CN1685830A - Nano silver antibacterial powder and its preparation method - Google Patents
Nano silver antibacterial powder and its preparation method Download PDFInfo
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- CN1685830A CN1685830A CN 200510049756 CN200510049756A CN1685830A CN 1685830 A CN1685830 A CN 1685830A CN 200510049756 CN200510049756 CN 200510049756 CN 200510049756 A CN200510049756 A CN 200510049756A CN 1685830 A CN1685830 A CN 1685830A
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Abstract
An antibacterial nano-Ag powder for ceramics is prepared from Ag nanoparticles and zeolite as carrier proportionally. Its advantages are high refractory performance and high antibacterial effect.
Description
Technical field
The present invention relates to a kind of antimicrobial powder, especially relate to a kind of nano-silver antimicrobial powder and preparation method.
Background technology
In recent years, microorganisms such as bacterium, virus are infected and cause multiple infectious disease to occur, and cause the instability of enormous economic loss and society.After China was subjected to the SARS virus challenge, people had had deeper requirement to antibacterial, antibiotic daily necessities.Present antimicrobial product is various, wherein a kind of is antimicrobial powder, using always in the existing antimicrobial powder is the antimicrobial powder of sterilization main body with the nano silver powder, introduced a kind of preparation method of carrying nano silver antimicrobial powder in the disclosed No. 200410016338.2 Chinese invention patent application specifications as on December 29th, 2004, it is to be to add ultra-fine carrier in 0.01～5.0% the silver nitrate aqueous solution with percent concentration, through ultrasonic oscillation after 0.5～4 hour, adding concentration is 0.01～5.0% surperficial adjuvant water solution, adding concentration is 0.001～1.0% hydrazine hydrate aqueous solution in stirring, continue to stir 10～30 minutes, obtain to contain the solution of carrier nano silver powder.Through separation, washing, drying, obtain the carrying nano silver antimicrobial powder of silver content 0.1～20%.But it is found that in actual applications this invents prepared antimicrobial powder when being used to make anti-bacteria ceramic, can be because high temperature sintering makes the anti-microbial property of the anti-bacteria ceramic that is made into that a bigger reduction be arranged.
Summary of the invention
Technical problem to be solved by this invention is that a kind of have safety, lasting, broad-spectrum antiseptic, premium properties such as heat-resisting, the nano-silver antimicrobial powder and the preparation method that can be effectively applied to make anti-bacteria ceramic are provided at above-mentioned prior art present situation.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of nano-silver antimicrobial powder, it is to be the powder that carrier constitutes with the zeolite by Nano Silver, the granularity of described powder is 25～70 μ m, described content of nanometer silver is 1.0～20%, and the granularity of described Nano Silver is 1～50nm.
The present invention solves the problems of the technologies described above another technical scheme that is adopted: a kind of preparation method of nano-silver antimicrobial powder, and it may further comprise the steps:
(1) the zeolite powder is immersed in 1～20% the liquor argenti nitratis ophthalmicus 10～20 hours, silver ion fully is adsorbed in the hole of zeolite;
(2) be in the mixed liquor adding reactor of 0.01～5.0% surperficial adjuvant water solution and step (1) with concentration, add deionized water, mixed liquor and deionized water weight ratio are 1: 1～20, dripping concentration with measuring pump in stirring is 0.001～1.0% hydrazine hydrate solution, liquid pH value to be mixed reaches 7.0～7.1, stopping to add hydrazine hydrate, and continue to stir 10～30min, is Nano Silver simple substance with silver ion reduction;
(3) the reacted liquid of step (2) is taken out, left standstill 4～10 days, fully sedimentation, decantation is used deionized water washing sediment 2～5 times, decantation liquid circulation washing of precipitate;
(4) sediment that step (3) is obtained is at 80～90 ℃ of dry moisture of removing, and ball milling to 25～70 μ m obtains the nano silver powder that zeolite is a carrier, and the granularity of described Nano Silver is 1～50nm, and described content of nanometer silver is 1.0～20%.
Described zeolite can be clinoptilolite, modenite and their mixture.
Described surperficial auxiliary agent can be dodecyl sodium sulfate, polyvinylpyrrolidone, lauryl sodium sulfate, sodium polyphosphate, one or more of sodium citrate.
Compared with prior art, the invention has the advantages that the anti-microbial property that utilizes Nano Silver, with the zeolite is carrier, have resistant to elevated temperatures characteristics, the antimicrobial powder of making adds in the ceramic glaze, and the ceramic of firing has significant antibacterial effect, bacterial classifications such as Escherichia coli, staphylococcus aureus, Candida albicans is suppressed the rate of killing extremely can reach more than 99%, be mainly used in china sanitary ware, domestic ceramics, fields such as architectural pottery.
