CN110200013A - A kind of antibacterial mildew inhibitor and the preparation method and application thereof - Google Patents
A kind of antibacterial mildew inhibitor and the preparation method and application thereof Download PDFInfo
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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
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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
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- A01N59/20—Copper
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to antibacterial mildew inhibitors, specifically provide a kind of antibacterial mildew inhibitor and the preparation method and application thereof.Antibacterial mildew inhibitor of the present invention is the copper oxide/zinc oxide compound nano particle for mixing amount of copper 0.5%-10%, particle size 20-300nm.The present invention mixes copper Zinc oxide nanoparticle with very excellent antibacterial and mouldproof performance, and when additive amount is 1% or more bulk material weight, antibiotic rate reaches 0 grade up to 99% or more (level-one), mould proof grade.Antibacterial mildew inhibitor preparation process of the present invention is simple, and product is well dispersed, and anti-microbial property is lasting, and high-efficiency broad spectrum is easy to use, will not impact to bulk material properties after addition, is suitble to industrial mass production and popularization.
Description
Technical field
The present invention relates to antibacterial mildew inhibitors, and in particular to mixes copper zinc oxide antibacterial mildew inhibitor and the preparation method and application thereof.
Background technique
It is learnt in the global necrology data in 2016 announced according to the World Health Organization (WHO), the whole world is because of bacterium, disease
Death caused by poison etc. infects is still the big factor of human death, and especially in low income country, sanitary condition difference is caused
Death toll be even more up to total death toll half it is even more.In all implementations with " big health " environment, people
Higher and higher to the concern of own health problem, antibacterial consciousness generally improves, and the demand to antimicrobial product is also growing.One side
There are various bacterial drug resistances due to the abuse of antibiotic in face.On the other hand, the growth of mould is equally to the daily of people
It is even more that will cause serious property loss etc. that life, which causes the mildew of inconvenience, especially vital document and coin etc.,.It is inorganic
The appearance of antibacterial agent can well solve the problem of bacterial drug resistance.Inorganic antiseptic relatively conventional at present includes nano silver
And silver ion antimicrobial agent, Nanometer Copper and nano zine oxide etc..But nano silver is at high price, and Nanometer Copper is oxidizable and reunites, and receives
In contrast advantage is larger for rice zinc oxide.But the anti-mold effect of nano silver and nano zine oxide is less managed in traditional inorganic antiseptic
Think.
Summary of the invention
For improve antibacterial effect especially anti-mold effect, the present invention a kind of antibacterial mildew inhibitor is provided, have efficiently, wide spectrum,
Durable antibiotic antimildew function.
The research of the invention finds that can both be significantly improved after mixing a certain amount of copper oxide in Zinc oxide nanoparticle
Antibacterial effect, it has been unexpectedly discovered that anti-mold effect can be significantly improved, to propose the present invention.
Specifically, the present invention provides a kind of antibacterial mildew inhibitor, it is copper oxide/zinc oxide compound nano particle；Wherein, it mixes
Amount of copper is 0.5%-10%, particle size 20-300nm.
The weight percentage of the present invention mixed amount of copper and refer to copper in the antibacterial mildew inhibitor.
Further, in the antibacterial mildew inhibitor mix amount of copper be 2%-6%, particularly preferably 4%.
In particular embodiments of the invention, in the antibacterial mildew inhibitor mix amount of copper be respectively 0.5%, 1%, 2%,
3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
The research of the invention finds that it is too high or too low when mixing amount of copper in the antibacterial mildew inhibitor, such as higher than 10% or be lower than
Antibacterial and mouldproof effect declines when 0.5%.And mix amount of copper 0.5%-10%, especially 2%-6% it is special 4% when, can obtain
Excellent antibacterial and mouldproof performance expands antimicrobial spectrum.
Preferably, the particle size of the antibacterial mildew inhibitor is 50-100nm.
Further the study found that the antibacterial mildew inhibitor particle size has significant shadow for antibacterial and mouldproof performance performance
It rings, particle size is excessive or too small, such as particle size is greater than when 300nm or particle size are less than 20nm under antibacterial and mouldproof effect
Drop.And particle size can obtain excellent antibacterial and mouldproof performance in 20-300nm especially 50-100nm, expand antibacterial
Spectrum.In addition, particle powder is easy to reunite, and mistake although anti-microbial property is preferable when the antibacterial mildew inhibitor particle is smaller
Thin particle powder when in use (such as when being added in coating), is also not easy to disperse, and causes mixing uneven and reaches not
To the effect of good antibacterial and mouldproof.
