CN110980721B - Preparation method of nano graphite powder and method for preparing nano graphite slurry by using nano graphite powder - Google Patents
Preparation method of nano graphite powder and method for preparing nano graphite slurry by using nano graphite powder Download PDFInfo
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Abstract
The invention provides a preparation method of nano graphite powder and a method for preparing nano graphite slurry by using the same, wherein the method comprises the following steps: placing the explosive column in an explosion container, vacuumizing, and filling protective gas to ensure that the pressure in the explosion container is not higher than 1000Pa; detonating the explosive column, reacting in the explosion container, collecting powder in the container after the product subsides, screening and washing to obtain the nano graphite powder. According to the method, the graphite powder is prepared by adopting an explosion method, the particle size of a product is regulated and controlled by controlling the initial gas pressure by utilizing the uniqueness of the reaction condition of the explosion method, and the obtained product has a narrow particle size distribution range and good uniformity; the particle size characteristics of the prepared nano graphite powder are suitable for preparing nano graphite slurry, and the obtained nano graphite slurry is uniform and stable; the method has the advantages of simple operation procedure and short processing time, and can effectively improve the production efficiency.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a preparation method of nano graphite powder and a method for preparing nano graphite slurry by using the nano graphite powder.
Background
The carbon industry belongs to the basic raw material industry and is an essential basic material for economic development. Among them, the nano-sized graphite material belongs to a popular research material, and has wide application fields, such as a kinescope of electronic information, a black matrix conductive coating in the display manufacturing industry, and is used as a catalyst, an adsorbent, a conductive agent, a lubricant, etc. in the chemical industry.
The production process of the nano graphite material is generally complex, so that the price of the nano graphite is high, and the agglomeration and sedimentation are easy to occur due to the large specific surface area of the nano graphite, so that the preparation and the application of the nano graphite are difficult and challenging due to the factors. The existing method for preparing the nano graphite powder comprises a nano diamond powder heating phase transformation method and a common graphite powder high-energy ball milling method; the method comprises the steps of preparing nano diamond powder by detonation of mixed explosive, then chemically purifying, and then heating the nano diamond powder to isolate oxygen and convert the nano diamond powder into nano graphite powder; the latter is to put the ordinary graphite powder into a high-energy ball mill for mechanical ball milling, the required time is long and reaches several hours to tens of hours, and the production efficiency is low.
Among the above methods, the detonation method is adopted to prepare the nano carbon material, and CN 101164682a discloses a method for synthesizing nano polycrystalline diamond by explosion, which comprises the following steps: firstly preparing a graphite compact, placing the graphite compact below an explosion device, detonating the explosion device, enabling a fly sheet to strike the graphite compact for reaction, then recovering graphite ash, screening the graphite ash, and carrying out chemical post-treatment on the graphite ash, wherein in the method, polycrystalline diamond is mainly prepared, and the adjustment of the size of a product is not involved.
At present, a method for preparing nano graphite by adopting an explosion method or a detonation method is also available, and CN 101003369A discloses a method for preparing flaky nano graphite powder by detonation, which comprises the steps of preparing a graphite interlayer compound, preparing an explosive, detonating and collecting, and specifically comprises the steps of mixing graphite with strong oxidizing acid, adding a reducing substance or explosive to prepare explosives, detonating the explosives in an explosion reaction kettle, and collecting a product from the reaction kettle after deposition to obtain flaky nano graphite powder. The method mainly emphasizes the composition of explosives, but does not clearly control the size of the obtained nano graphite powder, and the problem that the particle size is difficult to control still exists.
In summary, the preparation of the nano graphite powder by the explosion method also needs to study the influence of the reaction parameters, so that the particle size of the nano graphite can be regulated and controlled while the reaction time is shortened, and the nano graphite powder can be better suitable for subsequent application.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a preparation method of nano graphite powder and a method for preparing nano graphite slurry by using the same, wherein the method adopts an explosion method to prepare graphite powder, and the particle size of a product is regulated and controlled by controlling parameters such as gas pressure and the like, so that the product is suitable for the preparation of the subsequent nano graphite slurry, and the obtained slurry is uniform and stable; the method is simple to operate, short in processing time and capable of effectively improving production efficiency.
To achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a method for preparing nano graphite powder, which comprises the following steps:
(1) Placing the explosive column in an explosion container, vacuumizing, and filling protective gas to ensure that the pressure in the explosion container is not higher than 1000Pa;
(2) Detonating the explosive column, reacting in the explosion container, collecting powder in the container after the product subsides, screening and washing to obtain the nano graphite powder.
In the invention, the nano graphite powder is prepared by adopting an explosion method, under the negative oxygen balance condition, the explosive is decomposed to generate free carbon, a series of processes of aggregation, structural rearrangement and the like of carbon atoms are generated under the high temperature and high pressure action of detonation products, the state of the explosive is converted from a gaseous state to a solid state, and the crystal state and the size of the final product depend on factors such as thermodynamic conditions generated by detonation, detonation environment and the like. According to the invention, the particle size of the graphite powder is regulated by controlling the initial protective gas pressure so as to obtain a product with the required particle size, so that the subsequent use is convenient; the method has the advantages of simple operation procedure, short required time and extremely high production efficiency.
The following technical scheme is a preferred technical scheme of the invention, but is not a limitation of the technical scheme provided by the invention, and the technical purpose and beneficial effects of the invention can be better achieved and realized through the following technical scheme.
As a preferable technical scheme of the invention, the grain in the step (1) is a pure TNT grain.
Preferably, the explosion container in the step (1) is a closed container.
In a preferred embodiment of the present invention, the absolute pressure in the explosion container after the evacuation in the step (1) is not higher than 200Pa, for example, 200Pa, 180Pa, 160Pa, 150Pa, 140Pa, 120Pa or 100Pa, but is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
Preferably, the protective gas of step (1) comprises any one or a combination of at least two of nitrogen, carbon dioxide or an inert gas, wherein the inert gas comprises helium, neon or argon, typical but non-limiting examples of such combinations are: a combination of nitrogen and carbon dioxide, a combination of carbon dioxide and argon, a combination of nitrogen, carbon dioxide and neon, a combination of helium, neon and argon, and the like.
Preferably, the absolute pressure in the explosion vessel after the protective gas is filled in step (1) is 200 to 600Pa, for example, 200Pa, 300Pa, 350Pa, 400Pa, 450Pa, 500Pa or 600Pa, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferable technical scheme of the invention, the mode of detonating the grain in the step (2) is ignition detonation or detonator detonation.
Preferably, the waste gas is discharged after the product of the step (2) is settled.
Preferably, the screening in the step (2) is performed by using a screen having a particle size of 100 to 150 mesh, and the undersize is collected, and the mesh size of the screen selected may be 100 mesh, 110 mesh, 120 mesh, 130 mesh, 140 mesh, 150 mesh, or the like, but is not limited to the recited values, and other non-recited values within the range of the recited values are equally applicable.
In the invention, the screening treatment is mainly used for removing residues, sundries and the like of larger particles generated after explosion, and carrying out primary separation.
As a preferred embodiment of the present invention, the washing in the step (2) includes acid washing and water washing which are sequentially performed.
Preferably, the acid used for the acid wash comprises any one or a combination of at least two of hydrochloric acid, sulfuric acid or nitric acid, typical but non-limiting examples of which are: a combination of hydrochloric acid and sulfuric acid, a combination of sulfuric acid and nitric acid, a combination of hydrochloric acid, sulfuric acid and nitric acid, and the like.
In the present invention, the acid washing is actually an acid treatment to remove metal impurities or metal oxide impurities possibly contained in the powder by reaction, so as to obtain pure graphite powder.
Preferably, the water wash is washing the powder with water to neutrality.
As a preferable technical scheme of the invention, the washing in the step (2) further comprises a drying treatment.
The particle diameter of the nano graphite powder obtained in the step (2) is preferably 0.2 to 1. Mu.m, for example, 0.2. Mu.m, 0.3. Mu.m, 0.4. Mu.m, 0.5. Mu.m, 0.6. Mu.m, 0.7. Mu.m, 0.8. Mu.m, 0.9. Mu.m, or 1. Mu.m, etc., but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned value range are applicable.
According to the invention, the graphite powder prepared by the method can control the particle size to be between 0.4 and 0.8 mu m, has smaller particle size and uniform distribution, is easy to disperse in water, and the obtained nano graphite slurry is uniform and stable.
