Preparation method of low-cost negative electrode material

Abstract

The invention discloses a preparation method of a low-cost negative electrode material. The preparation method comprises the following steps: crushing treatment, purification treatment, graphitization treatment, coating carbonization treatment and demagnetizing screening. The carbon deposit is selected as a raw material, the carbon deposit is used as a fuel, and when the carbon deposit and lubricating oil serially connected into a combustion chamber of an internal combustion engine cannot be completely combusted, generated colloid is low in cost, renewable and in accordance with the concept of sustainable development, moreover, the number of scrapped automobiles and replaced automobiles in 2024 exceeds 65000000, and the carbon deposit is selected for preparing a negative electrode material to promote recycling of resources.

Description

Technical Field

[0001] The present invention relates to the technology of anode materials, and in particular to a preparation method of low-cost anode materials. Background Art

[0002] New energy vehicles refer to vehicles that use unconventional vehicle fuels as power sources or use conventional vehicle fuels and adopt new in-vehicle power devices, integrating advanced technologies in the power control and drive aspects of vehicles, and forming vehicles with advanced technical principles, new technologies, and new structures. Specifically, new energy vehicles include pure electric vehicles, range-extended electric vehicles, hybrid vehicles, fuel cell electric vehicles, hydrogen engine vehicles, etc. Currently, the best-developed new energy vehicles are pure electric vehicles, and the lithium batteries selected for pure electric vehicles are all lithium batteries.

[0003] With the increase in the sales volume of new energy vehicles, the output of lithium batteries has also increased accordingly. Most of the anode materials of lithium batteries are made of natural graphite, and natural graphite is a non-renewable resource. Excessive use will lead to the depletion of graphite resources, which does not conform to the concept of sustainable development. Therefore, it is necessary to propose a new solution to solve the above problems. Summary of the Invention

[0004] In view of this, in view of the deficiencies of the existing technology, the main purpose of the present invention is to provide a preparation method of low-cost anode materials, which can solve the problem that the anode of the existing lithium battery is made of non-renewable natural graphite and does not conform to the concept of sustainable development.

[0005] To achieve the above purpose, the present invention adopts the following technical solutions:

[0006] A preparation method of low-cost anode materials, which includes the following steps:

[0007] (1) Crushing treatment: Continuously dry the carbon deposit at a drying temperature of 150-180 °C for 60 min, and then use a crusher to crush it to obtain material A;

[0008] (2) Purification treatment: Place the material A obtained in step (1) in hydrochloric acid for the first water bath heating, the first water bath temperature is 50 °C, and the first water bath time is 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, place the acid-washed product in a sodium hydroxide solution for the second water bath heating, the second water bath temperature is 50 °C, and the second water bath time is 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, material B is obtained;

[0009] (3) Graphitization treatment: Graphitize the material B obtained in step (2) at a graphitization temperature of 2800-3000 °C, and then disperse it to obtain material C;

[0010] (4) Coating carbonization treatment: Put the material C obtained in step (3) and high-temperature pitch into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:(5 - 7). Stir for 60 min at a stirring speed of 1000 revolutions / min to obtain a coated material. Then put the coated material into a crucible and carbonize it under an inert atmosphere. The carbonization temperature is 1200 - 1300 °C, and the carbonization time is 8 h to obtain material D;

[0011] (5) Demagnetization screening: Demagnetize the material D obtained in step (4) by an electromagnetic demagnetizer with a background intensity of 8000 GS, and then screen it through a 400-mesh sieve to obtain the negative electrode material.

[0012] As a preferred solution, the D50 of the material A in step (1) is 10 - 12 μm.

[0013] As a preferred solution, the mass fraction of hydrochloric acid in step (2) is 15%.

[0014] As a preferred solution, the concentration of the sodium hydroxide solution in step (2) is 0.5 mol / L.

[0015] As a preferred solution, the D50 of the material C in step (3) is 10 - 11 μm.

[0016] As a preferred solution, the carbon deposit in step (1) is a hard carbon deposit.

[0017] Compared with the prior art, the present invention has obvious advantages and beneficial effects. Specifically, as can be seen from the above technical solutions:

[0018] By using carbon deposits as raw materials, when the carbon deposits are used as fuel and the lubricating oil introduced into the internal combustion engine combustion chamber cannot be completely burned, the generated colloid is low-cost and renewable, meeting the concept of sustainable development. Moreover, in 2024, the number of scrapped and replaced vehicles exceeded 6.5 million. Using carbon deposits to prepare negative electrode materials promotes the recycling and utilization of resources.

