CN114345480A - Wet grinding method for preparing graphite cathode material - Google Patents
Wet grinding method for preparing graphite cathode material Download PDFInfo
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- CN114345480A CN114345480A CN202111477868.7A CN202111477868A CN114345480A CN 114345480 A CN114345480 A CN 114345480A CN 202111477868 A CN202111477868 A CN 202111477868A CN 114345480 A CN114345480 A CN 114345480A
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Abstract
The invention relates to a wet grinding method for preparing a graphite cathode material, belonging to the technical field of wet grinding methods for preparing graphite cathode materials; the technical problem to be solved is as follows: an improvement of a wet grinding method for preparing a graphite cathode material is provided; the technical scheme for solving the technical problems is as follows: weighing coke powder with a certain mass of 13-20 mu m as a wet grinding raw material; measuring deionized water to enable the solid-liquid ratio of materials to a solvent in a mixed system to be 1: 1-1: 5; measuring 1-5 per mill of dispersant; weighing zirconium beads with a certain mass of 0.5-3mm as a wet grinding medium; after the sand mill is installed, sequentially pouring coke powder and water into the charging barrel; then, starting a sand mill, and pre-stirring at a low speed to fully mix the carbon powder and the deionized water; then the operation is carried out at the rotating speed of 1000-; sampling slurry every 2 hours, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down; the invention is applied to grinding of graphite cathode materials.
Description
Technical Field
The invention discloses a wet grinding method for preparing a graphite cathode material, and belongs to the technical field of wet grinding methods for preparing graphite cathode materials.
Background
With the development of new energy industry, graphite cathode material production lines such as bamboo shoots in spring after rain are rapidly developed all over the country. At present, various units adopt a dry crushing mode to process raw materials of a negative electrode material, such as needle coke, petroleum coke, pitch coke, coal coke and the like, so as to obtain coke powder with a proper particle size. The crushed materials are further subjected to ash removal treatment by chemical purification through reagents such as hydrofluoric acid with certain concentration. From the process end, in the treatment process of drying-crushing-chemical purification, materials undergo a redundant drying process.
When the existing dry crushing process and the purification and ash removal process are combined, a redundant drying process exists. In addition, the common fine pulverization treatment process of the cathode material usually comprises three procedures of dry grinding, shaping and grading. They have the following drawbacks:
(1) the dry pulverization method is classified into a mechanical pulverization method and an air current pulverization method, and means that materials are pulverized by shearing force, impact force and friction force, and powder smaller than 10 micrometers can be prepared by adopting air current pulverization. However, dry grinding has disadvantages of low grinding efficiency, poor dispersion of the powder material, and large ultimate grinding particle size.
(2) The shaping process is usually to passivate the sharp corners of the powder particles under the action of external forces to improve the filling characteristics of the powder. The dry powder is easy to agglomerate to form loose agglomerates due to the actions of electrostatic attraction, van der waals force, adhesion and the like among the ultrafine powder, so that the action and the shaping action force on the particles are offset, and the general effect of dry shaping is poor.
(3) Under the current conditions, the fineness and the particle size distribution of the classified product are not ideal enough, and the high-standard requirement of users is difficult to meet.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to solve the technical problems that: an improvement in a wet milling process for the preparation of graphite anode materials is provided.
In order to solve the technical problems, the invention adopts the technical scheme that: a wet grinding method for preparing a graphite anode material comprises the following steps:
(1) raw materials: weighing coke powder with a certain mass of 13-20 mu m as a wet grinding raw material, wherein the granularity of the raw material is shown in the table;
(2) solvent: measuring deionized water to ensure that the solid-liquid ratio of materials to a solvent in a mixed system is 1: 1-1: 5;
(3) dispersing agent: measuring 1-5 per mill of dispersant;
(4) grinding medium: zirconium beads with the particle size of 0.5-3mm are used as a wet grinding medium, and the addition amount of the zirconium beads with different particle sizes is shown in the following table;
(5) installing a sand mill: fastening a stainless steel material cylinder at the center of the instrument, inserting a polyurethane sand grinding disc into the material cylinder, and adjusting the height of the sand grinding disc to enable the bottom of the sand grinding disc to be 0.5mm away from the bottom of the material cylinder;
pouring zirconium beads with a certain volume to submerge the lower edge of the dispersion disc and expose the upper edge of the dispersion disc;
(6) and (3) wet grinding: after the height of the sand grinding disc and the volume of the zirconium beads are adjusted, coke powder and water are poured into the charging barrel in sequence; then, starting a sand mill, and pre-stirring at a low speed to fully mix the carbon powder and the deionized water; then the operation is carried out at the rotating speed of 1000-;
(7) sampling and detecting: sampling slurry every 2 hours, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down;
(8) and (3) post-treatment: sieving and separating the slurry and the zirconium beads, sealing the slurry in a sample bag, and then drying; and cleaning and drying the zirconium beads, the stainless steel material cylinder and the screen mesh for later use.
