CN112442893A - Special efficient nano copper antibacterial agent and preparation method thereof - Google Patents
Special efficient nano copper antibacterial agent and preparation method thereof Download PDFInfo
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- CN112442893A CN112442893A CN202011347855.3A CN202011347855A CN112442893A CN 112442893 A CN112442893 A CN 112442893A CN 202011347855 A CN202011347855 A CN 202011347855A CN 112442893 A CN112442893 A CN 112442893A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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Abstract
The invention relates to the technical field of bactericides, in particular to an ultra-high-efficiency nano copper antibacterial agent and a preparation method thereof, aiming at providing the ultra-high-efficiency nano copper antibacterial agent and the preparation method thereof, wherein the high-efficiency nano copper antibacterial agent has the performances of high antibacterial property, high washing resistance, low cost, environmental protection, extremely low consumption of antibacterial raw materials and the like; the ultra-high-efficiency nano copper antibacterial agent consists of core-shell type copper nano particles and phosphate buffer solution, wherein the core-shell type copper nano particles and the phosphate buffer solution comprise the core-shell type copper nano particles 1 multiplied by 10 in parts by weight‑7‑2×10‑5Preparing; 5-95 parts of phosphate buffer solution; the beneficial effects are that: the high-efficiency antibacterial rate of the ultra-high-efficiency nano copper antibacterial agent can reach more than 99 percent under the condition of extremely low copper addition amount. High-efficiency washable antibacterial textile and maximum washingThe frequency range is 10-100 times, and different application fields are met.
Description
Technical Field
The invention relates to the technical field of bactericides, in particular to an ultra-high-efficiency nano copper antibacterial agent and a preparation method thereof.
Background
In recent years, many bactericides have appeared on the market, mainly biocides and biostatic agents, leaching and binding bactericides, controlled release barriers and detergent-resistant agents. Biocides are capable of interrupting the regular metabolism of microorganisms and inhibiting their growth, thus imparting antibacterial and antifungal activity to cotton fabric fibers. Common in the textile industry is the leaching of biocides which do not chemically bond to cotton fabrics or fibers. In a humid environment, the leaching germicide is released gradually and continuously from the cotton fabric into the surrounding environment by a controlled release mechanism, and is effective for most bacteria and fungi, but the germicide cannot withstand repeated washing. Bound antimicrobials include antimicrobials that are chemically bound to the fiber surface and which act as a barrier to contact of the fiber surface with microorganisms. Compared with the leached bactericide, the combined bactericide has the obvious advantage of improving the washing fastness of the cotton fabric. In addition, the surface of the combined bactericide is treated in an environment-friendly way, and no toxic substances are released into the environment. Although both natural and organic fungicides can be used for surface modification of cotton fabrics, the most widely used cotton fabric fungicides are inorganic fungicides. Inorganic antibacterial agents are central to the research of antibacterial agents because of their high safety, heat resistance and durability. Because metals such as silver, copper, zinc and the like have antibacterial property, the metals such as silver, copper, zinc, gold and the like are loaded on the surface of the cotton fiber by adopting a simple physical adsorption or solution impregnation method to prepare the cotton fiber with the antibacterial function. In summary, in the textile industry, antibacterial cotton fibers have been used in the manufacture of household garments including undergarments, sportswear and military apparel. In medical applications, it can be used for the preparation of surgical lines, wound dressings and medical bandages.
Disclosure of Invention
The invention mainly aims to provide an ultra-high-efficiency nano copper antibacterial agent and a preparation method thereof, and the high-efficiency nano copper antibacterial agent has the performances of high antibacterial property, high washing resistance, low cost, environmental protection, extremely low antibacterial raw material consumption and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
the ultra-high-efficiency nano copper antibacterial agent is characterized by consisting of core-shell copper nanoparticles and phosphate buffer solution, wherein the core-shell copper nanoparticles and the phosphate buffer solution comprise the core-shell copper nanoparticles 1 multiplied by 10 in parts by weight-7-2×10-5Preparing; 5-95 parts of phosphate buffer solution;
the preparation method of the ultra-high-efficiency nano copper antibacterial agent comprises the step of obtaining the ultra-high-efficiency nano copper antibacterial agent by ultrasonic dispersion of core-shell copper nanoparticles and phosphate buffer solution.
The application of the highly effective nano copper antibacterial agent is that nano copper particles are attached to the coating and the textile to prepare the antibacterial coating and the antibacterial textile.
The invention has the beneficial effects that: 1. compared with widely used silver-based antibacterial agents, the antibacterial agent and the antibacterial textile prepared from the core-shell type nano copper particles have the advantages of simple process, low cost, environmental friendliness and low biotoxicity. 2. The high-efficiency antibacterial rate of the ultra-high-efficiency nano copper antibacterial agent can reach more than 99 percent under the condition of extremely low copper addition amount. The antibacterial textile is efficient and washable, the maximum washing frequency range is 10-100 times, and different application fields are met.