The present invention also provides the preparation methods of above-mentioned antibacterial mildew inhibitor, comprising:
Mantoquita and zinc salt are taken according to the ratio, are dissolved in deionized water and solution is made；
Appropriate sodium hydroxide is added into the solution, stirs evenly；
The appropriate lauryl sodium sulfate ethanol solution for being heated to 50-120 DEG C is added, is sufficiently reacted；
By the reaction product cleaning, drying, grinding.
Further, the mantoquita is selected from one or more of copper sulphate, copper chloride etc..
Further, the zinc salt is selected from one or more of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride etc..
Further, the dosage of the mantoquita and zinc salt is so as to mix amount of copper up to 0.5%- in made antibacterial mildew inhibitor
10% is advisable.
Further, the form addition that solution is made in sodium hydroxide is advisable.
Preferably, the additional amount of the sodium hydroxide is 1-5 times, more preferably 2-3 times of mantoquita and zinc salt integral molar quantity.
It the advantage is that and not only can guarantee that mantoquita and zinc salt are totally converted, but also can control crystallization rate, to regulate and control copper oxide/oxygen of generation
Change the size of zinc composite nanometer particle.
In the present invention, conventional method in that art preparation is can be used in the lauryl sodium sulfate ethanol solution, such as with dense
The ethyl alcohol of degree 60%-80% is prepared by solvent, preferably using 80% ethyl alcohol as solvent.The lauryl sodium sulfate ethyl alcohol
The concentration of lauryl sodium sulfate is usually 0.01-0.05g/ml, such as 0.02g/ml in solution.
The research of the invention finds that lauryl sodium sulfate ethanol solution (solvent is preferably 80% ethyl alcohol) is heated in advance
50-120 DEG C (preferably 80 DEG C) is then added in mantoquita zinc solution, the advantage is that make be added copper zinc solution while, temperature
Degree can reach optimal reaction temperature, so that homogeneous precipitation, reduces the size distribution of gained nano powder.
Preferably, the weight ratio of the sum of mantoquita and zinc salt weight in the lauryl sodium sulfate and reaction system being added
Example is 0.1-5:1, more preferably 1-3:1.Under this condition, lauryl sodium sulfate is as dispersing agent, be coated on copper ion and
Zinc ion periphery, reduces the crystallization rate of copper zinc composite particles, reduces particle size；Anionic group big simultaneously, which is reduced, to be generated
Nano particle grow up and reunite, to improve the dispersibility of nano particle.
The method collecting reaction product of centrifugation can be used after the reaction was completed to above-mentioned, it usually can be with 3000-10000r/min
Speed is centrifuged 15-60min；Then it is eluted with water, it is usually 2-5 times washable.Generally in 60-120 DEG C of dry 6-24h.
Specifically, the preparation method of above-mentioned antibacterial mildew inhibitor, comprising:
S1, by appropriate mantoquita and zinc salt, be dissolved in deionized water, obtain solution A；
S2, according in solution A mantoquita and zinc salt total amount weigh a certain amount of sodium hydroxide, be dissolved in deionized water, obtain
To solution B；
S3, the resulting solution A of S1 is mixed with the solution B in S2, obtains solution C；
S4, it weighs a certain amount of lauryl sodium sulfate and is dissolved in the ethyl alcohol of concentration 60%-80%, obtain solution D, and add
Heat arrives 50-120 DEG C；
S5, the resulting solution C of S3 is added in the resulting solution D of S4,1-6h is reacted, with 3000-10000r/min speed
It is centrifuged 15-60min, resulting precipitating cleaning 2-5 after grinding, is obtained into copper oxide/oxygen in 60-120 DEG C of dry 6-24h after
Change zinc composite nanometer particle, antibacterial mildew inhibitor as of the present invention.
The invention also includes above-mentioned antibacterial mildew inhibitors for the application to material antibacterial and mouldproof.
