Preparation method of carbon powder and amino acid ion composite material

Abstract

The invention discloses a carbon powder and amino acid ion composite material preparation method, which comprises: carbon powder activation: taking carbon powder with uniform particle size and a silane coupling agent, adding into a reaction container according to a mass ratio of 1: (0.05-0.2), adding absolute ethyl alcohol with the use amount of 5-10 times of the mass of the carbon powder, mixing, and stirring by using a stirrer to obtain a mixture A; stirring and reacting for 1-3 hours under the constant-temperature water bath condition of 50-70 DEG C; after the reaction is finished, carrying out vacuum filtration by adopting a Buchner funnel, putting a filter cake into an air dry oven, and drying at 60-75 DEG C for 4-6 hours to remove a residual solvent, so as to obtain surface-modified activated carbon powder; the invention relates to the technical field of composite materials. According to the preparation method of the carbon powder and amino acid ion composite material, amino acid and an alkali reagent react to prepare an amino acid ion liquid, and in the step S2, the high purity and stability of the ion liquid are ensured by accurately controlling the pH value and reaction conditions.

Description

Technical Field

[0001] This invention relates to the field of composite material technology, specifically to a method for preparing a carbon powder and amino acid ion composite material. Background Technology

[0002] With the rapid development of new energy, environmental protection, and biomedicine, the demand for high-performance functional materials is increasing. Carbon materials, especially carbon nanoparticles, have shown great application potential in electrochemical energy storage, catalysis, adsorption, and sensors due to their advantages such as high specific surface area, excellent conductivity, stable chemical properties, and wide availability. However, untreated carbon powder has a chemically inert surface and strong van der Waals forces between particles, making it prone to agglomeration. This not only reduces its effective specific surface area but also results in poor dispersibility in the matrix, severely limiting its performance and the expansion of its application range.

[0003] To improve the surface properties of carbon materials, researchers often employ surface modification techniques. Silane coupling agent modification is a common method, introducing specific organic functional groups onto the carbon material surface to enhance its compatibility with polymers or other organic phases. However, traditional modification methods often suffer from problems such as unstable coupling agent hydrolysis and uneven modified layers, resulting in weak interfacial bonding and limited performance improvement in the composite material.

[0004] On the other hand, ionic liquids, as novel green solvents and functional materials, have attracted widespread attention due to their extremely low vapor pressure, good thermal stability, and designability. Amino acid ionic liquids, as an important member of the ionic liquid family, not only inherit the excellent properties of traditional ionic liquids but also incorporate the advantages of amino acids, such as biocompatibility, chirality, and biodegradability, showing unique promise in fields such as biosensing and drug delivery. However, amino acid ionic liquids themselves have relatively low mechanical strength, poor processability, and relatively high cost, which to some extent restricts their practical application.

[0005] Current research has attempted to combine carbon materials with ionic liquids to prepare composite materials that combine the advantages of both. However, existing composite technologies mostly employ simple physical mixing or adsorption methods, such as directly immersing activated carbon in ionic liquids. Composite materials prepared using this method exhibit weak bonding between the ionic liquid and the carbon support, primarily through physical adsorption. This weak bonding makes the composite material susceptible to leaching and loss of the ionic liquid during use, leading to structural instability and performance degradation.

[0006] Therefore, developing a novel preparation method that can uniformly and stably load amino acid ionic liquids onto the surface of activated carbon powder through strong chemical bonding, thereby obtaining carbon-based composite materials with stable structure, excellent performance and biocompatibility, has become a problem to be solved in this field. Summary of the Invention

[0007] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing a carbon powder and amino acid ion composite material, comprising the following steps:

[0008] S1. Carbon powder activation: Take carbon powder with uniform particle size and silane coupling agent, add them to the reaction vessel at a mass ratio of 1:(0.05-0.2), then add anhydrous ethanol. The amount of anhydrous ethanol is 5-10 times the mass of carbon powder. After mixing, stir with a stirrer and stir the reaction for 1-3 hours under a constant temperature water bath at 50-70℃.

[0009] After the reaction was completed, the filter cake was vacuum filtered using a Buchner funnel and placed in a forced-air drying oven to dry at 60-75℃ for 4-6 hours to remove residual solvent, thus obtaining surface-modified activated carbon powder.