Drawings
FIG. 1 is a colony number chart of the antibacterial agent with different nano-copper contents co-cultured with Escherichia coli for 24h in the invention;
FIG. 2 is a colony number chart of the antibacterial agent with different nano-copper contents and staphylococcus aureus co-cultured for 24 hours in the invention;
FIG. 3 is a colony number diagram of 24h of co-culture of the antibacterial textile fabrics with different nano-copper contents and Escherichia coli bacteria in the invention;
FIG. 4 is a colony count chart of 24h of co-culture of the antibacterial textile with different nano-copper content and Staphylococcus aureus in the invention;
FIG. 5 is a colony count chart of the antibacterial textile with different nano-copper content co-cultured with Escherichia coli for 24h after being washed for different times;
FIG. 6 is a scanning transmission microscope image of a textile at different magnifications in accordance with the present invention.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
Unless otherwise specified, various starting materials of the present invention are commercially available; or prepared according to conventional methods in the art. Unless defined or indicated otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
The highly effective copper nano-particle liquid antibacterial agent consists of core-shell type copper nano-particles and phosphate buffer solution, wherein the concentration of nano-copper is 1 multiplied by 10 respectively-7g/ml、2×10-7g/ml、3×10-7g/ml、3.5×10- 7g/ml、4×10-7g/ml; during preparation, 0.01g, 0.02g, 0.03g, 0.035g and 0.04g of nano-copper particles are respectively weighed, 5mL of PBS buffer solution is injected into a centrifuge tube, the nano-copper powder is respectively added, and ultrasonic dispersion is carried out for 10 min. By dilution, the final concentration is 1 × 10-7g/ml、2×10-7g/ml、3×10-7g/ml、3.5×10-7g/ml、4×10-7g/ml of nano copper antibacterial agent.
The antibacterial agents prepared in this example have different antibacterial rates at different concentrations. As shown in FIG. 1, the concentration of nano-copper is 1X 10-7g/ml、2×10-7g/ml、3×10-7g/ml、4×10-7The antibacterial rate of the antibacterial agent in g/ml to Escherichia coli for 24h is 77.2%, 92.0%, 97.6% and 100% respectively; as shown in fig. 2, the concentration for nano-copper is 2 × 10-7g/ml、3×10- 7g/ml、3.5×10-7g/ml、4×10-7The antibacterial rate of the gram/ml antibacterial agent to staphylococcus aureus for 24h is 92.9%, 98.7%, 99.6% and 100%, respectively. The copper addition of the antibacterial agent of the embodiment is in the order of one million, the cost is low, and the antibacterial performance is strong.
Example 2
The antibacterial textile is made of core-shell type copper nanoparticles serving as a main antibacterial material, is attached to the surface and the inside of textile fibers through an ultrasonic technology, and is simple in process and environment-friendly. The nano-copper concentration of the prepared high-efficiency copper nano-particle antibacterial textile is respectively 8 multiplied by 10-7g/ml、1×10-6g/ml、2×10-6g/ml. In preparation, the concentration was 8X 10 according to the method of example 1-7g/ml、1×10-6g/ml、2×10-6100ml of each g/ml of nano-copper dispersion liquid is subjected to ultrasonic treatment for 10min to uniformly disperse the nano-copper dispersion liquid, and then 1g of each boiled and cleaned textile is respectively put into the nano-copper dispersion liquid and subjected to ultrasonic treatment for 20 min. Finally, washing and airing by distilled water to obtain the ultra-high-efficiency nano-copper antibacterial textile.
The prepared antibacterial textile has high-efficiency antibacterial performance, and the treatment concentrations of copper are respectively 8 multiplied by 10 as shown in figure 3-7g/ml、1×10-6g/ml、2×10-6The antibacterial rate of the g/ml textile to 24h of escherichia coli is 76.0%, 92.0% and 100% respectively; as shown in FIG. 4, the antibacterial rate against Staphylococcus aureus for 24h was 88.9%, 100%, and 100%, respectively. Because the dosage of the nano copper particles is in the order of one millionth, the color, the luster and the elasticity of the original textile are not influenced after the treatment, the cost is low, and the method is suitable for large-scale popularization.
