CN1792508A - Nano silver using inorganic metallic oxide as carrier and preparation process thereof - Google Patents
Nano silver using inorganic metallic oxide as carrier and preparation process thereof Download PDFInfo
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Abstract
A nano-Ag carried by the inorganic metallic oxide chosen from SiO2, TiO2 and ZrO2 is prepared from Ag nano-particles and said inorganic metallic oxide through sol-gel method to attach the Ag nano-particles onto the surface of inorganic metallic oxide. Its advantage is high dispersity and stability of Ag nano-particles.
Description
Technical Field
The invention relates to a nano material, in particular to nano silver taking inorganic metal oxide as a carrier;
the invention also relates to a preparation method of the nano silver taking the inorganic metal oxide as the carrier.
Technical Field
The nano silver particles belong to nano noble metal particles, and refer to metal silver particles with the particle size of 1-100 mm, and are also called as ultramicro noble metal particles. The excellent performance of the nano silver material depends on the unique microstructure, and the nano silver particles have obvious surface effect, quantum size effect and macroscopic quantum tunneling effect, thereby showing the characteristics of biology, heat, light, electricity, magnetism, catalysis, sensitivity and the like different from the conventional materials, and being applied to many fields of biomedicine, optics, electronics, photoelectric materials, catalysts, magnetic materials and the like.
At present, the widely applied fields of nano silver include medical, antibacterial materials, conductive materials and the like. For example, Chinese patent CN87100231A (published in 11/18/1987) discloses an antibacterial deodorant fabric, which is prepared by sequentially combining acrylic fabric and Cu+And alkaline green 4 composite crosslinking, the product has antibacterial effect on staphylococcus aureus, staphylococcus albus, MRSA, candida albicans and the like, and can be used for deodorant underwear, socks, insoles and work clothes in the medicine and food industry. U.S. patent No. 5785972 (published 1998, 7/28) discloses an ointment for preventing burn and scald infection, which is prepared from nano-silver, honey and helichrysum oil and can be applied to wound to prevent infection. In U.S. patent No. 6136228, published 2000-10-24 days, a transparent conductive coating is prepared by mixing nano silver solution with a coating, and the coating can be used as an antistatic coating.
Because the nano silver particles are extremely small, the surface energy is very large and the nano silver particles are easy to agglomerate, the carriers are added for preparing the nano silver particles so as to increase the stability of the nano silver particles and prevent the nano silver particles from agglomerating. At present, the preparation method of nano silver mainly comprises a chemical reduction method and a ray irradiation method. For example, U.S. Pat. No. 6,6660058 (published 2003, 12/9) uses sodium dodecylsulfonate as a protecting agent to prepare a nanosilver solution. Chinese patent CN1583332A (published 2005, 2/23) adopts a silver sol redox reaction in which a dispersed protective colloid solution is mixed with a silver nitrate solution and a reducing agent solution to control the growth of silver particles, so as to obtain a nano silver sol. The nano silver prepared in the above patent reports exists in the form of colloidal nano silver. The colloidal silver is unstable, and nano silver aggregates and precipitates out of a dispersion medium in a certain time. Chinese patent CN1359775 (published 2002, 7, 24) discloses a method for preparing nano silver particles by laser gas phase, which comprises subjecting silver nitrate solution to ultrasonic atomization, mixing with photosensitive gas and carrier gas, allowing the mixture to enter a reaction chamber, allowing the mixture to orthogonally meet with laser beam, maintaining the pressure in the reaction chamber at a set value dynamically, and allowing the photosensitive gas SF to contact with the laser beam at a set value6Under the action of light energy absorption and transmission, the temperature of the reaction zone exceeds the thermal decomposition temperature of silver nitrate, so that the silver nitrate is completely decomposed to form silver particle cores, and nano silver particles are formed in the subsequent quenching process. Chinese patent CN1557588 (published 2004, 12/29/10) discloses a method for preparing nano silver particles by radiation chemistry, in the process, silver nitrate is mainly used as the source of silver particles, and Isopropanol (IPA) is used as an oxidative free scavenger in aqueous solution; and controlling the growth speed of crystal nucleus by using hydrophilic surfactant polyvinyl alcohol (PVA) to control the particle size, performing irradiation treatment by using electron beams generated by an electron accelerator, washing, centrifugally separating and drying the irradiated solution to obtain the nano-silver powder. The two methods are difficult to control and have small feasibility of industrial production.
In order to solve the problems of the above methods, chinese patent CN1623897 (published 2005, 6/8) issued a method for preparing silica powder containing nano silver. The preparation method comprises the steps of adding silver nitrate solid into deionized water for dissolving to prepare silver nitrate solution, adding solution of surfactant into the solution, adding reducing agent to generate nano silver sol with the particle size of 1-100 nanometers, then adding silicon dioxide colloid, and adsorbing nano silver onto nano silicon dioxide colloid particles to obtain the nano silver-loaded silicon dioxide colloid. However, such adsorption force is weak, and the nano silver particles are easily separated from the silica particles. In addition, the concentration of nano silver prepared by the method is not high enough.