The coke powder adopted in the step (1) can be replaced by needle coke or petroleum coke or asphalt coke or natural graphite containing less than 10% of moisture.
The dispersant in the step (3) is sodium tripolyphosphate.
The depth of the zirconium beads poured into the dispersion disc in the step (5) is 35-40 mm.
The low-speed pre-stirring speed range is 300-500 r/min.
And the sand mill adopted in the fifth step can be replaced by a ball mill.
The coke powder with a certain mass in the step (1) is specifically 100-200g of coke powder.
Compared with the prior art, the invention has the beneficial effects that: compared with the prior art, the wet grinding method for preparing the graphite cathode material has the advantages that the coke powder with high raw material humidity can be directly used for grinding, the drying procedure is omitted, and the waste of personnel and time caused by drying can be greatly reduced.
Drawings
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is an SEM photograph of example 1 of the present invention;
FIG. 2 is an SEM photograph of example 2 of the present invention.
Detailed Description
As shown in fig. 1 and 2, the main solution of the present invention is: (1) in the preparation process of fine coke powder (not limited to coke powder, and can cover other anode material powder), the dispersion effect of the particle bodies is a crucial key factor. Therefore, the problem of dispersion of the coke powder is an important prerequisite for ensuring the granularity index of the coke powder.
Because the volume and the mass of the fine coke powder are small, the acting force of the gravity field is weak, and in addition, the surface energy of the fine coke powder is large and easy to agglomerate, the preparation of the dry powder is complicated and difficult. In water, the coke powder is easily dispersed by physical dispersion means such as mechanical dispersion, ultrasonic dispersion, electromagnetic dispersion, and impact flow dispersion, and also easily dispersed chemically by the action of various dispersants such as inorganic electrolytes (LPL, SS, NaOH, and the like), organic polymers (natural polymers such as polyacrylamide series, polyethylene oxide series, tannin, lignin, and the like), and surfactants. By strengthening dispersion, the coke powder particle system is ensured to realize efficient crushing-shaping-grading operation.
(2) Redundant drying processes are reduced, and time cost, labor cost and the like are reduced.
The invention provides a wet grinding method for preparing a graphite cathode material, aiming at solving the problem of dispersion of coke powder and reducing redundant drying procedures, and the method comprises the following steps:
(1) raw materials: weighing coke powder with a certain mass of 13-20 micrometers as a wet grinding raw material, wherein the particle size of the raw material coke powder is shown in table 2;
(2) solvent (dispersion medium): measuring deionized water or other solvents, and ensuring that the solid-to-liquid ratio of materials to the solvents in a mixed system is 1: 1 to 1: 5;
(3) dispersing agent: measuring 1-5 per mill of dispersant;
(4) grinding medium: weighing zirconium beads with a certain mass of 0.5-3mm as a wet grinding medium, wherein the addition amount of the zirconium beads with different particle sizes is shown in table 1;
TABLE 1 addition amount of zirconium beads of different particle diameters
(5) Installing a sand mill: the stainless steel charging barrel is fastened at the center of the instrument, the polyurethane sanding disc extends into the charging barrel, and the height of the sanding disc is adjusted to enable the bottom of the sanding disc to be 0.5mm away from the bottom of the charging barrel. Pouring zirconium beads with a certain volume to submerge the lower edge of the dispersion disc and expose the upper edge of the dispersion disc, wherein the dispersion disc can fully rotate to drive the zirconium beads and the raw material powder (the depth of the zirconium beads is about 35-40 mm);
(6) and (3) wet grinding: after the height of the sand grinding disc and the volume of the zirconium beads are adjusted, coke powder and water are poured into the charging barrel in sequence. Then, starting a sand mill, and pre-stirring at a low speed to fully mix the carbon powder and the deionized water; then the operation is carried out at the rotating speed of 1000-;
(7) sampling and detecting: every 2 hours, sampling, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down;
(8) and (3) post-treatment: sieving and separating the slurry and the zirconium beads, sealing the slurry in a sample bag, and then drying; and cleaning and drying the zirconium beads, the stainless steel material cylinder and the screen mesh for later use.
