CN103509395B - The preparation method of slow-release composite antibacterial coating - Google Patents
The preparation method of slow-release composite antibacterial coating Download PDFInfo
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- CN103509395B CN103509395B CN201310420043.0A CN201310420043A CN103509395B CN 103509395 B CN103509395 B CN 103509395B CN 201310420043 A CN201310420043 A CN 201310420043A CN 103509395 B CN103509395 B CN 103509395B
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Abstract
The present invention relates to the preparation of antimicrobial coating, aim to provide a kind of preparation method of slow-release composite antibacterial coating.The method comprises: adopt water-based organic emulsion to prepare organic coating at cleaned substrates surface coatings; Before organic coating surface drying, by the alcohol dispersion liquid even spread of antimicrobial powder to organic coating layer surface, after solidification, obtain slow-release composite antibacterial coating.The present invention is using organic emulsion as one-tenth film base material, unloaded silver-colored microballoon in the mesoporous silicon oxide with sustained-release antibacterial characteristic is partially submerged in organic membrane, on the one hand by film forming crosslinked between silica sphere hydroxyl and organic emulsion, make hollow silica carry silver-colored microballoon and firmly load to coatingsurface; Carrying silver-colored microballoon by hollow silica is on the other hand partially submerged in organic membrane, effectively prevent the blocking of emulsion to the mesoporous passage of microballoon, guarantees the performance of sustained-release antibacterial characteristic.Carry the long-term slow releasing silver ions of mesoporous passage of silver-colored microsphere surface by hollow silica, play the effect of durable antibiotic.
Description
Technical field
The present invention relates to the preparation of antimicrobial coating, particularly a kind of preparation method of slow-release composite antibacterial coating.
Background technology
Antimicrobial coating is a kind of important application form of anti-biotic material, and can give matrix antibacterial by loading to different matrix surface, relative to the way of being mixed by antiseptic-germicide in matrix, antimicrobial coating has stronger economy, and the scope of application is more wide.At present, antimicrobial coating obtains widespread use in household electrical appliance, sanitary ware, plastics film, construction wall decoration etc.But, the easily a large amount of stripping and running off of the more silver system antimicrobial coating silver ions of current application, the problems such as ubiquity stability is bad, Durability of antimicrobial effect is low.Therefore, the preparation of slowly released type antibiotic coating becomes the important technology approach that solution silver is the low life problems of antimicrobial coating.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes deficiency of the prior art, provides a kind of preparation method of slow-release composite antibacterial coating.
For technical solution problem, the invention provides a kind of preparation method of slow-release composite antibacterial coating, comprise the steps:
(1) adopt solid content be 5% ~ 50% water-based organic emulsion prepare organic coating at cleaned substrates surface coatings;
(2) before organic coating surface drying, by mass concentration be the alcohol dispersion liquid even spread of the antimicrobial powder of 8 ~ 40g/L to organic coating layer surface, obtain slow-release composite antibacterial coating after solidification;
Described antimicrobial powder is that hollow silica carries silver-colored microballoon, prepares as follows:
A, be that to add mass percentage concentration be in the vitriol oil of 98% to 3 micron polystyrene microspheres by diameter, polystyrene microsphere in concentrated sulfuric acid mass concentration is 20g/L; Stir 6h at 50 DEG C, centrifugal, deionized water wash 4 times, is then re-dispersed in dehydrated alcohol, obtains the sulfonated polystyrene dispersion liquid that mass concentration is 5g/L repeatedly;
B, in above-mentioned sulfonated polystyrene dispersion liquid, the mass concentration adding quality same with this dispersion liquid is the tin protochloride aqueous solution of 5g/L, stirred at ambient temperature 30min, centrifugal, washing after, join in the silver ammino solution of the 0.05mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 6: 3: 1; Stirred at ambient temperature 1h, adds Virahol in the resulting mixture, and the volume ratio of Virahol and mixture is 2: 3, obtains carrying silver-colored polystyrene complex microsphere dispersion liquid;
C, in above-mentioned year silver-colored polystyrene complex microsphere dispersion liquid, add tetraethoxy and mass percentage concentration is the ammoniacal liquor of 28%, Virahol in mixed solution: ammoniacal liquor: the volume ratio of tetraethoxy is 60: 2: 1; Stirred at ambient temperature 24h, products therefrom through centrifugal, washing after, at 550 DEG C, calcine 2h, namely obtain hollow silica carry silver-colored microballoon.
In the present invention, the water-based organic emulsion in described step (1) is any one in benzene emulsion, organosilicon crylic acid latex, pure-acrylic emulsion, acrylate and vinyl acetate emulsion.
In the present invention, the preparation method of described organic coating and slow-release composite antibacterial coating is spin-coating method or spraying method.
In the present invention, described cleaned substrates be through water cleaning and dry surface without the pottery of obvious stain, concrete, paint film any one.
Compared with existing technology of preparing, the invention has the beneficial effects as follows:
The present invention is using organic emulsion as one-tenth film base material, unloaded silver-colored microballoon in the mesoporous silicon oxide with sustained-release antibacterial characteristic is partially submerged in organic membrane, on the one hand by film forming crosslinked between silica sphere hydroxyl and organic emulsion, make hollow silica carry silver-colored microballoon and firmly load to coatingsurface; Carrying silver-colored microballoon by hollow silica is on the other hand partially submerged in organic membrane, effectively prevent the blocking of emulsion to the mesoporous passage of microballoon, guarantees the performance of sustained-release antibacterial characteristic.This antimicrobial coating carries the long-term slow releasing silver ions of mesoporous passage of silver-colored microsphere surface by hollow silica, plays the effect of durable antibiotic.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph (apparent form photo) of unloaded silver-colored microballoon in mesoporous silicon oxide;
Fig. 2 is the stereoscan photograph (for microballoon spherical shell internal pictures) of unloaded silver-colored microballoon in mesoporous silicon oxide, and lighter colored particles is the nano-Ag particles of load in spherical shell inside;
Fig. 3 is the stereoscan photograph (amplifying 100 times, overall pattern) of slow-release composite antibacterial coating;
Fig. 4 is the stereoscan photograph of slow-release composite antibacterial coating: (amplifying 5000 times, local pattern).