Disclosure of Invention
The invention aims to provide a preparation method of nano silver by taking inorganic metal oxide as a carrier, which adopts a sol-gel method to ensure that nano silver particles are adsorbed on the surface of the metal oxide, so that the nano silver particles growing on the metal oxide powder carrier obtain high dispersibility and stability, the application range of the nano silver is wider, and the effect is better.
The invention also aims to provide the nano silver prepared by the method and taking the inorganic metal oxide as the carrier.
The invention relates to a method for preparing nano silver by taking inorganic metal oxide as a carrier, whichcomprises the following steps:
(1) mixing 0.15g-2.40g of silver nitrate with isopropanol, inorganic metal alkoxide and ammonia water, and stirring for 4-12 hours;
(2) filtering and washing the product obtained in the step (1) to obtain inorganic metal oxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the powder obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent to form a suspension;
(4) and (4) filtering, washing and drying the suspension obtained in the step (3) to obtain the nano silver particles taking the inorganic metal oxide as the carrier.
In the step (1), the inorganic metal alkoxide is preferably Si (OC)2H5)4、Ti(OC4H9)4Or Zr (OC)3H7)4。
The reducing agent in the step (3) is sodium borohydride or sodium citrate, the concentration of the aqueous solution of the reducing agent has no special requirement, and a saturated solution is generally adopted.
In the step (3), the reduction reaction time is preferably 10min-3 h.
The obtained nano silver particles with the metal oxide as the carrier are formed by attaching nano silver particles on the surface of metal oxide powder; wherein the content of the nano silver is 0.5-8% by weight; the particle size of the metal oxide powder is 1-100 microns, and the particle size of the nano silver is 10-50 nanometers.
Compared with the prior art, the invention has the following advantages: the method for preparing the composite nano silver is simple and easy to implement and easy to popularize and apply. The obtained product has high purity, uniformity and dispersibility, and the maximum silver content can reach 10%. The product has wider application, is a high-functional conductive, antibacterial and catalytic material, and can be widely applied to the fields of catalyst materials, battery electrode materials, antibacterial materials, photonic crystal materials, electronic and visual sensors, low-temperature heat conduction materials, conductive slurry and the like.
Detailed Description
Example 1 with SiO2Preparing a nano silver material as a carrier:
(1) 0.15g of silver nitrate was mixed with 450ml of isopropanol, 45ml of Si (OC)2H5)445ml of ammonia water are mixed and stirred for 4 hours;
(2) filtering and washing the product obtained in the step (1) to obtain silicon dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the silicon dioxide powder adsorbing the silver ammino ions obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent into the water for reaction for 10 min;
(4) and (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking the silicon dioxide powder as the carrier. Wherein, the grain diameter of the silicon dioxide is about 5 microns, and the grain diameter of the nano silver is about 15 nanometers. The content of the nano silver is 0.5 percent.
Example 2 with SiO2Preparing a nano silver material as a carrier:
(1) 0.3g of silver nitrate was mixed with 450ml of isopropanol, 45ml of Si (OC)2H5)445ml of aqueous ammoniaStirring for 12 hours;
(2) filtering andwashing the product obtained in the step (1) to obtain silicon dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the silicon dioxide powder adsorbing the silver ammino ions obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent into the water for reaction for 3 hours;
(4) and (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking the silicon dioxide powder as the carrier. Wherein, the grain diameter of the silicon dioxide is about 10 microns, and the grain diameter of the nano silver is about 20 nanometers. The content of the nano silver is 1 percent.
Example 3 with TiO2Preparing a nano silver material as a carrier:
(1) 0.6g of silver nitrate was mixed with 450ml of isopropanol, 80ml of Ti (OC)4H9)445ml of ammonia water and 4Hours;
(2) filtering and washing the product obtained in the step (1) to obtain titanium dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the titanium dioxide powder adsorbing the silver ammino ions obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent into the water for reaction for 30 min;
(4) and (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking titanium dioxide powder as a carrier. Wherein the grain diameter of the titanium dioxide is about 4 microns, and the grain diameter of the nano silver is about 25 nanometers. The content of the nano silver is 2 percent.
Example 4 with TiO2Preparing a nano silver material as a carrier:
(1) 1.2g of silvernitrate was mixed with 450ml of isopropanol, 80ml of Ti (OC)4H9)445ml of ammonia water are mixed and stirred for 12 hours;
(2) filtering and washing the product obtained in the step (1) to obtain titanium dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the titanium dioxide powder adsorbing the silver ammino ions obtained in the step (2) in water, dropwise adding an aqueous solution of a reducing agent into the water, and reacting for 1h
(4) And (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking titanium dioxide powder as a carrier. Wherein the grain diameter of the titanium dioxide is about 8 microns, and the grain diameter of the nano silver is about 30 nanometers. The content of the nano silver is 4 percent.
