CN103783081A - Preparation method of silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent - Google Patents
Preparation method of silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent Download PDFInfo
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Abstract
The invention discloses a preparation method of a silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent. The preparation method comprises the following steps: dissolving a template agent, a lower alcohol, a zirconium source and a stabilizing agent in water to form a zirconium precursor solution; dropwise adding a silver nitrate aqueous solution and a zinc chloride aqueous solution to the zirconium precursor solution in the stirring process and mixing the solutions to form gel; and carrying out radiation treatment on the gel under a light source after drying the gel and then carrying out high temperature treatment, thus obtaining the silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent. The antibacterial agent takes mesoporous zirconium dioxide as a network supporting body and elemental silver and copper oxide as active centers and has elemental silver content of 21-25%, copper oxide content of 11-15% and zirconium dioxide content of 60-68%. The prepared silver-loaded mesoporous inorganic antibacterial agent has specific surface area of 500-1200cm<2>/g, aperture of 5-30nm and pore volume of 5.0-10.0cm<3>/g. The preparation method is simple, has the advantages of broad-spectrum antibacterial property, lasting antibacterial effect and stable antibacterial properties and can be widely used in the fields such as ceramics, plastics, textiles, coatings and water treatment.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic antiseptic, be specifically related to a kind of preparation method of mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope.
Background technology
In recent years,, owing to being subject to the impact of " SARS (Severe Acute Respiratory Syndrome) ", " bird flu ", " H1N1 Flu-A ", people's health consciousness constantly strengthens, and the demand of anti-biotic material and goods thereof is improved greatly.In daily life environment, the microorganisms such as virus, bacterium, fungi are not only polluting environment, also cause generation and the infection of a lot of diseases, and human health is caused to great threat.Inorganic antiseptic is the metal ions such as silver, copper, zinc be loaded on the carriers such as zeolite, apatite, silica gel and form.Inorganic antiseptic, by the high efficiency of stability intrinsic inorganic material and antimicrobial component, popularity are combined, has broad spectrum antibacterial, and antibacterial efficacy is lasting, and anti-microbial property is stable, to features such as human body are nontoxic.
Since mesoporous material is found, the excellent specific property of mesoporous material has just been subject to scholar's extensive concern always, because it has orderly pore passage structure, high specific surface area and pore volume, regular one dimension six square cylindrical ducts, pore-size distribution homogeneous and controlled, chemical stability is high, and the template of synthetic this kind of mesoporous material is simple and easy to get, effectively reduces manufacturing cost, thereby has shown unique development potentiality in the field such as catalysis, absorption.
Chinese patent 200610024773.9 discloses Nanometer mesoporous Silver Anti-bacterial Agent And Preparation Method, and this patent is take mesoporous silicon oxide as carrier, loads silver ion, and then under high temperature protection gas, sintering obtains the inorganic antiseptic of Ag-bearing simple substance.Chinese patent 200910156605.9 discloses a kind of inorganic nanometer-sized mesoporous antibacterial agent and preparation method.First this patent prepares inorganic nanometer-sized mesoporous material, then carries out surface graft modification, and liquor argenti nitratis ophthalmicus is added dropwise to after the inorganic nanometer-sized mesoporous material after modification with formaldehyde reduction, obtains inorganic nanometer-sized mesoporous antibacterial agent.Chinese patent 201110228086.X discloses bearing copper silicon nano mesoporous inorganic antimicrobial agent of a kind of year silver and preparation method thereof.This patent, by water-soluble polyethylene glycol-propane diols-polyethyleneglycol block copolymer, adds silicon source, copper nitrate and silver nitrate, obtains gel, then passes through roasting direct, obtains the bearing copper silicon nano mesoporous inorganic antimicrobial agent of argentiferous simple substance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope, by water-soluble to template, low-carbon alcohols, zirconium source and stabilizing agent, form zirconium precursor liquid solution, in whipping process, silver nitrate aqueous solution and solder(ing)acid are added dropwise to zirconium precursor liquid solution, the mixed gel that forms, after gel is dried, under light source, carry out treatment with irradiation, then obtain the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope through high temperature treatment.
