A method for preparing a catalyst for graphitization of carbon material

By preparing carbon-coated catalysts by mixing rare earth metal solutions with metal compounds, the problems of long time, high temperature, and high energy consumption in the catalytic graphitization process were solved, thereby improving the degree of graphitization and reducing energy consumption, thus enhancing the discharge performance of lithium-ion batteries.

CN117619372BActive Publication Date: 2025-11-28INNER MONGOLIA SHANSHAN TECH CO LTD
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Patent Information

Application Number
CN202311581220.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-24
Publication Date
2025-11-28
Estimated Expiration
2043-11-24

AI Technical Summary

Technical Problem

Existing catalysts suffer from problems such as long graphitization time, low graphitization degree, high graphitization temperature, and high energy consumption during the catalytic graphitization process, resulting in unsatisfactory discharge capacity and efficiency of artificial graphite in lithium-ion battery anode materials.

Method used

After mixing rare earth metal solution with metal compound, the catalyst is dried, granulated and carbonized to form a carbon-coated catalyst. A multi-layered carbon coating layer is generated on the surface of the catalyst, which promotes the graphitization process, increases the degree of graphitization and reduces the temperature.

Benefits of technology

It effectively improves the degree of graphitization, shortens the graphitization time, reduces energy consumption, and improves the discharge capacity and efficiency of graphite anode materials for lithium-ion batteries.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The application discloses a preparation method of a catalyst for graphitization of carbon materials, which comprises the following steps: (1) mixing; (2) drying; (3) granulating; and (4) carbonizing. The preparation method of the catalyst for graphitization of carbon materials has the beneficial effects that a small amount of rare earth metal is added, the rare earth metal is combined with carbon atoms to form graphite-like sheet layer clusters and is combined with edge carbon atoms, the graphitization process is effectively promoted, the graphitization degree is effectively improved, the graphitization time is shortened, the graphitization temperature is lowered, the energy consumption is reduced, the graphitization speed is accelerated, and the graphitization degree is improved. The artificial graphite catalyzed by the catalyst has higher discharge capacity and discharge efficiency when the artificial graphite is applied to a lithium ion battery graphite negative electrode material.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of functional catalytic material preparation, and particularly relates to a preparation method of a catalyst for graphitization of carbon materials. BACKGROUND

[0002] Graphite materials have the advantages of high electronic conductivity, large lithium ion diffusion coefficient, high lithium intercalation capacity and low lithium intercalation potential, and are widely sourced and low in price. Graphite materials are early applied negative electrode materials and are currently mainstream lithium ion battery negative electrode materials. Currently, the negative electrode materials on the market are mainly natural graphite and artificial graphite, and the total penetration rate of natural graphite and artificial graphite is about 90%, of which artificial graphite accounts for the largest proportion of 65%, natural graphite accounts for 25%, and other materials account for 10%.

[0003] With the development of new energy vehicles, market demand is continuously expanding. Natural graphite, as a non-renewable resource, cannot meet the demand for graphite raw materials in the future society, so the use of graphitizable carbon materials to prepare artificial graphite is gradually valued.

[0004] Under the traditional mode, artificial synthesis usually uses petroleum coke, pitch and other raw materials under high temperature (usually as high as 3000 DEG C) to effectively convert amorphous carbon structure into graphite structure. This synthesis method has many limitations and high economic cost, so adding a catalyst for catalytic graphitization has become an effective way and a new research direction in the field of artificial graphite technology.

[0005] The existing catalysts include Fe2O3, SiO2, SnO2 and ZnO. The above catalysts are used for catalytic graphitization in the process of artificial graphite, and have the problems of long graphitization time, low graphitization degree, high graphitization temperature and high energy consumption. The artificial graphite obtained by graphitization cannot achieve ideal discharge capacity and discharge efficiency when applied to lithium ion battery graphite negative electrode materials. SUMMARY

[0006] Therefore, the purpose of the present application is to provide a preparation method of a catalyst for graphitization of carbon materials. The catalyst for graphitization of carbon materials provided by the present application can effectively promote the graphitization process, thereby effectively improving the graphitization degree, shortening the graphitization time, and reducing the graphitization temperature and energy consumption.

