CN112174122A - Antibacterial graphene nano knife and preparation method and application thereof - Google Patents
Antibacterial graphene nano knife and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an antibacterial graphene nano knife and a preparation method and application thereof, and the antibacterial graphene nano knife is prepared from the following raw materials in parts by weight: 6-10 parts of graphite, 25-30 parts of acid liquor, 6-10 parts of intercalation agent, 0.2-1 part of dispersing agent, 99-99.8 parts of liquid carrier and 0.1-10 parts of phyllosilicate. According to the antibacterial graphene nano knife, the graphene nano knife paste body is processed by the preparation method, so that the antibacterial graphene nano knife paste body has super-strong antibacterial performance, and can be added into the fields needing bacteriostasis, such as facial masks, facial cleanser, medical hydrogel and the like to prepare healthy high-adsorption clean antibacterial products.
Description
Technical Field
The invention belongs to the field of antibacterial graphene preparation, and particularly relates to an antibacterial graphene nano knife and a preparation method and application thereof.
Background
The graphene material is the thinnest, the hardest and the best conductive nano material known at present, has strong flexibility and flexibility, and has good application prospects in the fields of lithium batteries, supercapacitors, conductive printing ink, flexible display screens, wearable equipment, chips, aerospace and the like. Currently, with the annual rise of the traditional manufacturing cost of the country, the "world factories" urgently need strategic transformation, and the national policies encourage the development of emerging high-tech strategic industries. The 2014 national ministry of industry and communications issues a key material upgrading and upgrading engineering implementation scheme, wherein the key development of the graphene industry is explicitly proposed. In the period of vigorous development of high-tech industry, any new subversive material will certainly lead to a new industrial revolution and further change the lives of people. Many scientists believe that graphene products are revolutionary new materials, and will push the electronic industry to step into a new development stage, leveraging at least the billion-level industry chain. Graphene has shown excellent characteristics in many aspects such as lithium ion secondary batteries, supercapacitors, conductive inks, flexible display devices, wearable devices, chip materials, heat dissipation materials, and the like. Discoverers of graphene since 2004 to 2010 obtain the nobel prize. The application development speed of graphene far exceeds that of fullerene and carbon nano tube in the current year, but the patent of graphene in the fields of biomedicine and health is relatively less.
In many fields, additives such as antibacterial agents are required to inhibit the growth of microorganisms in order to maintain human health. Currently, organic antibacterial agents such as imidazoles, quaternary ammonium salts, biguanides and the like and inorganic antibacterial agents of some rare metals such as silver and the like are commonly used. However, the organic antibacterial agent has the defects of drug resistance and adverse effect on environmental production after long-term use, and the inorganic antibacterial agent is expensive and non-renewable due to rare metals and is a waste of natural resources. The emergence of graphene antibacterial agents may be a new option. Because the graphene material has biological inertia, the biological drug resistance can not be generated. And the carbon material is easier to obtain and cheaper than rare metal, so the graphene antibacterial agent is a novel antibacterial material.
Disclosure of Invention
In view of this, the invention provides an antibacterial graphene nano-knife, and a preparation method and an application thereof, aiming at overcoming the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
an antibacterial graphene nano-knife is prepared from the following raw materials in parts by weight:
further, the intercalation agent is at least one of salicylic acid, salicylate, peroxyacetic acid, glycolic acid or citric acid; the dispersant is at least one of polyoxyethylene, polyethylene glycol, chitosan or EDTA; the phyllosilicate is white vermiculite. The silicate is in a layer shape, and the color depth of the paste can be controlled by adjusting the proportion of the silicate to the expanded graphite so as to meet the requirements of different use scenes.
Further, the particle size of the graphite is 10-50 μm; the liquid carrier is at least one of water or glycerol; the acid solution is a mixed solution of concentrated sulfuric acid and fuming nitric acid, wherein the mass ratio of the concentrated sulfuric acid to the fuming nitric acid is 1-3: 1.
The antibacterial graphene nanometer knife also comprises 0.1-1 part of defoaming agent; the defoaming agent is an organic silicon defoaming agent.
The preparation method of the antibacterial graphene nanometer knife comprises the following steps:
(1) adding graphite into acid liquor, adding an intercalation agent at the solution temperature of 60-80 ℃, then stirring, filtering, washing residues with hydrochloric acid until no sulfate is detected, washing the residues with deionized water until the pH value is 5-7, and then drying to obtain intercalated graphite;
(2) placing the intercalated graphite in microwave equipment, introducing nitrogen, and carrying out microwave treatment for 1-3 minutes to prepare expanded graphite;
(3) adding the dispersing agent into the liquid carrier, and uniformly stirring to prepare a mixed solution;
(4) adding the expanded graphite prepared in the step (2) into the mixed liquid prepared in the step (3) to prepare mixed liquid;
(5) adding phyllosilicate into the mixed material liquid prepared in the step (4), and performing high-speed fluid clash by using high-jet equipment to obtain a multilayer graphene mixed liquid;
(6) and (4) carrying out suction filtration or centrifugal concentration on the multilayer graphene mixed solution prepared in the step (5) to prepare the antibacterial graphene nanometer knife.
