CN112850688A - Preparation method of nanoscale carbon material - Google Patents
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Abstract
The invention discloses a preparation method of a nano-scale carbon material, and relates to the technical field of nano-carbon material preparation. The preparation method of the nanoscale carbon material comprises the following raw materials in parts by weight: 10-50 parts of hydrocarbon, 10-50 parts of oxygen-containing element compound and 1-3 parts of transition metal, and comprises eight steps of raw material dilution, solution mixing, raw material crystallization, grinding into powder, high-temperature reaction, taking out and soaking, drying and grinding. According to the preparation method of the nanoscale carbon material, in the preparation process, any catalyst does not need to be added, so that impurities in the catalyst are prevented from influencing the quality and performance of the finished product of the nanoscale carbon material, the stability of the prepared nanoscale carbon material is improved, the raw materials are mixed more uniformly, the raw materials are separated out by using a crystallization method after mixing, purer raw materials are obtained, the molecular gaps among the raw materials can be effectively reduced, the raw materials are mixed more uniformly and more pure, and the quality of the finished product of the nanoscale carbon material is improved.
Description
Technical Field
The invention relates to the technical field of nano carbon material preparation, in particular to a preparation method of a nano carbon material.
Background
The nano carbon material is a carbon material with a dispersion phase size of at least one dimension less than 100nm, the nano carbon material mainly comprises three types of carbon nano tubes, carbon nano fibers and nano carbon spheres, most of the preparation processes of partial nano carbon materials in the traditional nano carbon material preparation process need catalysts, the catalysts contain impurities, the quality and the performance of finished nano carbon materials are influenced, the reaction temperature needs to be controlled in the preparation process, the requirements on preparation equipment are high, the preparation cost is greatly increased, the preparation efficiency is low, the nano carbon material is not suitable for mass production, the requirements of markets on the nano carbon materials cannot be met, and therefore the nano carbon material is not convenient to popularize and use.
Disclosure of Invention
Technical problem to be solved
The invention aims to provide a preparation method of a nano-scale carbon material, which has the advantages of good stability, no impurities in a catalyst and low preparation cost, and solves the problems in the background technology.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a nanoscale carbon material comprises the following raw materials in parts by weight: 10-50 parts of hydrocarbon, 10-50 parts of oxygen-containing element compound and 1-3 parts of transition metal, and the preparation method comprises the following steps:
s1, raw material dilution: putting the corresponding parts of hydrocarbon into a container containing water, stirring, controlling the temperature to be 20-30 ℃, stopping adding the hydrocarbon when the solution is saturated, putting the corresponding parts of oxygen-containing element compound into the container containing water, stirring, controlling the temperature to be 20-30 ℃, and stopping adding the oxygen-containing element compound when the solution is saturated;
s2, mixing the solution: preparing a clean container, pouring two groups of diluted raw material solutions, and stirring the mixed solution, wherein the temperature is controlled to be 20-30 ℃ during stirring, and the stirring time is 5-10 minutes, so that the two solutions are uniformly mixed for later use;
s3, raw material crystallization: heating the mixed principle solution at 80-100 ℃ for 5-10 minutes, evaporating half of water, cooling, reducing the temperature along with the reduction of the temperature, reducing the solubility of the raw material, enabling the solution to reach a supersaturated state, further precipitating crystals, and filtering the precipitated crystals to obtain a product;
s4, grinding into powder: putting the crystal obtained in the step S3 into a drying box, setting the temperature of the drying box to be 80-100 ℃, drying for 5-10 minutes, removing water in the raw material, taking out and cooling for 1-2 hours, and putting the dried raw material into a grinding machine to be made into powder;
s5, high-temperature reaction: firstly putting the transition metal on a corundum boat, then putting the corundum boat into a muffle furnace, blowing the raw material powder ground in S4 into the muffle furnace by using protective gas, and then controlling the temperature of the muffle furnace to be 300-700 ℃ to react for 0.5-1 hour;
s6, taking out and soaking: after the reaction is finished, taking out the transition metal, preparing a container, pouring distilled water, putting the taken-out transition metal into a soaking pool, stirring soaking liquid of the transition metal once every 10-15 minutes during soaking, controlling the temperature at 20-30 ℃ during stirring, and taking out the transition metal;
s7, drying: opening the drying box, then putting the product solution obtained in the step S6 into the drying box, setting the temperature of the drying box at 80-100 ℃, and drying for 1-2 hours to obtain a dried product;
s8, grinding: and (4) putting the dried product obtained in the step (S7) into a grinding machine, and regulating the rotating speed of the grinding machine to be 300-500r/min, wherein the grinding time is 10-20 minutes, so as to obtain the powdery nanoscale carbon material.