[0010] By using carbon powder with a specific particle size and subjecting it to high-temperature carbonization, the structural stability and specific surface area of ​​the carbon powder are further improved, providing an ideal carrier for the uniform loading of amino acid ions, thereby significantly enhancing the interfacial compatibility and structural uniformity of the composite material.

[0011] S2. Preparation of amino acid ionic liquid: Select amino acids and alkaline reagents, add deionized water at a molar ratio of 1:(1-1.2), the amount of deionized water being 8-15 times the mass of amino acids; stir magnetically at 30-50℃ until the solid is completely dissolved;

[0012] During the process, a pH meter was used to monitor the pH value of the solution in real time, and the pH was controlled within the range of 7.5-9.0 to obtain a clear and transparent amino acid ionic solution.

[0013] By precisely controlling the pH value and reaction conditions, the high purity and stability of the ionic liquid are ensured.

[0014] S3. Composite reaction: Slowly add activated carbon powder to amino acid ionic liquid, control the mass ratio of carbon powder to amino acids to be 1:(0.3-1.5), introduce inert gas into the reaction system to replace air, then keep the inert gas continuously introduced, and raise the system temperature to 60-90℃, and stir the reaction at this temperature for 2-6 hours.

[0015] S4. Post-processing: After the reaction is completed, the reaction solution is transferred to a high-speed centrifuge for centrifugation, and the bottom solid product is collected. Then, the solid product is washed repeatedly 3-5 times with a mixture of deionized water and anhydrous ethanol. The volume ratio of deionized water to anhydrous ethanol in the mixture is 1:(1-3).

[0016] Finally, the washed solid was placed in a vacuum drying oven and dried for 8-12 hours at 60-80℃ and a vacuum degree ≤-0.09MPa. After drying, it was lightly ground in a mortar to control the particle size to 50-600nm, thus obtaining a carbon powder-amino acid ion composite material.

[0017] Preferably, the silane coupling agent in step S1 is selected from at least one of γ-aminopropyltriethoxysilane and vinyltriethoxysilane;

[0018] Before use, silane coupling agents need to be purified by vacuum distillation. The distillation temperature is controlled at 120-150℃ and the vacuum degree is controlled at ≤-0.08MPa. After purification, the purity of the silane coupling agent is ≥99.5%.

[0019] Preferably, the particle size of the toner in step S1 is 50-500 nm. The toner is first carbonized at 800-1000℃ for 2-4 hours in a high-purity nitrogen atmosphere. After carbonization, it is naturally cooled to room temperature and then activated.

[0020] Preferably, the amino acid in step S2 is selected from at least one of glutamic acid, aspartic acid, and lysine, and the amino acid is an L-isomer. The water content of the amino acid is ≤0.5%, and it needs to be stored in a desiccator. The desiccant in the desiccator is anhydrous calcium chloride.

[0021] Preferably, the alkaline reagent in step S2 is selected from at least one of sodium hydroxide, potassium hydroxide, and triethanolamine;

[0022] When the alkaline reagent is sodium hydroxide or potassium hydroxide, it needs to be prepared into an aqueous solution with a concentration of 0.5-2 mol / L. When preparing the solution, an ice-water bath should be used to cool it down to avoid the exothermic reaction of dissolution, which may cause the concentration to deviate.

[0023] When the alkaline reagent is triethanolamine, it should be added directly in pure form, and added slowly dropwise at a rate of 1-2 drops / second to prevent excessively high local concentrations.

[0024] Preferably, the concentration of the amino acid ionic liquid in step S2 is 0.1-0.5 g / mL, and the concentration is determined by weighing, with a weighing accuracy to 0.001 g.

[0025] The stirring rate during the preparation process is adjusted by the stirrer speed controller, with an adjustment error of ≤±20r / min. If the solution becomes turbid during the preparation process, it needs to be filtered through a 0.22μm organic phase filter membrane.

[0026] Preferably, a dispersant is also added in step S3, specifically polyethylene glycol 400 or Tween 80, and the amount of dispersant added is 0.1-1% of the total mass of the reaction system;

[0027] The dispersant is added by dissolving it in an amino acid ionic liquid before adding the activated carbon powder, followed by ultrasonic dispersion for 5-10 minutes at a power of 300-500W to ensure uniform distribution of the dispersant.