Further, the stirring step in the step (1) is carried out for 24-48 hours; the mass fraction of the hydrochloric acid in the step (1) is 9-18 wt%; the temperature of the drying step in the step (1) is 60-120 ℃.
The phyllosilicate in the step (5) is processed at 1000 ℃ for 30 min.
Further, the colliding fluid speed in the high-speed fluid colliding step in the step (5) is more than 50 m/s, and the colliding time is 5-10 min; and (4) the high-jet equipment in the step (5) is a high-pressure jet collider.
Furthermore, the thickness of the nanometer knife is 1.7-50nm, the lamella spacing is 0.34-500nm, the D50 is 0.1-20um, and the Dmax is 10-100 um.
The application of the antibacterial graphene nano knife is the application of the antibacterial graphene nano knife in preparing washing and protecting articles; the antibacterial graphene nano knife is applied to the preparation of facial cleanser; the antibacterial graphene nano knife is applied to preparation of medical hydrogel.
Further, the facial cleanser comprises 0.01-6 parts of antibacterial graphene nano knife and 0.1-5 parts of cyclic silicate; the medical hydrogel comprises 0.01-6 parts of antibacterial graphene nano knife. The cyclic silicate and the antibacterial graphene nanometer knife generate a synergistic effect in the use process of the facial cleanser, so that the facial microcirculation is promoted, and the skin quality is improved.
Further, the cyclic silicate is medical stone.
The medical hydrogel comprises a matrix material, wherein the matrix material is at least one of starch, cellulose, alginic acid, hyaluronic acid, chitosan, collagen, poly-L-lysine, poly-L-glutamic acid, polyvinyl alcohol, polyethylene glycol, polyethylene oxide, polyacrylic acid, polymethacrylic acid or polyacrylamide.
The facial cleanser comprises an oily component, a surfactant, an aqueous component and an additive, wherein the oily component is at least one of isopropyl myristate, isopropyl palmitate, glyceryl caprylate, glyceryl decanoate, lanolin, cetyl alcohol or stearyl alcohol; the surfactant is at least one of lauryl triethanolamine sulfate, cocamidopropyl betaine, coconut monoethanolamide, glyceryl monostearate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, polyoxyethylene, chitosan, polyvinyl alcohol or alkyl polyglucoside; the aqueous component is at least one of water, glycerol or propylene glycol; the additive is at least one of essence, antioxidant or whitening agent.
Compared with the prior art, the invention has the following advantages:
according to the antibacterial graphene nano knife, the graphene nano knife paste body is processed by the preparation method, so that the antibacterial graphene nano knife paste body has super-strong antibacterial performance, and can be added into the fields needing bacteriostasis, such as facial masks, facial cleanser, medical hydrogel and the like to prepare healthy high-adsorption clean antibacterial products.
According to the preparation method of the antibacterial graphene nanometer knife, disclosed by the invention, the interlayer agent, the reaction time and the temperature are limited, and the interlayer spacing interval is accurately controlled to obtain the graphene nanometer knife paste body with basically controllable layer number and interlayer spacing; the high-speed jet equipment provided by the invention can generate huge acting force to tear the graphite layer instantly while colliding a sample at a high speed, so that the expanded graphite can be processed into graphene in a very short time. The layered silicate acts like a blade during the process, helping the fluid to better exfoliate the expanded graphite into graphene, which acts synergistically with the high velocity jet equipment. The cream can be applied to the health field to realize the bacteriostatic effect more in an environment-friendly and healthy manner, and can be applied to the washing and protecting fields of facial cleanser and the like due to the high specific surface area and strong adsorbability of the graphene nano-knife, and can realize the high cleaning effect.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
An antibacterial graphene nano-knife is prepared from the following raw materials in parts by weight: 100g of natural graphite, 262.5g of sulfuric acid, 87.5g of nitric acid, 350g of salicylate, 30g of EDTA, 9870g of water and 50g of white vermiculite.
