CN110860272A - Graphene antibacterial carbon sphere and preparation method and application thereof - Google Patents
Graphene antibacterial carbon sphere and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a graphene antibacterial carbon sphere and a preparation method and application thereof, wherein the carbon sphere comprises the following components in percentage by mass: 80-90% of graphene grafted carbon powder; 5-15% of emulsifier; 0.1 to 5 percent of additive. According to the invention, carbon powder activation and graphene modification are adopted, so that grafting of graphene hydroxyl functional groups and nitro functional groups on activated carbon powder is facilitated, graphene grafted carbon is generated through high-temperature reaction under the protection of nitrogen, and meanwhile, generation of porous carbon is facilitated, and increase of the surface area of a final product is facilitated. The graphene composite activated carbon prepared by the method has excellent functions of resisting bacteria, removing peculiar smell and the like, and can be widely applied to places such as family living rooms, kitchens, toilets, refrigerators, washing machines and the like.
Description
Technical Field
The invention relates to the technical field of activated carbon, in particular to a graphene antibacterial carbon sphere and a preparation method and application thereof.
Background
The activated carbon is used as an excellent adsorption material, is commonly used for air purification, water purification, industrial waste gas recovery and the like, is applied to the fields of chemical industry, food processing, agriculture, national defense and the like, and plays an important role in environmental protection and human life. The adsorption characteristics of activated carbon depend on its developed pore structure and unique surface chemistry. However, most of the activated carbon is of a microporous structure, so that the adsorption performance of the activated carbon is limited.
Since the preparation of Graphene (Graphene) by mechanical exfoliation and the revealing of unique physical properties in 2004, scientists in the fields of physics, chemistry, materials, electronics and engineering all have paid a great deal of research interest, and their research promoters, anderley, haim and concutant, norwochoff, have won the prize on the physics in 2010 because of their pioneering work. The properties of graphene have been studied more deeply and show a wide application prospect: it can not only replace many current materials, realize the improvement of performance and the reduction of manufacturing cost, such as silicon in the semiconductor field; it can also be compounded with other materials to improve its performance and form a series of multifunctional composite materials.
In the prior art, for example, patent document CN 108840324a discloses a preparation method of an activated carbon-graphene composite material, which discloses that a graphene oxide material is dispersed in water, activated carbon is added, the mixture is stirred for 2 to 3 hours and fully mixed, then a NaBH4 solution is slowly dropped, and then the mixture is refluxed for 3 to 5 hours at 80 to 120 ℃, and filtered to obtain the activated carbon-graphene composite material, which has a function of adsorbing formaldehyde.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a graphene antibacterial carbon sphere and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
the invention provides a graphene antibacterial carbon sphere which comprises the following components in percentage by mass:
80-90% of graphene grafted carbon powder;
5-15% of emulsifier;
0.1 to 5 percent of additive.
Preferably, in the graphene grafted carbon powder, the mass content of graphene is 4-8%, and more preferably 5%.
Preferably, in the graphene grafted carbon powder, the carbon powder adopted is one or more of graphite carbon, biomass carbon, shell carbon, coal-based activated carbon and wood-based activated carbon.
Preferably, in the graphene grafted carbon powder, the adopted graphene is modified graphene.
Preferably, the emulsifier is any one or more of carboxylate, sulfate, sulfonate, N-dodecyl dimethylamine, polyoxyethylene ether and polyoxypropylene ether. In the invention, because the carbon powder particles are fine, static electricity is easy to generate in the stirring process, and the carbon powder particles are not easy to mix, so that the added emulsifier can disperse charges. The emulsifier adopted by the invention is a surfactant capable of stabilizing emulsion, the graphene has hydroxyl and carboxyl functional groups and has the characteristics of water phase and oil phase, and the added emulsifier can be mixed with the graphene grafted carbon, so that carbon ball forming is easy.
More preferably, the emulsifier is a compound of carboxylate and a polyoxypropylene ether emulsifier; and the optimal compounding ratio is 1: 5.
Preferably, the additive is one or more of diethylenetriamine, sodium hexametaphosphate, lysine, ferric nitrate, ferrous sulfate, sodium bicarbonate and ammonium bicarbonate.
More preferably, the additive is a mixture of diethylenetriamine, sodium hexametaphosphate and lysine; and the optimal mixing ratio is 2:3: 5.
