CN115336592A - Preparation method of nano copper oxide antibacterial material - Google Patents
Preparation method of nano copper oxide antibacterial material Download PDFInfo
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- CN115336592A CN115336592A CN202210853922.1A CN202210853922A CN115336592A CN 115336592 A CN115336592 A CN 115336592A CN 202210853922 A CN202210853922 A CN 202210853922A CN 115336592 A CN115336592 A CN 115336592A
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- copper oxide
- nano copper
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/14—Boron; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a preparation method of a nano copper oxide antibacterial material, which comprises the following steps: sodium borate is used as a precipitator, a copper acetate solution and a sodium borate solution are mixed according to a certain proportion, a surfactant cetyl trimethyl ammonium bromide is dripped into the mixture, the mixture is ultrasonically dispersed by an ultrasonic instrument and then is moved into a high-pressure reaction kettle to react under a certain hydrothermal condition, and the nano copper oxide particles are prepared. The nano copper oxide particles prepared by the method are in a special water drop shape, have a sharp-angled structure, are small in particle size, narrow in distribution and good in dispersity, and have stronger penetrability on microbial cell membranes and more excellent antibacterial performance compared with common spherical nano copper oxide particles.
Description
Technical Field
The invention belongs to the technical field of antibacterial materials, and particularly relates to a preparation method of a nano copper oxide antibacterial material.
Background
Common copper oxide is mostly used as a colorant and pigment of ceramics and glass to manufacture artificial gems, colored glass and the like; in addition, the copper oxide can also be used as an anti-wrinkling agent, a bactericide and a metallurgical reagent of the paint. The copper oxide has wide application in industrial production, when the particle size of the copper oxide powder reaches the nanometer level, the copper oxide powder can show unique performance due to the influence of small size effect, macroscopic quantum tunnel effect, surface effect and volume effect, and has special physical and chemical properties in the aspects of light absorption, thermal resistance, magnetism, melting point, chemical activity and the like, and meanwhile, the nano copper oxide particles also have the remarkable characteristics of no toxicity, environmental protection, high stability, recyclability and the like, so that the copper oxide powder can be more widely applied in the fields of science, engineering, pharmacy and the like.
The textile is easy to breed microorganisms, microbial communities in the nature widely exist in the surrounding environment, once the textile meets appropriate humidity, nutrients and temperature, the microorganisms bred on the textile not only affect the use performance of the textile, but also damage the body health of a user, and therefore how to inhibit or kill the microorganisms attached to the textile is a problem which needs to be solved urgently in the textile industry. As an inorganic material, the nano copper oxide not only has excellent antibacterial performance, but also meets the requirements of people on health and environmental protection, so that the nano copper oxide is more and more valued and has huge market potential.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a nano copper oxide antibacterial material, and the nano copper oxide particles prepared by the method are in a special water drop shape, have a sharp-angled structure, small particle size, narrow distribution and good dispersibility, and have stronger penetrability on microbial cell membranes and more excellent antibacterial performance compared with common spherical nano copper oxide particles.
The invention provides a preparation method of a nano copper oxide antibacterial material, which comprises the following steps:
the method comprises the following steps: respectively weighing copper acetate solid and sodium borate solid, adding deionized water, and stirring on a magnetic stirrer until the solids are completely dissolved to obtain copper acetate aqueous solution and sodium borate aqueous solution;
step two: adding the sodium borate solution into the copper acetate solution which is continuously stirred, and carrying out ultrasonic dispersion for 15min in an ultrasonic instrument at the temperature of 30 ℃;
step three: dropwise adding a surfactant cetyl trimethyl ammonium bromide solution into the mixed solution prepared in the second step, and ultrasonically dispersing for 15min in an ultrasonic instrument at the temperature of 30 ℃;
step four: and (4) transferring the blue mixed solution prepared in the third step into a reaction kettle, naturally cooling to room temperature after reaction to obtain a product, centrifuging, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the black nano-copper oxide powder.
Preferably, in step one, the sodium borate solid is sodium tetraborate decahydrate crystalline.
Preferably, in the first step, the molar ratio of the copper acetate to the sodium borate is 1 (10-20).
Preferably, in the second step and the third step, the ultrasonic dispersion frequency of the ultrasonic instrument is 60 to 100kHz.