[0007] The technical scheme of the present application discloses a preparation method of a catalyst for graphitization of carbon materials, which comprises the following steps:

[0008] (1) mixing: a rare earth metal solution with a concentration of 1%-50% and a metal compound are fully mixed to obtain a mixture, wherein the rare earth metal solution is 1%-25% and the rest is the metal compound, according to 100% by mass;

[0009] (2) drying: drying the mixture in step (1) at a temperature of 100-300℃ for 2-15h to obtain a mixed powder;

[0010] (3) granulation: mixing the mixed powder in step (2) with a precursor in a mass ratio of 1:1-1:3, and adding it into a reaction kettle, controlling the temperature in the reaction kettle to rise to 100-500℃ at a rate of 2-5℃ / min, and keeping it at this temperature for 2-10h, during which it is stirred at a speed of 50r / min-300r / min, and inert gas is continuously introduced into the reaction kettle for protection, and after the heat preservation is completed, it is naturally cooled to room temperature to obtain a mixed granule;

[0011] (4) carbonization: sending the mixed granule in step (3) to a carbonization furnace with a temperature of 600-1050℃ for 1-19h, while continuously introducing nitrogen into the carbonization furnace for protection, and after the heat preservation is completed, it is naturally cooled to room temperature to obtain a carbon-coated catalyst.

[0012] Further, the rare earth metal ions in the rare earth metal solution in step (1) include one or more of lanthanum ions, cerium ions, praseodymium ions, and yttrium ions.

[0013] Further, the solvent in the rare earth metal solution in step (1) consists of 30-50% water, 25%-35% acidic solvent, and 25%-35% organic solvent by mass fraction; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent.

[0014] Further, the acidic solvent is nitric acid solution or hydrochloric acid solution; the organic solvent is ethyl acetate solution or acetone solution.

[0015] Further, the metal compound in step (1) is one or more of silicon oxide, iron oxide, tin oxide, zinc oxide, boron oxide, silicon carbide, iron carbide, tin carbide, zinc carbide, and boron carbide.

[0016] Further, the particle size of the metal compound in step (1) is 5-10μm.

[0017] Further, the mixing and stirring speed in step (1) and step (3) is 50r / min-300r / min, and the mixing and stirring time is 0.5-2h.

[0018] Further, the precursor in step (3) is one or more of CMC, PVC, and resin.

[0019] Further, step (4) also includes: crushing and screening: crushing and screening the carbon-coated catalyst obtained in step (4) to obtain a catalyst finished product with a particle size of 6-15 μm.

[0020] Advantages of the present application:

[0021] 1. The preparation method of the catalyst for graphitization of carbon material provided by the present application effectively promotes the graphitization process, effectively improves the graphitization degree, shortens the graphitization time, and reduces the graphitization temperature and energy consumption by adding a small amount of rare earth metal, which combines with carbon atoms to form graphite-like sheet layer clusters and combines with edge carbon atoms.

[0022] 2. The preparation method of the catalyst for graphitization of carbon material provided by the present application produces a carbon-coated layer with multiple levels and multiple segments around the surface of the catalyst through carbonization, which fully connects rare earth metal ions and metal compounds, accelerates the reaction of activated molecules, atoms, ions, and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the disordered state of graphite crystallites to the ordered state, accelerates the graphitization speed, and improves the graphitization degree.

[0023] 3. The artificial graphite catalyzed by the catalyst of the present application has higher discharge capacity and discharge efficiency when applied to lithium ion battery graphite negative materials. DETAILED DESCRIPTION

[0024] The present application will be further described in detail through examples.

[0025] Example 1: A preparation method of a catalyst for graphitization of carbon material, which includes the following steps:

[0026] (1) Mixing: fully mix a lanthanum nitrate solution with a concentration of 25% and iron oxide with a particle size of 5-10 μm, the mixing and stirring speed is 50-300 r / min, and the mixing and stirring time is 0.5-2 h, to obtain a mixture, wherein the lanthanum nitrate solution is 5% and the rest is iron oxide according to 100% by mass fraction.

[0027] The solvent in the lanthanum nitrate solution is composed of 30-50% water, 25-35% acidic solvent, and 25-35% organic solvent by mass fraction; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent, which effectively dissolves the lanthanum nitrate; the acidic solvent is nitric acid solution or hydrochloric acid solution; the organic solvent is ethyl acetate solution or acetone solution.

[0028] (2) drying: drying the mixture in step (1) at a temperature of 100-300 DEG C for 2-15 h to obtain a mixed powder.