Preferably, the preparation method of the graphene grafted carbon powder comprises the following steps:
a1, carbon powder activation: dispersing carbon powder in a nitric acid solution, carrying out reflux treatment at 60-90 ℃ for 0.5-3 hours, filtering, cleaning and drying to obtain acid-treated activated carbon;
a2, preparing modified graphene: adding graphene into deionized water, carrying out ultrasonic treatment at normal temperature, then adding a surfactant, stirring, and carrying out ultrasonic treatment to obtain a modified graphene dispersed aqueous solution;
a3, preparing graphene composite activated carbon: adding acid-treated activated carbon into the modified graphene dispersion aqueous solution, stirring, heating to 60-100 ℃, reacting for 4-10h, cooling and drying to obtain graphene composite activated carbon;
a4, preparing graphene grafted carbon powder: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10-15 ℃/min to 350-500 ℃, and keeping the temperature for 0.5-3 hours; and then continuously heating to 700-900 ℃ at the heating speed of 10-12 ℃/min, keeping the temperature for 1-3h, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
The invention adopts the high-temperature heat treatment of the step A3, so that the solution is easy to be uniformly mixed; and the graphene composite activated carbon is obtained only by the heat treatment in the step A3, and belongs to the hydrogen bond action at normal temperature, the reaction degree is not large, and the acting force is weak. Therefore, further heat treatment is required. In the step A4, the first heat treatment is carried out to enable the hydrogen bonding effect of the graphene composite activated carbon to generate chemical bonding effect at high temperature, and graphene grafted carbon powder is generated through reaction; and the second high-temperature reaction is easy to generate holes on the graphene with the sheet structure, so that the surface area of the graphene grafted carbon powder is increased, and the antibacterial active sites are increased.
Preferably, in the step A1, the specific surface area of the activated carbon is 1500-2Per gram, the particle diameter is 10-100 mu m; the mass fraction of the nitric acid solution is 15 percent;
in the step A2, the concentration of a solution formed by adding the graphene into deionized water is 0.1%;
in the step A2, the surfactant is any one or more of stearic acid, sodium dodecyl benzene sulfonate, polyethylene glycol, fatty glyceride, sorbitan fatty acid, polyvinylpyrrolidone (PVP), dodecyl pyrrolidone and Dimethylformamide (DMF); the addition amount of the surfactant is 5% of the graphene content.
The invention also provides a preparation method of the graphene antibacterial carbon spheres, which comprises the following steps: and uniformly mixing the graphene grafted carbon powder, an emulsifier and an additive according to a proportion, and then carrying out extrusion forming to obtain the carbon spheres.
The invention also provides application of the graphene antibacterial carbon spheres in the fields of air purification and water purification.
According to the invention, carbon powder activation and graphene modification are adopted, so that grafting of graphene hydroxyl functional groups and nitro functional groups on activated carbon powder is facilitated, graphene grafted carbon is generated through high-temperature reaction under the protection of nitrogen, and meanwhile, generation of porous carbon is facilitated, and increase of the surface area of a final product is facilitated. The graphene has antibacterial performance, and the porous graphene microporous antibacterial carbon ball increases the adsorption capacity on peculiar smell.
Compared with the prior art, the invention has the following beneficial effects:
the graphene composite activated carbon prepared by the invention has excellent antibacterial and peculiar smell removing functions, and can be widely applied to places such as family living rooms, kitchens, toilets, refrigerators, washing machines and the like. This patent uses active carbon as the raw materials, through modified graphene grafting technique, prepares antibiotic carbon sphere of graphite alkene micropore. The microporous ball has ultramicroporosity, antibacterial contact sites are added, bacteria and peculiar smell can fully contact the surface of the whole ball body and inside micropores, and the antibacterial effect is greatly improved. The main technical key is the preparation of the graphene grafted carbon powder.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The graphene antibacterial carbon sphere comprises the following components in percentage by mass:
80% of graphene grafted carbon powder (graphene content is 4%);
15% of emulsifier (sodium carboxylate);
5% of additive (diethylenetriamine).