Preferably, the hydrocarbon in S1 is any one of a free chain saturated hydrocarbon, a chain unsaturated hydrocarbon, a cyclic saturated hydrocarbon, an aromatic hydrocarbon, an alcohol, and an ether.
Preferably, the oxygen compound in S1 is any one of acetaldehyde, ethylene oxide, ethylene glycol, formaldehyde, water and hydrogen peroxide.
Preferably, the stirring time in the S1 is 10-20 minutes.
Preferably, the temperature of the S3 is reduced to 0-20 ℃ and kept for 20-30 minutes.
Preferably, the rotation speed of the grinder in S4 is 100-200r/min, and the grinding time is 10-20 minutes.
Preferably, the protective gas in S5 is any one of nitrogen or argon.
Preferably, the transition metal is completely immersed in the water in the step S6 for 1 to 2 hours, so that the product on the transition metal is completely dropped in the water.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of a nanoscale carbon material, which has the following beneficial effects:
1. the preparation method of the nano-scale carbon material does not need to add any catalyst in the preparation process, thereby preventing impurities in the catalyst from influencing the quality and performance of the finished product of the nano-scale carbon material, increasing the stability of the prepared nano-scale carbon material, uniformly mixing raw material compounds in the preparation process, enabling the raw materials to be more uniformly mixed, separating out the raw materials by using a crystallization method after mixing to obtain purer raw materials, effectively reducing the molecular gap between the raw materials, enabling the raw materials to be more uniformly mixed and purer, increasing the quality of the finished product of the nano-scale carbon material, simultaneously increasing the precision of the finished product of the nano-scale carbon material, blowing the raw materials into a muffle furnace by using protective gas, increasing the pressure in the muffle furnace, promoting the yield of the nano-scale carbon material, and simultaneously facilitating the dispersing and adding of the raw materials, the high-temperature reaction of the raw materials is more thorough, and the yield of the nano-scale carbon material is increased.
2. According to the preparation method of the nanoscale carbon material, in the preparation process, the prepared nanoscale carbon material has high applicability, the preparation efficiency of the nanoscale carbon material is high, the preparation method is suitable for mass production, the requirement on reaction equipment is low, the added raw materials are easy to obtain, the preparation cost can be effectively reduced, the popularization and the use are convenient, the operation method is simple, the preparation time of the nanoscale carbon material can be saved, the prepared nanoscale carbon material can meet the market requirement on the nanoscale carbon material, the popularization is convenient, and the plasticity of the preparation method is increased.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows: a preparation method of a nanoscale carbon material comprises the following raw materials in parts by weight: 10 parts of hydrocarbon, 10 parts of oxygen-containing element compound and 1 part of transition metal, and the preparation method comprises the following steps:
step one, diluting raw materials: putting a corresponding part of hydrocarbon into a container containing water, wherein the hydrocarbon is any one of free chain saturated hydrocarbon, chain unsaturated hydrocarbon, cyclic saturated hydrocarbon, aromatic hydrocarbon, alcohol and ether, stirring the hydrocarbon, controlling the temperature to be 20 ℃, stopping adding the hydrocarbon until the solution is saturated, putting a corresponding part of oxygen-containing element compound into the container containing water, and stirring the oxygen-containing element compound for 10 minutes, controlling the temperature to be 20 ℃, and stopping adding the oxygen-containing element compound until the solution is saturated;
step two, solution mixing: preparing a clean container, pouring two groups of diluted raw material solutions, and stirring the mixed solution, wherein the temperature is controlled to be 20 ℃ during stirring, and the stirring time is 5 minutes, so that the two solutions are uniformly mixed for later use;
step three, raw material crystallization: heating the mixed principle solution at 80 ℃ for 5 minutes, evaporating half of water, cooling, reducing the temperature to 0 ℃, keeping the temperature for 20 minutes, reducing the solubility of the raw materials along with the temperature reduction, enabling the solution to reach a supersaturated state, further precipitating crystals, and filtering the precipitated crystals to obtain a product;
step four, grinding into powder: putting the crystal obtained in the step three into a drying box, setting the temperature of the drying box to be 80 ℃, drying for 5 minutes, removing water in the raw material, taking out and cooling for 1 hour, putting the dried raw material into a grinding machine, and making the raw material into powder, wherein the rotating speed of the grinding machine is 100r/min, and the grinding time is 10 minutes;
