CN111584865A - Granulation process for high-compaction microcrystalline graphite negative electrode material - Google Patents
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- B01J2/28—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using special binding agents
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention discloses a granulation process for a high-compaction microcrystalline graphite cathode material, which comprises the steps of firstly putting small-particle-size microcrystalline graphite powder and a large-particle-size adhesive into a fusion machine for mixing, then heating the fusion machine to a temperature 2-4 ℃ lower than the softening point of the adhesive, and carrying out fusion granulation for 60-120 min to obtain softened composite particles of the microcrystalline graphite and the adhesive; and then, heating the temperature of the fusion machine to 500-700 ℃, preserving the heat for 1-3 hours, finally cooling the material to room temperature, graphitizing, screening, demagnetizing and packaging to obtain the secondary composite particles for the high-compaction microcrystalline graphite cathode material. The method solves the problems of heavy load, abrasion and easy failure of granulation equipment caused by high content of the high-viscosity agent.
Description
Technical Field
The invention relates to a granulation process of a graphite material for a lithium ion battery, in particular to a granulation process special for a high-compaction microcrystalline graphite negative electrode material.
Background
The microcrystalline graphite has abundant mineral products but low utilization rate and weak related deep processing technology in China, and the microcrystalline graphite is developed into the lithium ion battery cathode material, so that the problem of insufficient microcrystalline graphite deep processing technology can be solved, and the cathode material with excellent rate capability can be obtained by utilizing the advantages of small microcrystalline graphite grains and low OI value.
However, the problem of low pole piece compaction density of the microcrystalline graphite negative electrode material generally exists, the pole piece compaction performance can be improved by increasing the particle size, but the rate performance of the material is also negatively affected, and in order to obtain a high-compaction product on the premise of ensuring excellent rate performance, secondary granulation can be carried out on microcrystalline graphite.
The secondary granulation refers to that single particles with small particle sizes are bonded together through an adhesive to form composite particles with larger particle sizes, and the secondary particles can have the rate capability of small particle products and also have the high compaction performance of large particles.
Patents [ CN201910492402.0 ] and [ CN201910491666.4 ] both report a granulation process of microcrystalline graphite, and it can be found that, because microcrystalline graphite has a porous characteristic, a phenomenon that a binder is easily filled into microcrystalline graphite is easily caused in a composite granulation process, which causes a shortage of the binder content on the surface of microcrystalline graphite, and further causes a poor granulation effect of secondary particles. Therefore, in order to obtain a high-compaction microcrystalline graphite negative electrode material, the prior art solution is to increase the amount of the binder, however, too much binder increases the viscosity of the granulating material, and the high viscosity of the material is very easy to cause high-load operation of granulating equipment and cause failure.
The invention provides a new idea for a granulation process of high-compaction microcrystalline graphite.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a granulation process for a high-compaction microcrystalline graphite negative electrode material.
The invention is realized by the following technical scheme:
a granulation process for a high-compaction microcrystalline graphite negative electrode material comprises the following steps:
s1, mixing: mixing small-particle-size microcrystalline graphite powder and a large-particle-size binder according to a mass ratio of 100: 25-30, putting into a fusion machine, and then starting the fusion machine for mixing;
s2, low softening point granulation: heating the fusion machine to a temperature 2-4 ℃ lower than the softening point of the adhesive, and performing fusion granulation for 60-120 min to obtain softened composite particles with microcrystalline graphite embedded in the adhesive;
s3, preheating: reducing the rotating speed of the fusion machine, raising the temperature of the fusion machine to 500-700 ℃, preserving the heat for 1-3 hours, and then cooling to room temperature to prepare primary particles of microcrystalline graphite and adhesive;
s4, graphitizing the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3, wherein the graphitizing temperature is controlled to be 3000-3400 ℃, and graphitizing composite particles are obtained;
and S5, screening, demagnetizing and packaging the graphitized composite particles to obtain the secondary composite particles for the high-compaction microcrystalline graphite negative electrode material.
Further, in step S1, the small-particle-size microcrystalline graphite powder is microcrystalline graphite powder having a particle size of 3 to 8 μm, and the large-particle-size binder is binder having a particle size of 13 to 20 μm.
