CN104497647B - 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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- CN104497647B CN104497647B CN201410722695.4A CN201410722695A CN104497647B CN 104497647 B CN104497647 B CN 104497647B CN 201410722695 A CN201410722695 A CN 201410722695A CN 104497647 B CN104497647 B CN 104497647B
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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, more particularly to for for the automatically cleaning anti-corrosion colloidal sol preparation side of metal base
Method.
Background technology
Inorganic ceramic paint is a kind of new organo-mineral complexing coating, is received based on the organic-inorganic of sol-gel technique
Rice composite coating (inorganic ceramic film) makes coating not only have the pliability of organic coating and inorganic painting concurrently by the introducing of organic group
The corrosion resistance characteristic of layer, and easy construction, by (100～250 DEG C) solidifications of low temperature can obtain with high rigidity, it is corrosion-resistant,
It is wear-resisting, heat-resisting, do not fire, low stain, the coating of ceramic quality, become a kind of environmental protection of metal coating corrosion-resistant field, cleaning and replace
Dai Pin, can be widely applied to alternative environment in the air corrosion-resistant field of the metal or alloy such as aluminium, iron seriously polluted, harmful
Chromium oxide coating pretreatment coating, have broad application prospects.The sheet metal of another aspect applying coating is in outdoor
During environment use, coating surface easily accumulates the dirts such as dust, organic emission and affects the outward appearance of coating.Automatically cleaning work(
The performance that material surface energy is maintained in the clean condition automatically can be referred to.The coating of self-cleaning function must have following two functions：
1) there is coating surface Superhydrophilic (less contact angle) to make dirt be easy to be pulled away under the washing away of rainwater or running water；
2) there is photocatalysis performance under the conditions of natural lighting, greasy dirt can be automatically removed.At present, the contact angle size of material surface is weighing apparatus
The leading indicator of amount coating self-cleaning performance.Anatase titanium dioxide is a kind of good photocatalytic semiconductor material, is had
Excellent self-cleaning performance.For the problems referred to above, anatase-type nanometer titanium dioxide of the present invention has good photocatalysis performance,
The present invention introduces nano TiO 2 powder on the basis of early stage, makes coating while anti-corrosion, with more preferable self-cleaning property
Can, reduce the maintenance cost of coating.
The content of the invention
The technical problem to be solved in the present invention is to overcome deficiency of the prior art, there is provided a kind of for metal base
Automatically cleaning anti-corrosion colloidal sol preparation method.
The invention provides a kind of automatically cleaning anti-corrosion colloidal sol preparation method for metal base, comprises the steps：
(1) under the stirring condition of 300r/min, by one or two the mixing in methyl silicate, tetraethyl orthosilicate
Thing is added into the saturation alcoholic solvent of the ammonia of 1～5 mass times, is subsequently adding water, and make water and the mol ratio of element silicon be 6～
10∶1；After reacting 8h at 60 DEG C, rotated removed by evaporation adds 30% mass of alcoholic solvent, obtains the particle of high solids content
Type nano silicon dioxide sol；
(2) under the stir speed (S.S.) of 800r/min, Al (OH) is added in corpuscular type nano silicon dioxide sol3Colloidal sol,
The mol ratio for keeping Si: Al is 5～1: 1；After being aged 24 hours at 50 DEG C, Al (OH) is obtained3Colloidal sol in-situ modified cladding is answered
Close silicon dioxide gel；
(3) under the mixing speed of 500r/min, nanometer titanium dioxide titanium valve is added in aforementioned composite silicon dioxide colloidal sol
Body, adds bead, makes dioxide composite Ludox: nano-titanium dioxide powder: the mass ratio of bead is 10: 1: 5；Stir
After mixing 8h, colloidal sol obtains titania additive dioxide composite Ludox by the strainer filtering of 200 mesh；
(4) under the stirring condition of 300r/min, add for adjusting in titania additive dioxide composite Ludox
The catalyst of section pH value, the pH value for making colloidal sol is maintained at 1～5；After stirring 0.5h, organosiloxane is added dropwise over into above-mentioned colloidal sol
In, it is 2: 1～1: 2 to control organosiloxane with the mass ratio of dioxide composite Ludox, after reacting 6h at 30 DEG C, is obtained suitable
For the automatically cleaning anti-corrosion colloidal sol of metal base.