Description of drawings
Fig. 1 is that zeolite of the present invention is the preparation flow figure of the nano silver powder of carrier;
Fig. 2 is to be the process chart that the nano silver powder of carrier prepares anti-bacteria ceramic with zeolite;
Fig. 3 is that zeolite of the present invention is the X-ray diffractogram of the nano silver powder of carrier.
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one: a kind of preparation method of nano-silver antimicrobial powder, and it may further comprise the steps:
(1) 12.0g AgNO3 is dissolved in the 200ml deionized water, adds 76.0g clinoptilolite (granularity is 25 μ m) and soaked 10 hours, obtain suspension;
(2) 3.0g lauryl sodium sulfate and 12.0g polyvinylpyrrolidone fully are dissolved in the 500ml deionized water, join the solution that obtains and the suspension of step (1) in the reactor jointly, add deionized water to 6L, drip 0.25% hydrazine hydrate solution under the stirring with measuring pump, silver ion in the reducing solution, reach 7.0～7.1 until the pH value, stop to add hydrazine hydrate, continue to stir 10 minutes;
(3) reactant liquor that step (2) is obtained left standstill 7 days, fully sedimentation, and the decantation supernatant liquor is used deionized water washing sediment 2 times;
(4) with the drying precipitate after step (3) washing, ball milling to 25 μ m obtains the nano silver powder that zeolite is a carrier, and the granularity of Nano Silver is 2nm, and silver content is 10%;
(5) get 10g glaze (rain clouds board WG3001) and 0.05g nano silver powder, add the 20ml deionized water, mix grinding 20 minutes makes the glaze slurry;
(6) step (5) is made the glaze slurry, impose on ready-made ceramic body surface, 40 ℃ of dryings 3 hours make glaze uniformly attached to the ceramic body surface;
(7) with the ceramic body of step (6) at 1200 ℃, 14 hours following sintering of firing period make anti-bacteria ceramic;
(8) adopt dull and stereotyped viable bacteria counting method that pottery is made antibacterial test.
Embodiment two: a kind of preparation method of nano-silver antimicrobial powder, and it may further comprise the steps:
(1) 12.0g AgNO3 is dissolved in the 1L deionized water, adds 76.0g modenite (granularity is 70 μ m) and soaked 20 hours, obtain suspension;
(2) 4.0g lauryl sodium sulfate and 10.0g polyvinylpyrrolidone fully are dissolved in the 500ml deionized water, join the solution that makes and the suspension of step (1) in the reactor jointly, add deionized water to 6L, drip 0.1% hydrazine hydrate solution under the stirring with measuring pump, reach 7.0～7.1 until the pH value, stop to add hydrazine hydrate, continue to stir the silver ion in the reducing solution 15 minutes;
(3) reactant liquor with step (2) left standstill 10 days, fully sedimentation, and the decantation supernatant liquor is used deionized water washing sediment 3 times;
(4) drying precipitate after the washing that step (3) is obtained, ball milling to 70 μ m obtains the nano silver powder that zeolite is a carrier, and the granularity of Nano Silver is 10nm, and silver content is 20%;
(5) preparation contains the solution 200ml of Nano Silver 500ppm, and sonic oscillation is uniformly dispersed powder in water.
(6) take by weighing 10g glaze (rain clouds board WG3001), be dissolved into the 20ml deionized water, impose on behind the mix grinding 10min and make the ceramic body surface in advance, 40 ℃ of dry 2h make glaze uniformly attached to the ceramic body surface;
(7) the described Nano silver solution of step (6) is sprayed on billet surface after the glazing, natural seasoning 4～6h sprays Nano silver solution again, and natural seasoning circulates 3 times;
(8) with the base substrate of step (7) at 1200 ℃, 14 hours following sintering of firing period make anti-bacteria ceramic.
(9) adopt dull and stereotyped viable bacteria counting method that pottery is made antibacterial test.