The step of the technical solution used in the present invention is as follows:
(1) be that 0.01～0.1:0.1～0.5:1 is evenly mixed by template, low-carbon (LC) alcohol and water according to mol ratio, stir to clarify, add again successively zirconium source and stabilizing agent, wherein the mass percent of zirconium source and template is 0.05～0.2:1, the mass percent of stabilizing agent and template is 0.01～0.05:1, under 200～400 revs/min, stir 6～12 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.19～0.25:1, the mass percent in copper chloride and zirconium source is 0.10～0.16:1, in dropping process, zirconium precursor liquid solution stirs 6～12 hours under 300～500 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, be 300～700 nanometers at wavelength again, luminous intensity is to irradiate 2～6 hours under the light source of 10000～50000 candelas, then at 400～700 ℃ of temperature, it is heat-treated 2～10 hours, obtain the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide accounts for the mass percent 60～68% of the mesoporous ZrO 2 antibacterial agent of described silver-copper oxide codope, copper oxide accounts for the mass percent 11～15% of the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope, and simple substance silver accounts for the mass percent 21～25% of the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope.
Described template is polyethylene glycol-propane diols-polyethyleneglycol block copolymer, neopelex, softex kw or lauryl sodium sulfate.
Described low-carbon alcohols is methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol or the tert-butyl alcohol.
Described zirconium source is zirconic acid four n-propyls, zirconic acid four isopropyl esters or tetrabutyl zirconate.
Described stabilizing agent is diethylene glycol, acetylacetone,2,4-pentanedione or triethanolamine.
Compared with background technology, the beneficial effect that the present invention has is:
1) the present invention is take mesoporous ZrO 2 as carrier, mesoporous ZrO 2 has the aperture of orderly pore passage structure, homogeneous, larger specific surface area and pore volume, the load capacity of silver simple substance and copper oxide is high, utilizes the synergy of silver-colored simple substance and copper oxide antibiotic property, can significantly improve antibacterial effect.
2) preparation method of the present invention is simple, has broad spectrum antibacterial, and antibacterial efficacy is lasting, and anti-microbial property is stable, to features such as human body are nontoxic, can be widely used in the fields such as pottery, plastics, weaving, coating and water treatment.
Embodiment
Embodiment 1:
(1) be that 0.01:0.1:1 is evenly mixed by polyethylene glycol-propane diols-polyethyleneglycol block copolymer, first alcohol and water according to mol ratio, stir to clarify, add again successively zirconic acid four n-propyls and diethylene glycol, wherein the mass percent of zirconic acid four n-propyls and polyethylene glycol-propane diols-polyethyleneglycol block copolymer is 0.05:1, the mass percent of diethylene glycol and polyethylene glycol-propane diols-polyethyleneglycol block copolymer is 0.01:1, under 200 revs/min, stir 12 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.19:1, the mass percent in copper chloride and zirconium source is 0.10:1, in dropping process, zirconium precursor liquid solution stirs 12 hours under 300 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, then be 300 nanometers at wavelength, luminous intensity is to irradiate 6 hours under the light source of 10000 candelas, then at 400 ℃ of temperature, it is heat-treated 10 hours, obtains the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide: copper oxide: the mass percent of simple substance silver is 68:11:21.
The specific surface area of carrying silver-colored mesoporous inorganic antibacterial (being labeled as Sample A) of preparation is 500cm
2/ g, aperture is 5nm, pore volume is 5.0cm
3/ g, finally for Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans, Trichophyton rubrum antibacterial experiment.