Further, in step S1, mixing microcrystalline graphite powder of 3-8 μm and binder of 13-20 μm in a mass ratio of 100: 25-30 of the raw materials are put into a fusion machine, and then the fusion machine is started to mix, wherein the rotating speed of the fusion machine is 500-1500 rpm, and the mixing time is 10-30 min.
Further, in step S2, the softening point of the adhesive is 105 to 110 ℃, the rotation speed of the fusion machine is adjusted to 50 to 200rpm, the temperature of the fusion machine is raised to a temperature 2 to 4 ℃ lower than the softening point of the adhesive, and the fusion and granulation are carried out for 60 to 120min to obtain the softened composite particles with the microcrystalline graphite embedded in the adhesive.
Further, in step S2, the softening point of the adhesive is 105 to 110 ℃, the rotation speed of the fusion machine is adjusted to 50 to 200rpm, the temperature of the fusion machine is raised to a temperature 3 ℃ lower than the softening point of the adhesive, and fusion granulation is performed for 60 to 120min to obtain the softened composite particles with microcrystalline graphite embedded in the adhesive.
Further, in step S2, the binder is high-temperature asphalt, including petroleum asphalt and coal asphalt.
Further, in step S3, the rotating speed of the fusion machine is reduced to 20-30 rpm, the temperature of the fusion machine is raised to 600 ℃, the temperature is kept for 1-3 h, then an electric heating switch of the fusion machine is closed, the fusion machine is cooled to room temperature through external circulating water, a blanking valve is opened, reverse blanking is started, and the primary particles of the microcrystalline graphite and the adhesive are prepared.
Further, in step S4, the graphitization is performed by adding the primary particles formed by compounding the microcrystalline graphite and the adhesive into an acheson furnace at a graphitization temperature of 3000-3400 ℃.
A high-compaction microcrystalline graphite negative electrode material is characterized in that: the high-compaction microcrystalline graphite negative electrode material is prepared according to the granulation process for the high-compaction microcrystalline graphite negative electrode material.
Further, the high-compaction microcrystalline graphite negative electrode material is formed by compounding primary particles of 3-8 mu m, and the granularity of the high-compaction microcrystalline graphite negative electrode material formed by compounding is 14-23 mu m; after the high-compaction microcrystalline graphite negative electrode material is made into a pole piece, the compaction density of the pole piece is more than or equal to 1.60 g/cc.
The invention has the following technical effects:
in the prior art, a secondary granulation process with high adhesive dosage is needed for high-compaction of the microcrystalline graphite cathode material, the load and abrasion of granulation equipment are increased due to the high adhesive content, equipment failure is easily caused, and energy consumption of the equipment is increased. The invention provides two innovative ideas of 'small-granularity microcrystalline graphite is matched with large-granularity adhesive' and 'low-softening-point granulation', and the 'biting' granulation of the small-granularity microcrystalline graphite on the large-granularity adhesive is completed under the condition that the adhesive is not completely melted (the 'biting' granulation refers to a granulation method that the small-granularity microcrystalline graphite is inlaid and adhered on the large-granularity adhesive which is not completely melted). The compacted density of the microcrystalline graphite cathode material prepared by the method is closer to that of soft carbon (less than or equal to 1.3 g/cc), and the microcrystalline graphite cathode product with the compacted density of more than or equal to 1.60g/cc is obtained by a novel granulation technology.
The innovation points of the invention are as follows:
(1) matching small-granularity microcrystalline graphite with a large-granularity adhesive:
in the conventional granulation process, the particle size of primary particles is generally not less than 6 μm, and the particle size of the binder is generally not more than 5 μm, so that the granulation process is that "large-particle-size primary particles are matched with small-particle-size binder", so that the large-particle-size binder is not adopted, and the larger the particle size of the binder is, the more difficult the binder is to be completely melted in a short time, so people often adopt small-particle-size binder. The invention adopts the technology of pricking the adhesive with large particle size by primary particles with small particle size, and the technology is one of the innovative points of the invention.
(2) Low softening point granulation:
the traditional granulating process is completed at the temperature higher than the softening point of the adhesive, has the advantages that the adhesive is in a molten state at the temperature, has certain fluidity and can uniformly bond single particles, and the defects that when the using amount of the adhesive is higher, the viscosity of granulating materials is higher and the load of granulating equipment is heavier.
