CN104448960A - Preparation method of nano titanium dioxide/zinc oxide super-hydrophobic compound coating - Google Patents
Preparation method of nano titanium dioxide/zinc oxide super-hydrophobic compound coating Download PDFInfo
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- CN104448960A CN104448960A CN201410766399.4A CN201410766399A CN104448960A CN 104448960 A CN104448960 A CN 104448960A CN 201410766399 A CN201410766399 A CN 201410766399A CN 104448960 A CN104448960 A CN 104448960A
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Abstract
The invention provides a preparation method of a nano titanium dioxide/zinc oxide super-hydrophobic compound coating. The preparation method comprises the following steps: (1) uniformly mixing ZnO, TiO2, ethanol, sodium dodecyl sulfate and deionized water, and magnetically stirring at normal temperature for 30 minutes to prepare TiO2/ZnO compound particles; then, putting stearic acid into absolute ethyl alcohol for ultrasonic full dissolution and finally mixing the dissolved stearic acid with the TiO2/ZnO composite particles, and magnetically stirring for 6 hours under a condition that the temperature is 45-55 DEG C and the pH is 3-5 to prepare a modified compound sol; and (2) soaking a steel substrate which is cleaned on the surface in the modified compound sol for dipping, lifting and coating to obtain a compound thin film, and finally, after drying the dipped and lifted steel substrate at room temperature, roasting till the coating is fully cured to prepare the nano titanium dioxide/zinc oxide super-hydrophobic compound coating. The static contact angle of the compound coating and water is 165.3 degrees and the rolling angle is 4 degrees.
Description
Technical field
The present invention relates to the preparation method of nano titanium oxide/zinc oxide super-hydrophobic compound coating.
Background technology
Body surface has automatically cleaning and anti-corrosion function is nanosecond science and technology age study problem the most widely, it is the target that people pursue that process differing materials surface makes it have ultra-hydrophobicity, as: people the accessory such as shoes, clothes worn do not get wet, the antifogging self-cleaning of kitchen tile and bathroom glass, the hydrophobic preservative property of building external paint and water pipe inwall.
Super-hydrophobic composite material surface, because have excellent hydrophobic ability and good antiseptic property, has a wide range of applications in industry and life.In recent years, find that a kind of preparation technology is simple, with low cost, method environmental protection, stable performance and the antifouling anticorrosion super-hydrophobic coat had both be current developing direction.
Summary of the invention
In order to solve problems of the prior art, the invention provides the preparation method of nano titanium oxide/zinc oxide super-hydrophobic compound coating.
The invention provides the preparation method of a kind of nano titanium oxide/zinc oxide super-hydrophobic compound coating, step is as follows: (1) is by 10 mass parts ZnO, 20 mass parts TiO
2, 8 parts by volume of ethanol, 1 mass parts sodium laurylsulfonate and a certain amount of deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles; Then 2.7 mass parts stearic acid are placed on ultrasonic abundant dissolving in dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 45-55 DEG C, the condition lower magnetic force of pH=3-5 stirs 6h, the complex sol of obtained modification;
(2) steel matrix clean for surface treatment is immersed in the complex sol of modification, then carry out Best-Effort request plated film, obtain certain thickness laminated film; Finally, after steel matrix complete for Best-Effort request at room temperature dry 20 ~ 30min, 200 DEG C of bakings, until coating is fully solidified, obtain nano-TiO
2/ ZnO super hydrophobic composite coating.
Preferably, in step (1) be by dissolve after stearic acid and TiO
2/ ZnO composite particles mixes, 50 DEG C, the condition lower magnetic force of pH=4 stirs 6h, the complex sol of obtained modification.
The present invention passes through mechanical stirring and surface modification, by TiO
2nano-TiO is mixed to form with ZnO
2/ ZnO compound coating, electrostatic force, Van der Waals force make them be cross-linked with each other together, the coated TiO of ZnO
2form the three-dimensional network-like structure stablizing porous.Stearic acid is made up of wetting ability carboxyl and nonpolar hydrophobic alkane long-chain, comprises the hydrophobicity alkane of hydrophilic carboxyl and nonpolar long-chain in stearic acid, when stearic acid solution adds TiO
2time in/ZnO complex sol, compound coating surface is a large amount of
in OH group and stearic acid
cOOH group generation dehydrating condensation, forms the film of super-hydrophobicity.Mainly due to two reasons, nano-TiO on the one hand
2the coarse structure of/ZnO laminated film surface mesh porous, provides architecture basics for having super-hydrophobicity; On the other hand, stearic modified to compound coating, effectively reduce the free energy of coatingsurface.Combine through both, form the dual rough surface structure of micro-/ nano of low surface energy, air deposits and is adsorbed on the surface of coarse structure, can effectively prevent water droplet from penetrating in hole.
