CN104497647A - Preparation method of self-cleaning anticorrosion sol for metal substrate - Google Patents
Preparation method of self-cleaning anticorrosion sol for metal substrate Download PDFInfo
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- CN104497647A CN104497647A CN201410722695.4A CN201410722695A CN104497647A CN 104497647 A CN104497647 A CN 104497647A CN 201410722695 A CN201410722695 A CN 201410722695A CN 104497647 A CN104497647 A CN 104497647A
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Abstract
The invention relates to the preparation technology of a sol, and aims at providing a preparation method of a self-cleaning anticorrosion sol for a metal substrate. The method comprises the following steps: feeding tetramethyl orthosilicate or tetraethoxysilane into a saturated alcohol solvent of ammonia gas under an agitating condition; then feeding water to react; performing rotary evaporation to remove some alcohol solvent to obtain high-solid-content particular colloidal silica sol; further feeding Al(OH)3 sol; ageing; further feeding nanometer titanium dioxide powder and glass beads; agitating; filtering the sol; further feeding a catalyst for regulating the pH; dropwise adding organo-siloxane to react to obtain the self-cleaning anticorrosion sol. According to the method, anatase titanium dioxide powder is introduced on the basis of Al(OH3) sol in-situ coated and modified coated silica sol and is grinded and uniformly dispersed into the Al(OH3) sol in-situ coated and modified coated silica sol, and therefore, the anatase titanium dioxide powder can be uniformly dispersed in the prepared coating to effectively improve the self-cleaning performance of the coating on the substrate while the corrosion resistance is ensured.
Description
Technical field
The present invention relates to colloidal sol technology of preparing, particularly for the anticorrosion colloidal sol preparation method of automatically cleaning for metal base.
Background technology
Inorganic ceramic paint is a kind of novel organo-mineral complexing coating, based on the organic-inorganic nanocomposite coating (inorganic ceramic film) of sol-gel technique by the introducing of organic group, make coating not only with the snappiness of organic coating and the corrosion resistance characteristic of inorganic coating, and easy construction, can obtain that there is high rigidity by low temperature (100 ~ 250 DEG C) solidification, corrosion-resistant, wear-resisting, heat-resisting, do not fire, low stain, the coating of pottery quality, become a kind of environmental protection of metallic coating corrosion-resistant field, clean substitute, aluminium can be widely used in, in the air corrosion-resistant field of the metal or alloy such as iron, alternative environment is seriously polluted, the pretreatment coating of harmful chromium oxide coating, have broad application prospects.The sheet metal of applying coating is in outdoor environment use procedure on the other hand, and coatingsurface easily accumulates the dirt such as dust, organic emission and affects the outward appearance of coating.Self-cleaning function refers to the performance that material surface energy is maintained in the clean condition automatically.The coating of self-cleaning function must have following two kinds of functions: 1) coatingsurface has Superhydrophilic (less contact angle) and makes dirt be easy to be pulled away under the washing away of rainwater or tap water; 2) under natural lighting condition, there is photocatalysis performance, automatically can remove greasy dirt.At present, the contact angle size of material surface weighs the leading indicator of coating self-cleaning performance.Anatase titanium dioxide is a kind of well photocatalytic semiconductor material, has excellent self-cleaning performance.For the problems referred to above, anatase-type nanometer titanium dioxide of the present invention has good photocatalysis performance, and the present invention is on early stage basis, introduce nano TiO 2 powder, make coating at rot-resistant simultaneously, there is better self-cleaning performance, reduce the maintenance cost of 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 automatically cleaning for metal base anticorrosion colloidal sol preparation method.
The invention provides the anticorrosion colloidal sol preparation method of a kind of automatically cleaning for metal base, comprise the steps:
(1) under the agitation condition of 300r/min, the mixture of one or both in methyl silicate, tetraethoxy is added in the saturated alcohol solvent of 1 ~ 5 quality ammonia doubly, then add water, and make the mol ratio of water and element silicon be 6 ~ 10: 1; React 8h at 60 DEG C after, remove 30% quality of added alcoholic solvent through rotary evaporation, obtain the corpuscular type nano silicon dioxide sol of high solids content;
(2) under the stir speed (S.S.) of 800r/min, in corpuscular type nano silicon dioxide sol, Al (OH) is added
3colloidal sol, the mol ratio keeping Si: Al is 5 ~ 1: 1; 50 DEG C of ageings after 24 hours, obtain Al (OH)
3the in-situ modified coated dioxide composite silicon sol of colloidal sol;
(3) under the stirring velocity of 500r/min, in aforementioned composite silicon dioxide colloidal sol, add nano-titanium dioxide powder, then add granulated glass sphere, make dioxide composite silicon sol: nano-titanium dioxide powder: the mass ratio of granulated glass sphere is 10: 1: 5; After stirring 8h, colloidal sol obtains titania additive dioxide composite silicon sol by 200 object strainer filterings;
(4) under the agitation condition of 300r/min, in titania additive dioxide composite silicon sol, add the catalyzer for adjust ph, make the pH value of colloidal sol remain on 1 ~ 5; After stirring 0.5h, dropwise added by organo-siloxane in above-mentioned colloidal sol, the mass ratio controlling organo-siloxane and dioxide composite silicon sol is 2: 1 ~ 1: 2, react 6h at 30 DEG C after, and the obtained anticorrosion colloidal sol of automatically cleaning being applicable to metal base.
