CN106256205A - A kind of preparation method carrying silver titanium oxide antimicrobial powder - Google Patents
A kind of preparation method carrying silver titanium oxide antimicrobial powder Download PDFInfo
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- CN106256205A CN106256205A CN201610852541.6A CN201610852541A CN106256205A CN 106256205 A CN106256205 A CN 106256205A CN 201610852541 A CN201610852541 A CN 201610852541A CN 106256205 A CN106256205 A CN 106256205A
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Abstract
The invention discloses a kind of preparation method carrying silver titanium oxide antimicrobial powder, concrete technology step is as follows: weigh 10g titanium oxide, joins in the deionized water of 200mL and stirs, and regulates pH to 3.0～3.2 with dust technology；Add the silver nitrate solution of 30mL 10g/L, under room temperature, stir 15～30min；In reaction solution, add 2.5g citric acid again or 0.5g molecular weight is the polyvinylpyrrolidone of 10000, continue stirring 15～30min；Improve reaction temperature, add the sodium hydroxide solution 10ml that mass concentration is 10%, react 1～2h；Being centrifuged by reaction solution, abandon supernatant, the solid of collection is placed in baking oven drying；Solid abrasive after drying processes, and at the Muffle kiln roasting 0.5～1h of 300～550 DEG C, i.e. obtains carrying silver titanium oxide antimicrobial powder.The present invention has height simple for process, repeatable, advantage with low cost, it is to avoid titanium oxide needs special equipment production line to cause price high or the problem of environmental pollution in synthesis.
Description
Technical field
The present invention relates to a kind of preparation method, particularly relate to a kind of preparation method carrying silver titanium oxide antimicrobial powder, belong to
Compou nd synthesis technical field.
Background technology
Silver-series antibacterial agent and titanium dioxide photocatalyst antibacterial are the most most popular inorganic series antibacterial agent at present.Silver
Series antibacterial agent has good anti-bacterial effect, the feature that toxic hazard is little, but it there is also simultaneously that cost is higher, illumination and high temperature variable
The shortcoming of color；By contrast, the antimicrobial efficiency of titanium dioxide photocatalyst antibacterial is relatively low, but can bear illumination and hot conditions, right
The effect of light and heat is stable, has safe and reliable, nontoxic, non-stimulated advantage, but there is also bactericidal property master simultaneously
Will be by ultraviolet excitation, defect that photocatalysis efficiency is low.Therefore, the excellent of silver-series antibacterial agent and titanium dioxide photocatalyst antibacterial is utilized
Gesture is complementary, and developing novel load silver titanium oxide antibacterial has become international study hotspot.But the current existing silver that carries aoxidizes
The preparation method of titanium antibacterial yet suffers from the defect that technical process is loaded down with trivial details, repetition reliability is low, relatively costly.
Summary of the invention
In order to solve the weak point existing for above-mentioned technology, the invention provides and a kind of carry silver titanium oxide antimicrobial powder
Preparation method.
In order to solve above technical problem, the technical solution used in the present invention is: a kind of carry silver titanium oxide antimicrobial powder
Preparation method, weighs the titanium oxide that 10g size is 20nm and puts in beaker, adds the deionized water stirring of 200mL all
Even；Configuration volume ratio is concentrated nitric acid: deionized water is the dilute nitric acid solution of 1:2, is slowly added dropwise dilute nitric acid solution to titanium oxide
In aqueous solution, the pH to 3.0～3.2 of regulation titanium oxide aqueous solution；
Take the silver nitrate solution of 30mL 10g/L, add to the titanium oxide solution mixing up pH；Reaction beaker is placed in electricity
On dynamic agitator, stirring 15～30min at room temperature, controlling mixing speed is 200r/min～400r/min；After having stirred
Adding 2.5g citric acid or 0.5g molecular weight in reaction solution is the polyvinylpyrrolidone of 10000, continue stirring 15～
30min；
Improve reaction temperature to 20～60 DEG C, dropping or add mass concentration in the way of toppling over and be in reaction system
The sodium hydroxide solution 10ml of 10%, stops stirring after reaction 1～2h；
Pouring reaction solution after being placed in centrifuge tube by freshness protection package into, trim, with the centrifugation 5min of 5000r/min；
Remove supernatant after centrifugal end, propose freshness protection package and solid, solid is placed in the baking oven of 80～120 DEG C and dries；
Take out the solid after drying to be ground processing, be ground into the powder of 400～500 mesh；Again by above-mentioned powder
At the Muffle kiln roasting 0.5～1h of 300～550 DEG C, i.e. obtain carrying silver titanium oxide antimicrobial powder.
The present invention uses low temperature can synthesize load silver titanium oxide antimicrobial powder, it is to avoid titanium oxide is in synthesis
Need special equipment production line to cause price high or the problem of environmental pollution, have height simple for process, repeatable,
Advantage with low cost.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further detailed explanation.