[0029] (3) granulation: the mixed powder in step (2) is mixed with CMC at a mass ratio of 1:2 at a mixing and stirring speed of 50-300 r / min for 0.5-2 h, and then added into a reaction kettle, the temperature in the reaction kettle is raised to 100-500 DEG C at a rate of 2-5 DEG C / min, and kept at the temperature for 2-10 h, during which the stirring speed is 50-300 r / min, and inert gas is continuously fed into the reaction kettle for protection, and after the temperature keeping, the reaction kettle is naturally cooled to room temperature to obtain mixed particles.

[0030] (4) carbonization: the mixed particles in step (3) are sent to a carbonization furnace at a temperature of 600-1050 DEG C for 1-19 h, and nitrogen is continuously fed into the carbonization furnace for protection, and after the temperature keeping, the carbonization furnace is naturally cooled to room temperature to obtain a carbon-coated catalyst; a multi-layer and multi-segment carbon coating layer is produced around the surface of the catalyst, the coating layer fully connects the rare earth metal ions and the metal compounds, accelerates the reaction of activated molecules, atoms, ions and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the disordered state to ordered state transformation process of graphite crystallites, and accelerates the graphitization speed.

[0031] (5) crushing and screening: the carbon-coated catalyst obtained in step (4) is crushed and screened to obtain a catalyst finished product with a particle size of 6-15 μm.

[0032] The present application effectively promotes the graphitization process by adding a small amount of rare earth metal, which combines with carbon atoms to form graphite-like sheet layer clusters and combines with edge carbon atoms, thereby effectively improving the graphitization degree, shortening the graphitization time, and reducing the graphitization temperature and energy consumption.

[0033] Example 2: a preparation method of a catalyst for graphitization of carbon materials, comprising the following steps:

[0034] (1) mixing: a cerium nitrate solution with a concentration of 25% is mixed with silicon oxide with a particle size of 5-10 μm at a mixing and stirring speed of 50-300 r / min for 0.5-2 h to obtain a mixture, wherein the cerium nitrate solution accounts for 5% and the rest is silicon oxide according to 100% by mass.

[0035] The solvent in the cerium nitrate salt solution is composed of 30-50% water, 25%-35% acidic solvent and 25%-35% organic solvent by mass fraction; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent, effectively dissolving the cerium nitrate salt; the acidic solvent is nitric acid solution or hydrochloric acid solution; and the organic solvent is ethyl acetate solution or acetone solution.

[0036] (2) drying: drying the mixture in step (1), the drying temperature is 100-300 DEG C, the drying time is 2-15h, to obtain a mixed powder.

[0037] (3) granulation: the mixed powder in step (2) is mixed with CMC according to the mass ratio of 1:2, the mixing and stirring speed is 50r / min-300r / min, the mixing and stirring time is 0.5-2h, then added into the reaction kettle, the temperature in the reaction kettle is controlled to rise to 100-500 DEG C at the rate of 2-5 DEG C / min, and kept at this temperature for 2-10h, during which the stirring speed is 50r / min-300r / min, and inert gas is continuously introduced into the reaction kettle for protection, after the completion of the heat preservation, it is naturally cooled to room temperature, to obtain a mixed granule.

[0038] (4) carbonization: the mixed granule in step (3) is sent to a carbonization furnace with a temperature of 600-1050 DEG C for 1-19h, and nitrogen is continuously introduced into the carbonization furnace for protection, after the completion of the heat preservation, it is naturally cooled to room temperature, to obtain a carbon-coated catalyst; a multi-layer and multi-segment carbon coating layer is produced around the surface of the catalyst, which fully connects the rare earth metal ions and metal compounds, accelerates the reaction of activated molecules, atoms, ions and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the disordered state to ordered state transformation process of graphite crystallites, and accelerates the speed of graphitization.

[0039] (5) crushing and screening: the carbon-coated catalyst obtained in step (4) is crushed and screened to obtain a catalyst finished product with a particle size of 6-15um.

[0040] The present application effectively promotes the graphitization process by adding a small amount of rare earth metal, which combines with carbon atoms to form graphite-like sheet layer clusters and combines with edge carbon atoms, thereby effectively improving the graphitization degree, shortening the graphitization time, and reducing the graphitization temperature and energy consumption.

[0041] Example 3: a preparation method of a catalyst for graphitization of carbon material, comprising the following steps:

[0042] (1)Mixing: a praseodymium nitrate solution with a concentration of 25% is mixed with tin oxide with a particle size of 5-10 μm, the mixing stirring speed is 50-300 r / min, the mixing stirring time is 0.5-2 h, to obtain a mixture, according to 100% by mass, the praseodymium nitrate solution is 5%, and the rest is tin oxide.