Embodiment three: a kind of preparation method of nano-silver antimicrobial powder, and it may further comprise the steps:
(1) 12.0g AgNO3 is dissolved in the 1L deionized water, adds 38.0g clinoptilolite (granularity is 25 μ m) and 38.0g modenite (granularity is 70 μ m) mixture, soaked 14 hours, obtain suspension;
(2) 1.0g sodium citrate and 12.0g polyvinylpyrrolidone fully are dissolved in the 500ml deionized water, join the solution that makes and the suspension of step (1) in the reactor jointly, add deionized water to 6L, drip 0.25% hydrazine hydrate solution under the stirring with measuring pump, reach 7.0～7.1 until the pH value, stop to add hydrazine hydrate, continue to stir the silver ion in the reducing solution 15 minutes;
(3) reactant liquor with step (2) left standstill 6 days, fully sedimentation, and the decantation supernatant liquor is used deionized water washing sediment 3 times;
(4) drying precipitate after the washing that step (3) is obtained, ball milling to 70 μ m obtains the nano silver powder that zeolite is a carrier, and the granularity of Nano Silver is 10nm, and silver content is 20%;
(5) preparation contains the solution 200ml of Nano Silver 500ppm, and sonic oscillation is uniformly dispersed powder in water.
(6) take by weighing 15g glaze (rain clouds board WG3001), be dissolved into the 20ml deionized water, impose on behind the mix grinding 10min and make the ceramic body surface in advance, 40 ℃ of dry 2h make glaze uniformly attached to the ceramic body surface;
(7) the described Nano silver solution of step (6) is sprayed on billet surface after the glazing, natural seasoning 6h sprays Nano silver solution again, and natural seasoning circulates 3 times;
(8) with the base substrate of step (7) at 1200 ℃, 15 hours following sintering of firing period make anti-bacteria ceramic.
(9) adopt dull and stereotyped viable bacteria counting method that pottery is made antibacterial test.
Embodiment four: a kind of preparation method of nano-silver antimicrobial powder, and it may further comprise the steps:
(1) 9.0g AgNO3 is dissolved in the 1L deionized water, adds 22.0g clinoptilolite (granularity is 25 μ m) and 38.0g modenite (granularity is 70 μ m) mixture, soaked 16 hours, obtain suspension;
(2) 3.0g sodium polyphosphate and 13.0g polyvinylpyrrolidone fully are dissolved in the 500ml deionized water, join the solution that makes and the suspension of step (1) in the reactor jointly, add deionized water to 8L, drip 1% hydrazine hydrate solution under the stirring with measuring pump, reach 7.0～7.1 until the pH value, stop to add hydrazine hydrate, continue to stir the silver ion in the reducing solution 20 minutes;
(3) reactant liquor with step (2) left standstill 8 days, fully sedimentation, and the decantation supernatant liquor is used deionized water washing sediment 4 times;
(4) drying precipitate after the washing that step (3) is obtained, ball milling to 50 μ m obtains the nano silver powder that zeolite is a carrier, and the granularity of Nano Silver is 35nm, and silver content is 20%;
(5) preparation contains the solution 100ml of Nano Silver 500ppm, and sonic oscillation is uniformly dispersed powder in water.
(6) take by weighing 20g glaze (rain clouds board WG3001), be dissolved into the 40ml deionized water, impose on behind the mix grinding 10min and make the ceramic body surface in advance, 40 ℃ of dry 2h make glaze uniformly attached to the ceramic body surface;
(7) the described Nano silver solution of step (6) is sprayed on billet surface after the glazing, natural seasoning 5h sprays Nano silver solution again, and natural seasoning circulates 4 times;
(8) with the base substrate of step (7) at 1200 ℃, 14 hours following sintering of firing period make anti-bacteria ceramic.
(9) adopt dull and stereotyped viable bacteria counting method that pottery is made antibacterial test.
As can be seen from Figure 3, silver content is 10%, and the particle mean size of silver-colored particle is 20nm, and remaining diffraction maximum is a zeolite.
Claims (4)
1, a kind of nano-silver antimicrobial powder is characterized in that it is is the powder that carrier constitutes with the zeolite by Nano Silver, and the granularity of described powder is 25～70 μ m, and described content of nanometer silver is 1.0～20%, and the granularity of described Nano Silver is 1～50nm.
2, a kind of preparation method of nano-silver antimicrobial powder is characterized in that it may further comprise the steps:
(1) the zeolite powder is immersed in 1～20% the liquor argenti nitratis ophthalmicus 10～20 hours, silver ion fully is adsorbed in the hole of zeolite;
(2) be in the mixed liquor adding reactor of 0.01～5.0% surperficial adjuvant water solution and step (1) with concentration, add deionized water, mixed liquor and deionized water weight ratio are 1: 1～20, dripping concentration with measuring pump in stirring is 0.001～1.0% hydrazine hydrate solution, liquid pH value to be mixed reaches 7.0～7.1, stopping to add hydrazine hydrate, and continue to stir 10～30 minutes, is Nano Silver simple substance with silver ion reduction;
(3) the reacted liquid of step (2) is taken out, left standstill 4～10 days, fully sedimentation, decantation is used deionized water washing sediment 2～5 times, decantation liquid circulation washing of precipitate;
(4) sediment that step (3) is obtained is at 80～90 ℃ of dry moisture of removing, and ball milling to 25～70 μ m obtains the nano silver powder that zeolite is a carrier, and wherein the granularity of Nano Silver is 1～50nm, and content of nanometer silver is 1.0～20%.