[0028] Preferably, the reaction in step S3 is carried out under the protection of an inert gas, which is argon or helium with a purity ≥ 99.99%.

[0029] The heating process is divided into two stages:

[0030] The first stage involves raising the temperature from room temperature to 40-50℃ and maintaining this temperature for 30-60 minutes.

[0031] The second stage involves raising the temperature from 40-50℃ to 60-90℃ and maintaining this temperature for 2-6 hours.

[0032] Preferably, during the drying process in step S4, the vacuum level and temperature are recorded every 2 hours. After drying, the product needs to be cooled to room temperature before being taken out to avoid moisture absorption after contact with air.

[0033] Preferably, the deionized water used for washing in step S4 is ultrapure water with a resistivity ≥18.2 MΩ•cm, and the anhydrous ethanol is of analytical grade with a purity ≥99.7% and a water content ≤0.1%.

[0034] The washing endpoint is determined by taking the last wash solution and adding 0.1 mol / L silver nitrate solution. If no white precipitate is formed, the washing is considered complete.

[0035] This invention provides a method for preparing a carbon powder and amino acid ion composite material. It has the following beneficial effects:

[0036] (I) The preparation method of the toner and amino acid ion composite material involves surface activation treatment of the toner with a silane coupling agent, which effectively improves the surface activity and dispersibility of the toner, enabling it to combine more fully with the amino acid ion liquid in the subsequent composite process.

[0037] In step S1, carbon powder with a specific particle size is used and subjected to high-temperature carbonization treatment, which further improves the structural stability and specific surface area of ​​the carbon powder, providing an ideal carrier for the uniform loading of amino acid ions, thereby significantly enhancing the interfacial compatibility and structural uniformity of the composite material.

[0038] (II) The preparation method of this carbon powder and amino acid ionic composite material involves preparing an amino acid ionic liquid by reacting amino acids with an alkaline reagent. In step S2, the high purity and stability of the ionic liquid are ensured by precisely controlling the pH value and reaction conditions. This method uses a variety of amino acids, all of which are biocompatible L-isomers. Combined with the flexible selection of alkaline reagents, the prepared composite material is not only environmentally friendly but also has good controllability, making it suitable for various high-end applications such as biomedicine and flexible electronics.

[0039] (III) The preparation method of this toner and amino acid ion composite material effectively prevents the oxidation and deterioration of toner and amino acid ion liquid at high temperatures by introducing inert gas protection and a staged heating mechanism during the composite reaction, thereby improving the controllability and reproducibility of the reaction. Simultaneously, by adding dispersants such as polyethylene glycol 400 or Tween 80 and combining them with ultrasonic treatment, the uniform dispersion of toner in the ion liquid is further promoted, avoiding agglomeration and ensuring that the composite material has a consistent nanoscale particle size and excellent surface properties.

[0040] (iv) The preparation method of the carbon powder and amino acid ion composite material is scientifically and rationally designed through post-processing. Through high-speed centrifugation and multiple washing with mixed solvents, unreacted amino acids and other impurities are effectively removed, ensuring the high purity of the product.

[0041] The vacuum drying process, combined with precise temperature control and vacuum monitoring, avoids performance degradation caused by high temperatures or moisture absorption. The resulting composite material has a controllable particle size of 50–600 nanometers, combining the high conductivity and high specific surface area of ​​carbon materials with the biocompatibility and reactivity of amino acid ions, thus expanding its application potential in catalysis, energy storage, and biosensors. Detailed Implementation

[0042] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0043] Example 1: The present invention provides a technical solution:

[0044] A method for preparing a carbon powder and amino acid ion composite material includes the following steps:

[0045] S1. Carbon powder activation: Take carbon powder with uniform particle size and silane coupling agent, add them to the reaction vessel at a mass ratio of 1:0.05, then add anhydrous ethanol. The amount of anhydrous ethanol is 5 times the mass of carbon powder. After mixing, stir with a stirrer and stir the reaction for 1 hour under a constant temperature water bath at 50℃.