Embodiment 2:
(1) be that 0.1:0.5:1 is evenly mixed by neopelex, second alcohol and water according to mol ratio, stir to clarify, add again successively zirconic acid four isopropyl esters and acetylacetone,2,4-pentanedione, wherein the mass percent of zirconic acid four isopropyl esters and neopelex is 0.2:1, the mass percent of acetylacetone,2,4-pentanedione and neopelex is 0.05:1, under 400 revs/min, stir 6 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.25:1, the mass percent in copper chloride and zirconium source is 0.16:1, in dropping process, zirconium precursor liquid solution stirs 6 hours under 500 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, then be 700 nanometers at wavelength, luminous intensity is to irradiate 2 hours under the light source of 50000 candelas, then at 700 ℃ of temperature, it is heat-treated 2 hours, obtains the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide: copper oxide: its mass percent of simple substance silver is 60:15:25.
The specific surface area of carrying silver-colored mesoporous inorganic antibacterial (being labeled as sample B) of preparation is 1200cm
2/ g, aperture is 30nm, pore volume is 10.0cm
3/ g, finally for Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans, Trichophyton rubrum antibacterial experiment.
Embodiment 3:
(1) be that 0.04:0.2:1 is evenly mixed by softex kw, normal propyl alcohol and water according to mol ratio, stir to clarify, add again successively tetrabutyl zirconate and triethanolamine, wherein the mass percent of tetrabutyl zirconate and softex kw is 0.1:1, the mass percent of triethanolamine and softex kw is 0.02:1, under 250 revs/min, stir 10 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.20:1, the mass percent in copper chloride and zirconium source is 0.12:1, in dropping process, zirconium precursor liquid solution stirs 8 hours under 450 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, then be 500 nanometers at wavelength, luminous intensity is to irradiate 4 hours under the light source of 30000 candelas, then at 600 ℃ of temperature, it is heat-treated 4 hours, obtains the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide: copper oxide: its mass percent of simple substance silver is 64:12:24.
The specific surface area of carrying silver-colored mesoporous inorganic antibacterial (being labeled as sample C) of preparation is 800cm
2/ g, aperture is 18nm, pore volume is 6.0cm
3/ g, finally for Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans, Trichophyton rubrum antibacterial experiment.
Embodiment 4:
(1) be that 0.08:0.4:1 is evenly mixed by lauryl sodium sulfate, isopropyl alcohol and water according to mol ratio, stir to clarify, add again successively zirconic acid four n-propyls and diethylene glycol, wherein the mass percent of zirconic acid four n-propyls and lauryl sodium sulfate is 0.14:1, the mass percent of diethylene glycol and lauryl sodium sulfate is 0.04:1, under 350 revs/min, stir 8 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.22:1, the mass percent in copper chloride and zirconium source is 0.14:1, in dropping process, zirconium precursor liquid solution stirs 11 hours under 350 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, then be 400 nanometers at wavelength, luminous intensity is to irradiate 3 hours under the light source of 40000 candelas, then at 550 ℃ of temperature, it is heat-treated 6 hours, obtains the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide: copper oxide: its mass percent of simple substance silver is 63:14:23.
The specific surface area of carrying silver-colored mesoporous inorganic antibacterial (being labeled as sample D) of preparation is 1000cm
2/ g, aperture is 22nm, pore volume is 8.0cm
3/ g, finally for Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans, Trichophyton rubrum antibacterial experiment.
Above-mentioned 4 embodiment carry out antibacterial experiment according to the antibacterial industry standard of Japan to Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans and Trichophyton rubrum, obtain minimal inhibitory concentration in each embodiment, be listed in the table below 1, each embodiment has all shown that Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans and Trichophyton rubrum are had to good antibacterial ability.
The minimal inhibitory concentration of the each embodiment antibacterial agent of table 1 to Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, Candida albicans, Trichophyton rubrum.
