CN112429728A - Preparation method of graphene material suitable for cold spraying - Google Patents
Preparation method of graphene material suitable for cold spraying Download PDFInfo
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Abstract
The invention relates to a preparation method of a graphene material suitable for cold spraying, which comprises the following steps: comprises a step 1, a step 2, a step 3 and a step 4. And 3, continuously heating the mixture obtained in the third step, adding an initiator, a coagulant and a silane coupling agent, evaporating to remove an organic solvent, heating to completely solidify the high molecular polymer, fully stirring and granulating in the heating process to obtain the graphite composite material with the surface coated with the high molecular polymer, cooling to room temperature, and carrying out conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer cooled in the third step. The invention has the advantages of ensuring that the polymer is completely coated on the graphite surface and ensuring that the coating amount is the same each time.
Description
Technical Field
The invention relates to the technical field of preparation methods of graphene materials, in particular to a preparation method of a graphene material suitable for cold spraying.
Background
Graphene (Graphene) is a two-dimensional honeycomb crystal structure formed by closely arranging sp2 hybridized carbon atoms, and belongs to graphite materials. The material has excellent Young modulus (1100GPa), high thermal conductivity (about 5000J. (m · K · s) & lt-1 & gt), high carrier mobility (2 x 105cm 2. (V · s) & lt-1 & gt), high specific surface area (a theoretical calculation value of 2630m2 · g < -1 >), quantum Hall effect, quantum tunneling effect, excellent impermeability and the like, so that the material has great application prospect in the fields of electronic devices, composite materials, functional coatings and the like. However, graphene is very easy to agglomerate due to strong pi-pi interaction and van der waals force between layers, and the excellent performance of graphene is related to the number of layers; in addition, graphene can only be dispersed in a few solvents with extremely strong polarity, and most of the solvents are toxic and are not beneficial to the sustainable development of the environment and people, so that the application of graphene is greatly limited. Therefore, the dispersibility of the graphene in common organic solvents and inorganic solvents is simply and efficiently improved, and the method has very important practical significance for the application of the graphene.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a graphene material suitable for cold spraying, which has the advantages of ensuring that a polymer is completely coated on the surface of graphite and ensuring that the coating amount is the same each time.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a graphene material suitable for cold spraying is characterized by comprising the following steps: the method comprises the following steps:
step 1: pre-oxidizing graphene, namely weighing phosphorus pentoxide, potassium persulfate and concentrated sulfuric acid, sealing the phosphorus pentoxide, the potassium persulfate and the concentrated sulfuric acid in a container, heating the mixture in a water bath to 75-85 ℃, stirring the mixture in the water bath until the raw materials are completely dissolved, slowly adding the graphene in a small amount for multiple times, keeping the temperature for reaction for 4-8h, washing the mixture to be neutral by using deionized water after the reaction is finished, and drying the mixture for 20-28h at 40-60 ℃ for later use, wherein the weight ratio of the phosphorus pentoxide to the potassium persulfate to the concentrated sulfuric acid to the graphite powder is 8: 2: 30: 15, dissolving the pre-oxidized graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05-0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% -7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: (18-22);
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1-2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
Preferably, the high molecular polymer is epoxy resin.
Preferably, zinc oxide and calcium oxide are further added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
In conclusion, the invention has the following beneficial effects:
the invention combines the dipping and the solvent evaporation treatment in the heating and curing process, thereby simplifying the process; the prepared modified graphene solution does not agglomerate, does not need crushing treatment, reduces equipment investment and is beneficial to large-scale production; the modified graphite, especially the modified natural graphite, as the carbon negative electrode material has longer cycle life and better heavy current discharge performance, and zinc oxide and calcium oxide are added to enhance the overall physical performance.
Detailed Description
The present invention is further explained.