[0046] The silane coupling agent is selected from γ-aminopropyltriethoxysilane;

[0047] Before use, silane coupling agents need to be purified by vacuum distillation. The distillation temperature is controlled at 120℃ and the vacuum degree is controlled at ≤-0.08MPa. After purification, the purity of the silane coupling agent is ≥99.5%.

[0048] The toner has a particle size of 50nm. The toner is first carbonized at 800℃ for 2 hours in a high-purity nitrogen atmosphere. After carbonization, it is naturally cooled to room temperature and then activated.

[0049] After the reaction was completed, the mixture was vacuum filtered using a Buchner funnel. The filter cake was placed in a forced-air drying oven and dried at 60°C for 4 hours to remove residual solvent, yielding surface-modified activated carbon powder.

[0050] S2. Preparation of amino acid ionic liquid: Select amino acids and alkaline reagents, add deionized water at a molar ratio of 1:1, and the amount of deionized water is 8 times the mass of amino acids; stir magnetically at 30°C until the solid is completely dissolved.

[0051] The amino acid is selected from glutamic acid, and the amino acid is an L-isomer. The water content of the amino acid is ≤0.5%. It needs to be stored in a desiccator, and the desiccant in the desiccator is anhydrous calcium chloride.

[0052] The alkaline reagent is selected from potassium hydroxide;

[0053] When the alkaline reagent is sodium hydroxide or potassium hydroxide, it needs to be prepared into an aqueous solution with a concentration of 0.5 mol / L. During preparation, an ice-water bath should be used to cool the solution to avoid exothermic dissolution that could lead to concentration deviation.

[0054] When the alkaline reagent is triethanolamine, it should be added directly in pure form, and added slowly drop by drop, with the dropping rate controlled at 1 drop / second to prevent excessively high local concentrations.

[0055] The concentration of the amino acid ionic liquid was 0.1 g / mL, and the concentration was determined by weighing with an accuracy of 0.001 g.

[0056] The stirring rate during the preparation process is adjusted by the stirrer speed controller, with an adjustment error of ≤±20r / min. If the solution becomes turbid during the preparation process, it needs to be filtered through a 0.22μm organic phase filter membrane.

[0057] During the process, a pH meter was used to monitor the pH value of the solution in real time and control the pH within the range of 7.5 to obtain a clear and transparent amino acid ionic solution.

[0058] S3. Composite reaction: Slowly add activated carbon powder to amino acid ionic liquid, control the mass ratio of carbon powder to amino acids to be 1:0.3, introduce inert gas into the reaction system to replace air, then keep the inert gas continuously introduced, and raise the system temperature to 60℃, and stir the reaction at this temperature for 2 hours.

[0059] The reaction is carried out under the protection of an inert gas, which is argon or helium with a purity ≥ 99.99%.

[0060] The heating process is divided into two stages:

[0061] The first stage involves raising the temperature from room temperature to 40°C and maintaining this temperature for 30 minutes.

[0062] The second stage involves raising the temperature from 40℃ to 60℃ and maintaining this temperature for 2 hours.

[0063] A dispersant, specifically polyethylene glycol 400, was added to the amino acid ionic liquid while the activated carbon powder was slowly added. The amount of dispersant added was 0.1% of the total mass of the reaction system.

[0064] The dispersant is added by dissolving it in an amino acid ionic liquid before adding the activated carbon powder, followed by ultrasonic dispersion for 5 minutes at a power of 300W to ensure uniform distribution of the dispersant.

[0065] S4. Post-processing: After the reaction is completed, the reaction solution is transferred to a high-speed centrifuge for centrifugation, and the bottom solid product is collected. Then, the solid product is washed three times with a mixture of deionized water and anhydrous ethanol, with a volume ratio of deionized water to anhydrous ethanol of 1:1.

[0066] Finally, the washed solid was placed in a vacuum drying oven and dried for 8 hours at 60℃ and a vacuum degree ≤-0.09MPa. After drying, it was lightly ground in a mortar and pestle to control the particle size to 50nm, thus obtaining a carbon powder-amino acid ion composite material.

[0067] The vacuum level and temperature were recorded every 2 hours during the drying process. After drying, the product was cooled to room temperature before being taken out to avoid moisture absorption after contact with air.

