CN115519133A - Preparation method of nickel-coated graphite powder - Google Patents
Preparation method of nickel-coated graphite powder Download PDFInfo
- Publication number
- CN115519133A CN115519133A CN202211291344.3A CN202211291344A CN115519133A CN 115519133 A CN115519133 A CN 115519133A CN 202211291344 A CN202211291344 A CN 202211291344A CN 115519133 A CN115519133 A CN 115519133A
- Authority
- CN
- China
- Prior art keywords
- graphite powder
- nickel
- solution
- coated graphite
- reducing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemically Coating (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of nickel-coated graphite powder, belonging to the technical field of preparation of electromagnetic shielding composite materials. The method specifically comprises the following steps: stirring and mixing graphite powder and deionized water at the temperature of 45-60 ℃, then sequentially adding nickel salt, complexing agent, buffering agent and wetting agent, and continuously stirring in the adding process to obtain a graphite powder mixed solution; adding a catalyst and a reducing agent solution into the graphite powder mixed solution; when a large amount of bubbles appear in the solution, slowly dripping a reducing agent solution, continuously stirring for reaction, and obtaining a product mixed solution after the reaction is finished; and carrying out solid-liquid separation, washing and drying on the product mixed solution to obtain the nickel-coated graphite powder. The method has the advantages of simple process flow, easy operation, high safety, good weather resistance and low resistivity of the prepared nickel-coated graphite powder, and the preparation process is carried out under the conditions of normal pressure and medium and low temperature.
Description
Technical Field
The invention belongs to the technical field of preparation of electromagnetic shielding composite materials, and particularly relates to a preparation method of nickel-coated graphite powder.
Background
The nickel-coated graphite powder is a coated composite powder material formed by coating a layer of metallic nickel on the surface of graphite particles serving as cores, has excellent lubricating property of graphite, and also has good electrical conductivity and thermal conductivity of metal, low density and low material cost. Is widely applied to the fields of electromagnetic shielding, wave absorption, thermal spraying and the like.
Because graphite powder does not have the capacity of generating autocatalytic reaction in a nickel solution, the prior art mainly adopts the following process flows: degreasing → washing → sensitization → washing → activation → washing- → chemical nickel plating/hydrogen pressure reduction, namely, a series of surface pretreatment needs to be carried out on the graphite powder, and then the chemical nickel plating or the hydrogen pressure reduction can be carried out. Therefore, the prior art has the problems of complex process flow, high production cost, great difficulty in waste liquid treatment and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the nickel-coated graphite powder, the nickel-coated graphite powder prepared by the method has the advantages of simple process flow, easy operation, high safety, good weather resistance and low resistivity, and the preparation process is carried out under the conditions of normal pressure, medium and low temperature.
The technical scheme adopted by the invention is as follows:
a preparation method of nickel-coated graphite powder comprises the following steps:
s1, stirring and mixing graphite powder and deionized water at the temperature of 45-60 ℃, then sequentially adding nickel salt, a complexing agent, a buffering agent and a wetting agent, and continuously stirring in the adding process to obtain a graphite powder mixed solution;
s2, adding a catalyst and a reducing agent solution into the graphite powder mixed solution;
s3, when a large number of bubbles appear in the solution in the step S2, slowly dropwise adding a reducing agent solution, continuously stirring for reaction, and obtaining a product mixed solution after the reaction is finished;
and S4, carrying out solid-liquid separation, washing and drying on the product mixed solution to obtain the nickel-coated graphite powder.
Optionally, the graphite powder is flake graphite powder, and the median particle diameter D50 is 1 μm to 250 μm.
Optionally, the mass ratio of the graphite powder to the deionized water is 9:50-200.
Optionally, in step S1:
the stirring speed is 200-600r/min;
adding nickel salt, complexing agent, buffering agent and wetting agent, and stirring for 15-20min.