Embodiment
Below by way of example, the present invention is further described.
The preparation method of slow-release composite antibacterial coating provided by the invention, comprises the steps:
(1) adopt solid content be 5% ~ 50% water-based organic emulsion prepare organic coating at cleaned substrates surface coatings;
(2) before organic coating surface drying, by mass concentration be the alcohol dispersion liquid even spread of the antimicrobial powder of 8 ~ 40g/L to organic coating layer surface, obtain slow-release composite antibacterial coating after solidification;
Described antimicrobial powder is that hollow silica carries silver-colored microballoon, prepares as follows:
A, polystyrene microsphere is added mass percentage concentration is in the vitriol oil of 98%, and polystyrene microsphere in concentrated sulfuric acid mass concentration is 20g/L; Stir 6h at 50 DEG C, centrifugal, deionized water wash 4 times, is then re-dispersed in dehydrated alcohol, obtains the sulfonated polystyrene dispersion liquid that mass concentration is 5g/L repeatedly;
B, in above-mentioned sulfonated polystyrene dispersion liquid, the mass concentration adding quality same with this dispersion liquid is the tin protochloride aqueous solution of 5g/L, stirred at ambient temperature 30min, centrifugal, washing after, join in the silver ammino solution of the 0.05mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 6: 3: 1; Stirred at ambient temperature 1h, adds Virahol in the resulting mixture, and the volume ratio of Virahol and mixture is 2: 3, obtains carrying silver-colored polystyrene complex microsphere dispersion liquid;
C, in above-mentioned year silver-colored polystyrene complex microsphere dispersion liquid, add tetraethoxy and mass percentage concentration is the ammoniacal liquor of 28%, Virahol in mixed solution: ammoniacal liquor: the volume ratio of tetraethoxy is 60: 2: 1; Stirred at ambient temperature 24h, products therefrom through centrifugal, washing after, at 550 DEG C, calcine 2h, namely obtain hollow silica carry silver-colored microballoon.
In each embodiment, except the difference to some extent of testing data in following table, all the other testing datas are all identical.
Finally, it is also to be noted that enumerate above be only specific embodiments of the invention son.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (2)
1. a preparation method for slow-release composite antibacterial coating, is characterized in that, comprises the steps:
(1) adopt solid content be 5% ~ 50% water-based organic emulsion prepare organic coating at cleaned substrates surface coatings;
(2) before organic coating surface drying, by mass concentration be the alcohol dispersion liquid even spread of the antimicrobial powder of 8 ~ 40g/L to organic coating layer surface, obtain slow-release composite antibacterial coating after solidification;
The preparation method of described organic coating and slow-release composite antibacterial coating is spin-coating method or spraying method;
Described antimicrobial powder is that hollow silica carries silver-colored microballoon, prepares as follows:
A, be that to add mass percentage concentration be in the vitriol oil of 98% to 3 micron polystyrene microspheres by diameter, polystyrene microsphere in concentrated sulfuric acid mass concentration is 20g/L; Stir 6h at 50 DEG C, centrifugal, deionized water wash 4 times, is then re-dispersed in dehydrated alcohol, obtains the sulfonated polystyrene dispersion liquid that mass concentration is 5g/L repeatedly;
B, in above-mentioned sulfonated polystyrene dispersion liquid, the mass concentration adding quality same with this dispersion liquid is the tin protochloride aqueous solution of 5g/L, stirred at ambient temperature 30min, centrifugal, washing after, join in the silver ammino solution of the 0.05mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 6: 3: 1; Stirred at ambient temperature 1h, adds Virahol in the resulting mixture, and the volume ratio of Virahol and mixture is 2: 3, obtains carrying silver-colored polystyrene complex microsphere dispersion liquid;
C, in above-mentioned year silver-colored polystyrene complex microsphere dispersion liquid, add tetraethoxy and mass percentage concentration is the ammoniacal liquor of 28%, Virahol in mixed solution: ammoniacal liquor: the volume ratio of tetraethoxy is 60: 2: 1; Stirred at ambient temperature 24h, products therefrom through centrifugal, washing after, at 550 DEG C, calcine 2h, namely obtain hollow silica carry silver-colored microballoon;
Water-based organic emulsion in described step (1) is any one in benzene emulsion, organosilicon crylic acid latex, pure-acrylic emulsion, acrylate and vinyl acetate emulsion.
2. method according to claim 1, is characterized in that, described cleaned substrates be through water cleaning and dry surface without the pottery of obvious stain, concrete, paint film any one.
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JPH10179403A (en) * | 1996-12-20 | 1998-07-07 | Nikkei Prod:Kk | Cooking vessel and production of its parts |
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CN1470574A (en) * | 2003-06-16 | 2004-01-28 | 上海维来新材料科技有限公司 | Antibacterial negative ion coating |
CN101613556A (en) * | 2009-07-16 | 2009-12-30 | 浙江大学 | The preparation method of titanium silver-based antimildew and antibacterial emulsion paint interior wall paint |
CN102079929A (en) * | 2009-11-30 | 2011-06-01 | 钱高鹏 | Silver-zinc titanium dioxide paint |
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