In the present invention, in the saturated alcohol solvent of step (1) ammonia, alcoholic solvent is wherein a kind of or wherein several combination of methyl alcohol, ethanol, Virahol.
In the present invention, step (3) nano-titanium dioxide powder is the powder of anatase-type nanometer titanium dioxide, and mean particle size is at 80nm ~ 100nm.
In the present invention, step (3) granulated glass sphere is grinding medium, and diameter is 6mm.
In the present invention, in step (4), catalyzer is HCl, HNO
3, wherein a kind of or wherein several combination of formic acid.
In the present invention, organo-siloxane is wherein a kind of or wherein several combination of methyltrimethoxy silane, methacryloxypropyl trimethoxy silane, phenyl triethoxysilane in step (4).
Compared with existing technology of preparing, the present invention has following beneficial effect:
The present invention is in employing Al (OH)
3on the basis of colloidal sol original position coating modification coated silica colloidal sol, introduce anatase titania nanopowder, make it be dispersed in Al (OH) by grinding distribution
3in colloidal sol original position coating modification coated silica colloidal sol, then through preparing the anticorrosion colloidal sol of the metal base with self-cleaning performance with organosilicon compound.Make nanometer anatase titania dispersed in the coating of preparation, on the base material of coating antiseptic, effectively can improve the self-cleaning performance of coating.
Embodiment
Below by way of example, the present invention is further described.
For the anticorrosion colloidal sol preparation method of the automatically cleaning of metal base in the present invention, comprise following several step:
(1) under the agitation condition of 300r/min, the mixture of one or both in methyl silicate, tetraethoxy is added in the saturated alcohol solvent of 1 ~ 5 quality ammonia doubly, then add water, and make the mol ratio of water and element silicon be 6 ~ 10: 1; React 8h at 60 DEG C after, remove 30% quality of added alcoholic solvent through rotary evaporation, obtain the corpuscular type nano silicon dioxide sol of high solids content;
(2) under the stir speed (S.S.) of 800r/min, in corpuscular type nano silicon dioxide sol, Al (OH) is added
3colloidal sol, the mol ratio keeping Si: Al is 5 ~ 1: 1; 50 DEG C of ageings after 24 hours, obtain Al (OH)
3the in-situ modified coated dioxide composite silicon sol of colloidal sol;
(3) under the stirring velocity of 500r/min, in aforementioned composite silicon dioxide colloidal sol, add nano-titanium dioxide powder, then add granulated glass sphere, make dioxide composite silicon sol: nano-titanium dioxide powder: the mass ratio of granulated glass sphere is 10: 1: 5; After stirring 8h, colloidal sol obtains titania additive dioxide composite silicon sol by 200 object strainer filterings;
(4) under the agitation condition of 300r/min, in titania additive dioxide composite silicon sol, add the catalyzer for adjust ph, make the pH value of colloidal sol remain on 1 ~ 5; After stirring 0.5h, dropwise added by organo-siloxane in above-mentioned colloidal sol, the mass ratio controlling organo-siloxane and dioxide composite silicon sol is 2: 1 ~ 1: 2, react 6h at 30 DEG C after, and the obtained anticorrosion colloidal sol of automatically cleaning being applicable to metal base.
For the using method of the anticorrosion colloidal sol of the automatically cleaning of metal base in the present invention:
Sample colloidal sol in metal aluminum sheet surface-coated, after 100 DEG C of surface drying 10min, forms the automatically cleaning corrosion protection coating of 3 ~ 5 micron thickness by spraying method after 250 DEG C of thermal treatment 20min.
Testing data in each embodiment sees the following form: as can be seen from the table, coating contact angle prepared by the sample colloidal sol (sequence number 1 to 9) adding nano titanium oxide is all within 10 degree, there is good self-cleaning performance, and coating contact angle prepared by the example colloidal sol of non-plus nano titanium dioxide comparatively large (67 degree).Other performances of coating as: there is not considerable change in pencil hardness, corrosion resistance nature (neutral salt spray test) etc.Visible, nano titanium oxide be added in the prerequisite not affecting other performances of coating under improve the self-cleaning performance of coating largely.
Coating adopts following standard testing various aspects of performance:
1) coating pencil hardness adopts U.S. material association ASTM3363 standard testing;
2) the German KRUSS contact angle instrument of coating contact angle is tested;
3) coating neutral salt spray test adopts paint film property testing standard GB-T1771-1991 test.