Optionally, the nickel salt is one or more of nickel sulfamate, nickel chloride, nickel nitrate, nickel oxalate, nickel acetate, nickel sulfate and nickel sulfate hexahydrate;
the complexing agent is one or more of ammonia water, citric acid and sodium citrate;
the buffer is one or more of ammonium chloride, sodium acetate and boric acid;
the wetting agent is one or more of 2-ethylhexyl sulfate sodium salt, sodium dodecyl sulfate and dioctyl sodium sulfosuccinate;
the reducing agent is one or more of hydrazine hydrate, sodium hypophosphite and sodium hypophosphite;
the catalyst is one or more of sodium borohydride, methyl ammonia borane, nickel powder, zinc powder and nickel-coated graphite powder.
Optionally, the concentration of nickel salt in the graphite powder mixed solution obtained in the step S1 is 200-600g/L, the concentration of the buffer is 100-300g/L, and the concentration of graphite is 45-90g/L.
Optionally, the reducing agent solution is a sodium hypophosphite solution with a concentration of 1000 g/L;
and 10-20mL of reducing agent solution is added into the S2.
Optionally, the catalyst is added in an amount of 0.5 to 2.0g.
Optionally, the stirring speed when the reducing agent solution is dripped in step S3 is 20-50r/min, and when no bubble is generated, the reaction is completed, and the dripping of the reducing agent is stopped.
Optionally, step S4 specifically includes:
filtering, suction filtering, filter pressing or centrifugal separation is carried out on the product mixed liquor to obtain a solid matter;
washing the solid matter until the washing liquid is neutral, and then carrying out suction filtration;
and (4) transferring the graphite powder into vacuum and nitrogen protection atmosphere, drying for 6-12h at 90-120 ℃, and obtaining the nickel-coated graphite powder after drying.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the nickel-coated graphite powder does not need to carry out surface pretreatment on the graphite powder, but stirs and mixes the graphite powder with deionized water and a nickel plating reagent at a proper temperature to fully wet the graphite powder, and directly carries out chemical nickel plating under the initiation of a catalyst, and the method has simple process flow and only comprises the following steps: mixing, chemical nickel plating, washing and drying, and the operation is simple; the whole preparation process is carried out under the conditions of normal pressure and medium and low temperature (45-60 ℃), is easy to control and has high safety; the prepared nickel-coated graphite powder coating is completely coated, uniform and compact, and has good weather resistance and conductivity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a flow chart of the preparation method of nickel-coated graphite powder of the present invention.
Fig. 2 is a scanning electron microscope image of the nickel-coated graphite powder prepared in example 1.
Detailed Description
In the following, certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the claimed embodiments. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, an embodiment of the present invention provides a method for preparing nickel-coated graphite powder, including the following steps:
s1, adding graphite powder into a reaction kettle filled with deionized water, controlling the temperature of the deionized water within the range of 45-60 ℃, and quickly and fully stirring to fully mix the graphite powder and the deionized water; and then adding nickel salt, a complexing agent, a buffering agent, a wetting agent and the like in sequence, continuously stirring in the adding process, and continuously stirring for a certain time after the adding is finished to fully wet the graphite powder to obtain a graphite powder mixed solution.
And S2, adding a small amount of catalyst and reducing agent solution into the obtained graphite powder mixed solution for contacting the surface of the wetted graphite powder to initiate a nickel plating reaction.
And S3, when the solution in the step S2 causes a nickel plating reaction to generate a large amount of bubbles under the action of a small amount of catalyst and reducing agent, slowly dropwise adding a reducing agent solution into the solution, continuously stirring for reaction until no bubbles are generated, and stopping dropwise adding the reducing agent solution when the solution is clarified to indicate that the reaction is finished to obtain a product mixed solution.
And S4, carrying out solid-liquid separation on the obtained product solution to obtain a solid matter, and then washing and drying the solid matter to finally obtain the required nickel-coated graphite powder.
Furthermore, the graphite powder raw material adopts flake graphite powder with the median particle diameter D50 of 1-250 μm.
Controlling the mass ratio of the graphite powder to the deionized water to be 9: in the range of 50-200.