On the other hand, the invention provides a preparation method of nano graphite slurry, wherein the method takes the prepared nano graphite powder as a raw material, and the method comprises the following steps:
mixing a dispersing agent and water, performing sizing treatment, mixing and ball milling the obtained glue solution and the prepared nano graphite powder, and stirring the ball-milled material to obtain nano graphite slurry.
As a preferable technical scheme of the invention, the mass ratio of the dispersing agent to the water is (1-10): (20-80), such as 1:20, 1:40, 1:60, 1:80, 2:20, 2:60, 3:35, 5:20, 6:40, 7:20 or 10:20, etc., but the dispersing agent is not limited to the listed values, and other non-listed values in the numerical range are equally applicable.
Preferably, the dispersant comprises polyvinylpyrrolidone and/or acetone.
Preferably, the sizing treatment is carried out in a ball mill.
Preferably, the time of the sizing treatment is 20 to 80min, for example, 20min, 30min, 40min, 50min, 60min, 70min or 80min, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
According to the invention, the dispersing agent and the solvent can be fully mixed by the sizing treatment, so that the powder can be rapidly dispersed when the powder is mixed with the nano graphite powder later, and the problem that the powder particles are aggregated and difficult to uniformly disperse is avoided.
In a preferred embodiment of the present invention, the mass ratio of the gum solution to the nano graphite powder is (50-100): (1-40), for example, 100:1, 50:1, 50:2, 60:3, 60:5, 70:10, 80:20, 90:30, 100:40 or 50:40, etc., but the present invention is not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
In the invention, the solid content of the nano graphite slurry is one of important parameters, so the mass ratio of the nano graphite powder to the glue solution is a factor for determining the solid content of the nano graphite powder, and the selection of the mass ratio is related to the particle size of the powder particles and the application occasion of the powder particles.
Preferably, the rotation speed of the ball mill is 1200-1500 r/min, for example 1200r/min, 1250r/min, 1280r/min, 1300r/min, 1320r/min, 1350r/min, 1400r/min, 1450r/min, 1500r/min, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the ball milling time is 1 to 4 hours, such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, or 4 hours, etc., but is not limited to the recited values, and other non-recited values within the range are equally applicable.
In a preferred embodiment of the present invention, the rotation speed of the stirring treatment is 1200 to 1800r/min, for example, 1200r/min, 1300r/min, 1400r/min, 1500r/min, 1600r/min, 1700r/min, 1800r/min, etc., but the stirring treatment is not limited to the listed values, and other non-listed values within the range of the values are equally applicable.
Preferably, the stirring treatment is performed for a period of time ranging from 1 to 4 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, or 4 hours, but the stirring treatment is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the nano-graphite slurry is an aqueous nano-graphite slurry.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, the graphite powder is prepared by adopting an explosion method, the particle size of a product is regulated and controlled by controlling the initial gas pressure by utilizing the uniqueness of the reaction condition of the explosion method, and the obtained product has a narrow particle size distribution range and good uniformity;
(2) The particle size characteristics of the nano graphite powder prepared by the method are suitable for preparing nano graphite slurry, and the obtained nano graphite slurry is uniform and stable;
(3) The method has simple operation procedures and short processing time, and can effectively improve the production efficiency.
Drawings
Fig. 1 is an SEM image of the nano graphite powder provided in example 1 of the present invention;
fig. 2 is an SEM image of the nano-graphite slurry provided in example 4 of the present invention.
Detailed Description
For better illustrating the present invention, the technical scheme of the present invention is convenient to understand, and the present invention is further described in detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
The invention provides a preparation method of nano graphite powder, which comprises the following steps:
(1) Placing the explosive column in an explosion container, vacuumizing, and filling protective gas to ensure that the pressure in the explosion container is not higher than 1000Pa;
(2) Detonating the explosive column, reacting in the explosion container, collecting powder in the container after the product subsides, screening and washing to obtain the nano graphite powder.
The following are exemplary but non-limiting examples of the invention:
example 1:
the embodiment provides a preparation method of nano graphite powder, which comprises the following steps:
(1) Placing the explosive column in a closed explosion container, vacuumizing to ensure that the absolute pressure in the explosion container is 150Pa, and then filling nitrogen as protective gas to ensure that the pressure in the explosion container is 400Pa;
(2) Igniting and detonating the explosive column, reacting in the explosive container, discharging waste gas after the product subsides, collecting powder on the inner wall and the bottom of the container, sieving with a 100-mesh sieve to remove large-particle impurities, washing the undersize with hydrochloric acid, washing with water to neutrality, and drying to obtain the nano graphite powder.