[0068] The deionized water used for washing is ultrapure water with a resistivity ≥18.2 MΩ•cm, and the anhydrous ethanol is analytical grade with a purity ≥99.7% and a water content ≤0.1%.

[0069] The washing endpoint is determined by taking the last wash solution and adding 0.1 mol / L silver nitrate solution. If no white precipitate is formed, the washing is considered complete.

[0070] Example 2: Based on Example 1, the present invention provides a technical solution:

[0071] A method for preparing a carbon powder and amino acid ion composite material includes the following steps:

[0072] S1. Activation of carbon powder: Take carbon powder with uniform particle size and silane coupling agent, add them to the reaction vessel at a mass ratio of 1:0.2, then add anhydrous ethanol. The amount of anhydrous ethanol is 10 times the mass of carbon powder. After mixing, stir with a stirrer and stir the reaction for 3 hours under a constant temperature water bath at 70℃.

[0073] The silane coupling agent is selected from vinyltriethoxysilane;

[0074] Before use, silane coupling agents need to be purified by vacuum distillation. The distillation temperature is controlled at 150℃ and the vacuum degree is controlled at ≤-0.08MPa. After purification, the purity of the silane coupling agent is ≥99.5%.

[0075] The toner has a particle size of 500nm. The toner is first carbonized at 1000℃ for 4 hours in a high-purity nitrogen atmosphere. After carbonization, it is naturally cooled to room temperature and then activated.

[0076] After the reaction was completed, the filter cake was vacuum filtered using a Buchner funnel and placed in a forced-air drying oven to dry at 75°C for 6 hours to remove residual solvent, thus obtaining surface-modified activated carbon powder.

[0077] S2. Preparation of amino acid ionic liquid: Select amino acids and alkaline reagents, add deionized water at a molar ratio of 1:1.2, and the amount of deionized water is 15 times the mass of amino acids; stir magnetically at 50°C until the solid is completely dissolved.

[0078] The amino acid selected is aspartic acid, which is an L-isomer. The water content of the amino acid is ≤0.5%. It needs to be stored in a desiccator with anhydrous calcium chloride as the desiccant.

[0079] The alkaline reagent is selected from sodium hydroxide;

[0080] When the alkaline reagent is sodium hydroxide or potassium hydroxide, it needs to be prepared into an aqueous solution with a concentration of 2 mol / L. During preparation, an ice-water bath should be used to cool the solution to avoid exothermic dissolution and subsequent concentration deviation.

[0081] When the alkaline reagent is triethanolamine, it should be added directly in pure form, and added slowly drop by drop at a rate of 2 drops / second to prevent excessively high local concentrations.

[0082] The concentration of the amino acid ionic liquid was 0.3 g / mL, and the concentration was determined by weighing with an accuracy of 0.001 g.

[0083] The stirring rate during the preparation process is adjusted by the stirrer speed controller, with an adjustment error of ≤±20r / min. If the solution becomes turbid during the preparation process, it needs to be filtered through a 0.22μm organic phase filter membrane.

[0084] During the process, a pH meter was used to monitor the pH value of the solution in real time and control the pH within the range of 8.0 to obtain a clear and transparent amino acid ionic liquid;

[0085] S3. Composite reaction: Slowly add activated carbon powder to amino acid ionic liquid, control the mass ratio of carbon powder to amino acids to be 1:1.2, introduce inert gas into the reaction system to replace air, then keep the inert gas continuously introduced, and raise the system temperature to 70℃, and stir the reaction at this temperature for 3h.

[0086] The reaction is carried out under the protection of an inert gas, which is argon or helium with a purity ≥ 99.99%.

[0087] The heating process is divided into two stages:

[0088] The first stage involves raising the temperature from room temperature to 45°C and maintaining this temperature for 50 minutes.

[0089] The second stage involves raising the temperature from 45℃ to 80℃ and maintaining this temperature for 4 hours.

[0090] A dispersant, specifically Tween 80, was added to the amino acid ionic liquid while the activated carbon powder was slowly added. The amount of dispersant added was 0.5% of the total mass of the reaction system.

[0091] The dispersant is added by dissolving it in an amino acid ionic liquid before adding the activated carbon powder, followed by ultrasonic dispersion for 8 minutes at a power of 400W to ensure uniform distribution of the dispersant.