The stearic acid of the present invention's low surface energy is to nano-TiO
2/ ZnO composite particles modifying surface, best modified condition is: stearic acid dosage is 9%, experimental temperature 50 DEG C, pH=4.The contact angle of coatingsurface increases along with the increase of stearic acid content, and when stearic acid content is greater than 9%, contact angle starts to reduce, and hydrophobicity also decreases.FTIR and TG analyzes and shows, TiO
2have hydrophobic with the grafting of ZnO particle surface
cH
3group, when temperature coating quality loss between 318 DEG C ~ 440 DEG C is 10.1%, mainly stearic acid decomposition causes.When coating thermal treatment temp is 200 DEG C, coating hydrophobic effect is best.Sem analysis shows, compound coating is the super hydrophobic surface of the dual coarse structure of micro-/ nano at steel matrix surface construction, is 165.3 ° with the static contact angle of water, roll angle 4 °.
Embodiment
Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is ordinary method.
embodiment 1
The preparation method of nano titanium oxide of the present invention/zinc oxide super-hydrophobic compound coating is as follows:
(1) by mechanical stirring by 10g ZnO, 20g TiO
2, 8mL ethanol, 1g sodium laurylsulfonate and a certain amount of deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles.Then 2.7g stearic acid is placed on ultrasonic abundant dissolving in 10mL dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 50 DEG C, the condition lower magnetic force of pH=4 stirs 6h, the complex sol of obtained modification.
(2) steel matrix prepared with sand papering, until after surperficial no marking, is dipped in ethanol and acetone and is removed spot, and clean with deionized water rinsing, dry for standby.
(3) steel matrix clean for surface treatment is immersed in modified complex sol, then carry out Best-Effort request plated film.Because the superficial attractive forces of particle and chemical binding force effect, will form the uniform laminated film of one deck in steel matrix in complex sol, obtain certain thickness laminated film for several times through repetitive operation.Finally, after steel matrix complete for Best-Effort request at room temperature dry 20 ~ 30min, 200 DEG C of bakings, until coating is fully solidified, obtain nano-TiO
2/ ZnO super hydrophobic composite coating.
The performance test of compound coating prepared by the present invention: (1) when stearic addition be ZnO and TiO
2gross weight 9% time, water reaches 165.3 ° at the contact angle of coatingsurface, presents excellent super-hydrophobicity.When stearic addition is greater than 9%, because stearic acid is to TiO
2/ ZnO too much the modification in surface makes it form double-deck absorption, and the wetting ability carboxyl now in stearic acid can be exposed on compound coating surface, and contact angle on surface of coating and hydrophobicity are declined thereupon.
(2) nano-TiO will obtained
2/ ZnO super hydrophobic composite coating, puts into water, acetone, ethanol and toluene solution respectively and soaks 4 days, then takes out sample and dries in atmosphere, and measure the contact angle of specimen surface.Result shows, and after soaking in water, acetone, ethanol and toluene solution, water droplet has small reduction at the contact angle of coatingsurface, and all maintain more than 155 °, this shows nano-TiO
2under/ZnO compound coating remains on different solvents for a long time, still there is good solvent resistance and excellent ultra-hydrophobicity.
(3) compound coating is placed on
within the scope of 20 DEG C ~ 300 DEG C, cooling and heating 20min, then dry in atmosphere and measure surperficial contact angle.Result shows, and the change of compound coating contact angle is less, still keeps good super-hydrophobicity, and this illustrates that high and low temperature environment is to nano-TiO
2the impact of/ZnO compound coating hydrophobicity is less.