Claims (5)
1. a preparation method for the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope, is characterized in that, carries out according to the following steps:
(1) be that 0.01～0.1:0.1～0.5:1 is evenly mixed by template, low-carbon (LC) alcohol and water according to mol ratio, stir to clarify, add again successively zirconium source and stabilizing agent, wherein the mass percent of zirconium source and template is 0.05～0.2:1, the mass percent of stabilizing agent and template is 0.01～0.05:1, under 200～400 revs/min, stir 6～12 hours, obtain zirconium precursor liquid solution;
(2) silver nitrate aqueous solution that is 0.2% by mass percent concentration and mass percent concentration are that 0.1% copper chloride solution drops in zirconium precursor liquid solution simultaneously, wherein the mass percent in silver nitrate and zirconium source is 0.19～0.25:1, the mass percent in copper chloride and zirconium source is 0.10～0.16:1, in dropping process, zirconium precursor liquid solution stirs 6～12 hours under 300～500 revs/min, then in room temperature ageing, dry, obtain gel;
(3) gel is dry under vacuum, be 300～700 nanometers at wavelength again, luminous intensity is to irradiate 2～6 hours under the light source of 10000～50000 candelas, then at 400～700 ℃ of temperature, it is heat-treated 2～10 hours, obtain the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope; Wherein: zirconium dioxide accounts for the mass percent 60～68% of the mesoporous ZrO 2 antibacterial agent of described silver-copper oxide codope, copper oxide accounts for the mass percent 11～15% of the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope, and simple substance silver accounts for the mass percent 21～25% of the mesoporous ZrO 2 antibacterial agent of silver-copper oxide codope.
2. the preparation method of the mesoporous ZrO 2 antibacterial agent of a kind of silver-copper oxide codope according to claim 1, is characterized in that: described template is polyethylene glycol-propane diols-polyethyleneglycol block copolymer, neopelex, softex kw or lauryl sodium sulfate.
3. the preparation method of the mesoporous ZrO 2 antibacterial agent of a kind of silver-copper oxide codope according to claim 1, is characterized in that: described low-carbon alcohols is methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol or the tert-butyl alcohol.
4. the preparation method of a kind of year according to claim 1 silver-colored mesoporous inorganic antibacterial, is characterized in that: described zirconium source is zirconic acid four n-propyls, zirconic acid four isopropyl esters or tetrabutyl zirconate.
5. the preparation method of a kind of year according to claim 1 silver-colored mesoporous inorganic antibacterial, is characterized in that: described stabilizing agent is diethylene glycol, acetylacetone,2,4-pentanedione or triethanolamine.
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Cited By (6)
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| CN105885604A (en) * | 2016-06-12 | 2016-08-24 | 铜陵青铜时代雕塑有限公司 | Zirconium n-Butoxide modified high-hardness and abrasion-resisting coating for urban copper-cast sculpture and preparation method thereof |
| CN108976475A (en) * | 2018-07-18 | 2018-12-11 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| CN109310355A (en) * | 2016-06-30 | 2019-02-05 | 拓自达电线株式会社 | Electrode material |
| CN112575448A (en) * | 2020-12-11 | 2021-03-30 | 浙江理工大学 | Preparation method of porous non-woven fabric with antibacterial function |
| CN112979163A (en) * | 2021-02-07 | 2021-06-18 | 深圳市阳光晶玻科技有限公司 | Ultrathin flexible glass material and preparation method and application thereof |
| US11490846B2 (en) | 2016-06-30 | 2022-11-08 | Tatsuta Electric Wire & Cable Co., Ltd. | Bioelectrode and method for producing bioelectrode |
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| CN112575448A (en) * | 2020-12-11 | 2021-03-30 | 浙江理工大学 | Preparation method of porous non-woven fabric with antibacterial function |
| CN112979163A (en) * | 2021-02-07 | 2021-06-18 | 深圳市阳光晶玻科技有限公司 | Ultrathin flexible glass material and preparation method and application thereof |
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Application publication date: 20140514 |