[0019] To more clearly illustrate the structural features and functions of the present invention, the present invention will be described in detail below with specific embodiments. Detailed implementation mode

[0020] The present invention discloses a preparation method of a low-cost negative electrode material, which includes the following steps:

[0021] (1) Crushing treatment: Continuously dry the carbon deposit at a drying temperature of 150 - 180 °C for 60 min, and then use a crusher to crush it to obtain Material A; the D50 of Material A is 10 - 12 μm. The carbon deposit is a hard carbon deposit, which is obtained by scraping and collecting the carbon deposit on the cylinder with a stainless steel scraper and removing the gel-like substances.

[0022] (2) Purification treatment: Place the Material A obtained in step (1) in hydrochloric acid for the first water bath heating. The first water bath temperature is 50 °C, and the first water bath time is 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, place the acid-washed product in a sodium hydroxide solution for the second water bath heating. The second water bath temperature is 50 °C, and the second water bath time is 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, Material B is obtained; among them, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0023] (3) Graphitization treatment: Graphitize the Material B obtained in step (2) at a graphitization temperature of 2800 - 3000 °C, and then disperse it to obtain Material C; the D50 of Material C is 10 - 11 μm.

[0024] (4) Coating carbonization treatment: Put the Material C obtained in step (3) and high-temperature pitch into a mixer for coating. The mass ratio of Material C to high-temperature pitch is 100:(5 - 7). Stir for 60 min at a stirring speed of 1000 revolutions / min to obtain a coated material. Then, put the coated material into a crucible and carbonize it under an inert atmosphere. The carbonization temperature is 1200 - 1300 °C, and the carbonization time is 8 h to obtain Material D;

[0025] (5) Demagnetization screening: Demagnetize the Material D obtained in step (4) with an electromagnetic demagnetizer with a background intensity of 8000 GS, and screen it through a 400-mesh sieve to obtain the negative electrode material.

[0026] The following is a detailed analysis in combination with multiple embodiments.

[0027] Example 1

[0028] (1) Crushing treatment: Continuously dry the hard carbon deposit at a drying temperature of 150 °C for 60 min, and then use a crusher to crush it to obtain Material A; the D50 of Material A is 11 μm.

[0029] (2) Purification treatment: The material A obtained in step (1) is placed in hydrochloric acid for the first water bath heating. The temperature of the first water bath is 50 °C, and the time of the first water bath is 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, the acid-washed product is placed in a sodium hydroxide solution for the second water bath heating. The temperature of the second water bath is 50 °C, and the time of the second water bath is 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, material B is obtained; wherein, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0030] (3) Graphitization treatment: The material B obtained in step (2) is subjected to graphitization treatment. The graphitization temperature is 2900 °C, and then it is dispersed to obtain material C; the D50 of material C is 10 μm.

[0031] (4) Coating carbonization treatment: The material C obtained in step (3) and high-temperature pitch are put into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:6. The stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, the coated material is put into a crucible and carbonized under an inert atmosphere. The carbonization temperature is 1250 °C, and the carbonization time is 8 h to obtain material D.

[0032] (5) Demagnetization screening: The material D obtained in step (4) is demagnetized by an electromagnetic demagnetizer with a background intensity of 8000 GS and screened by a 400-mesh sieve to obtain the negative electrode material.

[0033] Example 2

[0034] (1) Crushing treatment: The hard carbon deposit is continuously dried at a drying temperature of 180 °C and a drying time of 60 min, and then crushed using a crusher to obtain material A; the D50 of material A is 11 μm.

[0035] (2) Purification treatment: The material A obtained in step (1) is placed in hydrochloric acid for the first water bath heating. The temperature of the first water bath is 50 °C, and the time of the first water bath is 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, the acid-washed product is placed in a sodium hydroxide solution for the second water bath heating. The temperature of the second water bath is 50 °C, and the time of the second water bath is 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, material B is obtained; wherein, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0036] (3) Graphitization treatment: The material B obtained in step (2) is subjected to graphitization treatment. The graphitization temperature is 2800 - 3000 °C, and then it is dispersed to obtain material C; the D50 of material C is 10 μm.

[0037] (4) Coating carbonization treatment: Put the material C obtained in step (3) and high-temperature pitch into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:6. The stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, put the coated material into a crucible and carbonize it under an inert atmosphere. The carbonization temperature is 1250 °C, and the carbonization time is 8 h to obtain material D.

[0038] (5) Demagnetization screening: Demagnetize the material D obtained in step (4) with an electromagnetic demagnetizer with a background intensity of 8000 GS, and screen it through a 400-mesh sieve to obtain the negative electrode material.

