CN109179507A - A kind of slow-release long-acing nano anti-biotic material and its methods for making and using same - Google Patents
A kind of slow-release long-acing nano anti-biotic material and its methods for making and using same Download PDFInfo
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- CN109179507A CN109179507A CN201811220380.4A CN201811220380A CN109179507A CN 109179507 A CN109179507 A CN 109179507A CN 201811220380 A CN201811220380 A CN 201811220380A CN 109179507 A CN109179507 A CN 109179507A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
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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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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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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Abstract
The invention discloses a kind of slow-release long-acing nano anti-biotic material and its methods for making and using sames, adulterate bismuth tungstate nano particle using one step hydro thermal method synthesis silver ion, and be blended with waterglass ball milling and slow-release long-acing nano anti-biotic material is made.Silver ion is uniform and stable in the nano anti-biotic material is scattered in bismuth tungstate lattice, and silver ion gradually discharges in use process, while using the Strong oxdiative reducing power of bismuth tungstate electron-hole pair, generating synergetic antibacterial effect with silver ion.Heat resistance of the present invention is good, after can mixing with different materials such as macromolecule, metal, glass, ceramics, coating, paint, using high temperature process, heat treatment sintering or curing process, has sustained release, long-acting, wide spectrum, stable antibacterial, sterilization, antimildew function.
Description
Technical field
The present invention relates to anti-biotic material technical field more particularly to a kind of slow-release long-acing nano anti-biotic material and its preparations
Method.
Background technique
Raising with people to modern life quality, people more and more pay close attention to air quality and living environment, especially
It is the indoor air quality and living environment that itself lives.It among these include that the households such as indoor wall, glass and sofa are raw
Product are applied flexibly, they are extremely easy the unwanted particles such as dust, bacterium, the virus of absorption, if such particle long-term accumulation will endanger
Evil people's health.How to inhibit or kill the nocuousness such as bacterium, the virus in the home life supplieshome life supplies such as wall, glass and sofa
Particle becomes an important issue concerning life and health.
Common anti-biotic material can be summarized as organic, inorganic and natural class etc..There are non-for traditional organic anti-bacterial material
Broad-spectrum antiseptic, chemical stability are poor, heat resistance is poor, the deadly defects such as easy to aging；Natural class anti-biotic material is usually in 150-
180 DEG C begin to charing and decompose, and application range is narrow；Inorganic antibacterial material has many advantages, such as broad-spectrum antiseptic, heat-resist.However,
Inorganic antiseptic common at present is mainly using the oxide containing antibacterial ions such as silver, copper, zinc or simple substance particle and zeolite, phosphorus
The carriers such as hydrochlorate, hydroxyapatite or soluble glass mix, and it is long to improve antibacterial to make it through certain slow releasing function
Effect property, but the dispersion of its antibacterial ion is uneven, and antibacterial ion rate of release is too fast and random uncontrollable, when slow releasing function is sustainable
Between it is short, anti-microbial property long-time stability are poor, these carriers and antibacterial ion do not have synergetic antibacterial effect.The antibacterials such as silver, copper from
The chemical property of son is active, is easily changed into the silver oxide of brown, the copper oxide of black or redox into the elemental silver of black,
White and light material product can not be applied, and the discoloration problem for solving inorganic antiseptic is global problem.
Summary of the invention
Technical problem: the present invention is to solve above-mentioned inorganic antiseptic to disperse uneven, antibacterial ion release speed in the carrier
Spend it is fast and it is random it is uncontrollable, the slow releasing function sustainable time is short, anti-microbial property long-time stability are poor, carrier and antibacterial ion
The problems such as do not have to change colour after synergetic antibacterial effect, long-time service, provides a kind of slow-release long-acing nano anti-biotic material and its system
Standby and methods for using them.
Technical solution: a kind of slow-release long-acing nano anti-biotic material of the invention adulterates bismuth tungstate nano particle by silver ion
Be blended and be made through ball milling with waterglass powder, wherein silver ion doping bismuth tungstate nano particle content be by weight percent
10%-80%, the waterglass that remaining is silica and sodium oxide molybdena molar ratio is 0.8:1-2:1, silver ion adulterate bismuth tungstate nanometer
Silver ion doping is 0.01%-5%, partial size 2nm-100nm in particle.
A kind of slow-release long-acing nano anti-biotic material of the invention and preparation method thereof the following steps are included:
1) one step hydro thermal method synthesis silver ion adulterates bismuth tungstate nano particle: by enuatrol and Bi (NO3)3·5H2O is added
Into deionized water, stir 0.2-2 hours, then by AgNO3It is added in above-mentioned mixed liquor, magnetic agitation 0.5-2 hours, then
By Na2WO4·2H2O is added in above-mentioned solution, and magnetic agitation 0.5-2 hours, obtained mixed liquor is then added to poly- four
In the reactor tank of vinyl fluoride, 160-220 DEG C hydro-thermal 18-32 hours；It is cooled to room temperature, the precipitating n-hexane and second that will be obtained
Repeatedly, the powder obtained after dry 5-10 hour at 50-80 DEG C is silver ion doping bismuth tungstate nano particle for alcohol cleaning；
2) preparation of nano anti-biotic material: in proportion by the silver ion doping bismuth tungstate nano particle and water of step 1) preparation
Glass powder is blended 1-10 hours by mechanical ball mill, and nano anti-biotic material is made after evenly mixing.
Wherein: the enuatrol, Bi (NO3)3·5H2O、AgNO3、Na2WO4·2H2The molar ratio of O is (1-5), (0.1-
2)、(0.01-0.2)、(0.1-2)。
A kind of application method of slow-release long-acing nano anti-biotic material of the invention, the nano anti-biotic material and high score
After son, metal, glass, ceramics, coating, paint different materials mixing, using high temperature process, heat treatment sintering or curing molding
After use.
The utility model has the advantages that the advantageous effect of the invention is as follows:
1, one step hydro thermal method carries out impurity synthesis silver ion and adulterates bismuth tungstate nano particle through the invention, obtained
Antimicrobial spray in silver ion is uniform and stable is scattered in bismuth tungstate lattice, on this basis, will be silver-colored in conjunction with ball milling blending technology
Ion doping bismuth tungstate nano particle even dispersion is distributed in the intrinsic micropore of waterglass itself, further collaboration enhancing antibacterial from
Sustained release effect of son, antibacterial ion rate of release is stably and controllable in use process, and the slow releasing function sustainable time is long, antibiotic property
Energy long-time stability are good.
2, there is synergetic antibacterial effect between antibacterial ion and bismuth tungstate nanoparticle vector.Bismuth tungstate itself has relatively narrow
Forbidden bandwidth, under the irradiation of visible light, valence-band electrons are easy to be excited to form photo-generated carrier, then its by oxygen molecule also
Original shape is at the O with strong oxidizing property2 -Free radical.Meanwhile valence band hole and hydrone occur oxidation reaction and form strong oxidizing property
OH-Free radical, this O with strong oxidizing property2 -Free radical and OH-Free radical with virus, bacterium contacts to occur
Redox reaction, and then virus and bacterium are killed, and the O of strong oxidizing property2 -Free radical and OH-Free radical can be by bismuth tungstate
The monovalence silver ion adulterated in lattice, which further aoxidizes, forms the stronger trivalent silver iron of sterilizing ability, and collaboration enhancing silver ion is certainly
The antibacterial effect of body；Meanwhile silver ion is incorporated into bismuth tungstate lattice, can form more crystal defects, increases electronics-sky
The excitation probability in cave pair increases the quantity of electron-hole pair and the O with strong oxidizing property indirectly2 -Free radical and OH-
Free radical quantity, and then the trivalent silver iron of more strong sterilizing ability is caused to generate, there is significant Synergistic antimicrobial effect.
3, the discoloration problem of inorganic antiseptic is efficiently solved.Uniform and stable point of silver ion in nano anti-biotic material of the present invention
It dissipates in bismuth tungstate lattice, is not easy to be changed into the elemental silver of the silver oxide of brown or black, this may refrain from and solve silver-colored antibacterial
Metachroic problem is used for a long time in agent.
Specific embodiment
A kind of silver ion that slow-release long-acing nano anti-biotic material is synthesized by one step hydro thermal method doping bismuth tungstate of the present invention is received
Rice grain is blended through ball milling with waterglass powder and is made, wherein the content that silver ion adulterates bismuth tungstate nano particle presses quality hundred
Score is 10%-80%, and the waterglass that remaining is silica and sodium oxide molybdena molar ratio is 0.8:1-2:1, silver ion adulterates wolframic acid
Silver ion doping is 0.01%-5%, partial size 2nm-100nm in bismuth nano particle.
The preparation method of the anti-biotic material, comprising the following steps:
1) one step hydro thermal method synthesis silver ion adulterates bismuth tungstate nano particle: by 1-5mmol enuatrol and 0.1-2mmol
Bi(NO3)3·5H2O is add to deionized water, and is stirred 0.2-2 hours, then by 0.01-0.2mmol AgNO3It is added to
It states in mixed liquor, magnetic agitation 0.5-2 hours, then by 0.1-2mmol Na2WO4·2H2O is added in above-mentioned solution, and magnetic force stirs
It mixes 0.5-2 hours, then obtained mixed liquor is added in the reactor tank of polytetrafluoroethylene (PTFE), in 160-220 DEG C of hydro-thermal 18-32
Hour.It is cooled to room temperature, obtained precipitating is cleaned 3-6 times with n-hexane and ethyl alcohol, at 50-80 DEG C after dry 5-10 hours
The powder arrived is that silver ion adulterates bismuth tungstate nano particle.
2) preparation of nano anti-biotic material: in proportion by the silver ion doping bismuth tungstate nano particle and water of step 1) preparation
Glass powder is blended 1-10 hours by mechanical ball mill, and nano anti-biotic material is made after evenly mixing.
After the nano anti-biotic material can be mixed with different materials such as macromolecule, metal, glass, ceramics, coating, paint,
Using high temperature process, heat treatment sintering or curing molding after use.
Anti-biotic material obtained is subjected to antibiotic property test to more plants of test strains, antimicrobial spectrum measurement result shows antibacterial
Spray has broad spectrum antibacterial, and antibiotic rate is 99% or more.
Combined with specific embodiments below, present invention is further described in detail.The following examples are intended to illustrate the invention,
But it is not intended to limit the scope of the invention.
Embodiment 1
By 2.2mmol enuatrol and 0.4mmol Bi (NO3)3·5H2O is added in 40ml deionized water, and stirring 0.3 is small
When, then by 0.01mmol AgNO3It is added in above-mentioned mixed liquor, stirs 30 minutes, then by 0.4mmol Na2WO4·2H2O
It is added in above-mentioned solution, magnetic agitation 2 hours, then obtained mixed liquor is added to the reactor tank of 50ml polytetrafluoroethylene (PTFE)
In, 180 DEG C hydro-thermal 18 hours.It is cooled to room temperature, obtained precipitating n-hexane and ethyl alcohol are cleaned 3 times, at 60 DEG C dry 5
The powder obtained after hour is that silver ion adulterates bismuth tungstate nano particle.
The water glass for being 90% by mass fraction 10% and mass fraction by the silver ion doping bismuth tungstate nano particle of preparation
(silica and sodium oxide molybdena molar ratio pass through mechanical ball mill 2 hours glass powder for 0.8:1), uniformly mix, and obtain nano-antibacterial material
Material.
Embodiment 2
By 4.4mmol enuatrol and 0.8mmol Bi (NO3)3·5H2O is added in 40ml deionized water, and stirring 0.4 is small
When, then by 0.01mmol AgNO3It is added in above-mentioned mixed liquor, stirs 1 hour, then by 0.8mmol Na2WO4·2H2O adds
Enter into above-mentioned solution, magnetic agitation 1 hour, then obtained mixed liquor is added to the reactor tank of 50ml polytetrafluoroethylene (PTFE)
In, 200 DEG C hydro-thermal 24 hours.It is cooled to room temperature, obtained precipitating n-hexane and ethyl alcohol are cleaned 6 times, at 70 DEG C dry 8
The powder obtained after drying after hour is that silver ion adulterates bismuth tungstate nano particle.
The water glass for being 60% by mass fraction 40% and mass fraction by the silver ion doping bismuth tungstate nano particle of preparation
(silica and sodium oxide molybdena molar ratio pass through mechanical ball mill 1 hour glass powder for 1:1), uniformly mix, and obtain nano anti-biotic material.
Embodiment 3
By 1mmol enuatrol and 0.1mmol Bi (NO3)3·5H2O is added in 40ml deionized water, is stirred 0.2 hour,
Then by 0.01mmol AgNO3It is added in above-mentioned mixed liquor, stirs 0.5 hour, then by 0.1mmol Na2WO4·2H2O adds
Enter into above-mentioned solution, magnetic agitation 0.5 hour, then obtained mixed liquor is added to the reactor tank of 50ml polytetrafluoroethylene (PTFE)
In, 160 DEG C hydro-thermal 18 hours.It is cooled to room temperature, obtained precipitating n-hexane and ethyl alcohol are cleaned 3 times, at 50 DEG C dry 5
The powder obtained after drying after hour is that silver ion adulterates bismuth tungstate nano particle.
The water glass for being 40% by mass fraction 60% and mass fraction by the silver ion doping bismuth tungstate nano particle of preparation
(silica and sodium oxide molybdena molar ratio pass through mechanical ball mill 1 hour glass powder for 0.8:1), uniformly mix, and obtain nano-antibacterial material
Material.
Embodiment 4
By 5mmol enuatrol and 2mmol Bi (NO3)3·5H2O is added in 40ml deionized water, stirring 2 hours, then
By 0.2mmol AgNO3It is added in above-mentioned mixed liquor, stirs 2 hours, then by 2mmol Na2WO4·2H2O is added to above-mentioned molten
In liquid, magnetic agitation 2 hours, then obtained mixed liquor is added in the reactor tank of 50ml polytetrafluoroethylene (PTFE), in 220 DEG C of water
Heat 32 hours.It is cooled to room temperature, obtained precipitating n-hexane and ethyl alcohol are cleaned 6 times, it is dry after 10 hours dry at 80 DEG C
The powder obtained afterwards is that silver ion adulterates bismuth tungstate nano particle.
The water glass for being 20% by mass fraction 80% and mass fraction by the silver ion doping bismuth tungstate nano particle of preparation
(silica and sodium oxide molybdena molar ratio pass through mechanical ball mill 10 hours glass powder for 2:1), uniformly mix, and obtain nano-antibacterial material
Material.
The anti-biotic material as made from embodiment is to staphylococcus aureus, bacillus subtilis, Candida albicans, large intestine
Bacillus carries out antibiotic property test, their antibiotic rate is respectively 99.4%, 99.6%, 99.3%, 99.3%.
Claims (4)
1. a kind of slow-release long-acing nano anti-biotic material, it is characterised in that: the nano anti-biotic material adulterates bismuth tungstate by silver ion
Nano particle is blended through ball milling with waterglass powder and is made, wherein the content that silver ion adulterates bismuth tungstate nano particle presses quality
Percentage is 10%-80%, the waterglass that remaining is silica and sodium oxide molybdena molar ratio is 0.8:1-2:1, silver ion Doped Tungsten
Silver ion doping is 0.01%-5%, partial size 2nm-100nm in sour bismuth nano particle.
2. a kind of slow-release long-acing nano anti-biotic material a kind of as described in claim 1 and preparation method thereof, it is characterised in that:
The preparation method of the anti-biotic material the following steps are included:
1) one step hydro thermal method synthesis silver ion adulterates bismuth tungstate nano particle: by enuatrol and Bi (NO3)3·5H2O is added to
In ionized water, stir 0.2-2 hours, then by AgNO3It is added in above-mentioned mixed liquor, magnetic agitation 0.5-2 hours, then will
Na2WO4·2H2O is added in above-mentioned solution, and magnetic agitation 0.5-2 hours, obtained mixed liquor is then added to polytetrafluoro
In the reactor tank of ethylene, 160-220 DEG C hydro-thermal 18-32 hours；It is cooled to room temperature, the precipitating n-hexane and ethyl alcohol that will be obtained
Repeatedly, the powder obtained after dry 5-10 hour at 50-80 DEG C is silver ion doping bismuth tungstate nano particle for cleaning；
2) preparation of nano anti-biotic material: in proportion by the silver ion doping bismuth tungstate nano particle and waterglass of step 1) preparation
Powder is blended 1-10 hours by mechanical ball mill, and nano anti-biotic material is made after evenly mixing.
3. a kind of slow-release long-acing nano anti-biotic material according to claim 2 and preparation method thereof, it is characterised in that: institute
State enuatrol, Bi (NO3)3·5H2O、AgNO3、Na2WO4·2H2The molar ratio of O be (1-5), (0.1-2), (0.01-0.2),
(0.1-2)。
4. a kind of a kind of application method of slow-release long-acing nano anti-biotic material as described in claim 1, it is characterised in that: institute
State nano anti-biotic material and macromolecule, after metal, glass, ceramics, coating, paint different materials mix, using high temperature process,
It is used after heat treatment sintering or curing molding.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484710A (en) * | 2020-05-12 | 2020-08-04 | 同曦集团有限公司 | Antibacterial and antiviral master batch for transparent mask, preparation method of antibacterial and antiviral master batch and antibacterial and antiviral transparent mask |
| CN111704816A (en) * | 2020-06-29 | 2020-09-25 | 长沙标朗住工科技有限公司 | Long-acting slow-release bactericidal antiviral coating and preparation method and application thereof |
| CN115445616A (en) * | 2022-10-21 | 2022-12-09 | 厦门理工学院 | Preparation method and application of silver-doped bismuth tungstate heterojunction photocatalyst |
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| CN101618322A (en) * | 2009-07-30 | 2010-01-06 | 中国科学院上海硅酸盐研究所 | Photocatalysis antibacterial material excited by visible light and application thereof |
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| CN105457663A (en) * | 2015-11-17 | 2016-04-06 | 中国科学院海洋研究所 | Bi2WO6 / Ag3PO4 composite photocatalytic fungicide and preparation method thereof |
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| CN115445616A (en) * | 2022-10-21 | 2022-12-09 | 厦门理工学院 | Preparation method and application of silver-doped bismuth tungstate heterojunction photocatalyst |
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