Preferably, in the third step, the mole ratio of the surfactant cetyl trimethyl ammonium bromide to the copper acetate is 1 (80-100).
Preferably, in the third step, the dropping speed of the surfactant cetyl trimethyl ammonium bromide is 30-40 drops/min.
Preferably, in the fourth step, the reaction temperature in the reaction kettle is 160-200 ℃ and the time is 10-12 h.
Preferably, in the fourth step, the centrifugal rate is 10000-30000 rpm.
The invention has the following beneficial effects:
(1) The invention selects sodium borate as a precipitator, adds a surfactant cetyl trimethyl ammonium bromide, and prepares nano copper oxide particles in a special drop shape under certain hydrothermal conditions. The antibacterial principle of copper oxide is that the copper surface and the bacterial outer membrane directly interact to break the bacterial outer membrane, and the copper oxide enters the cell from the broken hole to block the metabolism of the cell, so that the bacteria can not breathe, eat, digest and generate energy until the bacteria shrink. Compared with the common spherical copper oxide particles, the water-drop-shaped copper oxide particles have a sharp-angled structure, small particle size, narrow distribution, good dispersibility, a large head and a rapidly contracted tail, so that the resistance of the particles entering the interior of bacteria is smaller, the speed is higher, the death of the bacteria is accelerated, and the antibacterial property is more excellent.
(2) The sodium borate has the effects of sterilization and disinfection, has the inhibiting effect on microorganisms such as escherichia coli, staphylococcus aureus, bacillus anthracis, candida albicans and the like, has quite wide application in washing products, cosmetics and medical treatment, is used as a precipitator to prepare nano copper oxide, can cooperate with copper oxide to exert antibacterial and bacteriostatic properties, and has more excellent antibacterial property.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a TEM image of the water-drop-shaped nano copper oxide particles prepared by the present invention.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A preparation method of a nano copper oxide antibacterial material comprises the following steps:
(1) Weighing copper acetate solid and sodium borate solid according to a molar ratio of 1;
(2) Adding the sodium borate solution into the copper acetate solution which is continuously stirred, and ultrasonically dispersing for 15min in an ultrasonic instrument at the temperature of 30 ℃;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of the cetyl trimethyl ammonium bromide to copper acetate of 1;
(4) And (4) transferring the blue mixed solution prepared in the step (3) into a reaction kettle, reacting at 160 ℃ for 10 hours, naturally cooling to room temperature after reaction to obtain a product, centrifuging, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain black nano copper oxide powder.
Example 2
A preparation method of a nano copper oxide antibacterial material comprises the following steps:
(1) Weighing copper acetate solid and sodium borate solid according to a molar ratio of 1;
(2) Adding the sodium borate solution into the copper acetate solution which is continuously stirred, and ultrasonically dispersing for 15min in an ultrasonic instrument at the temperature of 30 ℃;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of the cetyl trimethyl ammonium bromide to copper acetate of 1;
(4) And (3) transferring the blue mixed solution prepared in the step (3) into a reaction kettle, reacting for 11h at 180 ℃, naturally cooling to room temperature after reaction to obtain a product, centrifuging the product, alternately washing the product with deionized water and absolute ethyl alcohol for three times, and drying the precipitate for 5h at 60 ℃ in a vacuum drying oven to obtain the black nano copper oxide powder.
Example 3
A preparation method of a nano copper oxide antibacterial material comprises the following steps:
(1) Weighing copper acetate solid and sodium borate solid according to a molar ratio of 1;
(2) Adding the sodium borate solution into the copper acetate solution which is continuously stirred, and carrying out ultrasonic dispersion for 15min in an ultrasonic instrument at the temperature of 30 ℃;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of the cetyl trimethyl ammonium bromide to copper acetate of 1;
(4) And (3) transferring the blue mixed solution prepared in the step (3) into a reaction kettle, reacting for 12 hours at 200 ℃, naturally cooling to room temperature after reaction to obtain a product, centrifuging the product, alternately washing the product with deionized water and absolute ethyl alcohol for three times, and drying the precipitate in a vacuum drying oven for 5 hours at 60 ℃ to obtain the black nano copper oxide powder.