Controlling the stirring speed of the graphite powder, the deionized water and the subsequent nickel plating reagent to be 200-600r/min; and continuously stirring for about 15-20min after adding nickel salt, complexing agent, buffering agent and wetting agent.
The flaky graphite powder can ensure that the specific surface area of the nickel-coated graphite powder prepared subsequently is large; the flaky graphite powder raw material and deionized water are in a layered state (floating on the upper part of the liquid and/or precipitating on the bottom of the liquid) at the beginning and cannot be well mixed, and the graphite powder can be effectively ensured to be fully dispersed and contacted with the deionized water and a solvent by controlling the stirring rotating speed to be about 200-600r/min, and the graphite powder structure is ensured not to be damaged; after the nickel plating reagent is added, the mixture is continuously stirred for a certain time, so that the graphite powder can be well fully wetted, the hydrophilicity of the graphite powder is increased, a chemical environment that the surface of the graphite powder can well adsorb nickel ions is provided, and preparation is made for subsequent nickel plating reaction.
Alternatively, the nickel salt in the nickel plating reagent may be one or a combination of more of nickel sulfamate, nickel chloride, nickel nitrate, nickel oxalate, nickel acetate, nickel sulfate hexahydrate, and the like;
the complexing agent can be one or more of ammonia water, citric acid, sodium citrate, etc.;
the buffer can be one or more of ammonium chloride, sodium acetate, boric acid and the like;
the wetting agent can be one or more of 2-ethylhexyl sulfate sodium salt, sodium lauryl sulfate, dioctyl sodium sulfosuccinate, and the like.
The catalyst can be one or more of sodium borohydride, methyl ammonia borane, nickel powder, zinc powder, nickel-coated graphite powder and the like.
The reducing agent can be one or more of hydrazine hydrate, sodium hypophosphite and the like.
In one embodiment, when preparing the graphite powder mixed solution in step S1, the concentration of the nickel salt in the graphite powder mixed solution is controlled to be in the range of 200 to 600g/L, the concentration of the buffer is in the range of 100 to 300g/L, and the concentration of graphite is in the range of 45 to 90g/L. The nickel ions in the nickel plating reagent can be completely plated and attached to the surface of the graphite powder, the nickel plating layer is uniformly plated, the nickel ions in the solution are less in residue after the nickel plating is finished, and the nickel concentration can be as low as a milligram level, so that the treatment difficulty of the waste liquid can be effectively reduced, and the treatment cost of the waste liquid can be reduced; meanwhile, the graphite powder can be well coated for nickel plating, and the condition of plating leakage or incomplete plating attachment is avoided.
In one embodiment, the reducing agent solution is sodium hypophosphite solution with a concentration of 1000g/L, i.e. the reducing agent is sodium hypophosphite. In step S2, 0.5-2.0g of catalyst and 10-20mL of the sodium hypophosphite solution are added at a time to initiate the nickel plating reaction.
The catalyst has catalytic activity, can contact with the surface of graphite powder with high hydrophilicity by adding a small amount of catalyst, and then initiates the graphite powder to carry out autocatalysis to generate chemical nickel plating reaction under the action of a reducing agent; a small amount of catalyst provides an active center for chemical nickel plating reaction, nickel ions adsorbed on the surface of graphite powder are slowly reduced to form a nickel plating point structure, and the nickel ions in the solution start to carry out rapid nickel plating reaction by taking the active center as a start, so that a compact and continuous chemical plating layer is formed. Sodium hypophosphite is used as a reducing agent, so that the obtained coating is a low-phosphorus nickel coating which has good weather resistance, namely the obtained nickel-coated graphite powder product has good weather resistance and low resistivity.