[0043] The solvent in the praseodymium nitrate solution is composed of 30-50% water, 25-35% acidic solvent and 25-35% organic solvent by mass fraction; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent, which effectively dissolves the praseodymium nitrate; the acidic solvent is nitric acid solution or hydrochloric acid solution; the organic solvent is ethyl acetate solution or acetone solution.

[0044] (2) Drying: the mixture in step (1) is dried, the drying temperature is 100-300℃, the drying time is 2-15 h, to obtain a mixed powder.

[0045] (3) Granulation: the mixed powder in step (2) is mixed with CMC according to a mass ratio of 1:2, the mixing stirring speed is 50-300 r / min, the mixing stirring time is 0.5-2 h, then added into a reaction kettle, the temperature in the reaction kettle is controlled to rise to 100-500℃ at a rate of 2-5℃ / min, and kept at this temperature for 2-10 h, during which the stirring speed is 50-300 r / min, and inert gas is continuously introduced into the reaction kettle for protection, after the heat preservation is completed, it is naturally cooled to room temperature, to obtain a mixed granule.

[0046] (4) Carbonization: the mixed granule in step (3) is sent to a carbonization furnace with a temperature of 600-1050℃ for 1-19 h, while nitrogen is continuously introduced into the carbonization furnace for protection, after the heat preservation is completed, it is naturally cooled to room temperature, to obtain a carbon-coated catalyst; a multi-level and multi-segment carbon coating layer is produced around the surface of the catalyst, which fully connects the rare earth metal ions and metal compounds, accelerates the reaction of activated molecules, atoms, ions and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the disordered state to ordered state transformation process of graphite crystallites, and accelerates the speed of graphitization.

[0047] (5) Crushing and screening: the carbon-coated catalyst obtained in step (4) is crushed and screened, to obtain a catalyst finished product with a particle size of 6-15 μm.

[0048] The present application effectively promotes the graphitization process, effectively improves the graphitization degree, shortens the graphitization time, and reduces the graphitization temperature and energy consumption by adding a small amount of rare earth metal, which is combined with carbon atoms as graphite-like sheet layer clusters and combined with edge carbon atoms.

[0049] Embodiment 4: A preparation method of a catalyst for graphitization of carbon material, comprising the following steps:

[0050] (1) Mixing: a yttrium nitrate solution with a concentration of 25% and zinc oxide with a particle size of 5-10 μm are fully mixed, the mixing stirring speed is 50-300 r / min, and the mixing stirring time is 0.5-2 h, to obtain a mixture, wherein the yttrium nitrate solution accounts for 5% and the rest is zinc oxide according to 100% by mass.

[0051] The solvent in the yttrium nitrate solution is composed of 30-50% water, 25-35% acidic solvent and 25-35% organic solvent by mass fraction; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent, which effectively dissolves the yttrium nitrate; the acidic solvent is nitric acid solution or hydrochloric acid solution; and the organic solvent is ethyl acetate solution or acetone solution.

[0052] (2) Drying: the mixture in step (1) is dried, the drying temperature is 100-300 ℃, and the drying time is 2-15 h, to obtain a mixed powder.

[0053] (3) Granulation: the mixed powder in step (2) and CMC are fully mixed according to a mass ratio of 1:2, the mixing stirring speed is 50-300 r / min, and the mixing stirring time is 0.5-2 h, and then added into a reaction kettle, the temperature in the reaction kettle is controlled to increase to 100-500 ℃ at a rate of 2-5 ℃ / min, and kept at the temperature for 2-10 h, during which the stirring is continuously carried out at a speed of 50-300 r / min, and inert gas is continuously introduced into the reaction kettle for protection, and after the heat preservation is completed, natural cooling is carried out to room temperature, to obtain mixed particles.

[0054] (4) Carbonization: the mixed particles in step (3) are sent to a carbonization furnace with a temperature of 600-1050 ℃ for heat preservation for 1-19 h, while nitrogen is continuously introduced into the carbonization furnace for protection, and after the heat preservation is completed, natural cooling is carried out to room temperature, to obtain a carbon-coated catalyst; a multi-layer and multi-segment carbon coating layer is produced around the surface of the catalyst, which fully connects the rare earth metal ions and metal compounds, accelerates the reaction of activated molecules, atoms, ions and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the ordered state transformation process of the disordered state of graphite microcrystals, and accelerates the graphitization speed.