The nano graphite powder is subjected to Scanning Electron Microscope (SEM) characterization, and an SEM image is shown in FIG. 1.
In this example, as can be seen from FIG. 1, the particle size of the powder is small and is mainly distributed in the range of 0.4 to 0.8. Mu.m, and the median particle size is about 0.6. Mu.m.
Example 2:
the embodiment provides a preparation method of nano graphite powder, which comprises the following steps:
(1) Placing the explosive column in a closed explosion container, vacuumizing to ensure that the absolute pressure in the explosion container is 100Pa, and then filling argon as protective gas to ensure that the pressure in the explosion container is 300Pa;
(2) Detonating powder column with detonator, reacting in explosion container, discharging waste gas after product subsidence, collecting powder on inner wall and bottom of container, sieving with 150 mesh sieve to remove large particle impurities, washing undersize with sulfuric acid, washing with water to neutrality, and drying to obtain nanometer graphite powder.
In this embodiment, the particle size of the powder is small and is mainly distributed in the range of 0.5-1 μm, and the median particle size is about 0.7 μm.
Example 3:
the embodiment provides a preparation method of nano graphite powder, which comprises the following steps:
(1) Placing the explosive column in a closed explosion container, vacuumizing to ensure that the absolute pressure in the explosion container is 200Pa, and then filling argon as protective gas to ensure that the pressure in the explosion container is 600Pa;
(2) Igniting and detonating the explosive column, reacting in the explosive container, discharging waste gas after the product subsides, collecting powder on the inner wall and the bottom of the container, sieving with a 125-mesh sieve to remove large-particle impurities, washing the undersize with nitric acid, washing with water to neutrality, and drying to obtain the nano graphite powder.
In this embodiment, the particle size of the powder is small and is mainly distributed in the range of 0.2 to 0.6 μm, and the median particle size is about 0.4 μm.
Example 4:
the embodiment provides a preparation method of nano graphite slurry, which adopts nano graphite powder prepared in the embodiment 1 as a raw material and specifically comprises the following steps:
(1) Performing sizing treatment on polyvinylpyrrolidone dispersing agent and water in a mass ratio of 7:60 in a ball mill for 50min to obtain a glue solution;
(2) Adding the nano graphite powder obtained in the example 1 into a ball mill, wherein the mass ratio of the glue solution to the nano graphite powder is 80:10, and ball milling for 2 hours at the rotating speed of 1400 r/min;
(3) And stirring the ball-milled material for 3 hours at a stirring rotation speed of 1500r/min to obtain the water-based nano graphite slurry.
The aqueous nano-graphite slurry is subjected to scanning electron microscope characterization, and an SEM (scanning electron microscope) diagram of the aqueous nano-graphite slurry is shown in FIG. 2.
In this example, as can be seen from fig. 2, the particle size of the graphite slurry is small, the particle size is mainly distributed in the range of 0.2-0.6 μm, and the slurry has good dispersibility, uniform concentration and good stability.
Example 5:
the embodiment provides a preparation method of nano graphite slurry, which adopts nano graphite powder prepared in the embodiment 2 as a raw material and specifically comprises the following steps:
(1) Performing sizing treatment on an acetone dispersing agent and water in a mass ratio of 2:50 in a ball mill for 20min to obtain a glue solution;
(2) Adding the nano graphite powder obtained in the example 2 into a ball mill, wherein the mass ratio of the glue solution to the nano graphite powder is 70:4, and ball milling for 4 hours at the rotating speed of 1200 r/min;
(3) Stirring the ball-milled material for 1h at a stirring rotation speed of 1800r/min to obtain the water-based nano graphite slurry.
In the embodiment, the particle size of the graphite slurry is smaller, the particle size is mainly distributed in the range of 0.4-0.8 mu m, and the slurry has good dispersibility, uniform concentration and good stability.