(4) by nano-TiO
2/ ZnO coatingsurface sprinkles one deck chalk dust, to investigate the self-cleaning property of coating, places with the pitch angle of 10 °.With syringe gradually to the coating instillation drop sprinkled with chalk dust, because the hydrophobicity of super hydrophobic surface excellence and minimum roll angle, water droplet tumbles fast along coatingsurface and takes away the chalk dust on surface, makes coatingsurface be restored to clean state.
embodiment 2
The preparation method of nano titanium oxide of the present invention/zinc oxide super-hydrophobic compound coating is as follows:
(1) by mechanical stirring by 10g ZnO, 20g TiO
2, 8mL ethanol, 1g sodium laurylsulfonate and a certain amount of deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles.Then 2.7g stearic acid is placed on ultrasonic abundant dissolving in 10mL dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 45 DEG C, the condition lower magnetic force of pH=5 stirs 6h, the complex sol of obtained modification.
(2) steel matrix prepared with sand papering, until after surperficial no marking, is dipped in ethanol and acetone and is removed spot, and clean with deionized water rinsing, dry for standby.
(3) steel matrix clean for surface treatment is immersed in modified complex sol, then carry out Best-Effort request plated film.Because the superficial attractive forces of particle and chemical binding force effect, will form the uniform laminated film of one deck in steel matrix in complex sol, obtain certain thickness laminated film for several times through repetitive operation.Finally, after steel matrix complete for Best-Effort request at room temperature dry 20 ~ 30min, 190 DEG C of bakings, until coating is fully solidified, obtain nano-TiO
2/ ZnO super hydrophobic composite coating.
embodiment 3
The preparation method of nano titanium oxide of the present invention/zinc oxide super-hydrophobic compound coating is as follows:
(1) by mechanical stirring by 10g ZnO, 20g TiO
2, 8mL ethanol, 1g sodium laurylsulfonate and a certain amount of deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles.Then 2.7g stearic acid is placed on ultrasonic abundant dissolving in 10mL dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 55 DEG C, the condition lower magnetic force of pH=3 stirs 6h, the complex sol of obtained modification.
(2) steel matrix prepared with sand papering, until after surperficial no marking, is dipped in ethanol and acetone and is removed spot, and clean with deionized water rinsing, dry for standby.
(3) steel matrix clean for surface treatment is immersed in modified complex sol, then carry out Best-Effort request plated film.Because the superficial attractive forces of particle and chemical binding force effect, will form the uniform laminated film of one deck in steel matrix in complex sol, obtain certain thickness laminated film for several times through repetitive operation.Finally, after steel matrix complete for Best-Effort request at room temperature dry 20 ~ 30min, 210 DEG C of bakings, until coating is fully solidified, obtain nano-TiO
2/ ZnO super hydrophobic composite coating.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the preparation method of nano titanium oxide/zinc oxide super-hydrophobic compound coating, is characterized in that: step is as follows: (1) is by 10 mass parts ZnO, 20 mass parts TiO
2, 8 parts by volume of ethanol, 1 mass parts sodium laurylsulfonate and a certain amount of deionized water Homogeneous phase mixing, after normal temperature magnetic agitation 30min, obtained TiO
2/ ZnO composite particles; Then 2.7 mass parts stearic acid are placed on ultrasonic abundant dissolving in dehydrated alcohol, finally by the stearic acid after dissolving and TiO
2/ ZnO composite particles mixes, 45-55 DEG C, the condition lower magnetic force of pH=3-5 stirs 6h, the complex sol of obtained modification;
(2) steel matrix clean for surface treatment is immersed in the complex sol of modification, then carry out Best-Effort request plated film, obtain certain thickness laminated film; Finally, after steel matrix complete for Best-Effort request at room temperature dry 20 ~ 30min, 190 DEG C-210 DEG C bakings, until coating is fully solidified, obtain nano-TiO
2/ ZnO super hydrophobic composite coating.
2. the preparation method of nano titanium oxide according to claim 1/zinc oxide super-hydrophobic compound coating, is characterized in that: in step (1) be by dissolve after stearic acid and TiO
2/ ZnO composite particles mixes, 50 DEG C, the condition lower magnetic force of pH=4 stirs 6h, the complex sol of obtained modification.
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| CN105295707A (en) * | 2015-10-28 | 2016-02-03 | 天长市润达金属防锈助剂有限公司 | Corrosion-preventive and rust-resistant sol for aluminum alloy and preparation method thereof |
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| CN113370603B (en) * | 2021-04-25 | 2022-05-31 | 青岛农业大学 | Super-hydrophobic biological composite membrane and preparation method and application thereof |
| CN113215862A (en) * | 2021-04-26 | 2021-08-06 | 杭州西红柿环保科技有限公司 | Fully-degradable fluorine-free paper pulp molded dinner plate and preparation method thereof |
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