step five, high-temperature reaction: putting the transition metal on a corundum boat, then putting the corundum boat into a muffle furnace, blowing the raw material powder ground in the fourth step into the muffle furnace by using protective gas, wherein the protective gas is any one of nitrogen or argon, and then controlling the temperature of the muffle furnace to be 300 ℃ to react for 0.5 hour;
step six, taking out and soaking: after the reaction is finished, taking out the transition metal, preparing a container, pouring distilled water, soaking the taken-out transition metal in the container to ensure that the transition metal is completely immersed in the water, completely removing products on the transition metal in the water when the soaking time is 1 hour, stirring the soaking solution in the soaking process, stirring once every 10 minutes, controlling the temperature during stirring to be 20 ℃, and then taking out the transition metal;
step seven, drying: opening a drying box, then putting the product solution obtained in the step six into the drying box, setting the temperature of the drying box to be 80 ℃, and drying for 1 hour to obtain a dried product;
step eight, grinding: and putting the dried product obtained in the seventh step into a grinding machine, and regulating the rotating speed of the grinding machine to 300r/min for 10 minutes to obtain the powdery nanoscale carbon material.
Example two: a preparation method of a nanoscale carbon material comprises the following raw materials in parts by weight: 30 parts of hydrocarbon, 30 parts of oxygen-containing element compound and 2 parts of transition metal, and the preparation method comprises the following steps:
step one, diluting raw materials: putting a corresponding part of hydrocarbon into a container containing water, wherein the hydrocarbon is any one of free chain saturated hydrocarbon, chain unsaturated hydrocarbon, cyclic saturated hydrocarbon, aromatic hydrocarbon, alcohol and ether, stirring the hydrocarbon, controlling the temperature to be 25 ℃, stopping adding the hydrocarbon until the solution is saturated, putting a corresponding part of oxygen-containing element compound into the container containing water, and stirring the oxygen-containing element compound for 15 minutes, controlling the temperature to be 25 ℃, and stopping adding the oxygen-containing element compound until the solution is saturated;
step two, solution mixing: preparing a clean container, pouring two groups of diluted raw material solutions, and stirring the mixed solution, wherein the temperature is controlled to be 25 ℃ during stirring, and the stirring time is 7.5 minutes, so that the two solutions are uniformly mixed for later use;
step three, raw material crystallization: heating the mixed principle solution at 90 ℃ for 7.5 minutes, evaporating half of water, cooling, reducing the temperature to 10 ℃, keeping the temperature for 25 minutes, reducing the solubility of the raw materials along with the temperature reduction, enabling the solution to reach a supersaturated state, further precipitating crystals, and filtering the precipitated crystals to obtain a product;
step four, grinding into powder: putting the crystal obtained in the step three into a drying box, setting the temperature of the drying box to be 90 ℃, drying for 7.5 minutes, removing water in the raw material, taking out and cooling for 1.5 hours, putting the dried raw material into a grinding machine, and making the raw material into powder, wherein the rotating speed of the grinding machine is 150r/min, and the grinding time is 15 minutes;
step five, high-temperature reaction: putting the transition metal on a corundum boat, then putting the corundum boat into a muffle furnace, blowing the raw material powder ground in the fourth step into the muffle furnace by using protective gas, wherein the protective gas is any one of nitrogen or argon, and then controlling the temperature of the muffle furnace to be 500 ℃ to react for 0.75 hour;
step six, taking out and soaking: after the reaction is finished, taking out the transition metal, preparing a container, pouring distilled water, soaking the taken-out transition metal in the distilled water for 1.5 hours to ensure that the product on the transition metal is completely removed from the distilled water, stirring the soaking solution in the soaking process, stirring once every 15 minutes, controlling the temperature during stirring to be 25 ℃, and then taking out the transition metal;
step seven, drying: opening a drying box, then putting the product solution obtained in the step six into the drying box, setting the temperature of the drying box to be 90 ℃, and drying for 1.5 hours to obtain a dried product;
step eight, grinding: and putting the dried product obtained in the seventh step into a grinding machine, and regulating the rotating speed of the grinding machine to 400r/min for 15 minutes to obtain the powdery nanoscale carbon material.
