CN103509396B - The preparation method of hydrophobic antimicrobial coating - Google Patents
The preparation method of hydrophobic antimicrobial coating Download PDFInfo
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- CN103509396B CN103509396B CN201310420130.6A CN201310420130A CN103509396B CN 103509396 B CN103509396 B CN 103509396B CN 201310420130 A CN201310420130 A CN 201310420130A CN 103509396 B CN103509396 B CN 103509396B
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Abstract
The present invention relates to the preparation of antimicrobial coating, aim to provide a kind of preparation method of hydrophobic antimicrobial coating.The method comprises: adopt modified fluorin resin at cleaned substrates surface coatings, prepare hydrophobic coating; Before this hydrophobic coating surface drying, hydrophobically modified hollow silica is carried silver-colored microballoon homogeneous dispersion and be applied to its surface, after solidification, obtain hydrophobic antimicrobial coating.The present invention is based on bionics techniques principle, utilize unloaded silver-colored microballoon in mesoporous silicon oxide to be partially submerged in fluorine-containing organic membrane, on the one hand by the coating surface structure that structure micro-nano is coarse, strengthen coating hydrophobic performance further; Utilize on the other hand the structure of unloaded silver-colored microballoon uniqueness in this, carried the long-term slow releasing silver ions of mesoporous passage of silver-colored microsphere surface by hollow silica, play the effect of durable antibiotic, thus realize the integrated of coating sustained-released antibacterial and super hydrophobic functional.
Description
Technical field
The present invention relates to the preparation of antimicrobial coating, particularly a kind of preparation method of hydrophobic antimicrobial coating.
Background technology
Be in the body surface often easy grow mold in wet environment for a long time, body surface done hydrophobization process and can effectively avoid moisture, dirt in body surface enrichment, reduce mould growing at body surface.At present, applying more is low surface energy fluorine material, and generally speaking monomer Oil repellent is higher, and hydrophobic performance is better, but price also can significantly improve.By research lotus leaf automatically cleaning phenomenon, Univ Bonn Germany researchist finds that lotus leaf top layer grows nano level wax crystalline substance, make lotus leaf surface hydrophobic, the micron mastoid process etc. of lotus leaf surface forms micro-roughened surface and strengthens its hydrophobicity further simultaneously, make dirt not easily at its surface enrichment, give its self-cleaning function.In addition, the hydrophobic coating function of current application is general comparatively single, although some researchs add antibacterial components in hydrophobic coating, realizes the integrated of hydrophobic function and antibacterial, but be in the easy a large amount of stripping of surperficial antibacterial active constituents and run off, causing coating Durability of antimicrobial effect to reduce.Therefore, how by surface structure design structure one hydrophobic, sustained-release antibacterial coating system efficiently, become and be rich in a challenging development.
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 hydrophobic antimicrobial coating.
For technical solution problem, the invention provides a kind of preparation method of hydrophobic antimicrobial coating, comprise the steps:
(1) adopt solid content be the modified fluorin resin of 5% ~ 40% at cleaned substrates surface coatings, prepare hydrophobic coating;
(2) before this hydrophobic coating surface drying, be that the hydrophobically modified hollow silica of 8 ~ 40g/L carries silver-colored microballoon homogeneous dispersion and is applied to its surface by mass concentration, after solidification, obtain hydrophobic antimicrobial coating;
Described hydrophobically modified hollow silica carries silver-colored microballoon dispersion liquid and prepares according to the following procedure:
A, polystyrene microsphere is added mass percentage concentration is in the vitriol oil of 98%, and polystyrene 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 0.1mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 10: 5: 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: 3: 5; 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;
D, this hollow silica carried silver-colored microballoon and to be distributed to identical type in step (1) and solid content is in the modified fluorin resin of 2%, after ageing 8h, obtain hydrophobically modified hollow silica and carry silver-colored microballoon dispersion liquid.
In the present invention, modified fluorin resin described in step (1) is the one in acrylic acid modified fluoro-resin or organic-silicon-modified fluoro-resin.
In the present invention, described in step (1), the preparation method of hydrophobic coating and hydrophobic antimicrobial 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 based on bionics techniques principle, utilize unloaded silver-colored microballoon in mesoporous silicon oxide to be partially submerged in fluorine-containing organic membrane, on the one hand by the coating surface structure that structure micro-nano is coarse, strengthen coating hydrophobic performance further; Utilize on the other hand the structure of unloaded silver-colored microballoon uniqueness in this, carried the long-term slow releasing silver ions of mesoporous passage of silver-colored microsphere surface by hollow silica, play the effect of durable antibiotic, thus realize the integrated of coating sustained-released antibacterial and super hydrophobic functional.
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 (be microballoon spherical shell internal pictures, lighter colored particles is the nano-Ag particles of load in spherical shell inside) of unloaded silver-colored microballoon in mesoporous silicon oxide;
Fig. 3 is the stereoscan photograph of hydrophobic antimicrobial coatingsurface;
Fig. 4 is contact angle contrast photo (water droplet at the contact angle of modified fluorin resin hydrophobic coating surface be 112.0 °) of different coating to water;
Fig. 5 is for different coating is to the contact angle contrast photo (contact angle of water droplet hydrophobic antimicrobial coatingsurface prepared by the identical modified fluorin resin of employing is 150.4 °) of water.
Embodiment
Below by way of example, the present invention is further described.