The process step of the invention is as follows:
Weigh the titanium oxide that 10g size is 20nm to put in beaker, add the deionized water stirring of 200mL all
Even；Configuration volume ratio is concentrated nitric acid: deionized water is the dilute nitric acid solution of 1:2, is slowly added dropwise dilute nitric acid solution to titanium oxide
In aqueous solution, the pH to 3.0～3.2 of regulation titanium oxide aqueous solution；
Take the silver nitrate solution of 30mL 10g/L, add to the titanium oxide solution mixing up pH；Reaction beaker is placed in electricity
On dynamic agitator, stirring 15～30min at room temperature, controlling mixing speed is 200r/min～400r/min；After having stirred
Adding 2.5g citric acid or 0.5g molecular weight in reaction solution is the polyvinylpyrrolidone of 10000, continue stirring 15～
30min；
Raising reaction temperature is to 20～60 DEG C, and in reaction system, the speed with 0.5～2/s drips or with the side toppled over
Formula adds the sodium hydroxide solution 10ml that mass concentration is 10%, stops stirring after reaction 1～2h；
Pouring reaction solution after being placed in centrifuge tube by freshness protection package into, trim, with the centrifugation 5min of 5000r/min；
Remove supernatant after centrifugal end, propose freshness protection package and solid, solid is placed in the baking oven of 80～120 DEG C and dries；
Take out the solid after drying to be ground processing, be ground into the powder of 400～500 mesh；Again by above-mentioned powder
At the Muffle kiln roasting 0.5～1h of 300～550 DEG C, i.e. obtain carrying silver titanium oxide antimicrobial powder.
Below by specific embodiment, the technique effect of the present invention is verified further.
Embodiment one:
According to following processing step preparation load silver titanium oxide antimicrobial powder:
Weigh the titanium oxide that 10g size is 20nm to put in beaker, add the deionized water stirring of 200mL all
Even；Configuration volume ratio is concentrated nitric acid: deionized water is the dilute nitric acid solution of 1:2, is slowly added dropwise dilute nitric acid solution to titanium oxide
In aqueous solution, the pH to 3.0 of regulation titanium oxide aqueous solution；
Take the silver nitrate solution of 30mL 10g/L, add to the titanium oxide solution mixing up pH；Reaction beaker is placed in electricity
On dynamic agitator, stirring 15min at room temperature, control mixing speed is 400r/min；Stir in backward reaction solution and added
Enter 2.5g citric acid, continue stirring 15min；
Raising reaction temperature is to 60 DEG C, and dripping mass concentration with the speed of 2/s in reaction system is the hydrogen-oxygen of 10%
Change sodium solution 10ml, after reaction 1h, stop stirring；
Pouring reaction solution after being placed in centrifuge tube by freshness protection package into, trim, with the centrifugation 5min of 5000r/min；
Remove supernatant after centrifugal end, propose freshness protection package and solid, solid is placed in the baking oven of 80 DEG C and dries；
Take out the solid after drying to be ground processing, be ground into the powder of 400 mesh；Again by above-mentioned powder 300
DEG C Muffle kiln roasting 1h, i.e. obtain carrying silver titanium oxide antimicrobial powder.
According to national standard " nano inorganic material anti-microbial property detection method ", embodiment one is carried out escherichia coli
ATCC8739, escherichia coli ATCC25922, staphylococcus aureus ATCC6538, the antibacterial reality of Candida albicans ATCC10231
Testing, the anti-bacterial result shows: the bacteriostasis rate of a pair above-mentioned four kinds of strain of the embodiment of the present invention is all higher than 99.8%, has and significantly presses down
Bacterium effect.
Weighing appropriate powder body and be positioned under ultraviolet lamp tube the whiteness change testing powder body, test result shows: powder body is in nothing
Whiteness during illumination is 76.5, and the whiteness when light irradiates 24h, 48h, 72h, 96h is respectively 72.5,69.5,66.5,65.8,
Therefore may determine that, the embodiment of the present invention one whiteness change under illumination condition is less, has certain discoloration-resisting.