The preparation method of the antibacterial graphene nanometer knife comprises the following steps:
(1) adding natural graphite (80 meshes) into acid liquor, adding an intercalation agent at the solution temperature of 65 ℃, then stirring for 24h, filtering, washing residues with 18 wt% hydrochloric acid until no sulfate is detected, washing the residues with deionized water until the pH value is 7, and then drying for 38h at 100 ℃ to obtain intercalated graphite;
(2) placing the intercalated graphite in microwave equipment, introducing nitrogen, and performing microwave treatment for 1 minute to prepare expanded graphite;
(3) adding the dispersing agent into the liquid carrier, and uniformly stirring to prepare a mixed solution;
(4) adding 50g of the expanded graphite prepared in the step (2) into the mixed solution prepared in the step (3) to prepare mixed solution;
(5) adding phyllosilicate into the mixed material liquid prepared in the step (4), and performing high-speed fluid clash for 5min by using high-jet equipment, wherein the clash fluid speed is 60 m/s, so as to obtain a multilayer graphene mixed liquid;
(6) and (4) carrying out suction filtration or centrifugal concentration on the multilayer graphene mixed solution prepared in the step (5) to prepare the antibacterial graphene nanometer knife with the solid content of 3%.
16.0g of white oil, 8.0g of caprylic triglyceride, 3.0g of isononyl alcohol ester, 2.5g of olive oil, 2.0g of glyceryl monostearate, 3.0g of polyglycerol ester, 5.0g of lauryl ether phosphate and 0.5g of essence are respectively weighed, 16g of antibacterial graphene nano knife, 2g of medical stone and 44g of deionized water are added, and the mixture is placed into a high-speed stirrer to be fully stirred for 30min to prepare the facial cleanser emulsion.
A polyvinyl alcohol antibacterial hydrogel is prepared by weighing 4g of polyvinyl alcohol, weighing 50ml of distilled water, stirring and dissolving at 90 ℃, slowly adding 3g of boric acid, adding 2g of potassium hydroxide after complete dissolution, adding 16g of graphene nano-knife paste, adding 25g of distilled water, stirring at a high speed for 8 hours at 30 ℃, standing for 48 hours, and washing with distilled water to be neutral.
Example 2
An antibacterial graphene nano-knife is prepared from the following raw materials in parts by weight: 100g of natural graphite, 262.5g of sulfuric acid, nitric acid: 87.5g, 350g of salicylate, 30g g of EDTA, 9870g of water and 30g of white vermiculite.
The preparation method of the antibacterial graphene nanometer knife comprises the following steps:
(1) adding natural graphite (80 meshes) into acid liquor, adding an intercalation agent at the solution temperature of 65 ℃, then stirring for 24h, filtering, washing residues with 18 wt% hydrochloric acid until no sulfate is detected, washing the residues with deionized water until the pH value is 7, and then drying for 38h at 100 ℃ to obtain intercalated graphite;
(2) placing the intercalated graphite in microwave equipment, introducing nitrogen, and performing microwave treatment for 1 minute to prepare expanded graphite;
(3) adding the dispersing agent into the liquid carrier, and uniformly stirring to prepare a mixed solution;
(4) adding 50g of the expanded graphite prepared in the step (2) into the mixed solution prepared in the step (3) to prepare mixed solution;
(5) adding phyllosilicate into the mixed material liquid prepared in the step (4), and performing high-speed fluid clash for 5min by using high-jet equipment, wherein the clash fluid speed is 50 m/s, so as to obtain a multilayer graphene mixed liquid;
(6) and (4) carrying out suction filtration or centrifugal concentration on the multilayer graphene mixed solution prepared in the step (5) to prepare the antibacterial graphene nanometer knife with the solid content of 3%.
16.0g of white oil, 8.0g of caprylic triglyceride, 3.0g of isononyl alcohol ester, 2.5g of olive oil, 2.0g of glyceryl monostearate, 3.0g of polyglycerol ester, 5.0g of lauryl ether phosphate and 0.5g of essence are respectively weighed, 16g of antibacterial graphene nano knife, 1g of medical stone and 44g of deionized water are added, and the mixture is placed into a high-speed stirrer to be fully stirred for 30min to prepare the facial cleanser emulsion.
A polyvinyl alcohol antibacterial hydrogel is prepared by weighing 4g of polyvinyl alcohol, weighing 50ml of distilled water, stirring and dissolving at 90 ℃, slowly adding 3g of boric acid, adding 2g of potassium hydroxide after complete dissolution, adding 16g of graphene nano-knife paste, adding 25g of distilled water, stirring at a high speed for 8 hours at 30 ℃, standing for 48 hours, and washing with distilled water to be neutral.
Comparative example 1
16.0g of white oil, 8.0g of caprylic triglyceride, 3.0g of isononyl alcohol ester, 2.5g of olive oil, 2.0g of glyceryl monostearate, 3.0g of polyglycerol ester, 5.0g of lauryl ether phosphate, 0.5g of essence, 2g of medical stone and 44g of deionized water are respectively weighed and put into a high-speed stirrer to be fully stirred for 30min, so that the facial cleanser emulsion is prepared.