Example 6:
the embodiment provides a preparation method of nano graphite slurry, which adopts nano graphite powder prepared in the embodiment 3 as a raw material and specifically comprises the following steps:
(1) Performing sizing treatment on polyvinylpyrrolidone dispersing agent and water in a mass ratio of 9:30 in a ball mill for 80min to obtain a glue solution;
(2) Adding the nano graphite powder obtained in the example 3 into a ball mill, wherein the mass ratio of the glue solution to the nano graphite powder is 60:30, and ball milling for 1h at the rotating speed of 1500 r/min;
(3) And stirring the ball-milled material for 4 hours at a stirring rotation speed of 1200r/min to obtain the water-based nano graphite slurry.
In the embodiment, the particle size of the graphite slurry is smaller, the particle size is mainly distributed in the range of 0.2-0.5 mu m, and the slurry has good dispersibility, uniform concentration and good stability.
According to the embodiment, the method adopts an explosion method to prepare the graphite powder, and utilizes the uniqueness of the reaction condition of the explosion method to control the initial gas pressure to regulate and control the particle size of the product, so that the obtained product has narrow particle size distribution range and good uniformity; the particle size characteristics of the prepared nano graphite powder are suitable for preparing nano graphite slurry, and the obtained nano graphite slurry is uniform and stable; the method has the advantages of simple operation procedure and short processing time, and can effectively improve the production efficiency.
The applicant states that the detailed apparatus and method of the present invention are described by the above embodiments, but the present invention is not limited to the detailed apparatus and method, i.e., it does not mean that the present invention must be implemented by the detailed apparatus and method. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions for the apparatus of the present invention, addition of auxiliary apparatus, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
Claims (21)
1. The preparation method of the nano graphite powder is characterized by comprising the following steps of:
(1) Placing the explosive column in an explosion container, vacuumizing, and filling protective gas to ensure that the pressure in the explosion container is not higher than 1000Pa;
(2) Detonating explosive column, reacting in explosive container, collecting powder in container after product subsides, screening and washing, the screening is to screen with 100-150 mesh sieve, collecting undersize to obtain nano graphite powder with 0.2-1 μm particle size.
2. The method of claim 1, wherein the cartridge of step (1) is a pure TNT cartridge.
3. The method of claim 1, wherein the detonation vessel of step (1) is a closed vessel.
4. The method of claim 1, wherein the absolute pressure in the detonation vessel after the evacuation in step (1) is not higher than 200Pa.
5. The method of claim 1, wherein the protective gas of step (1) comprises any one or a combination of at least two of nitrogen, carbon dioxide, or an inert gas.
6. The method according to claim 1, wherein the absolute pressure in the explosion vessel after the protective gas is filled in the step (1) is 200 to 600Pa.
7. The method of claim 1, wherein the step (2) detonates the cartridge in a firing or detonator firing manner.
8. The process of claim 1, wherein the step (2) is followed by settling and then removing the effluent.
9. The method according to claim 1, wherein the washing in step (2) comprises acid washing and water washing performed sequentially.
10. The method of claim 9, wherein the acid used for the acid washing comprises any one or a combination of at least two of hydrochloric acid, sulfuric acid, and nitric acid.
11. The method of claim 9, wherein the water washing is washing the powder with water to neutrality.
12. The method according to claim 1, further comprising a drying treatment after the washing in the step (2).
13. A method of preparing a nano-graphite slurry, the method comprising preparing a nano-graphite powder according to any one of claims 1-12, further comprising:
mixing a dispersing agent and water, and then performing sizing treatment, wherein the mass ratio of the dispersing agent to the water is (1-10) (20-80), the obtained glue solution and the nano graphite powder are mixed and ball-milled, the mass ratio of the glue solution to the nano graphite powder is (50-100) (1-40), and the ball-milled material is stirred to obtain the nano graphite slurry.
14. The method of preparation according to claim 13, wherein the dispersant comprises polyvinylpyrrolidone and/or acetone.
15. The method according to claim 13, wherein the sizing treatment is performed in a ball mill.
16. The method according to claim 13, wherein the time of the sizing treatment is 20 to 80 minutes.
17. The method according to claim 13, wherein the rotational speed of the ball mill is 1200-1500 r/min.
18. The method of claim 13, wherein the ball milling is performed for a period of 1 to 4 hours.
19. The method according to claim 13, wherein the stirring treatment is performed at a rotation speed of 1200 to 1800r/min.
20. The method according to claim 13, wherein the stirring treatment is performed for 1 to 4 hours.
21. The method of claim 13, wherein the nano-graphite slurry is an aqueous nano-graphite slurry.
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