[0055] (5) Pulverization and screening: the carbon-coated catalyst obtained in step (4) is pulverized and screened to obtain a catalyst product with a particle size of 6-15 μm.

[0056] The present application effectively promotes the graphitization process and effectively improves the graphitization degree by adding a small amount of rare earth metal, which combines with carbon atoms to form graphite-like sheet layer clusters and combines with edge carbon atoms, thereby shortening the graphitization time and reducing the graphitization temperature and energy consumption.

[0057] Example 5: The overall structure is the same as that of Example 1, except that there is no carbonization and pulverization and screening process.

[0058] Test 1: The catalysts of Examples 1-5, Fe2O3, SiO2, SnO2 and ZnO were mixed with petroleum needle coke granules in a ratio of 1:22 for graphitization, the graphitization time was 20 h, the graphitization temperature was 2800°C, and the graphitization degree is shown in Table 1.

[0059] Table 1 Graphitization degree of petroleum needle coke using different catalysts

[0060]

[0061] Under the same graphitization time and temperature, the catalysts of Examples 1-5 were used to catalyze the graphitization of petroleum needle coke, and the graphitization degree was significantly higher than that of using traditional Fe2O3, SiO2, SnO2 and ZnO catalysts to catalyze the graphitization of petroleum needle coke. It shows that the catalyst of the present application can improve the graphitization degree compared with the traditional catalyst.

[0062] Meanwhile, Example 5 is a catalyst without carbonization, and its catalytic graphitization degree of petroleum needle coke is significantly lower than that of the catalysts of Examples 1-4, which significantly produces a carbon-coated layer with multiple levels and multiple segments around the surface of the catalyst, which fully connects the rare earth metal ions and metal compounds, accelerates the reaction of activated molecules, atoms, ions and carbon ions, reduces the activation energy in the graphitization process, reduces the energy barrier of the ordered state to the disordered state of the graphitized microcrystalline, accelerates the graphitization speed, and improves the graphitization degree.

[0063] Test 2: The catalysts of Examples 1-4, Fe2O3, SiO2, SnO2 and ZnO were mixed with petroleum needle coke granules in a ratio of 1:22 for graphitization, the graphitization temperature was 2800°C, the graphitization time of the catalysts of Examples 1-4 was 15 h, and the graphitization time of Fe2O3, SiO2, SnO2 and ZnO was 20 h, and the graphitization degree is shown in Table 2.

[0064] Table 2 Graphitization degree of petroleum needle coke using different catalysts

[0065]

[0066] In the case of the same graphitization temperature, the graphitization time of petroleum needle coke using the catalysts of Examples 1-4 is shortened by 5h, but the graphitization degree is almost the same as that of petroleum needle coke catalyzed by conventional Fe203, Si02, Sn02and ZnO catalysts, or even higher than that of petroleum needle coke catalyzed by conventional Fe203, Si02, Sn02and ZnO catalysts. It is shown that the catalysts of Examples 1-4 can shorten the graphitization time compared with conventional catalysts.

[0067] Test 3: The catalysts of Examples 1-4, Fe203, Si02, Sn02and ZnO are mixed with the granulated petroleum needle coke at a ratio of 1:22 for graphitization, and the graphitization time is 20h, wherein the graphitization temperature of petroleum needle coke catalyzed by the catalysts of Examples 1-4 is 2600℃, and the graphitization temperature of petroleum needle coke catalyzed by Fe203, Si02, Sn02and ZnO is 2800℃, and the graphitization degree is shown in Table 3.

[0068] Table 3 Graphitization degree of petroleum needle coke using different catalysts

[0069]

[0070] In the case of the same graphitization time, the graphitization temperature of petroleum needle coke using the catalysts of Examples 1-4 is reduced by 200℃, but the graphitization degree is almost the same as that of petroleum needle coke catalyzed by conventional Fe203, Si02, Sn02and ZnO catalysts, or even higher than that of petroleum needle coke catalyzed by conventional Fe203, Si02, Sn02and ZnO catalysts. It is shown that the catalysts of Examples 1-4 can reduce the graphitization temperature and reduce the energy consumption of graphitization compared with conventional catalysts.