Aiming at the condition of large consumption of the microcrystalline graphite granulation adhesive, the granulation is carried out at the temperature slightly lower than the softening point of the adhesive, when the temperature of the large-particle-size adhesive is close to the softening point, the surface of the large-particle-size adhesive has certain viscosity, but the inside of the large-particle-size adhesive is still kept in a solid state, and the 'sting' of the small-particle-size microcrystalline graphite on the large-particle-size adhesive can be well realized by the low-softening-point granulation.
(3) The microcrystalline graphite has the advantages of high compaction, high multiplying power and low rebound
The prepared microcrystalline graphite negative pole piece is compacted to be more than or equal to 1.60g/cc, the discharge capacity ratio of 10/1C is more than or equal to 90%, and the full-electricity rebound is less than or equal to 15%.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
S1, mixing: mixing 6 mu m microcrystalline graphite powder and 15 mu m petroleum asphalt with a softening point of 110 ℃ by a fusion machine at a mixing mass ratio of 100:25, a rotation speed of the fusion machine of 500rpm and a mixing time of 10 min.
S2, low softening point granulation: and (3) heating the fusion machine to 107 ℃, adjusting the rotating speed of the fusion machine to 50-200 rpm, and performing fusion granulation for 60min to obtain the softened composite particles with the microcrystalline graphite embedded on the adhesive.
S3, preheating: reducing the rotating speed of the fusion machine to 20rpm, raising the temperature of the fusion machine to 500 ℃, preserving the heat for 3h, then closing an electric heating switch of the fusion machine, cooling to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the preliminary particles of the microcrystalline graphite and the adhesive in a composite mode.
S4, adding the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3 into an Acheson furnace for graphitization treatment at a graphitization temperature of 3200 ℃, and obtaining graphitized composite particles.
And S5, screening, demagnetizing and packaging the graphitized composite particles to obtain a sample No. 1.
Example 2
S1, mixing: mixing 3 μm microlite toner with 13 μm coal tar pitch with softening point of 110 deg.C at a mixing mass ratio of 100:25 at 500rpm for 10 min.
S2, low softening point granulation: and (3) heating the fusion machine to 107 ℃, adjusting the rotating speed of the fusion machine to 100rpm, and performing fusion granulation for 100min to obtain the softened composite particles with the microcrystalline graphite embedded on the adhesive.
S3, preheating: reducing the rotating speed of the fusion machine to 20rpm, raising the temperature of the fusion machine to 500 ℃, preserving the heat for 3h, then closing an electric heating switch of the fusion machine, cooling to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the preliminary particles of the microcrystalline graphite and the adhesive in a composite mode.
S4, adding the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3 into an Acheson furnace for graphitization treatment at 3400 ℃ to obtain graphitized composite particles.
And S5, screening, demagnetizing and packaging the graphitized composite particles to obtain a sample No. 2.
Example 3
S1, mixing: mixing 6 μm microcrystalline graphite powder and 18 μm petroleum asphalt with a softening point of 105 deg.C by a fusion machine at a mixing mass ratio of 100:25 and a rotation speed of 500rpm for 10 min.
S2, low softening point granulation: and (3) heating the fusion machine to the temperature of 102 ℃, adjusting the rotating speed of the fusion machine to 50rpm, and performing fusion granulation for 60min to obtain the softened composite particles with the microcrystalline graphite embedded on the adhesive.
S3, preheating: reducing the rotating speed of the fusion machine to 20rpm, raising the temperature of the fusion machine to 500 ℃, preserving the heat for 3h, then closing an electric heating switch of the fusion machine, cooling to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the preliminary particles of the microcrystalline graphite and the adhesive in a composite mode.
S4, adding the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3 into an Acheson furnace for graphitization treatment at 3400 ℃ to obtain graphitized composite particles.
S5, screening the graphitized composite particles by using a rotary vibration screen, wherein the screen mesh of the rotary vibration screen is two layers, namely 325 meshes and 200 meshes, and the particle size of the screened graphitized composite particles is smaller than 200 meshes; and demagnetizing the screened graphitized composite particles by adopting an electromagnet, and then packaging to obtain a 3# sample.
Example 4
S1, mixing: mixing 8-micron microcrystalline graphite powder and 20-micron petroleum asphalt with a softening point of 105 ℃ by a fusion machine at a mixing mass ratio of 100:27, the rotating speed of the fusion machine is 1000rpm, and the mixing time is 20 min.