Example 1: a preparation method of a graphene material suitable for cold spraying comprises the following steps:
step 1: pre-oxidizing graphene, namely weighing phosphorus pentoxide, potassium persulfate and concentrated sulfuric acid, sealing the phosphorus pentoxide, the potassium persulfate and the concentrated sulfuric acid in a container, heating the mixture in a water bath to 75-85 ℃, stirring the mixture in the water bath until the raw materials are completely dissolved, slowly adding the graphene in a small amount for multiple times, keeping the temperature for reaction for 4-8h, washing the mixture to be neutral by using deionized water after the reaction is finished, and drying the mixture for 20-28h at 40-60 ℃ for later use, wherein the weight ratio of the phosphorus pentoxide to the potassium persulfate to the concentrated sulfuric acid to the graphite powder is 8: 2: 30: 15, dissolving the pre-oxidized graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 18;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
Example 2: a preparation method of a graphene material suitable for cold spraying comprises the following steps:
step 1: pre-oxidizing graphene, namely weighing phosphorus pentoxide, potassium persulfate and concentrated sulfuric acid, sealing the phosphorus pentoxide, the potassium persulfate and the concentrated sulfuric acid in a container, heating the mixture in a water bath to 75-85 ℃, stirring the mixture in the water bath until the raw materials are completely dissolved, slowly adding the graphene in a small amount for multiple times, keeping the temperature for reaction for 4-8h, washing the mixture to be neutral by using deionized water after the reaction is finished, and drying the mixture for 20-28h at 40-60 ℃ for later use, wherein the weight ratio of the phosphorus pentoxide to the potassium persulfate to the concentrated sulfuric acid to the graphite powder is 8: 2: 30: 15, dissolving the pre-oxidized graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.1% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 6% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 20;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1.5 percent of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
Example 3: a preparation method of a graphene material suitable for cold spraying comprises the following steps:
step 1: pre-oxidizing graphene, namely weighing phosphorus pentoxide, potassium persulfate and concentrated sulfuric acid, sealing the phosphorus pentoxide, the potassium persulfate and the concentrated sulfuric acid in a container, heating the mixture in a water bath to 75-85 ℃, stirring the mixture in the water bath until the raw materials are completely dissolved, slowly adding the graphene in a small amount for multiple times, keeping the temperature for reaction for 4-8h, washing the mixture to be neutral by using deionized water after the reaction is finished, and drying the mixture for 20-28h at 40-60 ℃ for later use, wherein the weight ratio of the phosphorus pentoxide to the potassium persulfate to the concentrated sulfuric acid to the graphite powder is 8: 2: 30: 15, dissolving the pre-oxidized graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% -7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: 22;
and step 3: continuously heating the mixture obtained in the step two, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (4) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after cooling.
The high molecular polymer is epoxy resin.
Zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
The modified graphite obtained was used as a negative electrode, lithium cobaltate was used as a positive electrode, and a solution of 1M-LiPF6 EC, DMC, EMC 1:1 was used as an electrolyte to prepare a full cell, in which the 3C discharge capacity was 85% of the 0.5C discharge capacity, the 2C discharge capacity was 95% of the 0.5C discharge capacity, and the capacity retention rate was 91% after charging and discharging at 1C for 300 weeks.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the design concept of the present invention should be included in the scope of the present invention.
Claims (3)
1. A preparation method of a graphene material suitable for cold spraying is characterized by comprising the following steps: the method comprises the following steps:
step 1: pre-oxidizing graphene, namely weighing phosphorus pentoxide, potassium persulfate and concentrated sulfuric acid, sealing the phosphorus pentoxide, the potassium persulfate and the concentrated sulfuric acid in a container, heating the mixture in a water bath to 75-85 ℃, stirring the mixture in the water bath until the raw materials are completely dissolved, slowly adding the graphene in a small amount for multiple times, keeping the temperature for reaction for 4-8h, washing the mixture to be neutral by using deionized water after the reaction is finished, and drying the mixture for 20-28h at 40-60 ℃ for later use, wherein the weight ratio of the phosphorus pentoxide to the potassium persulfate to the concentrated sulfuric acid to the graphite powder is 8: 2: 30: 15, dissolving the pre-oxidized graphene solution in water to obtain a graphene solution, adding a dispersing agent and a high molecular polymer, and mixing and stirring to obtain a graphene dispersion solution, wherein the using amount of the dispersing agent is 0.05-0.2% of the mass of the graphene solution;
step 2: adding an acrylamide monomer and a cross-linking agent into the graphene dispersion liquid, mixing and stirring, and preheating to obtain a preheated solution, wherein the dosage of the acrylamide monomer is 5% -7% of the mass of the graphene dispersion liquid; the molar ratio of the cross-linking agent to the acrylamide monomer is 1: (18-22);
and step 3: continuously heating the mixture obtained in the step 2, and adding an initiator, a coagulant and a silane coupling agent, wherein the initiator is a persulfate initiator, the coagulant is tetramethylethylenediamine, and the dosage of the initiator is 1-2% of the total mass of the acrylamide monomer and the crosslinking agent; the using amount of the coagulant is 0.05 percent of the volume of the preheating solution, wherein the mass ratio of the graphene dispersion liquid to the boric acid is 100:2, the organic solvent is evaporated, then the temperature is raised to completely solidify the high molecular polymer, the graphite composite material with the surface coated with the high molecular polymer is obtained by fully stirring and granulating in the temperature raising process, and the graphite composite material is cooled to the room temperature;
and 4, step 4: and (3) performing conventional carbonization treatment on the graphite composite material with the surface coated with the high molecular polymer after being cooled in the step (3).
2. The method for preparing the graphene material suitable for cold spraying according to claim 1, wherein the method comprises the following steps: the high molecular polymer is epoxy resin.
3. The method for preparing the graphene material suitable for cold spraying according to claim 1, wherein the method comprises the following steps: zinc oxide and calcium oxide are also added in the step 3, wherein the mass ratio of the graphene dispersion liquid to the zinc oxide and the calcium oxide is 100:1: 1.
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