The preparation method of hydrophobic antimicrobial coating provided by the invention, comprises the steps:
(1) adopt solid content be the modified fluorin resin of 5% ~ 40% at cleaned substrates surface coatings, prepare hydrophobic coating;
(2) before this hydrophobic coating surface drying, be that the hydrophobically modified hollow silica of 8 ~ 40g/L carries silver-colored microballoon homogeneous dispersion and is applied to its surface by mass concentration, after solidification, obtain hydrophobic antimicrobial coating;
Described hydrophobically modified hollow silica carries silver-colored microballoon dispersion liquid and prepares according to the following procedure:
A, polystyrene microsphere is added mass percentage concentration is in the vitriol oil of 98%, and polystyrene 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 0.1mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 10: 5: 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: 3: 5; 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;
D, this hollow silica carried silver-colored microballoon and to be distributed to identical type in step (1) and solid content is in the modified fluorin resin of 2%, after ageing 8h, obtain hydrophobically modified hollow silica and carry silver-colored microballoon dispersion liquid.
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 (3)
1. a preparation method for hydrophobic antimicrobial coating, is characterized in that, comprises the steps:
(1) adopt solid content be the modified fluorin resin of 5% ~ 40% at cleaned substrates surface coatings, prepare hydrophobic coating;
(2) before this hydrophobic coating surface drying, be that the hydrophobically modified hollow silica of 8 ~ 40g/L carries silver-colored microballoon homogeneous dispersion and is applied to its surface by mass concentration, after solidification, obtain hydrophobic antimicrobial coating;
Described in step (1), the preparation method of hydrophobic coating and hydrophobic antimicrobial coating is spin-coating method or spraying method;
Described hydrophobically modified hollow silica carries silver-colored microballoon dispersion liquid and prepares according to the following procedure:
A, polystyrene microsphere is added mass percentage concentration is in the vitriol oil of 98%, and polystyrene 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 0.1mol/L being dissolved with Seignette salt, Seignette salt: silver-colored ammonium ion: tin protochloride mol ratio is 10: 5: 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: 3: 5; 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;
D, this hollow silica carried silver-colored microballoon and to be distributed to identical type in step (1) and solid content is in the modified fluorin resin of 2%, after ageing 8h, obtain hydrophobically modified hollow silica and carry silver-colored microballoon dispersion liquid.
2. method according to claim 1, is characterized in that, modified fluorin resin described in step (1) is acrylic acid modified fluoro-resin or organic-silicon-modified fluoro-resin.
3. 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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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103861657B (en) * | 2014-02-24 | 2015-07-08 | 浙江大学 | Preparation method of nano-silver loaded porous silicon dioxide |
| CN103894122B (en) * | 2014-04-14 | 2015-09-16 | 浙江大学 | The preparation method of soluble type drug loading microcapsules |
| CN104310795B (en) * | 2014-09-29 | 2016-11-02 | 北京师范大学 | A kind of preparation method of substrate surface antimicrobial coating |
| CN105921130A (en) * | 2016-05-25 | 2016-09-07 | 厦门建霖工业有限公司 | Slow-release antibacterial adsorption material for drinking water treatment and preparation method of material |
| CN106436284B (en) * | 2016-09-27 | 2018-10-12 | 天津傲卓菲科技有限公司 | A kind of simple self-spraying tank of rapid build super-double-hydrophobic surface |
| TW202037683A (en) * | 2019-04-02 | 2020-10-16 | 新福光塗裝工程股份有限公司 | Antibacterial coating and coating method which includes antibacterial particles that are all located near a surface of the paint with excellent abrasion resistance and adhesion performance |
| CN110592959B (en) * | 2019-08-27 | 2020-12-08 | 玉环市几偶孵化器有限公司 | Self-cleaning textile material for automotive interior and preparation method thereof |
| CN115121193B (en) * | 2022-07-25 | 2023-08-08 | 西安理工大学 | Preparation method of positively charged AgO@MgO hollow composite microspheres |
| CN116463024A (en) * | 2023-05-29 | 2023-07-21 | 杭州老板电器股份有限公司 | Hydrophobic oleophobic antibacterial film layer and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242511A (en) * | 1990-02-23 | 1993-09-07 | Asahi Kasei Kogyo Kabushiki Kaisha | Copper alloy compositions |
| CN101058687A (en) * | 2007-02-18 | 2007-10-24 | 张弛一智 | Enhancement self-cleaning antibiotic low surface energy coat capable of being monitored |
| CN102669178A (en) * | 2012-05-08 | 2012-09-19 | 浙江大学 | Method for preparing sustained-release silver-based antibacterial agent |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3316861B2 (en) * | 1991-11-06 | 2002-08-19 | 松下電器産業株式会社 | Antibacterial treatment material and its manufacturing method |
| JPH10179403A (en) * | 1996-12-20 | 1998-07-07 | Nikkei Prod:Kk | Cooking vessel and production of its parts |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242511A (en) * | 1990-02-23 | 1993-09-07 | Asahi Kasei Kogyo Kabushiki Kaisha | Copper alloy compositions |
| CN101058687A (en) * | 2007-02-18 | 2007-10-24 | 张弛一智 | Enhancement self-cleaning antibiotic low surface energy coat capable of being monitored |
| CN102669178A (en) * | 2012-05-08 | 2012-09-19 | 浙江大学 | Method for preparing sustained-release silver-based antibacterial agent |
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