In step S3, the reducing agent solution is dripped and stirred at the same time, the stirring speed is controlled within the range of 20-50r/min, and when no bubble is generated in the reaction solution, the reaction is finished, the dripping of the reducing agent and the stirring are stopped. The stirring speed is controlled within the range of 20-50r/min, so that the reducing agent and the reaction solution can be effectively and uniformly mixed, the bubble generation condition in the solution can be conveniently observed, and whether the reaction is finished or not can be conveniently judged. The method has the advantages that the reducing agent is slowly dripped for reaction, the dosage of the reducing agent can be effectively controlled, the nickel plating reaction is carried out at a constant speed, the formed nickel plating layer is uniform and compact, the impurities and the bubbles are few, and the resistivity of the generated nickel-coated graphite powder is low.
In step S4, when performing solid-liquid separation of the product mixed solution, filtering, suction filtration, filter pressing, centrifugal separation or other means may be employed to perform separation to obtain a solid; the solid matter can be washed by deionized water until the discharged washing liquid is neutral, and then the solid matter is filtered; and finally, transferring the graphite powder into a vacuum nitrogen drying box, drying the graphite powder for 6 to 12 hours at the temperature of between 90 and 120 ℃ in the vacuum nitrogen protection atmosphere, and obtaining the nickel-coated graphite powder product after drying.
In conclusion, the preparation method of the invention has simplified process flow, and only comprises the following steps: mixing, chemical nickel plating, washing and drying; the graphite powder is not required to be subjected to surface pretreatment, and chemical nickel plating is directly performed, so that the operation is simple; the whole process is carried out under the conditions of normal pressure and medium and low temperature (45-60 ℃), the operation is easy, and the safety is high; during nickel plating, a catalyst initiates a point reaction on the surface of graphite powder, and the graphite powder is connected into sheets through points to finally form a plating layer; the reducing agent is slowly dripped at a constant speed in the reaction process, the reaction is carried out at a constant speed, and the generated plating layer is uniform and compact and has no impurities or bubbles, so that the prepared nickel-coated graphite powder has good weather resistance and low resistivity, and further has good performance when being used as a conductive filler.
Example 1
A preparation method of nickel-coated graphite powder comprises the following steps:
step 1, adding flake graphite powder with the median particle size of D50=100 μm into a reaction kettle filled with deionized water, wherein the temperature in the reaction kettle is 45-60 ℃, the mass ratio of the graphite powder to the deionized water is 9, and the flake graphite powder and the deionized water are fully stirred and mixed at 300-400 r/min. And then continuously stirring, sequentially adding nickel salt hexahydrate nickel sulfate, complexing agent ammonia water, buffering agent ammonium chloride and wetting agent sodium dodecyl sulfate, and continuously stirring for 15-20min after the addition is finished so as to fully wet the graphite powder. And obtaining a graphite powder mixed solution, wherein the concentration of nickel sulfate in the graphite powder mixed solution is 300g/L, the concentration of ammonium chloride is 150g/L, and the concentration of graphite powder is 45g/L.
And 2, stopping stirring after the graphite powder is fully wetted, adding 0.5-2g of catalyst nickel-coated graphite powder or coated nickel-carbon powder into the solution, and adding 10-20mL of 1000g/L sodium hypophosphite solution at one time.
And 3, after adding the catalyst and the hypophosphorous acid solution, when a large amount of bubbles appear in the solution, slowly and uniformly dripping a reducing agent sodium hypophosphite solution with the concentration of 1000g/L into the solution, continuously stirring at a controlled rotating speed of 20-50r/min, stopping dripping the sodium hypophosphite solution and stopping stirring when the reaction solution has no bubbles, and thus obtaining a product mixed solution.
Step 4, filtering, suction filtering, filter pressing or centrifugal separation is carried out on the product mixed liquor to obtain a solid matter; washing the solid matter with deionized water, and performing suction filtration after washing liquid is neutral; and then transferring the solid matter into a vacuum nitrogen drying box, and drying for 12 hours at 90 ℃ in the vacuum and nitrogen protection atmosphere to obtain the nickel-coated graphite powder product.