In the present invention, in the saturation alcoholic solvent of step (1) ammonia alcoholic solvent be methyl alcohol, ethanol, isopropanol one of which or
Wherein several combinations.
In the present invention, step (3) nano-titanium dioxide powder for anatase-type nanometer titanium dioxide powder, particle mean size
In 80nm～100nm.
In the present invention, step (3) bead be abrasive media, a diameter of 6mm.
In the present invention, catalyst is HCl, HNO in step (4)3, formic acid one of which or wherein several combinations.
In the present invention, organosiloxane is MTMS, methacryloxypropyl front three in step (4)
TMOS, phenyl triethoxysilane one of which or wherein several combinations.
Compared with existing technology of preparing, the invention has the advantages that：
The present invention is using Al (OH)3On the basis of colloidal sol original position coating modification coated silica colloidal sol, sharp titanium is introduced
Ore deposit nano TiO 2 powder, makes it be dispersed in Al (OH) by grinding distribution3Colloidal sol original position coating modification cladding dioxy
In SiClx colloidal sol, then Jing is combined the metal base anti-corrosion colloidal sol prepared with self-cleaning performance with organosilicon.Make the sharp titanium of nanometer
Ore deposit titanium dioxide is dispersed in the coating for preparing, and on the base material of coating antiseptic, can effectively improve the self-cleaning property of coating
Energy.
Specific embodiment
Below by way of example, the present invention is further described.
It is used for the automatically cleaning anti-corrosion colloidal sol preparation method of metal base in the present invention, including following several steps：
(1) under the stirring condition of 300r/min, by one or two the mixing in methyl silicate, tetraethyl orthosilicate
Thing is added into the saturation alcoholic solvent of the ammonia of 1～5 mass times, is subsequently adding water, and make water and the mol ratio of element silicon be 6～
10∶1；After reacting 8h at 60 DEG C, rotated removed by evaporation adds 30% mass of alcoholic solvent, obtains the particle of high solids content
Type nano silicon dioxide sol；
(2) under the stir speed (S.S.) of 800r/min, Al (OH) is added in corpuscular type nano silicon dioxide sol3Colloidal sol,
The mol ratio for keeping Si: Al is 5～1: 1；After being aged 24 hours at 50 DEG C, Al (OH) is obtained3Colloidal sol in-situ modified cladding is answered
Close silicon dioxide gel；
(3) under the mixing speed of 500r/min, nanometer titanium dioxide titanium valve is added in aforementioned composite silicon dioxide colloidal sol
Body, adds bead, makes dioxide composite Ludox: nano-titanium dioxide powder: the mass ratio of bead is 10: 1: 5；Stir
After mixing 8h, colloidal sol obtains titania additive dioxide composite Ludox by the strainer filtering of 200 mesh；
(4) under the stirring condition of 300r/min, add for adjusting in titania additive dioxide composite Ludox
The catalyst of section pH value, the pH value for making colloidal sol is maintained at 1～5；After stirring 0.5h, organosiloxane is added dropwise over into above-mentioned colloidal sol
In, it is 2: 1～1: 2 to control organosiloxane with the mass ratio of dioxide composite Ludox, after reacting 6h at 30 DEG C, is obtained suitable
For the automatically cleaning anti-corrosion colloidal sol of metal base.
It is used for the using method of the automatically cleaning anti-corrosion colloidal sol of metal base in the present invention：
Sample colloidal sol is coated by spraying method on metal aluminum sheet surface, after 100 DEG C of surface drying 10min, in 250 DEG C of heat treatments
The automatically cleaning corrosion-inhibiting coating of 3～5 microns of thickness is formed after 20min.
Test data in each embodiment see the table below：As can be seen from the table, the sample colloidal sol of nano titanium oxide is added
Coating contact angle prepared by (sequence number 1 to 9) within 10 degree, with preferable self-cleaning performance, and non-plus nano titanium dioxide
Coating contact angle larger (67 degree) prepared by the example colloidal sol of titanium.Other performances of coating are such as：Pencil hardness, corrosion resistance
There is no significant change in energy (neutral salt spray test) etc..It can be seen that, being added in of nano titanium oxide do not affect coating other performances
On the premise of largely improve the self-cleaning performance of coating.