For example, the antibacterial mildew inhibitor can be usually added to electrostatic spraying coating (comprising epoxy resin powder/metal
Powder, titanium dioxide, lithopone, auxiliary agent and pigment) in, it is sieved after being sufficiently mixed, described will contain antibacterial using the method for electrostatic spraying
The electrostatic spraying coating of mould inhibitor is sprayed into material surface, and 80-200 DEG C is taken out after solidification 15-50 minutes.Or the antibacterial is prevented
Mould dose is added in the liquid such as glaze, paint, and being uniformly dispersed by way of stirring or sonic oscillation can be used.
Copper oxide obtained by the present invention/zinc oxide compound nano particle has very excellent antibacterial and mouldproof performance, can
For the antibacterial and mouldproof of the multiple materials such as timber, plastics, printed matter, powder, fluid, bulk material level-one antibacterial ability can be assigned
With II grades or more mould proof grade；And after durability test, remain to reach durable preceding same antibacterial and mouldproof effect.Antibacterial of the present invention
For mould inhibitor when additive amount is 1% or more bulk material weight, antibiotic rate reaches 0 grade up to 99% or more (level-one), mould proof grade.
Antibacterial mildew inhibitor preparation process of the present invention is simple, and product is well dispersed, and anti-microbial property is lasting, and high-efficiency broad spectrum is easy to use, addition
After bulk material properties will not be impacted, be suitble to industrial mass production and popularization.
Detailed description of the invention
Fig. 1 is 1 copper oxide of embodiment/zinc oxide compound nano particle anti-microbial property test result.
Fig. 2 is 1 copper oxide of embodiment/zinc oxide compound nano particle fungicidal properties test result.
Fig. 3 is copper oxide/zinc oxide compound nano particle SEM figure that difference mixes amount of copper.
Fig. 4 is copper oxide/zinc oxide compound nano particle XRD diagram that difference mixes amount of copper.
Fig. 5 is 4 copper oxide of embodiment/zinc oxide compound nano particle XPS figure.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..It is not specified in embodiment specific
Technology or conditions person, described technology or conditions according to the literature in the art, or carried out according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be commercially available by regular distributor.
Embodiment 1
It weighs 0.25g cupric sulfate pentahydrate and 7.5g zinc nitrate hexahydrate is dissolved in 20ml deionized water, obtain solution A；
It weighs 40g sodium hydroxide to be dissolved in 20ml deionized water, obtains solution B；
Solution A and solution B are mixed to get solution C；
It weighs 10g lauryl sodium sulfate to be dissolved in the ethyl alcohol of concentration 80% of 500ml, obtains solution D, be heated to
Solution C is poured into after 80 DEG C, the reaction was continued 6h.
After solution is cooling, the revolving speed of final solution 8000r/min in centrifuge is centrifuged 30min, outwells supernatant
Liquid takes precipitating back and forth to be cleaned with water 5 times until cleaning, and what then will be cleaned is deposited in 120 DEG C of dry 12h in drying box, grinds
Up to copper oxide/zinc oxide compound nano particle.Wherein, which is 50-100nm, and mixing amount of copper is 4%.
Entrust Physical Chemistry Technology Inst., Chinese Academy of Sciences to copper oxide made from the present embodiment/zinc oxide compound nano particle
Antibacterial and mouldproof performance is detected, and (electrostatic spraying sample is anti-by the result is shown in Figure 1 (electrostatic spraying sample anti-microbial property test) and Fig. 2
Mould performance test).The result shows that its antibacterial and mouldproof is had excellent performance.
Embodiment 2
Difference with embodiment 1 is only that: the dosage of cupric sulfate pentahydrate is replaced with 0.125g.
Copper oxide made from the present embodiment/zinc oxide compound nano particle, size 50-100nm, mixing amount of copper is 2%.
Embodiment 3
Difference with embodiment 1 is only that: the dosage of cupric sulfate pentahydrate is replaced with 0.375g.
Copper oxide made from the present embodiment/zinc oxide compound nano particle, size 50-100nm, mixing amount of copper is 6%.
Embodiment 4
Difference with embodiment 1 is only that: the dosage of cupric sulfate pentahydrate is replaced with 0.625g.
Copper oxide made from the present embodiment/zinc oxide compound nano particle, size 50-100nm, mixing amount of copper is 10%
Embodiment 5
Difference with embodiment 1 is only that: the dosage of cupric sulfate pentahydrate is replaced with 0.031g.
Copper oxide made from this comparative example/zinc oxide compound nano particle, size 50-100nm, mixing amount of copper is 0.5%
Comparative example 1
Difference with embodiment 1 is only that: 7.75g zinc nitrate hexahydrate is used only and 20ml deionized water prepares solution
A；Remaining step is same as Example 1.
Zinc oxide nanoparticle made from this comparative example, size 50-100nm, mixing amount of copper is 0%.
Comparative example 2
Difference with embodiment 1 is only that: 7.75g cupric sulfate pentahydrate is used only and 20ml deionized water prepares solution A；Its
Remaining step is same as Example 1.
Copper oxide nanometer particle made from this comparative example, size 50-100nm are free of zinc.
Experimental example 1
Fig. 3 is copper oxide/zinc oxide compound nano particle SEM figure that difference mixes amount of copper, and wherein Fig. 3 A is made for comparative example 1
Zinc oxide nanoparticle (mix amount of copper be 0%) pattern, Fig. 3 B is copper oxide/zinc oxide compound nano made from embodiment 1
The pattern of particle (mixing amount of copper is 4%), Fig. 3 C is that (mix amount of copper is copper oxide made from embodiment 3/zinc oxide compound nano particle
6%) pattern, Fig. 3 D are the pattern of copper oxide made from embodiment 4/zinc oxide compound nano particle (mixing amount of copper is 10%).
Fig. 3 is as it can be seen that the ZnO for not mixing copper that the method for comparative example 1 is prepared is diameter about 50nm, is about 5 μm of pinnacle six
The sea urchin shape particle that square column is self-assembled into, and with the variation for mixing amount of copper, the pattern of composite nanometer particle changes, embodiment
1 corresponding composite particles are the flower-shaped particle that nanometer sheet is self-assembled into, and nanometer sheet surface has about tens nanometers of subtle sheet
Nano particle, can further increase the specific surface area of composite particles, and continue growing with amount of copper is mixed, and nanometer sheet gradually becomes again
At leaf of bamboo shape, eventually become needle-shaped.
Fig. 4 is 1 Zinc oxide nanoparticle of embodiment 1,4 copper oxide of embodiment/zinc oxide compound nano particle and comparative example
XRD diagram, wherein " 4%Cu-ZnO ", " 10%Cu-ZnO " are respectively embodiment 1,4 composite nanometer particle of embodiment；" ZnO " is pair
1 Zinc oxide nanoparticle of ratio.
Fig. 4 illustrates that the ZnO crystallinity of this method preparation is fine as it can be seen that the background of all spectral peaks is very low, and with mixing amount of copper
Increase, become more apparent upon positioned at 32.5 °, 35.5 ° and 38.7 ° of the peak CuO, but simple substance Cu and Cu is not detected2The peak of O, says
The copper of bright incorporation mainly exists in the form of CuO.
Fig. 5 is 4 copper oxide of embodiment/zinc oxide compound nano particle XPS figure, wherein Fig. 5 A is that XPS is composed entirely, and Fig. 5 B is
The narrow spectrum of Cu2p.
Fig. 5 as it can be seen that the copper in composite particles in addition to there is also a small amount of simple substance Cu or Cu by CuO2O, that is, the copper chemical combination mixed
Valence is between 0~2, but due to Cu/Cu2O amount is very little, the detection limit lower than XRD, so not occurring corresponding spectrum in Fig. 4
Peak.
2 antibacterial experiment of experimental example
Separately verify the anti-microbial property of Zinc oxide nanoparticle prepared by embodiment 1-5 and comparative example 1-2.
Experimental method: referring to GB/T 21866-2008 " antibiotic paint (paint film) antibiotic property measuring method and antibacterial effect "；
Bacterium: Escherichia coli (Escherichia coli) AS1.90 is used in detection；
Staphylococcus aureus (Staphylococcus aureus) AS1.89；
Testing result see the table below 1.
Table 1
Table 1 the result shows that, copper oxide produced by the present invention/zinc oxide compound nano particle anti-microbial property is significantly better than oxygen
Change zinc composite nanometer particle (comparative example 1) and copper oxide nanometer particle (comparative example 2), and the moderate composite Nano for mixing amount of copper
The antibiotic property of grain is best, mixes that amount of copper is too high or too low all to make antibacterial effect reduce.
The mould proof experiment of experimental example 3
Separately verify the fungicidal properties of Zinc oxide nanoparticle prepared by embodiment 1-5 and comparative example 1-2.