Example 2
A method of preparing nickel-coated graphite powder, substantially as in example 1, with the following exceptions:
the median particle size D50=20 μm of the graphite powder added in the step 1, the mass ratio of the graphite powder to the deionized water is 3; the concentration of nickel sulfate in the prepared graphite powder mixed solution is 400g/L, the concentration of ammonium chloride is 200g/L, and the concentration of graphite powder is 60g/L.
The drying conditions in the step 4 are as follows: drying for 6h at 120 ℃ in vacuum and nitrogen protection atmosphere.
Example 3
A method of preparing nickel-coated graphite powder, substantially as in example 1, with the following exceptions:
the median particle size D50=200 μm of the graphite powder added in the step 1, the mass ratio of the graphite powder to the deionized water is 9; the concentration of nickel sulfate in the prepared graphite powder mixed solution is 600g/L, the concentration of ammonium chloride is 300g/L, and the concentration of graphite powder is 90g/L.
Example 4
A method of preparing nickel-coated graphite powder, substantially as in example 1, with the following exceptions:
the median particle size D50=50 μm of the graphite powder added in the step 1, the mass ratio of the graphite powder to the deionized water is 9; the concentration of nickel sulfate in the prepared graphite powder mixed solution is 600g/L, the concentration of ammonium chloride is 600g/L, and the concentration of graphite powder is 45g/L.
The drying conditions in the step 4 are as follows: drying for 6h at 120 ℃ in vacuum and nitrogen protection atmosphere.
Example 5
A method of preparing nickel-coated graphite powder, substantially as in example 1, with the following exceptions:
the mass ratio of the graphite powder added in the step 1 to the deionized water is 9; the concentration of nickel sulfate in the prepared graphite powder mixed solution is 200g/L, the concentration of ammonium chloride is 100g/L, and the concentration of graphite powder is 45g/L.
Example 6
A method for preparing nickel-coated graphite powder, which is substantially the same as that in example 1, except that:
the nickel salt added in the step 1 is nickel chloride, the complexing agent is citric acid, the buffering agent is sodium acetate, the concentration of the nickel chloride in the prepared graphite powder mixed solution is 300g/L, the concentration of the sodium acetate is 100g/L, and the concentration of the graphite powder is 60g/L.
Example 7
A method of preparing nickel-coated graphite powder, substantially as described in example 1, with the following exceptions:
the nickel salt added in the step 1 is nickel acetate, the buffering agent is boric acid, and the wetting agent is sodium dioctyl sulfosuccinate; the concentration of nickel acetate in the prepared graphite powder mixed solution is 400g/L, the concentration of boric acid is 150g/L, and the concentration of graphite powder is 60g/L.
The scanning electron microscope examination and analysis shows that the nickel-coated graphite powder coatings prepared in the examples 1 to 7 are completely coated, and the coatings are uniformly and compactly distributed. As shown in fig. 2, a scanning electron micrograph of the nickel-coated graphite powder obtained in example 1 is shown.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the nickel-coated graphite powder is characterized by comprising the following steps:
s1, stirring and mixing graphite powder and deionized water at the temperature of 45-60 ℃, then sequentially adding nickel salt, a complexing agent, a buffering agent and a wetting agent, and continuously stirring in the adding process to obtain a graphite powder mixed solution;
s2, adding a catalyst and a reducing agent solution into the graphite powder mixed solution;
s3, when a large number of bubbles appear in the solution in the step S2, slowly dropwise adding a reducing agent solution, continuously stirring for reaction, and obtaining a product mixed solution after the reaction is finished;
and S4, carrying out solid-liquid separation, washing and drying on the product mixed solution to obtain the nickel-coated graphite powder.
2. The method for preparing nickel-coated graphite powder according to claim 1, wherein the graphite powder is flake graphite powder and has a median particle diameter D50 of 1 to 250 μm.
3. The preparation method of nickel-coated graphite powder according to claim 1 or 2, wherein the mass ratio of the graphite powder to the deionized water is 9:50-200.
4. The method for preparing nickel-coated graphite powder according to claim 1, wherein in step S1:
the stirring speed is 200-600r/min;
adding nickel salt, complexing agent, buffering agent and wetting agent, and stirring for 15-20min.