[0071] Test 4: The artificial graphites prepared in test 1 using different catalysts are used to manufacture lithium ion battery graphite negative electrode materials, i.e. each of the prepared artificial graphites is mixed with the conductive agent super P and CMC, SBR in a weight ratio of 95.5:1:1.5:1.5, a uniform slurry is prepared with water as a solvent, coated on a current collector copper foil to press a working electrode. The copper foil coated with the sample is placed in a vacuum drying box, after drying, the sample is taken out, the electrode sheet is washed, and placed in a microne hand box, a metal lithium sheet is used as a counter electrode, an electrolyte is 1M LiPFB6 B DMC+EMC+EC (1:1:1), a porous polypropylene film of Celgard 2400 type is used as a separator, a 2032 type button cell is assembled to perform rate charge and discharge test, and the test results are shown in Table 4.

[0072] Table 4: Rate charge and discharge test results

[0073]

[0074]

[0075] The artificial graphites prepared by catalyzing petroleum needle coke graphitization using the catalysts of examples 1-5 have higher discharge capacity and discharge efficiency when applied to lithium ion battery graphite negative electrode materials compared with the artificial graphites prepared by catalyzing petroleum needle coke graphitization using traditional catalysts; the artificial graphites prepared by catalyzing petroleum needle coke graphitization using the catalyst of example 5 have significantly lower discharge capacity and discharge efficiency when applied to lithium ion battery graphite negative electrode materials compared with the artificial graphites prepared by catalyzing petroleum needle coke graphitization using the catalysts of examples 1-4.

[0076] The above is the preferred embodiment of the present application, and for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, which improvements and refinements should also be considered within the scope of protection of the present application.

Claims

1. A method for producing a catalyst for graphitization of carbon material, characterized by comprising the steps of: It comprises the following steps: ​ (1) mixing: the concentration of 1%-50% of rare earth metal solution and one or more of silicon oxide, iron oxide, tin oxide, zinc oxide, iron carbide, tin carbide, zinc carbide are mixed, the mixture is obtained, according to the mass percentage is 100%, wherein the rare earth metal solution is 1%-25%, the rest is one or more of silicon oxide, iron oxide, tin oxide, zinc oxide, iron carbide, tin carbide, zinc carbide; Wherein, the rare earth metal ion in the rare earth metal solution includes one or more of lanthanum ion, cerium ion, praseodymium ion, yttrium ion; (2) drying: the mixture in step (1) is dried, the drying temperature is 100-300℃, the drying time is 2-15h, the mixed powder is obtained; (3) granulation: the mixed powder in step (2) and the precursor are mixed according to the mass ratio of 1:1-1:3, and are added into the reaction kettle, the temperature in the reaction kettle is controlled to rise to 100-500℃ at the rate of 2-5℃ / min, and is kept at the temperature for 2-10h, during which the stirring is not stopped at the speed of 50r / min-300 r / min, at the same time, inert gas is continuously introduced into the reaction kettle for protection, after the heat preservation is completed, it is naturally cooled to room temperature, and the mixed particles are obtained; (4) carbonization: the mixed particles in step (3) are sent to the carbonization furnace with a temperature of 600-1050℃ for 1-19h, at the same time, nitrogen is continuously introduced into the carbonization furnace for protection, after the heat preservation is completed, it is naturally cooled to room temperature, and the carbon coated catalyst is obtained.

2. The method for producing a catalyst for graphitization of carbon material according to claim 1, characterized by, The solvent in the rare earth metal solution in step (1) is composed of 30-50% water, 25%-35% acidic solvent and 25%-35% organic solvent; or 70-90% water and 10-30% acidic solvent; or 70-90% water and 10-30% organic solvent.

3. The method for producing a catalyst for graphitization of carbon material according to claim 2, characterized by, The acidic solvent is nitric acid solution or hydrochloric acid solution; the organic solvent is ethyl acetate solution or acetone solution.

4. The method for preparing a catalyst for graphitization of carbon materials according to claim 1, characterized in that, The particle size of silicon oxide, iron oxide, tin oxide, zinc oxide, iron carbide, tin carbide, zinc carbide in step (1) is 5-10μm.

5. The method for preparing a catalyst for graphitization of carbon materials according to claim 1, characterized in that, The mixing stirring speed in step (1) and step (3) is 50r / min-300 r / min, and the mixing stirring time is 0.5-2h.

6. The method for preparing a catalyst for graphitization of carbon materials according to claim 1, characterized in that, The precursor in step (3) is one or more of CMC, PVC and resin.

7. The method for preparing a catalyst for graphitization of carbon materials according to claim 1, characterized in that, After step (4), it further comprises: crushing and screening: the carbon coated catalyst obtained in step (4) is crushed and screened, and the catalyst finished product with particle size of 6-15μm is obtained.

Citation Information

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