Example 3
The high-washable copper nanoparticle antibacterial textile has high-efficiency antibacterial propertyOn the basis, the fabric also has high washing resistance. Aiming at 50 times of washing resistance promoted in the current market, the antibacterial textile achieves 100 times of washing without failure. According to the raw material characteristics and the processing method of the embodiment, the washing can be carried out for 200 times, 500 times or even 1000 times without failure, and different use requirements in the civil market and the military field can be widely met. Considering the loss of antibacterial material before and after washing, on the basis of keeping the textile characteristics unchanged, the treatment concentrations of copper of 5X 10 respectively were developed-6g/ml、1×10-5g/ml、2×10-5g/ml high washing-resistant antibacterial textile. The preparation method is the same as example 2. Because the addition of copper is in the order of one hundred thousand, the product still has the characteristics of high-efficiency antibiosis and no change of the characteristics of the original textile.
The textile is washed by a simulated washing machine, 0.25g of soap is added into every 50ml of distilled water as washing liquid, 1g of antibacterial textile is added into every 50ml of washing liquid, magnetic stirring treatment is carried out under the parameter of 400r/min, and 1 washing is carried out every 15 min. And (4) after washing, carrying out the detection of the residual antibacterial performance by using a plate counting method. As shown in FIG. 5, the concentrations for the copper treatment were 5X 10, respectively-6g/ml、1×10-5g/ml、2×10-5The maximum washing times of the high-washable antibacterial textile per ml are respectively 10 times, 50 times and 100 times, and the escherichia coli resistant rates after washing are respectively 92.86%, 85.79% and 99.6%.
Analyzing the antibacterial textile by using a scanning electron microscope and an X-ray energy spectrum to prove that the nano-copper is successfully attached to the textile fiber; FIG. 6(a) - (d) are scanning transmission microscope images of the nano-copper antibacterial textile at different magnifications; FIG. 6(e) - (h) are scanning transmission microscope images of the common textile under different magnifications.
The antibacterial performance of the antibacterial agent is characterized by a flat plate counting method, and the antibacterial rate of different antibacterial agents and antibacterial textiles reaches 76-100 percent.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. The ultra-high-efficiency nano copper antibacterial agent is characterized by consisting of core-shell copper nanoparticles and phosphate buffer solution, wherein the core-shell copper nanoparticles and the phosphate buffer solution comprise the core-shell copper nanoparticles 1 multiplied by 10 in parts by weight-7-2×10-5Preparing; 5-95 parts of phosphate buffer solution;
the preparation method of the ultra-high-efficiency nano copper antibacterial agent comprises the step of obtaining the ultra-high-efficiency nano copper antibacterial agent by ultrasonic dispersion of core-shell copper nanoparticles and phosphate buffer solution.
2. The application of the highly effective nano copper antibacterial agent is that nano copper particles are attached to the coating and the textile to prepare the antibacterial coating and the antibacterial textile.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113954402A (en) * | 2021-09-30 | 2022-01-21 | 江苏佰家丽新材料科技有限公司 | Manufacturing method of antibacterial sound-absorbing board and antibacterial sound-absorbing board |
| CN115413674A (en) * | 2022-09-09 | 2022-12-02 | 兰州大学 | Nano-copper antibacterial agent for fusarium trilorum |
| CN116218071A (en) * | 2023-03-15 | 2023-06-06 | 佛山市瑞志医疗科技有限公司 | EVA antibacterial insole and preparation method thereof |
| CN116267989A (en) * | 2022-09-09 | 2023-06-23 | 兰州大学 | Nanometer iron antibacterial agent for fusarium trilineum |
| WO2023132756A1 (en) * | 2022-01-07 | 2023-07-13 | Nairotech Desarrollo E Innovación S.A. | Suspended metal nanoparticle |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113954402A (en) * | 2021-09-30 | 2022-01-21 | 江苏佰家丽新材料科技有限公司 | Manufacturing method of antibacterial sound-absorbing board and antibacterial sound-absorbing board |
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| CN115413674A (en) * | 2022-09-09 | 2022-12-02 | 兰州大学 | Nano-copper antibacterial agent for fusarium trilorum |
| CN115413674B (en) * | 2022-09-09 | 2023-03-31 | 兰州大学 | Nano-copper antibacterial agent for fusarium trilorum |
| CN116267989A (en) * | 2022-09-09 | 2023-06-23 | 兰州大学 | Nanometer iron antibacterial agent for fusarium trilineum |
| CN116267989B (en) * | 2022-09-09 | 2024-05-07 | 兰州大学 | Nanometer iron antibacterial agent for fusarium trilineum |
| CN116218071A (en) * | 2023-03-15 | 2023-06-06 | 佛山市瑞志医疗科技有限公司 | EVA antibacterial insole and preparation method thereof |
| CN116218071B (en) * | 2023-03-15 | 2023-11-21 | 佛山市瑞志医疗科技有限公司 | EVA antibacterial insole and preparation method thereof |
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