The specific preparation method of the graphene antibacterial carbon spheres comprises the following steps:
1. preparation of graphene grafted carbon powder
A1, carbon powder activation: dispersing carbon powder (hull carbon) in nitric acid solution with mass fraction of 15%, refluxing at 60 deg.C for 3 hr, filtering, cleaning, and drying to obtain acid-treated active carbon; the specific surface area of the activated carbon is 1500-2Per gram, the particle diameter is 10-100 mu m;
a2, preparing modified graphene: adding graphene into deionized water (prepared according to the concentration of 0.1%), carrying out ultrasonic treatment at normal temperature, then adding a surfactant (stearic acid, the addition amount is 5% of the content of the graphene), stirring, and carrying out ultrasonic treatment to obtain a modified graphene dispersed aqueous solution;
a3, preparing graphene composite activated carbon: adding the acid-treated activated carbon into the modified graphene dispersion aqueous solution, stirring, heating to 80 ℃, reacting for 8 hours, cooling and drying to obtain graphene composite activated carbon;
a4, preparing graphene grafted carbon powder: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10 ℃/min to 350 ℃, and keeping the temperature for 3 hours; and then continuously heating to 700 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 3h, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
2. Preparation of graphene antibacterial carbon spheres
And uniformly mixing the graphene grafted carbon powder, an emulsifier and an additive according to a proportion, and then carrying out extrusion forming to obtain the carbon spheres.
Example 2
The graphene antibacterial carbon sphere comprises the following components in percentage by mass:
87% of graphene grafted carbon powder (graphene content is 5%);
12.9% of emulsifier (N-dodecyl dimethylamine);
additive (lysine) 0.1%.
The specific preparation method of the graphene antibacterial carbon spheres comprises the following steps:
1. preparation of graphene grafted carbon powder
A1, carbon powder activation: dispersing carbon powder (biomass charcoal) in a nitric acid solution with the mass fraction of 15%, performing reflux treatment at 80 ℃ for 2 hours, and filtering, cleaning and drying to obtain acid-treated active carbon; the specific surface area of the activated carbon is 1500-2Per gram, the particle diameter is 10-100 mu m;
a2, preparing modified graphene: adding graphene into deionized water (prepared according to the concentration of 0.1%), carrying out ultrasonic treatment at normal temperature, then adding a surfactant (dodecyl pyrrolidone, the addition amount is 5% of the content of the graphene), stirring, and carrying out ultrasonic treatment to obtain a modified graphene dispersed aqueous solution;
a3, preparing graphene composite activated carbon: adding the acid-treated activated carbon into the modified graphene dispersion aqueous solution, stirring, heating to 60 ℃, reacting for 10 hours, cooling and drying to obtain graphene composite activated carbon;
a4, preparing graphene grafted carbon powder: heating the graphene composite activated carbon under the protection of gas at a heating rate of 15 ℃/min to 500 ℃ and keeping the temperature for 0.5 hour; and then continuously heating to 800 ℃ at the heating rate of 12 ℃/min, keeping the temperature for 2h, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
2. Preparation of graphene antibacterial carbon spheres
And uniformly mixing the graphene grafted carbon powder, an emulsifier and an additive according to a proportion, and then carrying out extrusion forming to obtain the carbon spheres.
Example 3
The graphene antibacterial carbon sphere comprises the following components in percentage by mass:
90% of graphene grafted carbon powder (graphene content is 8%);
5% of emulsifier (polyoxypropylene ether);
5% of additive (diethylene triamine and sodium hexametaphosphate 5:5 mixed).
The specific preparation method of the graphene antibacterial carbon spheres comprises the following steps:
1. preparation of graphene grafted carbon powder
A1, carbon powder activation: dispersing carbon powder (coal-based activated carbon) in a nitric acid solution with the mass fraction of 15%, performing reflux treatment at 90 ℃ for 0.5 hour, and filtering, cleaning and drying to obtain acid-treated activated carbon; the specific surface area of the activated carbon is 1500-2Per gram, the particle diameter is 10-100 mu m;
a2, preparing modified graphene: adding graphene into deionized water (prepared according to the concentration of 0.1%), carrying out ultrasonic treatment at normal temperature, then adding a surfactant (polyethylene glycol, the addition amount is 5% of the content of the graphene), stirring, and carrying out ultrasonic treatment to obtain a modified graphene dispersed aqueous solution;
a3, preparing graphene composite activated carbon: adding the acid-treated activated carbon into the modified graphene dispersion aqueous solution, stirring, heating to 100 ℃, reacting for 4 hours, cooling and drying to obtain graphene composite activated carbon;
a4, preparing graphene grafted carbon powder: heating the graphene composite activated carbon under the protection of gas at a heating rate of 12 ℃/min to 400 ℃ and keeping the temperature for 3 hours; and then continuously heating to 900 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 1h, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
2. Preparation of graphene antibacterial carbon spheres
And uniformly mixing the graphene grafted carbon powder, an emulsifier and an additive according to a proportion, and then carrying out extrusion forming to obtain the carbon spheres.