Coating adopts following standard testing various aspects of performance：
1) coating pencil hardness adopts the ASTM3363 standard testings of U.S. material association；
2) coating contact angle Germany KRUSS contact angle instruments test；
3) coating neutral salt spray test is tested using paint film property testing standard GB-T1771-1991.
Finally, in addition it is also necessary to it is noted that listed above is only that the present invention is embodied as example.Obviously, the present invention not
It is limited to above example, there can also be many deformations.One of ordinary skill in the art can be straight from present disclosure
The all deformations derived or associate are connect, protection scope of the present invention is considered as.
Claims (5)
1. the automatically cleaning anti-corrosion colloidal sol preparation method of metal base is used for, it is characterised in that comprised the steps：
(1) under the stirring condition of 300r/min, one or two the mixture in methyl silicate, tetraethyl orthosilicate is added
Enter into the saturation alcoholic solvent of the ammonia of 1～5 mass times, be subsequently adding water, and make water be 6～10 with the mol ratio of element silicon:
1；After reacting 8h at 60 DEG C, rotated removed by evaporation adds 30% mass of alcoholic solvent, obtains the corpuscular type of high solids content
Nano silicon dioxide sol；
(2) under the stir speed (S.S.) of 800r/min, Al (OH) is added in corpuscular type nano silicon dioxide sol3Colloidal sol, keeps Si
: the mol ratio of Al is 5～1: 1；After being aged 24 hours at 50 DEG C, Al (OH) is obtained3The compound dioxy of the in-situ modified cladding of colloidal sol
SiClx colloidal sol；
(3) under the mixing speed of 500r/min, nano-titanium dioxide powder is added in aforementioned composite silicon dioxide colloidal sol, then
The bead as abrasive media is added, dioxide composite Ludox: nano-titanium dioxide powder is made: the mass ratio of bead is
10∶1∶5；After stirring 8h, colloidal sol obtains titania additive dioxide composite Ludox by the strainer filtering of 200 mesh；
(4) under the stirring condition of 300r/min, add for adjusting pH in titania additive dioxide composite Ludox
The catalyst of value, the pH value for making colloidal sol is maintained at 1～5；After stirring 0.5h, organosiloxane is added dropwise in above-mentioned colloidal sol,
It is 2: 1～1: 2 that organosiloxane is controlled with the mass ratio of dioxide composite Ludox, after reacting 6h at 30 DEG C, is obtained and is suitable for
In the automatically cleaning anti-corrosion colloidal sol of metal base；
Alcoholic solvent is methyl alcohol, ethanol, isopropanol one of which or wherein several groups in the saturation alcoholic solvent of step (1) ammonia
Close.
2. method according to claim 1, it is characterised in that step (3) nano-titanium dioxide powder is received for Detitanium-ore-type
The powder of rice titanium dioxide, particle mean size is in 80nm～100nm.
3. method according to claim 1, it is characterised in that a diameter of 6mm of step (3) bead.
4. method according to claim 1, it is characterised in that catalyst is HCl, HNO in step (4)3, formic acid wherein one
Plant or wherein several combinations.
5. method according to claim 1, it is characterised in that organosiloxane is methyl trimethoxy epoxide silicon in step (4)
Alkane, methacryloxypropyl trimethoxy silane, phenyl triethoxysilane one of which or wherein several combinations.
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| CN105199446B (en) * | 2015-10-20 | 2017-07-28 | 河北新仟瑞新型建材有限公司 | Nano titanium oxide functional coating, its preparation method, the preparation method of base material prepared therefrom and the base material |
| 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 |
| CN115216163B (en) * | 2022-07-15 | 2023-05-16 | 李开天 | Inorganic electric heating coating material, preparation method and application thereof, and conductive fiber |
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| CN102134411B (en) * | 2011-01-18 | 2012-07-04 | 浙江大学 | Method for preparing organic-inorganic composite sol used for preventing corrosion on surface of metal aluminum plate |
| CN102784598A (en) * | 2012-06-25 | 2012-11-21 | 浙江赛凡新材料有限公司 | Method for preparing self-repairing nanocomposite sol used for long-lasting anticorrosion of metal plate |
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