A polyvinyl alcohol antibacterial hydrogel is prepared by weighing 4g of polyvinyl alcohol, weighing 50ml of distilled water, stirring and dissolving at 90 ℃, slowly adding 3g of boric acid, adding 2g of potassium hydroxide after complete dissolution, adding 25g of distilled water, stirring at a high speed for 8 hours at 30 ℃, standing for 48 hours, and washing with distilled water to be neutral.
Bacteriostatic tests were performed on the antibacterial graphene nanopitch, facial cleanser and hydrogel obtained in examples 1-2 and comparative example 1, and the results are shown in table 1.
TABLE 1 results of bacteriostasis
| Antibacterial rate of antibacterial graphene nano knife | Bacteriostatic ratio (%) of facial cleanser | Hydrogel bacteriostatic ratio (%) | |
| Example 1 | 99 | 98 | 99 |
| Example 2 | 96 | 95 | 96 |
| Comparative example 1 | - | 2 | 1 |
As can be seen from table 1, the graphene nanoputter has an obvious effect in the antibacterial field, and the addition of the phyllosilicate has a synergistic effect on the graphene nanoputter, so that the phyllosilicate is reduced, and the antibacterial effect of the nanoputter is slightly reduced.
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 that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An antibiotic graphite alkene nanometer sword which characterized in that: the nanometer knife is prepared from the following raw materials in parts by weight:
2. the antimicrobial graphene nanopitch of claim 1, wherein: the intercalation agent is at least one of salicylic acid, salicylate, peroxyacetic acid, glycolic acid or citric acid; the dispersant is at least one of polyoxyethylene, polyethylene glycol, chitosan or EDTA; the phyllosilicate is white vermiculite.
3. The antimicrobial graphene nanopitch of claim 1, wherein: the particle size of the graphite is 10-50 μm; the liquid carrier is at least one of water or glycerol; the acid solution is a mixed solution of concentrated sulfuric acid and fuming nitric acid, wherein the mass ratio of the concentrated sulfuric acid to the fuming nitric acid is 1-3: 1.
4. The method for preparing the antibacterial graphene nanoputter according to any one of claims 1 to 3, wherein: the method comprises the following steps:
(1) adding graphite into acid liquor, adding an intercalation agent at the solution temperature of 60-80 ℃, then stirring, filtering, washing residues with hydrochloric acid until no sulfate is detected, washing the residues with deionized water until the pH value is 5-7, and then drying to obtain intercalated graphite;
(2) placing the intercalated graphite in microwave equipment, introducing nitrogen, and carrying out microwave treatment for 1-3 minutes to prepare expanded graphite;
(3) adding the dispersing agent into the liquid carrier, and uniformly stirring to prepare a mixed solution;
(4) adding the expanded graphite prepared in the step (2) into the mixed liquid prepared in the step (3) to prepare mixed liquid;
(5) adding phyllosilicate into the mixed material liquid prepared in the step (4), and performing high-speed fluid clash by using high-jet equipment to obtain a multilayer graphene mixed liquid;
(6) and (4) carrying out suction filtration or centrifugal concentration on the multilayer graphene mixed solution prepared in the step (5) to prepare the antibacterial graphene nanometer knife.
5. The preparation method of the antibacterial graphene nanoputter according to claim 4, characterized in that: the stirring step in the step (1) is carried out for 24-48 hours; the mass fraction of the hydrochloric acid in the step (1) is 9-18 wt%; the temperature of the drying step in the step (1) is 60-120 ℃.
6. The preparation method of the antibacterial graphene nanoputter according to claim 4, characterized in that: the colliding fluid speed in the high-speed fluid colliding step in the step (5) is more than 50 m/s, and the colliding time is 5-10 min; and (4) the high-jet equipment in the step (5) is a high-pressure jet collider.
7. The preparation method of the antibacterial graphene nanoputter according to claim 4, characterized in that: the thickness of the nanometer knife is 1.7-50nm, the lamella spacing is 0.34-500nm, the D50 is 0.1-20um, and the Dmax is 10-100 um.
8. Use of the antibacterial graphene nanoputter according to any one of claims 1 to 3, characterized in that: the antibacterial graphene nano knife is applied to the preparation of washing and protecting products; the antibacterial graphene nano knife is applied to the preparation of facial cleanser; the antibacterial graphene nano knife is applied to preparation of medical hydrogel.
9. Use of the antibacterial graphene nanoputter according to claim 8, characterized in that: the facial cleanser comprises 0.01-6 parts of antibacterial graphene nano knife and 0.1-5 parts of cyclic silicate; the medical hydrogel comprises 0.01-6 parts of antibacterial graphene nano knife.
10. Use of the antibacterial graphene nanoputter according to claim 9, characterized in that: the cyclic silicate is medical stone.
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| CN202011058653.7A CN112174122A (en) | 2020-09-30 | 2020-09-30 | Antibacterial graphene nano knife and preparation method and application thereof |
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