CN108485329A - A kind of super-hydrophilic self-cleaning coating sol and its preparation and application - Google Patents
A kind of super-hydrophilic self-cleaning coating sol and its preparation and application Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses a kind of super-hydrophilic self-cleaning coating sols and its preparation method and application being combined using titanium dioxide and inorganic polysilazane.The present invention by nano-titanium dioxide and inorganic polysilazane it is compound prepare can the super-hydrophilic self-cleaning coating sol that bonds by force of self-curing, the Superhydrophilic that prepared coating has photocatalytic activity and stablizes；Preparation process of the present invention is simple, of low cost, environmentally protective, operating condition is easily-controllable, efficiently solves the problems, such as to have at present that coating photocatalytic activity is poor and preparation process is complicated, may advantageously facilitate the application and development of super hydrophilic technology.
Description
Technical field
The present invention relates to a kind of super-hydrophilic self-cleaning coating sols, specifically, being to be related to a kind of use titanium dioxide and nothing
The super-hydrophilic self-cleaning coating sol and its preparation method and application that machine polysilazane is combined.
Background technology
In recent years, the super wetting surface generated by controlling the wetability of the surface of solids receives the concern of industry,
Middle ultra-hydrophilic surface (contact angle of surface water is less than 10 °) is since it is in automatically cleaning, antifog, water-oil separating, fresh water collecting, air-conditioning
Possessing huge potential using value with fields such as heat exchangers becomes research hotspot.In order to obtain ultra-hydrophilic surface, also just need
One layer of coating with super hydrophilicity is coated in material surface.Therefore, coating material of the research and development with super hydrophilicity has
There are significant application value and economic benefit.
Titanium dioxide is most often used and because having powerful oxidability, high chemically stability and nontoxic characteristic
As the substance of photocatalyst.Photocatalyst can be used for handling the harmful chemical of low concentration in air, itself will not disengage harmful
Substance, therefore be splendid environmental purification catalyst.Photocatalytic activity is high, has smelly eliminating, sterilization, antibacterial, antifouling
With remove the functions such as harmful substance.In addition to this, titanium dioxide film materials have preferable Superhydrophilic, can form water droplet
Moisture film is uniformly sprawled on the surface thereof.Titania-based washcoats are prepared at present, generally chemical vapour deposition technique, magnetic control are used to splash
Penetrate method, sol-gal process etc..The usual amorphous state of coating of titanium dioxide prepared by chemical vapour deposition technique and magnetron sputtering method contains
Amount is high, and photocatalytic activity is relatively low, and preparation method is complicated, and equipment requirement is wanted；Coating of titanium dioxide prepared by sol-gel method,
High-temperature baking is needed, to improve caking property and photocatalytic activity.
Invention content
The technical problem to be solved in the present invention is, in the prior art the shortcomings that, provide that a kind of have can self-curing
Cohesive super-hydrophilic self-cleaning coating sol by force；
The further technical problems to be solved of the present invention are, provide it is a kind of have can the super-hydrophilic self-cleaning that bonds by force of self-curing apply
The preparation method of layer colloidal sol；
Super-hydrophilic self-cleaning coating sol provided by the invention has photocatalytic activity, and can keep super hydrophilic after film forming
Property.
The purpose of the present invention is realized by following proposal：
It is a kind of have can the super-hydrophilic self-cleaning coating sol that bonds by force of self-curing, including nano-titanium dioxide, inorganic polysilazane,
Solvent, catalyst；
The solvent be ethyl alcohol, methanol, isopropanol, n-butanol, toluene, n-butyl ether, dimethylbenzene, dichloromethane, water at least
It is a kind of；
The catalyst is at least one of 4,4'- trimethylenes bis- (1- methyl piperidines), 1- methyl piperidines, dimethylamine；
The nano-titanium dioxide is anatase-type nanometer titanium dioxide；
The average grain diameter of the nano-titanium dioxide is 0.1 ~ 50nm；
The inorganic polysilazane is perhydrogenating polysilazane, and structural formula is：
, wherein n is 1 ~ 3000.