Example 4
The embodiment provides a graphene antibacterial carbon sphere which comprises the following components in percentage by mass:
87% of graphene grafted carbon powder (graphene content is 4%);
10% of emulsifier (sodium sulfonate);
additive (lysine) 3%.
The preparation method is the same as in example 1.
Example 5
This embodiment provides an antibiotic carbon sphere of graphite alkene, compares with embodiment 3, the difference only lies in: in this example, the emulsifier used was a 1:5 complex of sodium carboxylate and polyoxypropylene ether.
The preparation method of the graphene antibacterial carbon spheres is the same.
Example 6
This embodiment provides an antibiotic carbon sphere of graphite alkene, compares with embodiment 3, the difference only lies in: in this example, the emulsifier used was a 1:5 complex of sodium sulfonate and polyoxypropylene ether.
The preparation method of the graphene antibacterial carbon spheres is the same.
Example 7
This embodiment provides an antibiotic carbon sphere of graphite alkene, compares with embodiment 3, the difference only lies in: in this example, the additive used was a 2:3:5 mixture of diethylenetriamine, sodium hexametaphosphate, and lysine.
The preparation method of the graphene antibacterial carbon spheres is the same.
Example 8
This embodiment provides an antibiotic carbon sphere of graphite alkene, compares with embodiment 3, the difference only lies in: in this example, the additive used was a 2:3:5 mixture of diethylenetriamine, ferrous sulfate, and lysine.
The preparation method of the graphene antibacterial carbon spheres is the same.
Comparative example 1
This comparative example provides an antibiotic carbon sphere of graphite alkene, compares with example 1, and the difference only lies in: in this example, the emulsifier content was 18% and the additive content was 2%.
The preparation method of the graphene antibacterial carbon spheres is the same.
Comparative example 2
This comparative example provides an antibiotic carbon sphere of graphite alkene, compares with example 3, and the difference only lies in: in this example, the emulsifier content was 3% and the additive content was 7%.
Comparative example 3
Compared with the embodiment 3, the difference is only that: in this embodiment, in the step 1 of the preparation method, the carbon powder activation treatment in the step a1 is not performed, and the activated carbon that is not subjected to the acid treatment is used in the step A3.
Comparative example 4
Compared with the embodiment 3, the difference is only that: in this embodiment, in the step 1 of the preparation method, in the preparation of the graphene grafted carbon powder, the step a4 includes the following steps: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10 ℃/min to 700 ℃, keeping the temperature for 6 hours, cooling after the reaction is finished, taking out a product, washing with water, and drying to obtain the graphene composite activated carbon.
Comparative example 5
Compared with the embodiment 3, the difference is only that: in this embodiment, in the step 1 of the preparation method, in the preparation of the graphene grafted carbon powder, the step a4 includes the following steps: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10 ℃/min to 350 ℃, keeping the temperature for 6 hours, cooling after the reaction is finished, taking out a product, washing with water, and drying to obtain the graphene composite activated carbon.