3, the preparation method of a kind of nano-silver antimicrobial powder as claimed in claim 2 is characterized in that described zeolite is clinoptilolite, modenite and their mixture.
4, the preparation method of a kind of nano-silver antimicrobial powder as claimed in claim 2 is characterized in that described surperficial auxiliary agent is a dodecyl sodium sulfate, polyvinylpyrrolidone, lauryl sodium sulfate, sodium polyphosphate, one or more of sodium citrate.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007040742A1 (en) * | 2007-08-28 | 2009-03-05 | Ahrenshof Vermögensverwaltungs-GmbH | Air purifier, useful for neutralizing bad smells, preferably for air purification in refrigerators, and for controlling bad smells e.g. in textiles and vacuum cleaners, comprises a silver zeolite with a nanoparticulate metallic silver |
| CN100551242C (en) * | 2006-09-11 | 2009-10-21 | 厦门大学 | Silver supported ammonium modified nano zeolite antibacterial agent and preparation method thereof |
| WO2012048638A1 (en) * | 2010-10-14 | 2012-04-19 | Ariston Thermo (China) Co., Ltd | Resistance for water heating with enhanced antibacterial effect |
| CN103289244A (en) * | 2013-06-21 | 2013-09-11 | 苏州市景荣科技有限公司 | Antibacterial deodorization HPVC foaming sole material |
| CN105638731A (en) * | 2016-01-30 | 2016-06-08 | 湘潭大学 | Preparation method of antibacterial sepiolite powder |
| CN105817642A (en) * | 2016-04-19 | 2016-08-03 | 南京农业大学 | Au/Ag core shell nanomaterial with efficient antibacterial property and preparation method of Au/Ag core shell nanomaterial |
| CN107629515A (en) * | 2017-11-05 | 2018-01-26 | 包红珠 | The anti-bacteria ceramic coating and its manufacture craft of a kind of annular blade formula air diffuser |
| CN115366512A (en) * | 2022-08-08 | 2022-11-22 | 浙江亚厦装饰股份有限公司 | Preparation method of high-hardness antibacterial wood plastic |
-
2005
- 2005-04-29 CN CN 200510049756 patent/CN1685830A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100551242C (en) * | 2006-09-11 | 2009-10-21 | 厦门大学 | Silver supported ammonium modified nano zeolite antibacterial agent and preparation method thereof |
| DE102007040742A1 (en) * | 2007-08-28 | 2009-03-05 | Ahrenshof Vermögensverwaltungs-GmbH | Air purifier, useful for neutralizing bad smells, preferably for air purification in refrigerators, and for controlling bad smells e.g. in textiles and vacuum cleaners, comprises a silver zeolite with a nanoparticulate metallic silver |
| WO2012048638A1 (en) * | 2010-10-14 | 2012-04-19 | Ariston Thermo (China) Co., Ltd | Resistance for water heating with enhanced antibacterial effect |
| CN102457998A (en) * | 2010-10-14 | 2012-05-16 | 阿里斯顿热能产品(中国)有限公司 | Resistor with enhanced antibacterial effect for heating water |
| CN103289244A (en) * | 2013-06-21 | 2013-09-11 | 苏州市景荣科技有限公司 | Antibacterial deodorization HPVC foaming sole material |
| CN105638731A (en) * | 2016-01-30 | 2016-06-08 | 湘潭大学 | Preparation method of antibacterial sepiolite powder |
| CN105638731B (en) * | 2016-01-30 | 2016-10-12 | 湘潭大学 | A kind of preparation method of meerschaum antibacterial powder |
| CN105817642A (en) * | 2016-04-19 | 2016-08-03 | 南京农业大学 | Au/Ag core shell nanomaterial with efficient antibacterial property and preparation method of Au/Ag core shell nanomaterial |
| CN105817642B (en) * | 2016-04-19 | 2018-04-13 | 南京农业大学 | A kind of Au/Ag core-shell nano materials with Efficient antibacterial performance and preparation method thereof |
| CN107629515A (en) * | 2017-11-05 | 2018-01-26 | 包红珠 | The anti-bacteria ceramic coating and its manufacture craft of a kind of annular blade formula air diffuser |
| CN115366512A (en) * | 2022-08-08 | 2022-11-22 | 浙江亚厦装饰股份有限公司 | Preparation method of high-hardness antibacterial wood plastic |
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