilizing negative pressure, uniformly stirring, closing a valve of the sample injection bottle, applying pressure to the interior of the reaction kettle, wherein the pressure is 0.08MPa, heating the reaction kettle by using a water bath, and uniformly stirring the solution in the reaction kettle for 30min at the water bath temperature of 40 ℃ to obtain a mixed solution.
And step three, carrying out suction filtration on the mixed solution obtained in the step two, carrying out suction filtration on the mixed solution to a non-flowing state, and then transferring the mixed solution into a reaction container to obtain a mixture, and simultaneously obtaining 12mL of sodium hydroxide solution with the mass fraction of 35% for subsequent purification.
Step four, roasting the mixture obtained in the step three through suction filtration for 2 hours at the temperature of 550 ℃, and washing the roasted spherical graphite out of a roasting container by using boiling water; mixing hot water at 80 ℃ with the roasted spherical graphite, performing ultrasonic treatment at the ultrasonic frequency of 40kHz for 5min, standing, discharging supernatant, and repeating the steps until the roasted spherical graphite is washed to be neutral.
Step five, carrying out suction filtration and dehydration on the spherical graphite washed to be neutral in the step four to obtain a spherical graphite filter cake, adding the spherical graphite filter cake into a reaction kettle, opening a vacuum pump to carry out vacuum pumping, keeping the vacuum degree at-0.07 Mpa for 30min, then closing a valve of the vacuum pump, opening a valve of a sample feeding bottle, and enabling hydrochloric acid with the volume fraction of 15% and placed in the sample feeding bottle in advance to flow into the reaction kettle as acid liquor through pressure difference, wherein the liquid-solid ratio of the hydrochloric acid to the spherical graphite filter cake is 1.5: closing a valve of a sample injection bottle, uniformly mixing and stirring acid liquor and graphite, opening a valve of a vacuum pump for pressurization, wherein the pressure is 0.07MPa, uniformly stirring for 2 hours in a water bath at 40 ℃ to obtain spherical graphite after acid leaching, mixing hot water at 80 ℃ with the spherical graphite after acid leaching for ultrasonic treatment, wherein the ultrasonic frequency is 40kHz, the ultrasonic time is 5 minutes, standing to discharge supernatant, repeating the steps until the spherical graphite after acid leaching is washed to be neutral, and then performing suction filtration and drying to obtain 8.6g of spherical graphite with the fixed carbon content of 99.9 percent.
And step six, mixing the obtained 8.6g of spherical graphite with the obtained 12mL of sodium hydroxide solution with the mass fraction of 35%, and repeating the step two to the step five to finally obtain the product with the fixed carbon content of 99.95%.
Example 3
The embodiment of the application provides an alkaline-acid method for purifying natural spherical graphite, which comprises the following steps:
step one, preparing a sodium hydroxide solution with the mass fraction of 40% by taking 16g of sodium hydroxide and 24mL of water, and putting the sodium hydroxide solution into a sample injection bottle for later use;
secondly, pressurizing and alkaline leaching by taking the alligator spherical graphite with the fixed carbon content of 95.56 percent as a raw material; weighing 10g of northwest spherical graphite, putting the northwest spherical graphite into a reaction kettle, vacuumizing the reaction kettle, maintaining the vacuum degree at-0.08 MPa for 30min, pumping the sodium hydroxide solution in the sample injection bottle into the reaction kettle by utilizing negative pressure, uniformly stirring, closing a valve of the sample injection bottle, applying pressure to the interior of the reaction kettle, wherein the pressure is 0.08MPa, heating the reaction kettle by using a water bath, and uniformly stirring the solution in the reaction kettle for 30min at the water bath temperature of 35 ℃ to obtain a mixed solution.
And step three, carrying out suction filtration on the mixed solution obtained in the step two, carrying out suction filtration on the mixed solution to a non-flowing state, and then transferring the mixed solution into a reaction container to obtain a mixture, wherein 10mL of 35% sodium hydroxide solution is obtained and can be used for subsequent purification.
Step four, roasting the mixture obtained in the step three through suction filtration for 1.5 hours at the temperature of 550 ℃, and washing the roasted spherical graphite out of a roasting container by using boiling water; mixing hot water at 70 ℃ with the roasted spherical graphite, performing ultrasonic treatment at the ultrasonic frequency of 30kHz for 5min, standing, discharging supernatant, and repeating the steps until the roasted spherical graphite is washed to be neutral.