Comparative example 6
Compared with the embodiment 3, the difference is only that: in this embodiment, in the step 1 of the preparation method, in the preparation of the graphene grafted carbon powder, the step a4 includes the following steps: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10 ℃/min to 350 ℃, and keeping the temperature for 3 hours; and then continuously heating to 600 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 3 hours, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
Effect verification:
the graphene antibacterial carbon spheres prepared in the examples and the comparative examples are subjected to effect verification and are tested by adopting the methods of ATCC 25922 and GB/T18801-2015, and the test results are as follows:
| antibacterial property | PM2.5 removal Rate | |
| Example 1 | 96.8％ | 97.2％ |
| Example 2 | 93.3％ | 92.7％ |
| Example 3 | 95.1％ | 94.9％ |
| Example 4 | 97.5％ | 98.5％ |
| Example 5 | 98.6％ | 99.1％ |
| Practice ofExample 6 | 96.2％ | 97.4％ |
| Example 7 | 99.9％ | 99.9％ |
| Example 8 | 96.8％ | 97.7％ |
| Comparative example 1 | 90.3％ | 90.2％ |
| Comparative example 2 | 85.4％ | 82.7％ |
| Comparative example 3 | 80.6％ | 76.6％ |
| Comparative example 4 | 75.2％ | 78.8％ |
| Comparative example 5 | 78.1％ | 77.5％ |
| Comparative example 6 | 70.7％ | 72.3％ |
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (10)
1. The graphene antibacterial carbon sphere is characterized by comprising the following components in percentage by mass:
80-90% of graphene grafted carbon powder;
5-15% of emulsifier;
0.1 to 5 percent of additive.
2. The graphene antibacterial carbon sphere according to claim 1, wherein the graphene grafted carbon powder contains 4-8% by mass of graphene.
3. The graphene antibacterial carbon sphere according to claim 1 or 2, wherein carbon powder adopted in the graphene grafted carbon powder is one or more of graphite carbon, biomass carbon, shell carbon, coal-based activated carbon and wood-based activated carbon.
4. The graphene antibacterial carbon sphere according to claim 1 or 2, wherein in the graphene grafted carbon powder, the adopted graphene is modified graphene.
5. The graphene antibacterial carbon sphere according to claim 1, wherein the emulsifier is one or more selected from the group consisting of carboxylate, sulfate, sulfonate, N-dodecyldimethylamine, polyoxyethylene ethers, and polyoxypropylene ethers.
6. The graphene antibacterial carbon sphere according to claim 1, wherein the additive is any one or more of diethylenetriamine, sodium hexametaphosphate, lysine, ferric nitrate, ferrous sulfate, sodium bicarbonate, and ammonium bicarbonate.
7. The graphene antibacterial carbon sphere according to claim 1 or 2, wherein the preparation method of the graphene grafted carbon powder comprises the following steps:
a1, carbon powder activation: dispersing carbon powder in a nitric acid solution, carrying out reflux treatment at 60-90 ℃ for 0.5-3 hours, filtering, cleaning and drying to obtain acid-treated activated carbon;
a2, preparing modified graphene: adding graphene into deionized water, carrying out ultrasonic treatment at normal temperature, then adding a surfactant, stirring, and carrying out ultrasonic treatment to obtain a modified graphene dispersed aqueous solution;
a3, preparing graphene composite activated carbon: adding acid-treated activated carbon into the modified graphene dispersion aqueous solution, stirring, heating to 60-100 ℃, reacting for 4-10h, cooling and drying to obtain graphene composite activated carbon;
a4, preparing graphene grafted carbon powder: heating the graphene composite activated carbon under the protection of gas at a heating rate of 10-15 ℃/min to 350-500 ℃, and keeping the temperature for 0.5-3 hours; and then continuously heating to 700-900 ℃ at the heating speed of 10-12 ℃/min, keeping the temperature for 1-3h, cooling after the reaction is finished, taking out the product, washing with water, and drying to obtain the catalyst.
8. The graphene antibacterial carbon sphere of claim 7, wherein in the step A1, the specific surface area of the activated carbon is 1500-2Per gram, the particle diameter is 10-100 mu m; the mass fraction of the nitric acid solution is 15 percent;
in the step A2, the concentration of a solution formed by adding the graphene into deionized water is 0.1%;
in the step A2, the surfactant is any one or more of stearic acid, sodium dodecyl benzene sulfonate, polyethylene glycol, fatty glyceride, sorbitan fatty acid, polyvinylpyrrolidone (PVP), dodecyl pyrrolidone and Dimethylformamide (DMF); the addition amount of the surfactant is 5% of the graphene content.
9. The preparation method of the graphene antibacterial carbon spheres according to claim 1, which is characterized by comprising the following steps: and uniformly mixing the graphene grafted carbon powder, an emulsifier and an additive according to a proportion, and then carrying out extrusion forming to obtain the carbon spheres.
10. The application of the graphene antibacterial carbon spheres of claim 1 in the fields of air purification and water purification.
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