CN115336592B - Preparation method of nano copper oxide antibacterial material - Google Patents

Preparation method of nano copper oxide antibacterial material Download PDF

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Publication number
CN115336592B
CN115336592B CN202210853922.1A CN202210853922A CN115336592B CN 115336592 B CN115336592 B CN 115336592B CN 202210853922 A CN202210853922 A CN 202210853922A CN 115336592 B CN115336592 B CN 115336592B
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copper oxide
nano copper
sodium borate
antibacterial material
solution
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CN115336592A (en
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吴惠民
余丽玲
彭超
力伟
林宇霖
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Fuzhou Fusu Science And Technology Research Institute Co ltd
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 preparation 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 transferred 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 angle structure, small particle size, narrow distribution and good dispersibility, have stronger penetrability to microbial cell membranes and have more excellent antibacterial performance compared with the common spherical nano copper oxide particles.

Description

Preparation method of nano copper oxide antibacterial material
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 precious stones, 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 paint. Copper oxide has wide application in industrial production, when the particle size of 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 tunneling effect, surface effect and volume effect, and shows special physical and chemical properties in the aspects of light absorption, thermal resistance, magnetism, melting point, chemical activity and the like, and meanwhile, the nanometer copper oxide particle also has the remarkable characteristics of no toxicity, environmental protection, high stability, recycling and the like, so that the copper oxide powder is widely applied to the fields of science, engineering, pharmacy and the like.
The textile is easy to grow microorganisms, microbial communities in nature widely exist in the surrounding environment, once proper humidity, nutrients and temperature are met, the microorganisms growing on the textile can rapidly grow, the service performance of the textile is affected, the physical health of a user is damaged, and therefore, how to inhibit or kill the microorganisms attached to the textile is an urgent problem to be solved by the textile industry. The nano copper oxide is used as an inorganic material, has excellent antibacterial property, meets the requirements of people on health and environmental protection, and therefore is more and more important 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 angle structure, small particle size, narrow distribution and good dispersibility, and have stronger penetrability to microbial cell membranes and more excellent antibacterial performance than the common spherical nano copper oxide particles.
The invention provides a preparation method of a nano copper oxide antibacterial material, which comprises the following steps:
step one: respectively weighing copper acetate solid and sodium borate solid, adding deionized water, and placing on a magnetic stirrer to stir until the solids are completely dissolved, thereby obtaining copper acetate aqueous solution and sodium borate aqueous solution;
step two: adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
step three: dripping a surfactant cetyl trimethyl ammonium bromide solution into the mixed solution prepared in the step two, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
step four: transferring the blue mixed solution prepared in the third step into a reaction kettle, naturally cooling to room temperature after reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
Preferably, in the first step, the sodium borate solid is sodium tetraborate decahydrate crystals.
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 frequency of the ultrasonic instrument during ultrasonic dispersion is 60-100 kHz.
Preferably, in the third step, the molar ratio of the hexadecyl trimethyl ammonium bromide to the copper acetate serving as the surfactant is 1 (80-100).
Preferably, in the third step, the dripping speed of the hexadecyl trimethyl ammonium bromide serving as the surfactant is 30-40 drops/min.
Preferably, in the fourth step, the reaction temperature in the reaction kettle is 160-200 ℃ and the reaction time is 10-12 h.
Preferably, in step four, the centrifugation rate is 10000 to 30000rpm.
The invention has the following beneficial effects:
(1) The invention selects sodium borate as a precipitator, adds hexadecyl trimethyl ammonium bromide as a surfactant, prepares nano copper oxide particles under certain hydrothermal conditions, and takes the form of special water drops. The principle of copper oxide antibiosis is that the copper surface and the outer bacterial membrane directly interact to break the outer bacterial membrane, and the copper oxide enters the inside of cells from the broken holes to obstruct the metabolism of the cells, so that the bacteria cannot breathe, eat, digest and produce energy until atrophy. Compared with the common spherical copper oxide particles, the water-drop-shaped copper oxide particles have the advantages of sharp angle structure, small particle size, narrow distribution, good dispersibility, large head and rapidly contracted tail, so that the resistance of entering the inside of bacteria is smaller, the speed is higher, the bacterial death is accelerated, and the water-drop-shaped copper oxide particles have more excellent antibacterial performance.
(2) The sodium borate has the functions of sterilization and disinfection, has the inhibition 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, adopts the sodium borate as a precipitator to prepare nano copper oxide, and can cooperate with the copper oxide to exert the antibacterial performance, and the prepared copper oxide has more excellent antibacterial performance.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a TEM image of water-droplet-shaped nano copper oxide particles produced by the present invention.
Detailed Description
The present invention will be described in more detail by way of specific examples, but the scope of the present invention is not limited to these examples.
Example 1
The preparation process of nanometer copper oxide as antiseptic material includes the following steps:
(1) Weighing copper acetate solids and sodium borate solids according to a molar ratio of 1:10, respectively dissolving the copper acetate solids and the sodium borate solids in 30mL of deionized water, and placing the deionized water on a magnetic stirrer for stirring until the solids are completely dissolved to obtain a copper acetate aqueous solution and a sodium borate aqueous solution;
(2) Adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of 1:100 with copper acetate, adding 20mL of deionized water to prepare a solution, dripping the solution into the mixed solution prepared in the step 2, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(4) Transferring the blue mixed solution prepared in the step 3 into a reaction kettle, reacting for 10 hours at 160 ℃, naturally cooling to room temperature after the reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