[0039] Example 3

[0040] (1) Crushing treatment: Continuously dry the hard coke deposits at a drying temperature of 180 °C and a drying time of 60 min, and then use a crusher to crush it to obtain material A; the D50 of material A is 10 μm.

[0041] (2) Purification treatment: Place the material A obtained in step (1) in hydrochloric acid for the first water bath heating. The first water bath temperature is 50 °C, and the first water bath time is 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, place the acid-washed product in a sodium hydroxide solution for the second water bath heating. The second water bath temperature is 50 °C, and the second water bath time is 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, material B is obtained; among them, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0042] (3) Graphitization treatment: Perform graphitization treatment on the material B obtained in step (2). The graphitization temperature is 2800 - 3000 °C, and then it is dispersed to obtain material C; the D50 of material C is 11 μm.

[0043] (4) Coating carbonization treatment: Put the material C obtained in step (3) and high-temperature pitch into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:6. The stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, put the coated material into a crucible and carbonize it under an inert atmosphere. The carbonization temperature is 1200 °C, and the carbonization time is 8 h to obtain material D.

[0044] (5) Demagnetization screening: Demagnetize the material D obtained in step (4) with an electromagnetic demagnetizer with a background intensity of 8000 GS, and screen it through a 400-mesh sieve to obtain the negative electrode material.

[0045] Example 4

[0046] (1) Crushing treatment: Continuously dry the hard carbon deposits at a drying temperature of 180 °C for 60 min, and then use a crusher to crush them to obtain Material A; the D50 of Material A is 12 μm.

[0047] (2) Purification treatment: Place the Material A obtained in step (1) in hydrochloric acid for the first water bath heating, with the first water bath temperature of 50 °C and the first water bath time of 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, place the acid-washed product in a sodium hydroxide solution for the second water bath heating, with the second water bath temperature of 50 °C and the second water bath time of 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, Material B is obtained; among them, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0048] (3) Graphitization treatment: Subject the Material B obtained in step (2) to graphitization treatment at a graphitization temperature of 2800 °C, and then disperse it to obtain Material C; the D50 of Material C is 10 μm.

[0049] (4) Coating carbonization treatment: Put the Material C obtained in step (3) and high-temperature pitch into a mixer for coating. The mass ratio of Material C to high-temperature pitch is 100:7, the stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, put the coated material into a crucible and carry out carbonization under an inert atmosphere at a carbonization temperature of 1300 °C for 8 h to obtain Material D.

[0050] (5) Demagnetization screening: Demagnetize the Material D obtained in step (4) with an electromagnetic demagnetizer with a background intensity of 8000 GS, and screen it through a 400-mesh sieve to obtain the negative electrode material.

[0051] Example 5

[0052] (1) Crushing treatment: Continuously dry the hard carbon deposits at a drying temperature of 160 °C for 60 min, and then use a crusher to crush them to obtain Material A; the D50 of Material A is 12 μm.

[0053] (2) Purification treatment: Place the Material A obtained in step (1) in hydrochloric acid for the first water bath heating, with the first water bath temperature of 50 °C and the first water bath time of 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, place the acid-washed product in a sodium hydroxide solution for the second water bath heating, with the second water bath temperature of 50 °C and the second water bath time of 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, Material B is obtained; among them, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0054] (3) Graphitization treatment: The material B obtained in step (2) is subjected to graphitization treatment at a graphitization temperature of 3000 °C, and then dispersed to obtain material C; the D50 of material C is 10 μm.

[0055] (4) Coating carbonization treatment: The material C obtained in step (3) and high-temperature pitch are put into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:5, the stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, the coated material is put into a crucible and carbonized under an inert atmosphere at a carbonization temperature of 1200 °C for a carbonization time of 8 h to obtain material D.

[0056] (5) Demagnetization screening: The material D obtained in step (4) is demagnetized by an electromagnetic demagnetizer with a background intensity of 8000 GS and then screened by a 400-mesh sieve to obtain the negative electrode material.

[0057] Example 6

[0058] (1) Crushing treatment: The hard carbon deposits are continuously dried at a drying temperature of 170 °C for a drying time of 60 min, and then crushed using a crusher to obtain material A; the D50 of material A is 12 μm.