Example 5
With ZrO2Preparing a nano silver material as a carrier:
(1) 1.8g of silver nitrate was mixed with 450ml of isopropanol, 50ml of Zr (OC)3H7)445ml of ammonia water are mixed and stirred for 4 hours;
(2) filtering and washing the product obtained in the step (1) to obtain zirconium dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the zirconium dioxide powder adsorbing silver ammino ions obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent into the water for reaction for 30 min;
(4) and (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking zirconium dioxide powder as a carrier. Wherein the grain diameter of the zirconium dioxide is about4 microns, and the grain diameter of the nano silver is about 40 nanometers. The content of the nano silver is 6 percent.
EXAMPLE 6 with ZrO2Preparing a nano silver material as a carrier:
(1) 2.4g of silver nitrate was mixed with 450ml of isopropanol, 50ml of Zr (OC)3H7)445ml of ammonia water are mixed and stirred for 12 hours;
(2) filtering and washing the product obtained in the step (1) to obtain zirconium dioxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the zirconium dioxide powder adsorbing silver ammino ions obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent into the water for reaction for 30 min;
(4) and (4) filtering and washing the suspension obtained in the step (3), and drying the obtained powder to obtain the nano silver particles taking zirconium dioxide powder as a carrier. Wherein the grain diameter of the zirconium dioxide is about 4 microns, and the grain diameter of the nano silver is about 50 nanometers. The content of the nano silver is 8 percent.
Example 7 the percent content of nano silver in the material was determined by titration method for the nano silver supported on inorganic metal oxide obtained in examples 1-6.
(1) Titration principle: weighing a certain amount of nano silver powder using inorganic metal oxide as carrier, firstly dissolving nano silver into silver ions (Ag) by using concentrated nitric acid+) And an indicator is added. Then adding NH which can react with silver ions to generate precipitates dropwise into the solution4SCN, continuously adding dropwise NH after silver ions are consumed4SCN can react with indicator NH in solution4Fe(SO4)2The chemical reaction takes place and the solution is bright reddish brown, which is the end point of the titration. By adding dropwise NH4The total amount of SCN can be used to calculate the mass of silver ions in solution, i.e. the mass of nano-silver. The reaction chemical equation is as follows:
(2) solution preparation:
solvent: 6M HNO3；
Indicator (b): 10% NH4Fe(SO4)2；
Titration solution: NH (NH)4SCN。
0.75g of NH are weighed4SCN was placed in a 1000ml volumetric flask and water was added to the scale.
(3) Preparation of standard silver solution:
weighing 1.0000g of Ag powder, adding 100ml of 6N HNO3And heating in water bath, and adding the volumetric flask to 1000ml when the silver powder is completely dissolved, wherein the concentration of the standard Ag solution is 1 mg/ml.
(4) Standard NH4Preparation of SCN solution:
taking 10ml of standard Ag solution, and sequentially adding 10ml of water and 6N HNO3(content of 1-10%), 1-2ml 10% NH4Fe(SO4)2And adding water to make the total volume reach 80-100 ml. With ready NH4SCN titrates, endpoint is reached and recorded. Three consecutive times were averaged and made to have an error of no more than 0.10 ml.
(5) Calibration analysis of nano silver particles
Weighing 100.0mg of nano silver powder taking inorganic metal oxide as carrier, adding 20-30ml of 6N HNO3Heating in low temperature water bath until the slightly boiling solution is colorless, diluting to 100ml, and adding 1-2ml NH4Fe(SO4)2Titration was started until the solution appeared bright reddish brown.
(6) The percentage of nano-silver can be determined by the following formula:
the nano silver powder prepared in examples 1, 2, 3, 4, 5 and 6, which uses inorganic metal oxide as a carrier, has a nano silver content of 0.5-8 wt% measured according to the above method.
Claims (5)
1. A method for preparing nano silver by taking inorganic metal oxide as a carrier is characterized by comprising the following steps:
(1) mixing 0.15g-2.40g of silver nitrate with isopropanol, inorganic metal alkoxide and ammonia water, and stirring for 4-12 hours;
(2) filtering and washing the product obtained in the step (1) to obtain inorganic metal oxide powder adsorbing silver-ammonia complex ions;
(3) dispersing the powder obtained in the step (2) in water, and dropwise adding an aqueous solution of a reducing agent to form a suspension;
(4) and (4) filtering, washing and drying the suspension obtained in the step (3) to obtain the nano silver taking the inorganic metal oxide as the carrier.