Example three: a preparation method of a nanoscale carbon material comprises the following raw materials in parts by weight: 50 parts of hydrocarbon, 50 parts of oxygen-containing element compound and 3 parts of transition metal, and the preparation method comprises the following steps:
step one, diluting raw materials: putting a corresponding part of hydrocarbon into a container containing water, wherein the hydrocarbon is any one of free chain saturated hydrocarbon, chain unsaturated hydrocarbon, cyclic saturated hydrocarbon, aromatic hydrocarbon, alcohol and ether, stirring the hydrocarbon, controlling the temperature to be 30 ℃, stopping adding the hydrocarbon until the solution is saturated, putting a corresponding part of oxygen-containing element compound into the container containing water, and stirring the oxygen-containing element compound for 20 minutes, controlling the temperature to be 30 ℃, and stopping adding the oxygen-containing element compound until the solution is saturated;
step two, solution mixing: preparing a clean container, pouring two groups of diluted raw material solutions, and stirring the mixed solution, wherein the temperature is controlled at 30 ℃ during stirring, and the stirring time is 10 minutes, so that the two solutions are uniformly mixed for later use;
step three, raw material crystallization: heating the mixed principle solution at 100 ℃ for 10 minutes, evaporating half of water, cooling to 20 ℃, keeping the temperature for 30 minutes, reducing the solubility of the raw materials along with the temperature reduction, enabling the solution to reach a supersaturated state, further precipitating crystals, and filtering the precipitated crystals to obtain a product;
step four, grinding into powder: putting the crystal obtained in the step three into a drying box, setting the temperature of the drying box to be 100 ℃, drying for 10 minutes, removing water in the raw material, taking out and cooling for 2 hours, putting the dried raw material into a grinding machine, and making the raw material into powder, wherein the rotating speed of the grinding machine is 200r/min, and the grinding time is 20 minutes;
step five, high-temperature reaction: putting the transition metal on a corundum boat, then putting the corundum boat into a muffle furnace, blowing the raw material powder ground in the fourth step into the muffle furnace by using protective gas, wherein the protective gas is any one of nitrogen or argon, and then controlling the temperature of the muffle furnace to be 700 ℃ to react for 1 hour;
step six, taking out and soaking: after the reaction is finished, taking out the transition metal, preparing a container, pouring distilled water, soaking the taken-out transition metal in the container for 2 hours to completely remove the product on the transition metal in the water, stirring the soaking solution in the soaking process once every 20 minutes, controlling the temperature during stirring to be 30 ℃, and then taking out the transition metal;
step seven, drying: opening a drying box, then putting the product solution obtained in the step six into the drying box, setting the temperature of the drying box to be 100 ℃, and drying for 2 hours to obtain a dried product;
step eight, grinding: and (5) putting the dried product obtained in the step seven into a grinding machine, regulating the rotating speed of the grinding machine to 500r/min, and grinding for 20 minutes to obtain the powdery nanoscale carbon material.