Comparative example 1
(1) Weighing the solid copper acetate and the solid sodium hydroxide according to a molar ratio of 1;
(2) Adding sodium hydroxide solution into copper acetate solution under stirring, and ultrasonically dispersing in an ultrasonic instrument at 30 deg.C for 15min;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of the cetyl trimethyl ammonium bromide to copper acetate of 1;
(4) And (3) transferring the blue mixed solution prepared in the step (3) into a reaction kettle, reacting for 11h at 180 ℃, naturally cooling to room temperature after reaction to obtain a product, centrifuging the product, alternately washing the product with deionized water and absolute ethyl alcohol for three times, and drying the precipitate for 5h at 60 ℃ in a vacuum drying oven to obtain the black nano copper oxide powder.
Comparative example 2
(1) Weighing copper acetate solid and sodium borate solid according to a molar ratio of 1;
(2) Adding the sodium borate solution into the copper acetate solution which is continuously stirred, and carrying out ultrasonic dispersion for 15min in an ultrasonic instrument at the temperature of 30 ℃;
(3) And (3) transferring the blue mixed solution prepared in the step (2) into a reaction kettle, reacting for 11h at 180 ℃, naturally cooling to room temperature after reaction to obtain a product, centrifuging the product, alternately washing the product with deionized water and absolute ethyl alcohol for three times, and drying the precipitate for 5h at 60 ℃ in a vacuum drying oven to obtain the black nano copper oxide powder.
The reactant ratios and reaction conditions of inventive examples 1 to 3 and comparative examples 1 to 2 are shown in Table 1.
TABLE 1 reactant proportions and reaction conditions for examples 1-3 and comparative examples 1-2
The nano copper oxide particles obtained in the above examples 1 to 3 and comparative examples 1 to 2 were subjected to a sedimentation test to analyze the dispersibility thereof. The settling velocity of particles in a dispersion medium is related to the size and mass of the particles, with large particles settling at a high rate and small particles settling at a low rate. Nanoparticles are small in size, have a very large specific surface area per unit volume, rapidly increase the number of surface atoms due to a sharp increase in surface area, and have a tendency to attract each other to stabilize them because of their high activity and extremely unstable state due to the increased number of surface atoms, insufficient coordination of atoms and high surface energy, which tends to make the particles easily agglomerate. Therefore, the dispersibility of the nano copper oxide in the aqueous solution and the agglomeration condition of the particles can be qualitatively judged through the complete settling time, and the longer the complete settling time is, the better the dispersibility is and the less agglomeration is caused among the particles. The following table 2 is a result of performing a settling experiment on the nano copper oxide particles obtained in examples 1 to 3 and comparative examples 1 to 2.
TABLE 2 complete settling time of the products of examples 1 to 3 and comparative examples 1 to 2
| Complete settling time/h | |
| Example 1 | 36 |
| Example 2 | 40 |
| Example 3 | 35 |
| Comparative example 1 | 24 |
| Comparative example 2 | 15 |
As can be seen from Table 2, the particles of examples 1 to 3 have longer complete settling time, when the molar ratio of copper acetate to sodium borate is 1:15, the molar ratio of the surfactant cetyl trimethyl ammonium bromide to copper acetate is 1:90, the reaction temperature of the reaction kettle is 180 ℃, and the reaction time is 11h, the obtained nano copper oxide particles have the longest complete settling time in the aqueous solution and the best dispersibility; comparative example 1 spherical nano copper oxide is prepared by using sodium hydroxide as a precipitator, and the dispersibility is general; comparative example 2 does not add cetyl trimethyl ammonium bromide as a surfactant, and the complete settling time of the nano copper oxide particles in the aqueous solution is short, and the dispersibility is poor.
Table 3 shows the antibacterial properties of nylon fibers prepared from the nano copper oxide particles obtained in examples 1 to 3 and comparative examples 1 to 2. As can be seen from Table 3, in examples 1-3, no bacterial colony is found on the surface of the culture dish in both Escherichia coli and Staphylococcus aureus, which indicates that the sterilization rate reaches 100%, and the water-drop-shaped nano copper oxide prepared by the invention has excellent antibacterial performance; comparative example 1 is spherical nanometer copper oxide prepared by using sodium hydroxide as a precipitator, and comparative example 2 is not added with surfactant cetyl trimethyl ammonium bromide, so that the prepared nylon fiber has the advantages that bacterial colony survival is found, and the antibacterial performance is general.