[0092] S4. Post-processing: After the reaction is completed, the reaction solution is transferred to a high-speed centrifuge for centrifugation, and the bottom solid product is collected. Then, the solid product is washed repeatedly 4 times with a mixture of deionized water and anhydrous ethanol. The volume ratio of deionized water to anhydrous ethanol in the mixture is 1:2.

[0093] Finally, the washed solid was placed in a vacuum drying oven and dried at 70℃ and vacuum degree ≤-0.09MPa for 12 hours. After drying, it was lightly ground in a mortar and pestle to control the particle size to 300nm, thus obtaining carbon powder-amino acid ion composite material.

[0094] The vacuum level and temperature were recorded every 2 hours during the drying process. After drying, the product was cooled to room temperature before being taken out to avoid moisture absorption after contact with air.

[0095] The deionized water used for washing is ultrapure water with a resistivity ≥18.2 MΩ•cm, and the anhydrous ethanol is analytical grade with a purity ≥99.7% and a water content ≤0.1%.

[0096] The washing endpoint is determined by taking the last wash solution and adding 0.1 mol / L silver nitrate solution. If no white precipitate is formed, the washing is considered complete.

[0097] Example 3: Based on Examples 1 and 2, the present invention provides a technical solution:

[0098] A method for preparing a carbon powder and amino acid ion composite material includes the following steps:

[0099] S1. Activation of carbon powder: Take carbon powder with uniform particle size and silane coupling agent, add them to the reaction vessel at a mass ratio of 1:0.2, then add anhydrous ethanol. The amount of anhydrous ethanol is 10 times the mass of carbon powder. After mixing, stir with a stirrer and stir the reaction for 3 hours under a constant temperature water bath at 70℃.

[0100] The silane coupling agent is selected from vinyltriethoxysilane;

[0101] Before use, silane coupling agents need to be purified by vacuum distillation. The distillation temperature is controlled at 150℃ and the vacuum degree is controlled at ≤-0.08MPa. After purification, the purity of the silane coupling agent is ≥99.5%.

[0102] The toner has a particle size of 500nm. The toner is first carbonized at 1000℃ for 4 hours in a high-purity nitrogen atmosphere. After carbonization, it is naturally cooled to room temperature and then activated.

[0103] After the reaction was completed, the filter cake was vacuum filtered using a Buchner funnel and placed in a forced-air drying oven to dry at 75°C for 6 hours to remove residual solvent, thus obtaining surface-modified activated carbon powder.

[0104] S2. Preparation of amino acid ionic liquid: Select amino acids and alkaline reagents, add deionized water at a molar ratio of 1:1.2, and the amount of deionized water is 15 times the mass of amino acids; stir magnetically at 50°C until the solid is completely dissolved.

[0105] The amino acid is selected from lysine, and the amino acid is an L-isomer. The water content of the amino acid is ≤0.5%. It needs to be stored in a desiccator, and the desiccant in the desiccator is anhydrous calcium chloride.

[0106] The alkaline reagent is selected from triethanolamine;

[0107] When the alkaline reagent is potassium hydroxide, it needs to be prepared into an aqueous solution with a concentration of 2 mol / L. During preparation, an ice-water bath should be used to cool the solution to avoid exothermic dissolution and subsequent concentration deviation.

[0108] When the alkaline reagent is triethanolamine, it should be added directly in pure form, and added slowly drop by drop at a rate of 2 drops / second to prevent excessively high local concentrations.

[0109] The concentration of the amino acid ionic liquid was 0.5 g / mL, and the concentration was determined by weighing with an accuracy of 0.001 g.

[0110] The stirring rate during the preparation process is adjusted by the stirrer speed controller, with an adjustment error of ≤±20r / min. If the solution becomes turbid during the preparation process, it needs to be filtered through a 0.22μm organic phase filter membrane.

[0111] During the process, a pH meter was used to monitor the pH value of the solution in real time and control the pH within the range of 9.0 to obtain a clear and transparent amino acid ionic liquid;

[0112] S3. Composite reaction: Slowly add activated carbon powder to amino acid ionic liquid, control the mass ratio of carbon powder to amino acids to be 1:1.5, introduce inert gas into the reaction system to replace air, then keep the inert gas continuously introduced, and raise the system temperature to 90℃, and stir the reaction at this temperature for 6 hours.