Example 2
The preparation process of nanometer copper oxide as antiseptic material includes the following steps:
(1) Weighing copper acetate solids and sodium borate solids according to a molar ratio of 1:15, respectively dissolving the copper acetate solids and the sodium borate solids in 30mL of deionized water, and placing the deionized water on a magnetic stirrer for stirring until the solids are completely dissolved to obtain a copper acetate aqueous solution and a sodium borate aqueous solution;
(2) Adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of 1:90 with copper acetate, adding 20mL of deionized water to prepare a solution, dripping the solution into the mixed solution prepared in the step 2, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(4) Transferring the blue mixed solution prepared in the step 3 into a reaction kettle, reacting for 11 hours at 180 ℃, naturally cooling to room temperature after the reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
Example 3
The preparation process of nanometer copper oxide as antiseptic material includes the following steps:
(1) Weighing copper acetate solids and sodium borate solids according to a molar ratio of 1:20, respectively dissolving the copper acetate solids and the sodium borate solids in 30mL of deionized water, and placing the deionized water on a magnetic stirrer for stirring until the solids are completely dissolved to obtain a copper acetate aqueous solution and a sodium borate aqueous solution;
(2) Adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of 1:80 with copper acetate, adding 20mL of deionized water to prepare a solution, dripping the solution into the mixed solution prepared in the step 2, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(4) 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 the reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
Comparative example 1
(1) Weighing copper acetate solids and sodium hydroxide solids according to a molar ratio of 1:15, respectively dissolving the copper acetate solids and the sodium hydroxide solids in 30mL of deionized water, and placing the deionized water on a magnetic stirrer for stirring until the solids are completely dissolved to obtain copper acetate aqueous solution and sodium hydroxide aqueous solution;
(2) Adding sodium hydroxide solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(3) Weighing a surfactant cetyl trimethyl ammonium bromide according to a molar ratio of 1:90 with copper acetate, adding 20mL of deionized water to prepare a solution, dripping the solution into the mixed solution prepared in the step 2, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(4) Transferring the blue mixed solution prepared in the step 3 into a reaction kettle, reacting for 11 hours at 180 ℃, naturally cooling to room temperature after the reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
Comparative example 2
(1) Weighing copper acetate solids and sodium borate solids according to a molar ratio of 1:15, respectively dissolving the copper acetate solids and the sodium borate solids in 30mL of deionized water, and placing the deionized water on a magnetic stirrer for stirring until the solids are completely dissolved to obtain a copper acetate aqueous solution and a sodium borate aqueous solution;
(2) Adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
(3) Transferring the blue mixed solution prepared in the step 2 into a reaction kettle, reacting for 11 hours at 180 ℃, naturally cooling to room temperature after the reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain the nano copper oxide black powder.
The ratios of the reactants and the reaction conditions of examples 1 to 3 and comparative examples 1 to 2 of the present invention are shown in Table 1.
TABLE 1 reactant ratios and reaction conditions for examples 1-3 and comparative examples 1-2
The nano copper oxide particles obtained in examples 1 to 3 and comparative examples 1 to 2 were subjected to a sedimentation experiment to analyze the dispersibility thereof. The sedimentation velocity of particles in a dispersion medium is related to the size and mass of the particles, and the sedimentation velocity of large particles is high and the sedimentation velocity of small particles is low. The nanoparticle size is small, the specific surface per unit volume is very large, the surface atomic number is rapidly increased by the rapid increase of the surface area, and the surface atomic number is increased, and the atomic coordination is insufficient and the surface energy is very high, so that the surface atoms have high activity and are in a very unstable state, and thus the particles tend to be attracted to each other to be stable, and the particles tend to be easily agglomerated. Therefore, the dispersibility of the nano copper oxide in the aqueous solution and the agglomeration condition of particles can be qualitatively judged through the complete sedimentation time, and the longer the complete sedimentation time is, the better the dispersibility is, and the less agglomeration is caused among particles. Table 2 below shows the results of sedimentation experiments performed on the nano copper oxide particles obtained in examples 1 to 3 and comparative examples 1 to 2.
TABLE 2 complete settling time for the products of examples 1-3 and comparative examples 1-2
Complete sedimentation 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 1-3 have longer complete sedimentation time, and when the molar ratio of copper acetate to sodium borate is 1:15, the molar ratio of the cetyl trimethyl ammonium bromide to the copper acetate serving as a surfactant is 1:90, the reaction temperature of the reaction kettle is 180 ℃, and the complete sedimentation time of the obtained nano copper oxide particles in the aqueous solution is longest and the dispersibility is best when the reaction time is 11 hours; comparative example 1 is a preparation of spherical nano copper oxide with sodium hydroxide as a precipitant, and the dispersibility is general; comparative example 2 was free of added surfactant cetyltrimethylammonium bromide, and the nano copper oxide particles had a shorter complete settling time in aqueous solution and poor dispersibility.
Table 3 shows 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 to 3, neither Escherichia coli nor Staphylococcus aureus was found on the surface of the petri dish, showing that the sterilization rate reached 100%, and the water-drop-shaped nano copper oxide prepared by the method of the present invention had excellent antibacterial properties; in comparative example 1, sodium hydroxide is used as a precipitant to prepare spherical nano copper oxide, and in comparative example 2, no surfactant cetyl trimethyl ammonium bromide is added, and all prepared nylon fibers find that colonies exist, and the antibacterial performance is general.
TABLE 3 antibacterial Properties of the nylon fibers prepared in examples 1 to 3 and comparative examples 1 to 2
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention.