It can be seen from this that: in the traditional preparation process of the nano-scale carbon material, most of the preparation processes of partial nano-scale carbon materials need catalysts, the catalysts contain impurities, the quality and the performance of finished products of the nano-scale carbon materials are influenced, the reaction temperature needs to be controlled in the preparation process, the requirements on preparation equipment are higher, the preparation cost is greatly increased, the method is not suitable for mass production, and the requirements of markets on the nano-scale carbon materials cannot be met, so the method is inconvenient to popularize and use, and the efficiency in preparation is low. The raw materials are separated out to obtain purer raw materials, the molecular gap between the raw materials can be effectively reduced, the mixing is more uniform, the raw materials are purer, the finished product quality of the nano-scale carbon material is improved, the finished product precision of the nano-scale carbon material is improved, the raw materials are blown into a muffle furnace by utilizing the protective gas, the pressure in the muffle furnace can be increased, the yield of the nano-scale carbon material is promoted, the raw materials are conveniently added in a dispersing way, the high-temperature reaction of the raw materials is more thorough, the yield of the nano-scale carbon material is increased, the prepared nano-scale carbon material has high applicability, the efficiency for preparing the nano-scale carbon material is high, the nano-scale carbon material is suitable for mass production, the requirement on reaction equipment is low, the added raw materials are easy to obtain, the preparation cost can be effectively reduced, the popularization and the use are convenient, meanwhile, and the prepared nano-scale carbon material can meet the requirement of the market on the nano-scale carbon material, is convenient to popularize and increases the plasticity of the preparation method.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for preparing a nanoscale carbon material is characterized by comprising the following steps: the composite material comprises the following raw materials in parts by weight: 10-50 parts of hydrocarbon, 10-50 parts of oxygen-containing element compound and 1-3 parts of transition metal, and the preparation method comprises the following steps:
s1, raw material dilution: putting the corresponding parts of hydrocarbon into a container containing water, stirring, controlling the temperature to be 20-30 ℃, stopping adding the hydrocarbon when the solution is saturated, putting the corresponding parts of oxygen-containing element compound into the container containing water, stirring, controlling the temperature to be 20-30 ℃, and stopping adding the oxygen-containing element compound when the solution is saturated;
s2, mixing the solution: preparing a clean container, pouring two groups of diluted raw material solutions, and stirring the mixed solution, wherein the temperature is controlled to be 20-30 ℃ during stirring, and the stirring time is 5-10 minutes, so that the two solutions are uniformly mixed for later use;
s3, raw material crystallization: heating the mixed principle solution at 80-100 ℃ for 5-10 minutes, evaporating half of water, cooling, reducing the temperature along with the reduction of the temperature, reducing the solubility of the raw material, enabling the solution to reach a supersaturated state, further precipitating crystals, and filtering the precipitated crystals to obtain a product;
s4, grinding into powder: putting the crystal obtained in the step S3 into a drying box, setting the temperature of the drying box to be 80-100 ℃, drying for 5-10 minutes, removing water in the raw material, taking out and cooling for 1-2 hours, and putting the dried raw material into a grinding machine to be made into powder;
s5, high-temperature reaction: firstly putting the transition metal on a corundum boat, then putting the corundum boat into a muffle furnace, blowing the raw material powder ground in S4 into the muffle furnace by using protective gas, and then controlling the temperature of the muffle furnace to be 300-700 ℃ to react for 0.5-1 hour;
s6, taking out and soaking: after the reaction is finished, taking out the transition metal, preparing a container, pouring distilled water, putting the taken-out transition metal into a soaking pool, stirring soaking liquid of the transition metal once every 10-15 minutes during soaking, controlling the temperature at 20-30 ℃ during stirring, and taking out the transition metal;
s7, drying: opening the drying box, then putting the product solution obtained in the step S6 into the drying box, setting the temperature of the drying box at 80-100 ℃, and drying for 1-2 hours to obtain a dried product;
s8, grinding: and (4) putting the dried product obtained in the step (S7) into a grinding machine, and regulating the rotating speed of the grinding machine to be 300-500r/min, wherein the grinding time is 10-20 minutes, so as to obtain the powdery nanoscale carbon material.
2. The method for producing a nanosized carbon material according to claim 1, wherein: the hydrocarbon in S1 is any one of a free chain saturated hydrocarbon, a chain unsaturated hydrocarbon, a cyclic saturated hydrocarbon, an aromatic hydrocarbon, an alcohol, and an ether.
3. The method for producing a nanosized carbon material according to claim 2, wherein: the oxygen element compound in the S1 is any one of acetaldehyde, ethylene oxide, ethylene glycol, formaldehyde, water and hydrogen peroxide.
4. The method for producing a nanosized carbon material according to claim 3, wherein: the stirring time in the S1 is 10-20 minutes.
5. The method for producing a nanosized carbon material according to claim 1, wherein: and S3, reducing the temperature to 0-20 ℃, and keeping the temperature for 20-30 minutes.
6. The method for producing a nanosized carbon material according to claim 1, wherein: the rotation speed of the grinder in the S4 is 100-200r/min, and the grinding time is 10-20 minutes.
7. The method for producing a nanosized carbon material according to claim 1, wherein: the protective gas in the S5 is nitrogen or argon.
8. The method for producing a nanosized carbon material according to claim 1, wherein: and in the S6, the transition metal is completely immersed in the water for 1-2 hours, so that the product on the transition metal is completely dropped into the water.
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Application publication date: 20210528 |