S2, low softening point granulation: and (3) heating the fusion machine to the temperature of 102 ℃, adjusting the rotating speed of the fusion machine to 100rpm, and performing fusion granulation for 90min to obtain the softened composite particles with the microcrystalline graphite embedded on the adhesive.
S3, preheating: reducing the rotating speed of the fusion machine to 25rpm, raising the temperature of the fusion machine to 600 ℃, preserving the heat for 2h, then closing an electric heating switch of the fusion machine, cooling the fusion machine to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the preliminary particles of the microcrystalline graphite and the adhesive in a composite mode.
S4, adding the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3 into an Acheson furnace for graphitization treatment at the graphitization temperature of 3000 ℃ to obtain graphitized composite particles.
And S5, screening, demagnetizing and packaging the graphitized composite particles to obtain a sample No. 4.
Example 5
S1, mixing: mixing 5-micron microcrystalline graphite powder and 16-micron petroleum asphalt with a softening point of 105 ℃ by a fusion machine at a mixing mass ratio of 100:30, the rotating speed of the fusion machine is 1500rpm, and the mixing time is 30 min.
S2, low softening point granulation: and (3) heating the fusion machine to the temperature of 102 ℃, adjusting the rotating speed of the fusion machine to 200rpm, and performing fusion granulation for 120min to obtain the softened composite particles with the microcrystalline graphite embedded on the adhesive.
S3, preheating: reducing the rotating speed of the fusion machine to 30rpm, raising the temperature of the fusion machine to 700 ℃, preserving the heat for 1h, then closing an electric heating switch of the fusion machine, cooling to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the preliminary particles of the microcrystalline graphite and the adhesive in a composite mode.
S4, adding the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3 into an Acheson furnace for graphitization treatment at a graphitization temperature of 3200 ℃, and obtaining graphitized composite particles.
And S5, screening, demagnetizing and packaging the graphitized composite particles to obtain a sample No. 5.
Comparative example
Mixing 4-micron microcrystalline graphite powder and 15-micron petroleum asphalt with a softening point of 105 ℃ by a fusion machine at a mixing mass ratio of 100:30, the rotating speed of the fusion machine is 1500rpm, and the mixing time is 30 min.
And (3) putting the uniformly mixed materials into a vertical reaction kettle, adjusting the stirring speed to 80rpm, adjusting the temperature to 500 ℃, stirring and granulating for 2 hours, then discharging into a cooling kettle, cooling to room temperature through circulating water, and discharging to obtain the composite material.
And (4) carrying out grading, graphitization, screening, demagnetization and packaging on the composite material to obtain a comparative sample.
The 1# to 5# samples prepared in the above examples and the comparative samples were tested, and the physicochemical indexes thereof are shown in the following table:
as can be seen from the above table, the microcrystalline graphite cathode material prepared by the method has the granularity of 16-18 microns, the pole piece compaction is more than or equal to 1.60g/cc, the 10/1C discharge capacity ratio is more than or equal to 90%, and the full-electricity rebound is less than or equal to 15%.
If the conventional granulation technology is adopted, the obtained comparative sample has low compounding degree (small granularity), low pole piece compaction, rate capability and full-electric rebound performance of the pole piece which are not as good as those of the microcrystalline graphite negative electrode material prepared by the method.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that various improvements and modifications within the structure and principle of the present invention can be realized by those skilled in the art, and the protection scope of the present invention should be considered.
Claims (10)
1. A granulation process for a high-compaction microcrystalline graphite negative electrode material is characterized by comprising the following steps of:
s1, mixing: mixing small-particle-size microcrystalline graphite powder and a large-particle-size binder according to a mass ratio of 100: 25-30, putting into a fusion machine, and then starting the fusion machine for mixing;
s2, low softening point granulation: heating the fusion machine to a temperature 2-4 ℃ lower than the softening point of the adhesive, and performing fusion granulation for 60-120 min to obtain softened composite particles with microcrystalline graphite embedded in the adhesive;
s3, preheating: reducing the rotating speed of the fusion machine, raising the temperature of the fusion machine to 500-700 ℃, preserving the heat for 1-3 hours, and then cooling to room temperature to prepare primary particles of microcrystalline graphite and adhesive;
s4, graphitizing the primary particles compounded by the microcrystalline graphite and the adhesive prepared in the step S3, wherein the graphitizing temperature is controlled to be 3000-3400 ℃, and graphitizing composite particles are obtained;
and S5, screening, demagnetizing and packaging the graphitized composite particles to obtain the secondary composite particles for the high-compaction microcrystalline graphite negative electrode material.
2. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in step S1, the small-particle microcrystalline graphite powder is microcrystalline graphite powder having a particle size of 3 to 8 μm, and the large-particle binder is binder having a particle size of 13 to 20 μm.
3. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in the step S1, mixing microcrystalline graphite powder of 3-8 μm and adhesive of 13-20 μm according to a mass ratio of 100: 25-30 of the raw materials are put into a fusion machine, and then the fusion machine is started to mix, wherein the rotating speed of the fusion machine is 500-1500 rpm, and the mixing time is 10-30 min.
4. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in step S2, the softening point of the adhesive is 105-110 ℃, the rotating speed of the fusion machine is adjusted to 50-200 rpm, the temperature of the fusion machine is raised to be 2-4 ℃ lower than the softening point of the adhesive, and fusion granulation is carried out for 60-120 min to obtain the softening composite particles with the microcrystalline graphite embedded in the adhesive.
5. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in step S2, the softening point of the adhesive is 105-110 ℃, the rotating speed of the fusion machine is adjusted to 50-200 rpm, the temperature of the fusion machine is raised to be 3 ℃ lower than the softening point of the adhesive, and fusion granulation is carried out for 60-120 min to obtain the softening composite particles with the microcrystalline graphite embedded in the adhesive.
6. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in step S2, the binder is high temperature asphalt, including petroleum asphalt and coal asphalt.
7. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: and step S3, reducing the rotating speed of the fusion machine to 20-30 rpm, raising the temperature of the fusion machine to 600 ℃, preserving the heat for 1-3 hours, then closing an electric heating switch of the fusion machine, cooling to room temperature through external circulating water, opening a blanking valve, and opening reverse blanking to prepare the primary particles compounded by the microcrystalline graphite and the adhesive.
8. The granulation process for the high-compaction microcrystalline graphite anode material as claimed in claim 1, wherein the granulation process comprises the following steps: in the step S4, the graphitization is to add the primary particles compounded by the microcrystalline graphite and the adhesive into an Acheson furnace for graphitization treatment, wherein the graphitization temperature is 3000-3400 ℃.
9. A high-compaction microcrystalline graphite negative electrode material is characterized in that: the high-compaction microcrystalline graphite negative electrode material is prepared by the granulation process for the high-compaction microcrystalline graphite negative electrode material according to any one of claims 1 to 8.
10. The high-compaction microcrystalline graphite anode material of claim 9, wherein: the high-compaction microcrystalline graphite negative electrode material is formed by compounding primary particles of 3-8 mu m, and the granularity of the high-compaction microcrystalline graphite negative electrode material formed by compounding is 14-23 mu m; after the high-compaction microcrystalline graphite negative electrode material is made into a pole piece, the compaction density of the pole piece is more than or equal to 1.60 g/cc.
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| CN112694087A (en) * | 2020-12-23 | 2021-04-23 | 东莞市和鸿升新材料科技有限公司 | Method for preparing low-cost negative electrode material by recycling resistance material |
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| CN1851963A (en) * | 2006-05-19 | 2006-10-25 | 湛江市聚鑫电子材料有限公司 | Lithium-ion cell composite carbon negative polar material and preparing method |
| JP2009158105A (en) * | 2007-12-25 | 2009-07-16 | Tokai Carbon Co Ltd | Method of manufacturing composite carbon material for negative electrode material of lithium ion secondary battery |
| CN103241731A (en) * | 2013-04-01 | 2013-08-14 | 东莞市凯金电池材料有限公司 | Preparation method of compound graphite material for lithium ion secondary battery |
| CN105304870A (en) * | 2015-09-22 | 2016-02-03 | 江西正拓新能源科技有限公司 | Secondary granulation lithium ion battery cathode material and preparation method thereof |
| CN108383116A (en) * | 2018-02-11 | 2018-08-10 | 珠海光宇电池有限公司 | Artificial plumbago negative pole material and preparation method thereof and negative electrode of lithium ion battery |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112694087A (en) * | 2020-12-23 | 2021-04-23 | 东莞市和鸿升新材料科技有限公司 | Method for preparing low-cost negative electrode material by recycling resistance material |
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