The wet grinding equipment can be replaced by a ball mill; the wet grinding raw material is not limited to coal-based coke powder, and needle coke, petroleum coke, pitch coke, natural graphite and the like containing certain moisture can be used instead.
The present invention is further illustrated below with reference to specific examples and comparative examples.
Example 1
(1) Raw materials: weighing 100g of coal-based coke powder with large particle size as a wet grinding raw material;
(2) solvent: measuring 300mL of deionized water;
(3) dispersing agent: measuring 1.5mL of sodium tripolyphosphate;
(4) grinding medium: weighing about 420g of 3mm zirconium beads;
(5) installing a sand mill: the stainless steel material cylinder is fastened in the center of the instrument, the polyurethane abrasive disc is inserted into the material cylinder, and the height of the abrasive disc is adjusted to make the bottom of the abrasive disc be 0.5mm away from the bottom of the material cylinder. Pouring zirconium beads with a certain volume to submerge the lower edge of the dispersion disc and expose the upper edge of the dispersion disc, wherein the dispersion disc can fully rotate to drive the zirconium beads and the raw material powder (the depth of the zirconium beads is about 35-40 mm);
(6) and (3) wet grinding: after the height of the sand mill and the volume of the zirconium beads are adjusted, the weighed coke powder, water, dispersing agent and grinding medium are poured into the charging barrel in sequence. Then, starting a sand mill, pre-stirring at a low speed to fully mix carbon powder and deionized water, and performing wet grinding at a rotating speed of 3000r/min after the operation is stable;
(7) sampling and detecting: every 2 hours, sampling, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down;
(8) and (3) post-treatment: sieving and separating the slurry and the zirconium beads, sealing the slurry in a sample bag, and then drying; and cleaning and drying the zirconium beads, the stainless steel material cylinder and the screen mesh for later use.
Example 2
(1) Raw materials: weighing 100g of coal-based coke powder with large particle size as a wet grinding raw material;
(2) solvent: measuring 300mL of deionized water;
(3) grinding medium: weighing about 522g of 1mm zirconium beads;
(4) installing a sand mill: the stainless steel material cylinder is fastened in the center of the instrument, the polyurethane abrasive disc is inserted into the material cylinder, and the height of the abrasive disc is adjusted to make the bottom of the abrasive disc be 0.5mm away from the bottom of the material cylinder. Pouring zirconium beads with a certain volume to submerge the lower edge of the dispersion disc and expose the upper edge of the dispersion disc, wherein the dispersion disc can fully rotate to drive the zirconium beads and the raw material powder (the depth of the zirconium beads is about 35-40 mm);
(5) and (3) wet grinding: after the height of the sand mill and the volume of the zirconium beads are adjusted, the weighed coke powder, water, dispersing agent and grinding medium are poured into the charging barrel in sequence. Then, starting a sand mill, pre-stirring at a low speed to fully mix carbon powder and deionized water, and performing wet grinding at a rotating speed of 3000r/min after the operation is stable;
(6) sampling and detecting: every 2 hours, sampling, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down;
(7) and (3) post-treatment: sieving and separating the slurry and the zirconium beads, sealing the slurry in a sample bag, and then drying; and cleaning and drying the zirconium beads, the stainless steel material cylinder and the screen mesh for later use.
Comparative example 1
The present comparative example provides a wet milling technique for the preparation of a graphite anode material, which is different from that of example 1 in that the present comparative example does not have step (3), i.e., 5 ‰ of dispersant is not added.
Comparative example 2
The comparison example provides a wet grinding technology for preparing a graphite cathode material, and compared with the method in example 1, the comparison example adopts 100g of small-particle-size coal-based coke powder as a raw material.
Comparative example 3
The present comparative example provides a wet grinding technique for the preparation of a graphite negative electrode material, which is different from that of example 1 in that the present comparative example uses 100g of coal-based coke powder having a small particle size as a raw material and does not have step (3), i.e., does not add 5 ‰ of a dispersant.
Comparative example 4
This comparative example provides a wet milling technique for the preparation of graphite anode material, which differs from example 2 in that about 570g of 0.5mm zirconium beads were used as the wet milling media.
Comparative example 5
The present comparative example provides a wet milling technique for the preparation of graphite anode material, which differs from example 2 in that about 420g of 3mm zirconium beads were used as the wet milling media.