Embodiment two:
According to following processing step preparation load silver titanium oxide antimicrobial powder:
Weigh the titanium oxide that 10g size is 20nm to put in beaker, add the deionized water stirring of 200mL all
Even；Configuration volume ratio is concentrated nitric acid: deionized water is the dilute nitric acid solution of 1:2, is slowly added dropwise dilute nitric acid solution to titanium oxide
In aqueous solution, the pH to 3.2 of regulation titanium oxide aqueous solution；
Take the silver nitrate solution of 30mL 10g/L, add to the titanium oxide solution mixing up pH；Reaction beaker is placed in electricity
On dynamic agitator, stirring 30min at room temperature, control mixing speed is 200r/min；Stir in backward reaction solution and added
Enter the polyvinylpyrrolidone that 0.5g molecular weight is 10000, continue stirring 30min；
Regulation reaction temperature, to 20 DEG C, adds the hydroxide that mass concentration is 10% in reaction system in the way of toppling over
Sodium solution 10ml, stops stirring after reaction 2h；
Pouring reaction solution after being placed in centrifuge tube by freshness protection package into, trim, with the centrifugation 5min of 5000r/min；
Remove supernatant after centrifugal end, propose freshness protection package and solid, solid is placed in the baking oven of 120 DEG C and dries；
Take out the solid after drying to be ground processing, be ground into the powder of 500 mesh；Again by above-mentioned powder 550
DEG C Muffle kiln roasting 0.5h, i.e. obtain carrying silver titanium oxide antimicrobial powder.
According to national standard " nano inorganic material anti-microbial property detection method ", embodiment two is carried out escherichia coli
ATCC8739, escherichia coli ATCC25922, staphylococcus aureus ATCC6538, the antibacterial reality of Candida albicans ATCC10231
Testing, the anti-bacterial result shows: the embodiment of the present invention two is all higher than 99.6% to the bacteriostasis rate of above-mentioned four kinds of strains, has prominent pressing down
Bacterium effect.
Weighing appropriate powder body and be positioned under ultraviolet lamp tube the whiteness change testing powder body, test result shows: powder body is in nothing
Whiteness during illumination is 77.3, and the whiteness when light irradiates 24h, 48h, 72h, 96h is respectively 74.8,71.6,70.9,68.5,
Therefore may determine that, the embodiment of the present invention two whiteness change under illumination condition is less, has overcome silver-series antibacterial agent illumination easy
The shortcoming of variable color, has certain discoloration-resisting.
The composite bactericidal powder body of present invention synthesis can preferably comprehensive inorganic silver-series antibacterial agent and photocatalytic titanium oxide touch
The respective advantage of matchmaker's antibacterial, and effectively overcome the shortcoming of the two, has that fungistatic effect is prominent, fastness is stablized in illumination, antibacterial
Without the advantage of ultraviolet excitation and simple for process, repeatable higher, with low cost, it is suitable for further grinding
Send out application.
Above-mentioned embodiment is not limitation of the present invention, and the present invention is also not limited to the example above, and this technology is led
Change that the technical staff in territory is made in the range of technical scheme, retrofit, add or replace, also belong to this
Bright protection domain.
Claims (1)
1. the preparation method carrying silver titanium oxide antimicrobial powder, it is characterised in that: the processing step of described method is as follows:
Weighing the titanium oxide that 10g size is 20nm to put in beaker, the deionized water adding 200mL stirs；Join
Putting volume ratio is concentrated nitric acid: deionized water is the dilute nitric acid solution of 1:2, is slowly added dropwise dilute nitric acid solution to titanium oxide aqueous solution
In, the pH to 3.0～3.2 of regulation titanium oxide aqueous solution；
Take the silver nitrate solution of 30mL 10g/L, add to the titanium oxide solution mixing up pH；Reaction beaker is placed in electric mixing
Mixing on device, at room temperature stirring 15～30min, controlling mixing speed is 200r/min～400r/min；Stirred backward instead
Answering addition 2.5g citric acid or 0.5g molecular weight in solution is the polyvinylpyrrolidone of 10000, continues stirring 15～30min；
Raising reaction temperature is to 20～60 DEG C, and dripping or add mass concentration in the way of toppling in reaction system is 10%
Sodium hydroxide solution 10ml, stops stirring after reaction 1～2h；
Pouring reaction solution after being placed in centrifuge tube by freshness protection package into, trim, with the centrifugation 5min of 5000r/min；Centrifugal
Remove supernatant after end, propose freshness protection package and solid, solid is placed in the baking oven of 80～120 DEG C and dries；
Take out the solid after drying to be ground processing, be ground into the powder of 400～500 mesh；Again by above-mentioned powder 300
～the Muffle kiln roasting 0.5～1h of 550 DEG C, i.e. obtain carrying silver titanium oxide antimicrobial powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539625A (en) * | 2022-02-28 | 2022-05-27 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano-gold antibacterial powder, antibacterial plastic master batch or material, preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539625A (en) * | 2022-02-28 | 2022-05-27 | 广东粤港澳大湾区国家纳米科技创新研究院 | Nano-gold antibacterial powder, antibacterial plastic master batch or material, preparation method and application |
| CN114539625B (en) * | 2022-02-28 | 2023-12-05 | 广东粤港澳大湾区国家纳米科技创新研究院 | Antibacterial nano gold powder, antibacterial plastic master batch or material, preparation method and application |
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