2. The method according to claim 1, wherein in step (1), the inorganic metal alkoxide is Si (OC)2H5)4、Ti(OC4H9)4Or Zr (OC)3H7)4。
3. The method according to claim 1 or 2, characterized in that the reducing agent in step (3) is sodium borohydride or sodium citrate.
4. The method according to claim 3, wherein in the step (3), the reduction reaction time is 10min to 3 h.
5. The nano silver supported on the metal oxide prepared by the method of any one of claims 1 to 4, wherein the nano silver is formed by attaching nano silver particles to the surface of metal oxide powder; wherein the content of the nano silver is 0.5-8% by weight; the particle size of the metal oxide powder is 1-100 microns, and the particle size of the nano silver is 10-50 nanometers.
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| CN 200510101485 CN1792508A (en) | 2005-11-25 | 2005-11-25 | Nano silver using inorganic metallic oxide as carrier and preparation process thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100591417C (en) * | 2008-06-26 | 2010-02-24 | 南京大学 | Silicon dioxide supported nano-silver catalyst, preparation and use thereof |
| CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
| CN103756155A (en) * | 2014-01-27 | 2014-04-30 | 河南联塑实业有限公司 | Antibacterial PPR pipe |
| CN103783081A (en) * | 2014-01-17 | 2014-05-14 | 浙江理工大学 | Preparation method of silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent |
| CN104741605A (en) * | 2015-04-10 | 2015-07-01 | 武汉大学 | Nano-silver wrapping type silicon dioxide nano-micron ball conductive powder and production method and application thereof |
| CN105195732A (en) * | 2015-09-10 | 2015-12-30 | 有研亿金新材料有限公司 | Platinum-ceramic composite powder and preparation method and application thereof |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN106513700A (en) * | 2016-11-01 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Nano-silver colloid carried by porous titanium dioxide and preparation and application of nano-silver colloid carried by porous titanium dioxide |
| CN109592189A (en) * | 2017-09-30 | 2019-04-09 | 上海住邦电器有限公司 | Nano-silver anion restraining and sterilizing bacteria liner enamelled vessel |
| CN114871426A (en) * | 2022-05-20 | 2022-08-09 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano-silver material, preparation method and application |
| CN115418013A (en) * | 2022-09-15 | 2022-12-02 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
-
2005
- 2005-11-25 CN CN 200510101485 patent/CN1792508A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100591417C (en) * | 2008-06-26 | 2010-02-24 | 南京大学 | Silicon dioxide supported nano-silver catalyst, preparation and use thereof |
| CN103350226A (en) * | 2013-07-16 | 2013-10-16 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
| CN103350226B (en) * | 2013-07-16 | 2015-07-01 | 合肥工业大学 | SiO2/Ag composite micron sphere and preparation method thereof |
| CN103783081A (en) * | 2014-01-17 | 2014-05-14 | 浙江理工大学 | Preparation method of silver-copper oxide co-doped mesoporous zirconium dioxide antibacterial agent |
| CN103756155A (en) * | 2014-01-27 | 2014-04-30 | 河南联塑实业有限公司 | Antibacterial PPR pipe |
| CN103756155B (en) * | 2014-01-27 | 2016-03-02 | 河南联塑实业有限公司 | A kind of Antibacterial PPR pipe |
| CN104741605B (en) * | 2015-04-10 | 2017-03-01 | 武汉大学 | Nanometer silver parcel silicon dioxide receives micron ball conductive powder and its preparation method and application |
| CN104741605A (en) * | 2015-04-10 | 2015-07-01 | 武汉大学 | Nano-silver wrapping type silicon dioxide nano-micron ball conductive powder and production method and application thereof |
| CN105195732A (en) * | 2015-09-10 | 2015-12-30 | 有研亿金新材料有限公司 | Platinum-ceramic composite powder and preparation method and application thereof |
| CN106283123A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of preparation method of nanometer silver coating |
| CN106513700A (en) * | 2016-11-01 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Nano-silver colloid carried by porous titanium dioxide and preparation and application of nano-silver colloid carried by porous titanium dioxide |
| CN109592189A (en) * | 2017-09-30 | 2019-04-09 | 上海住邦电器有限公司 | Nano-silver anion restraining and sterilizing bacteria liner enamelled vessel |
| CN109592189B (en) * | 2017-09-30 | 2021-04-30 | 上海住邦电器有限公司 | Nano-silver negative ion bacteriostatic and bactericidal inner container enamel container |
| CN114871426A (en) * | 2022-05-20 | 2022-08-09 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano-silver material, preparation method and application |
| CN114871426B (en) * | 2022-05-20 | 2023-12-22 | 爱科美材料科技(南通)有限公司 | Mesoporous alumina in-situ coated nano silver material, preparation method and application |
| CN115418013A (en) * | 2022-09-15 | 2022-12-02 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
| CN115418013B (en) * | 2022-09-15 | 2023-09-01 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
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