5. The method for preparing nickel-coated graphite powder according to claim 1 or 4, characterized in that:
the nickel salt is one or more of nickel sulfamate, nickel chloride, nickel nitrate, nickel oxalate, nickel acetate, nickel sulfate and nickel sulfate hexahydrate;
the complexing agent is one or more of ammonia water, citric acid and sodium citrate;
the buffer is one or more of ammonium chloride, sodium acetate and boric acid;
the wetting agent is one or more of 2-ethylhexyl sulfate sodium salt, sodium dodecyl sulfate and dioctyl sodium sulfosuccinate;
the reducing agent is one or more of hydrazine hydrate, sodium hypophosphite and sodium hypophosphite;
the catalyst is one or more of sodium borohydride, methyl ammonia borane, nickel powder, zinc powder and nickel-coated graphite powder.
6. The method for preparing nickel-coated graphite powder according to claim 5, wherein the concentration of nickel salt in the graphite powder mixed solution obtained in the step S1 is 200-600g/L, the concentration of the buffer is 100-300g/L, and the concentration of graphite is 45-90g/L.
7. The method for preparing nickel-coated graphite powder according to claim 5, wherein the reducing agent solution is a sodium hypophosphite solution with a concentration of 1000 g/L;
and 10-20mL of reducing agent solution is added into the S2.
8. The method for preparing nickel-coated graphite powder according to claim 5, wherein the amount of the catalyst is 0.5 to 2.0g.
9. The method for preparing nickel-coated graphite powder according to claim 1, wherein the stirring speed for dropping the reducing agent solution in step S3 is 20 to 50r/min, and when no bubble is generated, the reaction is completed and the dropping of the reducing agent is stopped.
10. The method for preparing nickel-coated graphite powder according to claim 1, wherein the step S4 specifically comprises:
filtering, suction filtering, filter pressing or centrifugal separation is carried out on the product mixed liquor to obtain a solid matter;
washing the solid matter until the washing liquid is neutral, and then carrying out suction filtration;
and (4) transferring the graphite powder into vacuum and nitrogen protection atmosphere, drying for 6-12h at 90-120 ℃, and obtaining the nickel-coated graphite powder after drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211291344.3A CN115519133B (en) | 2022-10-21 | 2022-10-21 | Preparation method of nickel-coated graphite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211291344.3A CN115519133B (en) | 2022-10-21 | 2022-10-21 | Preparation method of nickel-coated graphite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115519133A true CN115519133A (en) | 2022-12-27 |
| CN115519133B CN115519133B (en) | 2023-08-25 |
Family
ID=84703324
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211291344.3A Active CN115519133B (en) | 2022-10-21 | 2022-10-21 | Preparation method of nickel-coated graphite powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115519133B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691937A (en) * | 2013-12-31 | 2014-04-02 | 武汉理工大学 | Nickel-coated graphite composite particle preparation method |
| CN107225234A (en) * | 2017-04-21 | 2017-10-03 | 昆明理工大学 | A kind of Cr2The surface cladded with nickel layer method of N particles |
| CN109500385A (en) * | 2018-09-28 | 2019-03-22 | 中北大学 | A kind of laser fast shaping nickel/graphene composite powder preparation method |
| CN109518171A (en) * | 2018-12-24 | 2019-03-26 | 广州传福化学技术有限公司 | A kind of chemical nickel-plating liquid |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN111424266A (en) * | 2020-03-19 | 2020-07-17 | 西安工程大学 | Preparation method of nickel-coated graphite composite particles |
| US20210222302A1 (en) * | 2020-01-19 | 2021-07-22 | Beijing Institute Of Technology | Method for forming nickel plated graphene hollow sphere |
| CN114700490A (en) * | 2022-03-15 | 2022-07-05 | 东北大学 | Preparation method of nickel-coated graphite composite particles and application of nickel-coated graphite composite particles in electromagnetic shielding field |
-
2022