Step five, carrying out suction filtration and dehydration on the spherical graphite washed to be neutral in the step four to obtain a spherical graphite filter cake, adding the spherical graphite filter cake into a reaction kettle, opening a vacuum pump to carry out vacuum pumping, keeping the vacuum degree at-0.07 Mpa for 30min, then closing a valve of the vacuum pump, opening a valve of a sample feeding bottle, and enabling hydrochloric acid with the volume fraction of 20% and placed in the sample feeding bottle in advance to flow into the reaction kettle as acid liquor through pressure difference, wherein the liquid-solid ratio of the hydrochloric acid to the spherical graphite filter cake is 1.3: closing a valve of a sample injection bottle, uniformly mixing and stirring acid liquor and graphite, opening a valve of a vacuum pump for pressurization, wherein the pressure is 0.07MPa, uniformly stirring for 2 hours in a water bath at 40 ℃ to obtain spherical graphite after acid leaching, mixing hot water at 80 ℃ with the spherical graphite after acid leaching for ultrasonic treatment, wherein the ultrasonic frequency is 40kHz, the ultrasonic time is 5 minutes, standing to discharge supernatant, repeating the steps until the spherical graphite after acid leaching is washed to be neutral, and then performing suction filtration and drying to finally obtain 8.4g of high-grade spherical graphite with the fixed carbon content of 99.95 percent.
As shown in fig. 1, in the method for purifying natural spherical graphite by an alkaline-acid method provided in this embodiment of the present application, a sodium hydroxide solution and spherical graphite are uniformly mixed and reacted under negative pressure, then a pressurization manner is used for reaction at a predetermined temperature, then a mixed solution of graphite and alkaline solution is subjected to suction filtration to obtain an alkaline solution for recycling and a mixture, the mixture is calcined and then uniformly mixed and reacted with an acid solution under negative pressure, then a pressurization manner is used for reaction at a predetermined temperature, and finally, suction filtration and drying are performed to obtain high-grade spherical graphite, so that the alkaline solution and the acid solution can be favorably introduced into the interlayer of the spherical graphite by using the alternating action of negative pressure and pressurization, the reaction efficiency is improved, the usage amount of the alkaline solution and the acid solution can be effectively reduced, the purification cost is reduced, the spherical graphite with a fixed carbon content of 93-98% is purified to more than 99.95%, and ultrasonic-assisted water washing is used in the water washing process after alkali fusion and acid leaching, and the usage amount of washing water can be effectively reduced.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Claims (9)
1. An alkaline-acid method for purifying natural spherical graphite is characterized by comprising the following steps:
uniformly mixing a spherical graphite raw material with a sodium hydroxide solution with the mass fraction of 30-50% under the vacuum degree of-0.05-0.10 MPa, and then stirring for 0.5-1 h at the temperature of 30-40 ℃ under the pressure condition of 0.03-0.08 MPa to obtain a mixed solution;
filtering the mixed solution to obtain a mixture, and roasting the mixture at 500-600 ℃ for 1-2 h to obtain a roasted product;
mixing the roasted product with water, performing ultrasonic treatment, standing, discharging supernatant, and repeating the steps until the roasted product is washed to be neutral;
dehydrating the washed neutral roasted product to obtain a spherical graphite filter cake, uniformly mixing the spherical graphite filter cake with acid liquor under the vacuum degree of-0.05 to-0.10 Mpa, and stirring for 1 to 2 hours at the temperature of between 30 and 50 ℃ under the pressure condition of between 0.03 and 0.08Mpa to obtain acid-leached spherical graphite;
mixing the spherical graphite after acid leaching with water at 50-80 ℃, standing, discharging supernatant, and repeating the steps until the spherical graphite is washed to be neutral to obtain the purified spherical graphite.
2. The method for purifying natural spherical graphite according to claim 1, wherein the sodium hydroxide solution and the raw material for spherical graphite are mixed at a mass ratio of 1.6 to 2:1.
3. the method of purifying natural spheroidal graphite according to claim 1, wherein the raw material of spheroidal graphite is maintained in a vacuum degree of-0.05 to-0.10 MPa for 20 to 30min before the raw material of spheroidal graphite and the sodium hydroxide solution are uniformly mixed.
4. The method for purifying natural spherical graphite according to claim 1, wherein the ultrasonic treatment is performed at a frequency of 20 to 40kHz for 3 to 5min.
5. The alkaline-acid purification method of natural spherical graphite according to claim 1, wherein the acid solution is hydrochloric acid, nitric acid or a mixture of hydrochloric acid and nitric acid, and the volume fraction of the acid solution is 15-20%.
6. The method for purifying natural spherical graphite according to claim 1, wherein the spherical graphite cake is maintained at a vacuum degree of-0.05 to-0.10 MPa for 20 to 30min before the spherical graphite cake and the acid solution are uniformly mixed.
7. The alkaline-acid purification method of natural spherical graphite according to claim 1, wherein the mass ratio of the acid solution to the spherical graphite filter cake when mixed is 1 to 1.5:1.
8. the method for purifying natural spherical graphite by an alkaline-acid method according to claim 1, wherein the calcined product is washed out of the calcining container with boiling water, mixed with water of 50 to 80 ℃ and subjected to ultrasonic treatment, and then left to stand.
9. The method of claim 1, wherein the raw material of the natural spherical graphite has a fixed carbon content of 93 to 98%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116692850A (en) * | 2023-07-26 | 2023-09-05 | 牡丹江奥丰新材料科技有限责任公司 | Green purification method of natural graphite |
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