The indexes of the particle size of the wet-milled materials according to the above examples 1 and comparative examples 1 to 3 and examples 2 and comparative examples 4 to 5 are shown in the following table 2:
TABLE 2 index of particle size of wet-milled material in examples and comparative examples
In the above table: the ball-material ratio refers to the mass ratio of the grinding medium to the material; the K value is a parameter for measuring the particle size distribution concentration, and the calculation formula is
(ii) a Wherein D is10The particle size value is the corresponding particle size value when the cumulative distribution percentage from small to large in the particle size distribution reaches 10 percent; d50And D90、D97Respectively corresponding particle size values when the cumulative distribution percentage from small to large in the particle size distribution reaches 50 percent, 90 percent and 97 percent respectively; the grinding effect is to grind the material D after 8 hours90Value of (D) and before grinding90The ratio of the values of (a) to (b) is used to indicate the change in the particle size of the wet-milled material. Analysis of the data from table 2 leads to the following conclusions:
(1) from the particle size indexes of example 1 and comparative example 1, and comparative example 2 and comparative example 3, the particle size of the test coke powder without the dispersant is smaller under the same grinding time. But the particle size distribution of the test coke powder added with the dispersing agent is more concentrated (the K value is closer to 1);
(2) from the particle size indexes of example 1 and comparative example 2 and comparative example 1 and comparative example 3, the grinding effect of the coal-based coke powder is related to the matching of the particle size of the raw coke powder and the particle size of the grinding medium.
(3) From the particle size indexes of example 2, comparative example 4 and comparative example 5, the grinding effect of the coke powder is better than that of the grinding system added with the grinding medium of 0.5mm and the grinding medium of 1mm after 8 hours.
The test object of the invention is mainly to test the particle size of the coke powder raw material, the particle size (ball-to-material ratio) of the grinding medium to the coke powder raw material and the influence of the additive on the wet grinding effect. The granularity of the raw materials (large and small particles) is set to be the granularity index which can be achieved by the materials after actual production and coarse breaking, and the granularity of the grinding media is set to ensure that the test effect has stronger persuasion, so the grinding media with more particle sizes are selected for testing. Grinding media of a certain particle size generally have a better crushing effect.
It should be noted that, regarding the specific structure of the present invention, the connection relationship between the modules adopted in the present invention is determined and can be realized, except for the specific description in the embodiment, the specific connection relationship can bring the corresponding technical effect, and the technical problem proposed by the present invention is solved on the premise of not depending on the execution of the corresponding software program.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A wet grinding method for preparing a graphite cathode material is characterized by comprising the following steps: the method comprises the following steps:
(1) raw materials: weighing coke powder with a certain mass of 13-20 mu m as a wet grinding raw material, wherein the granularity of the raw material is shown in the table;
(2) solvent: measuring deionized water to ensure that the solid-liquid ratio of materials to a solvent in a mixed system is 1: 1-1: 5;
(3) dispersing agent: measuring 1-5 per mill of dispersant;
(4) grinding medium: zirconium beads with the particle size of 0.5-3mm are used as a wet grinding medium, and the addition amount of the zirconium beads with different particle sizes is shown in the following table;
(5) installing a sand mill: fastening a stainless steel material cylinder at the center of the instrument, inserting a polyurethane sand grinding disc into the material cylinder, and adjusting the height of the sand grinding disc to enable the bottom of the sand grinding disc to be 0.5mm away from the bottom of the material cylinder;
pouring zirconium beads with a certain volume to submerge the lower edge of the dispersion disc and expose the upper edge of the dispersion disc;
(6) and (3) wet grinding: after the height of the sand grinding disc and the volume of the zirconium beads are adjusted, coke powder and water are poured into the charging barrel in sequence; then, starting a sand mill, and pre-stirring at a low speed to fully mix the carbon powder and the deionized water; then the operation is carried out at the rotating speed of 1000-;
(7) sampling and detecting: sampling slurry every 2 hours, and then carrying out laser granularity test; after grinding for 8 hours, the instrument was shut down;
(8) and (3) post-treatment: sieving and separating the slurry and the zirconium beads, sealing the slurry in a sample bag, and then drying; and cleaning and drying the zirconium beads, the stainless steel material cylinder and the screen mesh for later use.
2. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: the coke powder adopted in the step (1) can be replaced by needle coke or petroleum coke or asphalt coke or natural graphite containing less than 10% of moisture.
3. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: the dispersant in the step (3) is sodium tripolyphosphate.
4. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: the depth of the zirconium beads poured into the dispersion disc in the step (5) is 35-40 mm.
5. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: the low-speed pre-stirring speed range is 300-500 r/min.
6. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: and the sand mill adopted in the fifth step can be replaced by a ball mill.
7. The wet grinding method for preparing the graphite anode material according to claim 1, characterized in that: the step (1) adopts a certain mass of coke powder, specifically 100g-200g of coke powder.
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