- 2022-10-21 CN CN202211291344.3A patent/CN115519133B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103691937A (en) * | 2013-12-31 | 2014-04-02 | 武汉理工大学 | Nickel-coated graphite composite particle preparation method |
| CN107225234A (en) * | 2017-04-21 | 2017-10-03 | 昆明理工大学 | A kind of Cr2The surface cladded with nickel layer method of N particles |
| CN109500385A (en) * | 2018-09-28 | 2019-03-22 | 中北大学 | A kind of laser fast shaping nickel/graphene composite powder preparation method |
| CN109518171A (en) * | 2018-12-24 | 2019-03-26 | 广州传福化学技术有限公司 | A kind of chemical nickel-plating liquid |
| US20210222302A1 (en) * | 2020-01-19 | 2021-07-22 | Beijing Institute Of Technology | Method for forming nickel plated graphene hollow sphere |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN111424266A (en) * | 2020-03-19 | 2020-07-17 | 西安工程大学 | Preparation method of nickel-coated graphite composite particles |
| CN114700490A (en) * | 2022-03-15 | 2022-07-05 | 东北大学 | Preparation method of nickel-coated graphite composite particles and application of nickel-coated graphite composite particles in electromagnetic shielding field |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115519133B (en) | 2023-08-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102002694B (en) | Method for preparing uniform silver conducting layer on surface of metal or nonmetal material | |
| US10995408B2 (en) | Method of electroless nickle plating on surface of silicon carbide powder | |
| Tan et al. | Pd-around-CeO 2− x hybrid nanostructure catalyst: three-phase-transfer synthesis, electrocatalytic properties and dual promoting mechanism | |
| CN102664275B (en) | Carbon-loaded kernel-shell copper-palladium-platinum catalyst for fuel battery and preparation method thereof | |
| CN1936078A (en) | Composite conducting microball and its preparing method | |
| CN108728835A (en) | A kind of preparation method of electroplate material | |
| CN109423637A (en) | A kind of preparation method of high conductive material | |
| CN102212801A (en) | Chemical silvering method for PS (polystyrene) microspheres | |
| CN109967113A (en) | A kind of preparation method of the monatomic catalyst of metal | |
| CN101054663A (en) | Activating process for nonmetal basal body chemical plating | |
| CN109423636A (en) | A kind of preparation method of secondary silver-plated highly conductive filler | |
| JPWO2019181788A1 (en) | Compound for positive electrode | |
| Sun et al. | Catalytic properties of Pd nanoparticles supported on Cu 2 O microspheres for hydrogen peroxide electroreduction | |
| CN101773825A (en) | Catalyst slurry for fuel cell double-effect oxygen electrode, preparation method and application thereof | |
| JP3871653B2 (en) | Method for producing conductive fine particles | |
| JP6840314B2 (en) | Carrier-supported palladium core platinum shell fine particle colloid, carrier-supported palladium core platinum shell fine particle catalyst, their manufacturing method, and battery | |
| JP6609758B2 (en) | Carrier-supported palladium core platinum shell fine particles and method for producing the same | |
| JP6573333B2 (en) | Carrier-supported palladium fine particle colloid, carrier-supported palladium core platinum shell fine particle colloid, carrier-supported palladium core platinum shell fine particle catalyst, method for producing them, and battery. | |
| CN115519133A (en) | Preparation method of nickel-coated graphite powder | |
| CN110586081B (en) | Palladium-carbon catalyst and preparation method and application thereof | |
| CN112981452A (en) | Water oxidation electrocatalyst and preparation method thereof, and water oxidation electrode and preparation method thereof | |
| CN101638796B (en) | Preparation method of anode catalyst for water electrolysis reaction | |
| CN112207276B (en) | Preparation method of micron nickel-plated aluminum powder | |
| CN114457325A (en) | Method for controlling thickness of nickel layer of nickel-plated polymer microsphere | |
| Babu et al. | Electroless Ni–P coated on graphite as catalyst for the electro-oxidation of dextrose in alkali solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |