CN109179507B - Slow-release long-acting nano antibacterial material and preparation and application methods thereof - Google Patents
Slow-release long-acting nano antibacterial material and preparation and application methods thereof Download PDFInfo
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Abstract
本发明公开了一种缓释型长效纳米抗菌材料及其制备和应用方法，采用一步水热法合成银离子掺杂钨酸铋纳米颗粒，并与水玻璃球磨共混制得缓释型长效纳米抗菌材料。该纳米抗菌材料中银离子均匀稳定分散于钨酸铋晶格，使用过程中银离子逐步释放，同时利用钨酸铋电子‑空穴对的强氧化还原能力，与银离子产生协同抗菌作用。本发明耐热性能好，可与高分子、金属、玻璃、陶瓷、涂料、油漆等不同材料混合后，再经过高温加工、热处理烧结或固化处理，具备缓释、长效、广谱、稳定的抗菌、杀菌、防霉功能。The invention discloses a slow-release long-acting nanometer antibacterial material and a preparation and application method thereof. A one-step hydrothermal method is used to synthesize silver ion-doped bismuth tungstate nanoparticles, and blend with water glass ball milling to obtain a slow-release long-acting nanoparticle. Effective nano antibacterial material. In the nano antibacterial material, silver ions are uniformly and stably dispersed in the lattice of bismuth tungstate, and the silver ions are gradually released during use. At the same time, the strong redox ability of the electron-hole pair of bismuth tungstate is utilized to produce a synergistic antibacterial effect with silver ions. The invention has good heat resistance, can be mixed with different materials such as polymers, metals, glass, ceramics, coatings, paints, etc., and then undergo high-temperature processing, heat treatment, sintering or curing treatment, and has slow-release, long-term, broad-spectrum and stable properties. Antibacterial, bactericidal and mildew proof functions.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a slow-release long-acting nano antibacterial material and a preparation method thereof.
Background
With the improvement of modern life quality, people pay more and more attention to air quality and living environment, especially to indoor air quality and living environment of self-living. The particles include indoor walls, glass, sofa and other household articles, and are easy to adsorb harmful particles such as dust, bacteria, viruses and the like, and if the particles are accumulated for a long time, the particles can harm the health of people. How to inhibit or kill harmful particles such as bacteria, viruses and the like on walls, glass, sofas and other household living goods becomes an important issue concerning life health.
The commonly used antibacterial materials can be classified into organic, inorganic and natural ones. The traditional organic antibacterial material has the fatal defects of non-broad-spectrum antibacterial property, poor chemical stability, poor heat resistance, easy aging and the like; the natural antibacterial material usually starts to be carbonized and decomposed at the temperature of 150-180 ℃, and the application range is narrow; the inorganic antibacterial material has the advantages of broad-spectrum antibacterial property, good heat resistance and the like. However, the common inorganic antibacterial agents at present are mainly prepared by mixing oxide or simple substance particles containing antibacterial ions such as silver, copper, zinc and the like with carriers such as zeolite, phosphate, hydroxyapatite or soluble glass and the like, so that the antibacterial long-acting property is improved through a certain slow release effect, but the antibacterial ions are not uniformly dispersed, the release speed of the antibacterial ions is too fast and random and uncontrollable, the sustained-release effect is short in sustainable time, the antibacterial property is poor in long-term stability, and the carriers and the antibacterial ions do not have a synergistic antibacterial effect. The chemical properties of antibacterial ions such as silver, copper and the like are active, and the antibacterial ions are easily converted into brown silver oxide, black copper oxide or simple substance silver which is oxidized and reduced into black, so that the antibacterial ions cannot be applied to white and light-colored products, and the problem of discoloration of inorganic antibacterial agents is a worldwide problem.
Disclosure of Invention
The technical problem is as follows: the invention provides a slow-release long-acting nano antibacterial material and a preparation method and an application method thereof, aiming at solving the problems that the inorganic antibacterial agent is not uniformly dispersed in a carrier, the release speed of antibacterial ions is too high and is random and uncontrollable, the sustained-release effect is short in sustainable time, the long-term stability of the antibacterial performance is poor, the carrier and the antibacterial ions have no synergistic antibacterial effect, the color is changed after long-term use and the like.
The technical scheme is as follows: the slow-release long-acting nano antibacterial material is prepared by ball-milling and blending silver ion-doped bismuth tungstate nano particles and water glass powder, wherein the content of the silver ion-doped bismuth tungstate nano particles is 10-80% by mass, the balance is water glass with the molar ratio of silicon oxide to sodium oxide being 0.8:1-2:1, the doping amount of silver ions in the silver ion-doped bismuth tungstate nano particles is 0.01-5%, and the particle size is 2-100 nm.
The invention relates to a slow-release long-acting nano antibacterial material and a preparation method thereof, wherein the preparation method comprises the following steps:
1) synthesizing silver ion doped bismuth tungstate nano particles by a one-step hydrothermal method: mixing sodium oleate with Bi (NO)3)3·5H2Adding O into deionized water, stirring for 0.2-2 hr, and adding AgNO3Adding into the above mixture, magnetically stirring for 0.5-2 hr, adding Na2WO4·2H2Adding O into the solution, magnetically stirring for 0.5-2 hours, adding the obtained mixed solution into a polytetrafluoroethylene reaction tank, and carrying out hydrothermal treatment at the temperature of 160-220 ℃ for 18-32 hours; cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for multiple times, and drying at 50-80 deg.C for 5-10 hr to obtain powder of silver ion doped bismuth tungstate nanoparticles;
2) preparing a nano antibacterial material: proportionally mixing the silver ion doped bismuth tungstate nano particles prepared in the step 1) with water glass powder by mechanical ball milling for 1-10 hours, and uniformly mixing to obtain the nano antibacterial material.
Wherein: the sodium oleate and Bi (NO)3)3·5H2O、AgNO3、Na2WO4·2H2The molar ratio of O is (1-5), (0.1-2), (0.01-0.2) and (0.1-2).
The invention relates to an application method of a slow-release long-acting nano antibacterial material, which is used after the nano antibacterial material is mixed with different materials such as high molecules, metals, glass, ceramics, coatings and paints and then is processed at high temperature, sintered by heat treatment or cured and molded.
Has the advantages that: the beneficial effects of the invention are as follows:
1. the silver ion doped bismuth tungstate nano particles are synthesized by carrying out lattice doping by a one-step hydrothermal method, the silver ions in the prepared antibacterial spray are uniformly and stably dispersed in bismuth tungstate lattices, and on the basis, the silver ion doped bismuth tungstate nano particles are uniformly dispersed and distributed in inherent micropores of water glass by combining a ball-milling blending process, so that the slow release effect of the antibacterial ions is further enhanced in a synergistic manner, the release speed of the antibacterial ions is stable and controllable in the use process, the sustained release effect of the antibacterial ions is long in sustainable time, and the long-term stability of the antibacterial performance is good.
2. The antibacterial ions and the bismuth tungstate nano particle carrier have a synergistic antibacterial effect. Bismuth tungstate has a narrow forbidden band width, and under the irradiation of visible light,valence band electrons are easily excited to form photogenerated carriers, which then reduce oxygen molecules to form O with strong oxidizing property2 -A free radical. Simultaneously, the valence band hole and water molecule are oxidized to form strong oxidizing OH-Free radical, such O having strong oxidizing property2 -Free radicals and OH-The free radicals are in contact with viruses and bacteria to generate oxidation-reduction reaction, thereby killing the viruses and bacteria, and the O with strong oxidizing property2 -Free radicals and OH-Monovalent silver ions doped in bismuth tungstate lattices can be further oxidized by the free radicals to form trivalent silver ions with stronger bactericidal capacity, and the antibacterial effect of the silver ions is synergistically enhanced; meanwhile, silver ions are doped into bismuth tungstate lattices, so that more crystal defects can be formed, the excitation probability of electron-hole pairs is increased, the number of the electron-hole pairs is indirectly increased, and O with strong oxidizing property2 -Free radicals and OH-The number of free radicals further causes more trivalent silver ions with stronger sterilization capacity to be generated, and the synergistic antibacterial effect is remarkable.
3. Effectively solves the problem of color change of the inorganic antibacterial agent. Silver ions in the nano antibacterial material are uniformly and stably dispersed in bismuth tungstate lattices and are not easy to be converted into brown silver oxide or black simple substance silver, so that the problem of color change of the silver antibacterial agent after long-term use is solved.
Detailed Description
The invention relates to a slow-release long-acting nano antibacterial material which is prepared by ball-milling and blending silver ion doped bismuth tungstate nano particles synthesized by a one-step hydrothermal method and water glass powder, wherein the content of the silver ion doped bismuth tungstate nano particles is 10-80% by mass percent, the balance is water glass with the molar ratio of silicon oxide to sodium oxide of 0.8:1-2:1, the doping amount of silver ions in the silver ion doped bismuth tungstate nano particles is 0.01-5%, and the particle size is 2-100 nm.
The preparation method of the antibacterial material comprises the following steps:
1) synthesizing silver ion doped bismuth tungstate nano particles by a one-step hydrothermal method: 1-5mmol of sodium oleate and 0.1-2mmol of Bi (NO)3)3·5H2Adding O into deionized water, stirring for 0.2-2 hr, and adding 0.01-0.2mmol AgNO3Adding into the above mixture, magnetically stirring for 0.5-2 hr, adding 0.1-2mmol Na2WO4·2H2O is added into the solution, magnetic stirring is carried out for 0.5 to 2 hours, then the obtained mixed solution is added into a reaction tank of polytetrafluoroethylene, and hydrothermal is carried out for 18 to 32 hours at the temperature of 160 ℃ and 220 ℃. Cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for 3-6 times, and drying at 50-80 deg.C for 5-10 hr to obtain powder of silver ion doped bismuth tungstate nanoparticles.
2) Preparing a nano antibacterial material: proportionally mixing the silver ion doped bismuth tungstate nano particles prepared in the step 1) with water glass powder by mechanical ball milling for 1-10 hours, and uniformly mixing to obtain the nano antibacterial material.
The nano antibacterial material can be mixed with different materials such as high polymer, metal, glass, ceramics, coating, paint and the like, and then is used after high-temperature processing, heat treatment sintering or curing molding.
The prepared antibacterial material is used for carrying out antibacterial property test on a plurality of test strains, and the antibacterial spectrum test result shows that the antibacterial spray has broad-spectrum antibacterial property, and the antibacterial rate is more than 99%.
The present invention will be described in further detail with reference to specific examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
2.2mmol of sodium oleate and 0.4mmol of Bi (NO)3)3·5H2O is added to 40ml of deionized water, stirred for 0.3 hour, and then 0.01mmol of AgNO is added3Adding into the above mixture, stirring for 30 min, adding 0.4mmol Na2WO4·2H2O is added into the solution, magnetic stirring is carried out for 2 hours, then the obtained mixed solution is added into a reaction tank of 50ml of polytetrafluoroethylene, and hydrothermal reaction is carried out for 18 hours at 180 ℃. Cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for 3 times, and drying at 60 ℃ for 5 hours to obtain powder which is silver ion doped bismuth tungstate nano-particles.
And (2) mechanically ball-milling the prepared silver ion doped bismuth tungstate nano particles according to the mass fraction of 10% and the mass fraction of 90% of water glass powder (the molar ratio of silicon oxide to sodium oxide is 0.8:1) for 2 hours, and uniformly mixing to obtain the nano antibacterial material.
Example 2
4.4mmol of sodium oleate and 0.8mmol of Bi (NO)3)3·5H2O is added to 40ml of deionized water, stirred for 0.4 hour, and then 0.01mmol of AgNO is added3Adding into the above mixture, stirring for 1 hr, adding 0.8mmol Na2WO4·2H2O is added into the solution, magnetic stirring is carried out for 1 hour, and then the obtained mixed solution is added into a reaction tank of 50ml of polytetrafluoroethylene and hydrothermal reaction is carried out for 24 hours at 200 ℃. Cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for 6 times, drying at 70 ℃ for 8 hours, and obtaining powder which is silver ion doped bismuth tungstate nano-particles.
And (2) mechanically ball-milling the prepared silver ion doped bismuth tungstate nano particles according to the mass fraction of 40% and the mass fraction of 60% of water glass powder (the molar ratio of silicon oxide to sodium oxide is 1:1) for 1 hour, and uniformly mixing to obtain the nano antibacterial material.
Example 3
1mmol of sodium oleate and 0.1mmol of Bi (NO)3)3·5H2O is added to 40ml of deionized water, stirred for 0.2 hour, and then 0.01mmol of AgNO is added3Adding into the above mixture, stirring for 0.5 hr, adding 0.1mmol Na2WO4·2H2O is added to the above solution, magnetically stirred for 0.5 hour, and then the resulting mixture is added to a 50ml polytetrafluoroethylene reaction tank and hydrothermally heated at 160 ℃ for 18 hours. Cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for 3 times, drying at 50 ℃ for 5 hours, and obtaining powder which is silver ion doped bismuth tungstate nano-particles.