[0059] (2) Purification treatment: The material A obtained in step (1) is placed in hydrochloric acid for the first water bath heating at a first water bath temperature of 50 °C for a first water bath time of 10 h. After washing and centrifugation, an acid-washed product is obtained. Then, the acid-washed product is placed in a sodium hydroxide solution for the second water bath heating at a second water bath temperature of 50 °C for a second water bath time of 15 h to obtain an alkali-washed product. After washing and centrifuging the alkali-fused product, material B is obtained; among them, the mass fraction of hydrochloric acid is 15%, and the concentration of the sodium hydroxide solution is 0.5 mol / L.

[0060] (3) Graphitization treatment: The material B obtained in step (2) is subjected to graphitization treatment at a graphitization temperature of 2900 °C, and then dispersed to obtain material C; the D50 of material C is 11 μm.

[0061] (4) Coating carbonization treatment: The material C obtained in step (3) and high-temperature pitch are put into a mixer for coating. The mass ratio of material C to high-temperature pitch is 100:6, the stirring time is 60 min, and the stirring speed is 1000 revolutions / min to obtain a coated material. Then, the coated material is put into a crucible and carbonized under an inert atmosphere at a carbonization temperature of 1200 °C for a carbonization time of 8 h to obtain material D.

[0062] (5) Demagnetization screening: The material D obtained in step (4) is demagnetized by an electromagnetic demagnetizer with a background intensity of 8000 GS and then screened by a 400-mesh sieve to obtain the negative electrode material.

[0063] Performance tests were conducted on the above-mentioned multiple embodiments, and the test results are shown in Table 1.

[0064]

[0065] Table 1

[0066] It can be clearly seen from the above table that the negative electrode material prepared by the preparation method of the present invention has a small particle size and a large specific surface area. Moreover, the negative electrode made of this negative electrode material is applied to a lithium battery, making the first discharge capacity of the battery ≥ 347.32 mAh / g, the first efficiency 92.05%, and the electrical performance excellent, which is more conducive to the popularization and application of lithium batteries.

[0067] The design focus of the present invention is that by using carbon deposit as the raw material, when the carbon deposit, as the fuel, and the lubricating oil introduced into the internal combustion engine combustion chamber cannot be completely burned, the produced colloid is low-cost and renewable, meeting the concept of sustainable development. Moreover, the number of scrapped and replaced automobiles in 2024 exceeded 6.5 million. Using carbon deposit to prepare the negative electrode material promotes the recycling and utilization of resources.

[0068] The above are only the preferred embodiments of the present invention, and do not impose any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and decorations made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a low-cost negative electrode material, characterized in that: The following steps are included: (1) Crushing treatment: The carbon deposits are continuously dried at a drying temperature of 150-180°C for 60 minutes, and then crushed using a crusher to obtain material A; (2) Purification treatment: placing the material A obtained in step (1) in hydrochloric acid for a first water bath heating, the first water bath temperature is 50° C., the first water bath time is 10 h, and then washing and centrifuging to obtain an acid-washed product. Then, placing the acid-washed product in a sodium hydroxide solution for a second water bath heating, the second water bath temperature is 50° C., the second water bath time is 15 h, to obtain an alkali-washed product. The alkali-melted product is washed and centrifuged to obtain material B; (3) Graphitization treatment: The material B obtained in step (2) is graphitized at a temperature of 2800-3000° C., and then broken up to obtain material C; (4) Coating and carbonization treatment: Material C obtained in step (3) and high temperature asphalt are placed in a mixer for coating, the mass ratio of material C to high temperature asphalt is 100:(5-7), the stirring time is 60 min, the stirring speed is 1000 rpm, and the coated material is obtained. The coated material is then placed in a sagger and carbonized under an inert atmosphere at a carbonization temperature of 1200-1300°C and a carbonization time of 8 h to obtain material D; (5) Demagnetization and screening: The material D obtained in step (4) was demagnetized by an electromagnetic iron remover with a background strength of 8000GS, and then sieved by a 400-mesh sieving machine to obtain the negative electrode material.

2. The method for preparing a low-cost negative electrode material according to claim 1, characterized in that: The D50 of material A in step (1) is 10-12 μm.

3. The method for preparing a low-cost negative electrode material according to claim 1, characterized in that: The mass fraction of hydrochloric acid in step (2) is 15%.

4. The method for preparing a low-cost negative electrode material according to claim 1, characterized in that: The concentration of the sodium hydroxide solution in step (2) is 0.5 mol / L.

5. The method for preparing a low-cost negative electrode material according to claim 1, characterized in that: The D50 of material C in step (3) is 10-11 μm.

6. The method for preparing a low-cost negative electrode material according to claim 1, characterized in that: The carbon deposits in step (1) are hard carbon deposits.

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