[0113] The reaction is carried out under the protection of an inert gas, which is argon or helium with a purity ≥ 99.99%.

[0114] The heating process is divided into two stages:

[0115] The first stage involves raising the temperature from room temperature to 50°C and maintaining this temperature for 60 minutes.

[0116] The second stage involves raising the temperature from 50℃ to 90℃ and maintaining this temperature for 6 hours.

[0117] A dispersant, specifically Tween 80, was added to the amino acid ionic liquid while the activated carbon powder was slowly added. The amount of dispersant added was 1% of the total mass of the reaction system.

[0118] The dispersant is added by dissolving it in an amino acid ionic liquid before adding the activated carbon powder, followed by ultrasonic dispersion for 10 minutes at a power of 500W to ensure uniform distribution of the dispersant.

[0119] S4. Post-processing: After the reaction is completed, the reaction solution is transferred to a high-speed centrifuge for centrifugation, and the bottom solid product is collected. Then, the solid product is washed repeatedly 5 times with a mixture of deionized water and anhydrous ethanol. The volume ratio of deionized water to anhydrous ethanol in the mixture is 1:3.

[0120] Finally, the washed solid was placed in a vacuum drying oven and dried at 80℃ and vacuum degree ≤-0.09MPa for 12 hours. After drying, it was lightly ground in a mortar and pestle to control the particle size to 600nm, thus obtaining carbon powder-amino acid ion composite material.

[0121] The vacuum level and temperature were recorded every 2 hours during the drying process. After drying, the product was cooled to room temperature before being taken out to avoid moisture absorption after contact with air.

[0122] The deionized water used for washing is ultrapure water with a resistivity ≥18.2 MΩ•cm, and the anhydrous ethanol is analytical grade with a purity ≥99.7% and a water content ≤0.1%.

[0123] The washing endpoint is determined by taking the last wash solution and adding 0.1 mol / L silver nitrate solution. If no white precipitate is formed, the washing is considered complete.

[0124] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0125] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for producing a carbon powder, amino acid ion composite material, characterized by, The method comprises the following steps: S1, carbon powder activation: take carbon powder with uniform particle size and silane coupling agent, add to the reaction container according to the mass ratio of 1:(0.05-0.2), then add anhydrous ethanol, the amount of anhydrous ethanol is 5-10 times the mass of carbon powder, mix and stir with a stirrer, and stir and react at 50-70 DEG C constant temperature water bath for 1-3h; After the reaction is completed, vacuum filtration is performed with a Buchner funnel, the filter cake is placed in a forced air drying oven, and dried at 60-75 DEG C for 4-6h to remove residual solvents, and the surface modified activated carbon powder is obtained; S2, preparation of amino acid ionic liquid: select amino acid and base reagent, add deionized water according to the molar ratio of 1:(1-1.2), the amount of deionized water is 8-15 times the mass of amino acid, and magnetic stirring is carried out at 30-50 DEG C until the solid is completely dissolved; During the process, the pH value of the solution is monitored in real time with a pH meter, and the pH value is controlled in the range of 7.5-9.0, and the clear and transparent amino acid ionic liquid is obtained; S3. Compound reaction: slowly add the activated carbon powder to the amino acid ionic liquid, control the mass ratio of carbon powder to amino acid to be 1:(0.3-1.5), introduce inert gas to replace air in the reaction system, then keep the inert gas continuously introduced, and raise the temperature of the system to 60-90 DEG C, and stir and react at the temperature for 2-6h; S4. Post-processing: after the reaction is completed, the reaction liquid is transferred to a high-speed centrifuge, the bottom solid product is collected, and then the solid product is washed repeatedly with a mixture of deionized water and anhydrous ethanol for 3-5 times, and the volume ratio of deionized water to anhydrous ethanol in the mixture is 1:(1-3); Finally, the washed solid is placed in a vacuum drying oven, dried at 60-80 DEG C and a vacuum degree of ≤-0.09MPa for 8-12h, and then slightly ground in a mortar after drying, and the particle size is controlled to be 50-600nm, and the carbon powder-amino acid ionic composite material is obtained.