And (3) mechanically ball-milling the prepared silver ion doped bismuth tungstate nano particles according to the mass fraction of 60% and the mass fraction of 40% of water glass powder (the molar ratio of silicon oxide to sodium oxide is 0.8:1) for 1 hour, and uniformly mixing to obtain the nano antibacterial material.
Example 4
5mmol of sodium oleate and 2mmol of Bi (NO)3)3·5H2O is added to 40ml of deionized water, stirred for 2 hours, and then 0.2mmol of AgNO is added3Adding into the above mixture, stirring for 2 hr, adding 2mmol Na2WO4·2H2O is added into the solution, magnetic stirring is carried out for 2 hours, and then the obtained mixed solution is added into a reaction tank of 50ml of polytetrafluoroethylene, and hydrothermal reaction is carried out for 32 hours at 220 ℃. Cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for 6 times, drying at 80 ℃ for 10 hours, and obtaining powder which is silver ion doped bismuth tungstate nano-particles.
And (2) mechanically ball-milling the prepared silver ion doped bismuth tungstate nano particles according to the mass fraction of 80% and the mass fraction of 20% of water glass powder (the molar ratio of silicon oxide to sodium oxide is 2:1) for 10 hours, and uniformly mixing to obtain the nano antibacterial material.
The antibacterial materials prepared in the examples are used for antibacterial tests on staphylococcus aureus, bacillus subtilis, candida albicans and escherichia coli, and the antibacterial rates of the antibacterial materials are 99.4%, 99.6%, 99.3% and 99.3%, respectively.
Claims (2)
1. A preparation method of a slow-release long-acting nano antibacterial material is characterized by comprising the following steps: the nano antibacterial material is prepared by ball-milling and blending silver ion-doped bismuth tungstate nano particles and water glass powder, wherein the content of the silver ion-doped bismuth tungstate nano particles is 10-80% by mass percent, the balance is water glass with the molar ratio of silicon oxide to sodium oxide being 0.8:1-2:1, the silver ion doping amount in the silver ion-doped bismuth tungstate nano particles is 0.01-5%, and the particle size is 2nm-100nm, and the preparation method of the antibacterial material comprises the following steps:
1) synthesizing silver ion doped bismuth tungstate nano particles by a one-step hydrothermal method: mixing sodium oleate with Bi (NO)3)3·5H2Adding O into deionized water, stirring for 0.2-2 hr, and adding AgNO3Adding into the above mixture, magnetically stirring for 0.5-2 hr, adding Na2WO4·2H2Adding O into the solution, magnetically stirring for 0.5-2 hours, adding the obtained mixed solution into a polytetrafluoroethylene reaction tank, and carrying out hydrothermal treatment at the temperature of 160-220 ℃ for 18-32 hours; cooling to room temperature, washing the obtained precipitate with n-hexane and ethanol for multiple times, and drying at 50-80 deg.C for 5-10 hr to obtain powder of silver ion doped bismuth tungstate nanoparticles;
2) preparing a nano antibacterial material: proportionally mixing the silver ion doped bismuth tungstate nano particles prepared in the step 1) with water glass powder by mechanical ball milling for 1-10 hours, and uniformly mixing to prepare a nano antibacterial material;
the sodium oleate and Bi (NO)3)3·5H2O、AgNO3、Na2WO4·2H2The molar ratio of O is (1-5), (0.1-2), (0.01-0.2) and (0.1-2).
2. A method for using the slow-release long-acting nano antibacterial material prepared by the method of claim 1, which is characterized in that: the nano antibacterial material is mixed with different materials such as polymer, metal, glass, ceramics, coating and paint, and then is used after high-temperature processing, heat treatment sintering or curing molding.
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| 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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| CN104549268A (en) * | 2015-01-21 | 2015-04-29 | 江南大学 | A kind of AgBi(WO4)2 photocatalytic material and preparation method thereof |
| CN104971720A (en) * | 2015-06-11 | 2015-10-14 | 西北师范大学 | Bismuth tungstate nanocomposite, and preparation method and application thereof |
| CN105457663A (en) * | 2015-11-17 | 2016-04-06 | 中国科学院海洋研究所 | A kind of Bi2WO6/Ag3PO4 composite photocatalytic bactericide and its preparation method |
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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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