Experimental method: referring to GB/T 1741-2007 " paint film fungus resistance measuring method "；
Detection is with bacterium: see the table below 2.
Testing result see the table below 2.
Table 2
Table 2 the result shows that, copper oxide produced by the present invention/zinc oxide compound nano particle fungicidal properties is significantly better than oxygen
Change zinc composite nanometer particle (comparative example 1) and copper oxide nanometer particle (comparative example 2), and the moderate composite Nano for mixing amount of copper
The mildew resistance of grain is best, mixes that amount of copper is too high or too low all to make anti-mold effect reduce.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of antibacterial mildew inhibitor is the copper oxide/zinc oxide compound nano particle for mixing amount of copper 0.5%-10%, the particle ruler
Very little 20-300nm.
2. antibacterial mildew inhibitor according to claim 1, which is characterized in that the amount of copper of mixing in the antibacterial mildew inhibitor is 2%-
6%, preferably 4%.
3. antibacterial mildew inhibitor according to claim 1 or 2, which is characterized in that the particle size of the antibacterial mildew inhibitor is
50-100nm。
4. the preparation method of any one of the claim 1-3 antibacterial mildew inhibitor characterized by comprising
Mantoquita and zinc salt are taken according to the ratio, are dissolved in deionized water and solution is made；
Appropriate sodium hydroxide is added into the solution, stirs evenly；
The appropriate lauryl sodium sulfate ethanol solution for being heated to 50-120 DEG C is added, is sufficiently reacted；
By the reaction product cleaning, drying, grinding.
5. the preparation method according to claim 4, which is characterized in that the mantoquita in copper sulphate, copper chloride one
Kind is several；And/or
The zinc salt is selected from one or more of zinc nitrate, zinc acetate, zinc sulfate, zinc chloride.
6. preparation method according to claim 4 or 5, which is characterized in that the additional amount of the sodium hydroxide be mantoquita and
1-5 times of zinc salt integral molar quantity, more preferably 2-3 times.
7. according to the described in any item preparation methods of claim 4-6, which is characterized in that the lauryl sodium sulfate that is added with
The weight ratio of the sum of mantoquita and zinc salt weight is 0.1-5:1, more preferably 1-3:1 in reaction system.
8. according to the described in any item preparation methods of claim 4-7 characterized by comprising
S1, by appropriate mantoquita and zinc salt, be dissolved in deionized water, obtain solution A；
S2, according in solution A mantoquita and zinc salt total amount weigh a certain amount of sodium hydroxide, be dissolved in deionized water, obtain molten
Liquid B；
S3, the resulting solution A of S1 is mixed with the solution B in S2, obtains solution C；
S4, it weighs a certain amount of lauryl sodium sulfate and is dissolved in the ethyl alcohol of concentration 60%-80%, obtain solution D, and be heated to
50-120℃；
S5, the resulting solution C of S3 is added in the resulting solution D of S4, reacts 1-6h, with the centrifugation of 3000-10000r/min speed
Resulting precipitating cleaning 2-5 after grinding, is obtained copper oxide/zinc oxide in 60-120 DEG C of dry 6-24h after by 15-60min
Composite nanometer particle.
9. the antibacterial mildew inhibitor of any one of claim 4-8 the method preparation.
10. any one of claim 1-3,9 antibacterial mildew inhibitor are for the application to material antibacterial and mouldproof.
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| CN112690289A (en) * | 2020-12-25 | 2021-04-23 | 南昌大学 | Antibacterial mildew preventive and preparation method thereof |
| CN113463224A (en) * | 2021-07-02 | 2021-10-01 | 和也健康科技有限公司 | Preparation method of nano antibacterial stone needle fiber material for cosmetic cotton |
| ES2904257A1 (en) * | 2020-10-02 | 2022-04-04 | Zapico Rodriguez Ines | Disinfection procedure (Machine-translation by Google Translate, not legally binding) |
| CN115039793A (en) * | 2022-07-05 | 2022-09-13 | 汕头市优森活新材料科技有限公司 | Indoor efficient antibacterial smell-cleaning agent and preparation method and application thereof |
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| CN113463224A (en) * | 2021-07-02 | 2021-10-01 | 和也健康科技有限公司 | Preparation method of nano antibacterial stone needle fiber material for cosmetic cotton |
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| Publication number | Publication date |
|---|---|
| CN110200013B (en) | 2020-04-14 |
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