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 (6)
1., for the anticorrosion colloidal sol preparation method of automatically cleaning of metal base, it is characterized in that, comprise the steps:
(1) under the agitation condition of 300r/min, the mixture of one or both in methyl silicate, tetraethoxy is added in the saturated alcohol solvent of 1 ~ 5 quality ammonia doubly, then add water, and make the mol ratio of water and element silicon be 6 ~ 10: 1; React 8h at 60 DEG C after, remove 30% quality of added alcoholic solvent through rotary evaporation, obtain the corpuscular type nano silicon dioxide sol of high solids content;
(2) under the stir speed (S.S.) of 800r/min, in corpuscular type nano silicon dioxide sol, Al (OH) is added
3colloidal sol, the mol ratio keeping Si: Al is 5 ~ 1: 1; 50 DEG C of ageings after 24 hours, obtain Al (OH)
3the in-situ modified coated dioxide composite silicon sol of colloidal sol;
(3) under the stirring velocity of 500r/min, in aforementioned composite silicon dioxide colloidal sol, add nano-titanium dioxide powder, then add granulated glass sphere, make dioxide composite silicon sol: nano-titanium dioxide powder: the mass ratio of granulated glass sphere is 10: 1: 5; After stirring 8h, colloidal sol obtains titania additive dioxide composite silicon sol by 200 object strainer filterings;
(4) under the agitation condition of 300r/min, in titania additive dioxide composite silicon sol, add the catalyzer for adjust ph, make the pH value of colloidal sol remain on 1 ~ 5; After stirring 0.5h, dropwise added by organo-siloxane in above-mentioned colloidal sol, the mass ratio controlling organo-siloxane and dioxide composite silicon sol is 2: 1 ~ 1: 2, react 6h at 30 DEG C after, and the obtained anticorrosion colloidal sol of automatically cleaning being applicable to metal base.
2. method according to claim 1, is characterized in that, in the saturated alcohol solvent of step (1) ammonia, alcoholic solvent is wherein a kind of or wherein several combination of methyl alcohol, ethanol, Virahol.
3. method according to claim 1, is characterized in that, step (3) nano-titanium dioxide powder is the powder of anatase-type nanometer titanium dioxide, and mean particle size is at 80nm ~ 100nm.
4. method according to claim 1, is characterized in that, step (3) granulated glass sphere is grinding medium, and diameter is 6mm.
5. method according to claim 1, is characterized in that, in step (4), catalyzer is HCl, HNO
3, wherein a kind of or wherein several combination of formic acid.
6. method according to claim 1, is characterized in that, organo-siloxane is wherein a kind of or wherein several combination of methyltrimethoxy silane, methacryloxypropyl trimethoxy silane, phenyl triethoxysilane in step (4).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105199446A (en) * | 2015-10-20 | 2015-12-30 | 河北新仟瑞新型建材有限公司 | Nano-titanium-dioxide functional coating, preparation method thereof, substrate prepared from nano-titanium-dioxide functional coating and preparation method of substrate |
| CN108003691A (en) * | 2017-11-22 | 2018-05-08 | 浙江加州国际纳米技术研究院台州分院 | Preparation method for ocean engineering anti-halobios adhersion coating |
| CN108117276A (en) * | 2017-12-16 | 2018-06-05 | 天津市职业大学 | A kind of design and preparation method of electro-conductive glass automatically cleaning antireflective coating |
| CN109370420A (en) * | 2018-10-22 | 2019-02-22 | 浙江大学 | A kind of high weather resistant water-thinned preparation method of anticorrosion paint |
| CN111117328A (en) * | 2018-10-30 | 2020-05-08 | 3M创新有限公司 | Preparation method of anti-fouling composition with photocatalytic performance |
| CN115216163A (en) * | 2022-07-15 | 2022-10-21 | 李开天 | Inorganic electric heating coating material, preparation method and application thereof, and conductive fiber |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199446A (en) * | 2015-10-20 | 2015-12-30 | 河北新仟瑞新型建材有限公司 | Nano-titanium-dioxide functional coating, preparation method thereof, substrate prepared from nano-titanium-dioxide functional coating and preparation method of substrate |
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| CN108003691A (en) * | 2017-11-22 | 2018-05-08 | 浙江加州国际纳米技术研究院台州分院 | Preparation method for ocean engineering anti-halobios adhersion coating |
| CN108117276A (en) * | 2017-12-16 | 2018-06-05 | 天津市职业大学 | A kind of design and preparation method of electro-conductive glass automatically cleaning antireflective coating |
| CN109370420A (en) * | 2018-10-22 | 2019-02-22 | 浙江大学 | A kind of high weather resistant water-thinned preparation method of anticorrosion paint |
| WO2020082703A1 (en) * | 2018-10-22 | 2020-04-30 | 浙江大学 | Method for manufacturing water-based anticorrosive coating having high weather resistance |
| CN111117328A (en) * | 2018-10-30 | 2020-05-08 | 3M创新有限公司 | Preparation method of anti-fouling composition with photocatalytic performance |
| CN115216163A (en) * | 2022-07-15 | 2022-10-21 | 李开天 | Inorganic electric heating coating material, preparation method and application thereof, and conductive fiber |
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