2. The method according to claim 1, wherein the carbon powder, amino acid ion composite material is prepared by the following steps. The silane coupling agent in step S1 is selected from at least one of γ-aminopropyl triethoxysilane and vinyl triethoxysilane; The silane coupling agent needs to be purified by vacuum distillation before use, the distillation temperature is controlled at 120-150 DEG C, and the vacuum degree is controlled at ≤-0.08MPa, and the purity of the purified silane coupling agent is ≥99.5%.

3. The method for preparing a carbon powder and amino acid ion composite material according to claim 2, characterized in that: The particle size of the carbon powder in step S1 is 50-500nm, the carbon powder is first carbonized at 800-1000 DEG C for 2-4h, the carbonization atmosphere is high-purity nitrogen, and the carbonized product is naturally cooled to room temperature before activation treatment.

4. The method for preparing a carbon powder and amino acid ion composite material according to claim 1, characterized in that: The amino acid in step S2 is selected from at least one of glutamic acid, aspartic acid and lysine, the amino acid is an L-type isomer, the water content of the amino acid is ≤0.5%, and the amino acid needs to be stored in a desiccator, and the drying agent in the desiccator is anhydrous calcium chloride.

5. The method for preparing a carbon powder and amino acid ion composite material according to claim 4, characterized in that: The base reagent in step S2 is selected from at least one of sodium hydroxide, potassium hydroxide and triethanolamine; When the base reagent is sodium hydroxide or potassium hydroxide, it needs to be prepared into an aqueous solution with a concentration of 0.5-2mol / L, and an ice water bath is used for cooling during preparation to avoid concentration deviation caused by heat release during dissolution; When the base reagent is triethanolamine, it is directly added in pure form, and the addition is slow and dropwise, with a dropwise addition rate of 1-2 drops / s.

6. The method for preparing a carbon powder and amino acid ion composite material according to claim 5, characterized in that: The concentration of the amino acid ionic liquid in step S2 is 0.1-0.5 g / mL, and the concentration is determined by weighing, with a weighing accuracy of 0.001 g; During the preparation process, the stirring rate is adjusted by a stirrer speed controller, and the adjustment error is ≤±20 r / min. If the solution is turbid during the preparation process, it needs to be filtered through a 0.22 μm organic phase filter.

7. The method according to claim 1, wherein the method is characterized by: In step S3, a dispersant is also added, which is specifically polyethylene glycol 400 or Tween 80, and the addition amount of the dispersant is 0.1-1% of the total mass of the reaction system. The dispersant is dissolved in the amino acid ionic liquid before the activated carbon powder is added, and then ultrasonic dispersion is performed, with an ultrasonic dispersion time of 5-10 min and an ultrasonic power setting of 300-500 W, to ensure uniform distribution of the dispersant.

8. The method for preparing a carbon powder and amino acid ion composite material according to claim 6, characterized in that: The reaction in step S3 is carried out under the protection of an inert gas, which is argon or helium with a purity of ≥99.99%; The temperature rising process is divided into two stages: The first stage is from room temperature to 40-50°C, and the temperature is kept at this temperature for 30-60 min. The second stage is from 40-50°C to 60-90°C, and the temperature is kept at this temperature for 2-6 h.

9. The method according to claim 1, wherein the method is characterized by: During the drying process in step S4, the vacuum degree and temperature are recorded every 2 h, and after the drying is completed, the product needs to be cooled to room temperature before being taken out, to avoid moisture absorption after contacting air.

10. The method according to claim 9, wherein the carbon powder, amino acid ion composite material is prepared by the following steps: 1) mixing a carbon powder and an amino acid ion to obtain a mixture; 2) heating the mixture to obtain a carbon powder, amino acid ion composite material. The deionized water used for washing in step S4 is ultrapure water with a resistivity of ≥18.2 MΩ·cm, and the anhydrous ethanol is of analytical purity with a purity of ≥99.7% and a water content of ≤0.1%. The end point of washing is determined by adding 0.1 mol / L silver nitrate solution to the last washing liquid, and no white precipitate is generated, indicating that the washing is complete.