Claims (5)

1. The preparation method of the nano copper oxide antibacterial material is characterized by comprising the following steps of:
step one: respectively weighing copper acetate solid and sodium borate solid, adding deionized water, and placing on a magnetic stirrer to stir until the solids are completely dissolved, thereby obtaining copper acetate aqueous solution and sodium borate aqueous solution;
step two: adding the sodium borate solution into the continuously stirred copper acetate solution, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
step three: dripping a surfactant cetyl trimethyl ammonium bromide solution into the mixed solution prepared in the step two, and performing ultrasonic dispersion in an ultrasonic instrument at 30 ℃ for 15min;
step four: transferring the blue mixed solution prepared in the third step into a reaction kettle, naturally cooling to room temperature after reaction, centrifuging the obtained product, alternately washing three times by using deionized water and absolute ethyl alcohol, and drying the precipitate in a vacuum drying oven at 60 ℃ for 5 hours to obtain nano copper oxide black powder;
the molar ratio of the copper acetate to the sodium borate is 1 (10-20);
the mole ratio of the hexadecyl trimethyl ammonium bromide to the copper acetate of the surfactant is 1 (80-100);
the reaction temperature in the reaction kettle is 160-200 ℃ and the reaction time is 10-12 h.
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 method for preparing a nano copper oxide antibacterial material according to claim 1, wherein in the second and third steps, the ultrasonic dispersion frequency of the ultrasonic instrument is 60-100 kHz.
4. The method for preparing a nano copper oxide antibacterial material according to claim 1, wherein in the third step, the dripping speed of the surfactant cetyl trimethyl ammonium bromide is 30-40 drops/min.
5. The method for preparing a nano copper oxide antibacterial material according to claim 1, wherein in the fourth step, the centrifugal speed is 10000-30000 rpm.
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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

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