TABLE 3 antibacterial Properties of Polyamide fibers prepared in examples 1 to 3 and comparative examples 1 to 2
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (8)
1. A preparation method of a nano copper oxide antibacterial material is characterized by comprising the following steps:
the method comprises the following steps: respectively weighing copper acetate solid and sodium borate solid, adding deionized water, and stirring on a magnetic stirrer until the solids are completely dissolved to obtain copper acetate aqueous solution and sodium borate aqueous solution;
step two: adding the sodium borate solution into the copper acetate solution which is continuously stirred, and ultrasonically dispersing for 15min in an ultrasonic instrument at the temperature of 30 ℃;
step three: dropwise adding a surfactant cetyl trimethyl ammonium bromide solution into the mixed solution prepared in the second step, and performing ultrasonic dispersion for 15min in an ultrasonic instrument at the temperature of 30 ℃;
step four: and (4) transferring the blue mixed solution prepared in the third step into a reaction kettle, naturally cooling to room temperature after reaction to obtain a product, centrifuging, alternately washing with deionized water and absolute ethyl alcohol for three times, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the black nano-copper oxide powder.
2. The method for preparing a nano copper oxide antibacterial material according to claim 1, wherein in the first step, the sodium borate solid is sodium tetraborate decahydrate crystal.
3. The preparation method of the nano copper oxide antibacterial material according to claim 1, wherein in the first step, the molar ratio of the copper acetate to the sodium borate is 1 (10 to 20).
4. The method for preparing the nano copper oxide antibacterial material according to claim 1, wherein in the second step and the third step, the frequency of the ultrasonic instrument during ultrasonic dispersion is 60 to 100kHz.
5. The preparation method of the nano copper oxide antibacterial material according to claim 1, characterized in that in the third step, the molar ratio of the surfactant cetyl trimethyl ammonium bromide to the surfactant copper acetate is 1 (80 to 100).
6. The preparation method of the nano copper oxide antibacterial material according to claim 1, characterized in that in the third step, the dropping speed of the surfactant cetyl trimethyl ammonium bromide is 30 to 40 drops/min.
7. The preparation method of the nano copper oxide antibacterial material according to claim 1, characterized in that in the fourth step, the reaction temperature in the reaction kettle is 160-200 ℃ and the reaction time is 10h to 12h.
8. The method for preparing the nano copper oxide antibacterial material according to claim 1, wherein in the fourth step, the centrifugal rate is 10000 to 30000rpm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030051580A1 (en) * | 2001-01-31 | 2003-03-20 | Lewis Kenrick M. | Preparation of nanosized copper and copper compounds |
| WO2014196881A1 (en) * | 2013-06-03 | 2014-12-11 | Eko-Styl Sp. Z O. O. | Method of wet washing to produce biocide textiles |
| CN106732668A (en) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials |
| US20190255730A1 (en) * | 2016-06-10 | 2019-08-22 | Prestech Limited | Submicron particle compositions |
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- 2022-07-20 CN CN202210853922.1A patent/CN115336592B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030051580A1 (en) * | 2001-01-31 | 2003-03-20 | Lewis Kenrick M. | Preparation of nanosized copper and copper compounds |
| WO2014196881A1 (en) * | 2013-06-03 | 2014-12-11 | Eko-Styl Sp. Z O. O. | Method of wet washing to produce biocide textiles |
| US20190255730A1 (en) * | 2016-06-10 | 2019-08-22 | Prestech Limited | Submicron particle compositions |
| CN106732668A (en) * | 2016-11-18 | 2017-05-31 | 中国计量大学 | A kind of hydrothermal preparing process of flower-shaped molybdenum bisuphide/cupric oxide composite nano materials |
Non-Patent Citations (4)
| Title |
|---|
| GÜNER ET AL.: ""SYNTHESIS AND CHARACTERIZATION OF COPPER HYDROXYNITRATE AND COPPER OXIDE BY HYDROTHERMAL METHOD"", 《JOTCSB》 * |
| ISSA M. EL-NAHHAL ET AL.: ""The efficacy of surfactants in stabilizing coating of nano-structured CuO particles onto the surface of cotton fibers and their antimicrobial activity"", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| 付育才: ""纳米氧化铜的制备及其性质的研究"", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技Ⅰ辑》 * |
| 朱刚等: ""不同形貌CuO的制备与表征"", 《硅酸盐通报》 * |
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