It is used for this invention, contain the repetitive unit and soluble inorganic poly- silicon nitrogen in a solvent represented by above-mentioned general formula
Alkane can be by any polysilazane made from method well known in the prior art.Contain above-mentioned general formula institute as preparing
The method of the inorganic polysilazane soluble in a solvent indicated, it includes any the one of method known in the state of the art that can use
Kind.In the present invention, it is preferable to use the perhydrogenating polysilazanes that number-average molecular weight is 400 ~ 50000 for inorganic polysilazane.
The mass ratio of the nano-titanium dioxide and inorganic polysilazane is 10:（0.1~5）；
The mass ratio of the inorganic polysilazane and catalyst is 10:（0.001~1）；
The solid content of the super-hydrophilic self-cleaning coating sol is 1 ~ 70%；
A kind of preparation method of super-hydrophilic self-cleaning coating sol, includes the following steps：
（1）The preparation of nanometer titanium dioxide titanium solution
Anatase-type nanometer titanium dioxide, modifying agent, solvent are mixed, is uniformly dispersed under ultrasound condition, obtains nanometer titanium dioxide
Titanium solution；
The modifying agent is hexamethyldisilazane, hexamethyldisiloxane, at least one of methyltriethoxysilane；
The anatase-type nanometer titanium dioxide, modifying agent, solvent mass ratio be 1:（0.001~0.1）：（1~1000）；
（2）The preparation of super-hydrophilic self-cleaning coating sol
Step（1）Obtained nanometer titanium dioxide titanium solution, inorganic polysilazane solution, solvent mixes, and is stirred under the conditions of 0 ~ 35 DEG C
1 ~ 40h is mixed, is sealed, super-hydrophilic self-cleaning coating sol is obtained；
The inorganic polysilazane solution includes inorganic polysilazane, solvent and catalyst；The inorganic polysilazane solution
Solid content is 1 ~ 60%.
The application method of the super-hydrophilic self-cleaning coating sol, i.e., super-hydrophilic self-cleaning coating sol film in base material
On, cure 1 under the conditions of 0 ~ 100 DEG C~for 24 hours to get to super-hydrophilic coating.
The thickness of the super-hydrophilic coating is 1~1000 μm.
In the present invention, catalyst used can be under room temperature or lower temperature（0~100℃）By inorganic poly- silicon nitrogen
Alkane is converted into the effect of silica；In the present invention, the catalyst is 4,4'- trimethylenes bis- (1- methyl piperidines), 1- first
At least one of phenylpiperidines, dimethylamine.
To obtain the super-hydrophilic self-cleaning coating sol of the present invention, on the one hand, the present invention utilizes sharp with photocatalytic activity
Titanium ore type nano-titanium dioxide is as matrix so that coating has photocatalyst characteristic；On the other hand, the present invention is by being centainly formulated
And process control, make inorganic polysilazane（Perhydrogenating polysilazane）It is combined with nano-titanium dioxide, super hydrophilic painting is collectively formed
Layer colloidal sol.The colloidal sol of the present invention is coated in substrate surface, under the action of catalyst, inorganic polysilazane is converted into hydrophily two
Silica, with anatase-type nanometer titanium dioxide be collectively formed it is of the present invention can self-curing by force bond super-hydrophilic coating.
For the super-hydrophilic self-cleaning coating sol of the present invention for obtaining stable, the present invention changes titanium dioxide by modifying agent
Property, the compatibility between titanium dioxide and inorganic polysilazane can be improved, to obtain stable super-hydrophilic self-cleaning coating sol.
In view of the Superhydrophilic that the preferable bonding characteristic of inorganic polysilazane and film forming matter are stablized, the painting prepared by the present invention
Layer not only has photocatalytic activity, and can keep Superhydrophilic.In addition, in view of the preferable bonding characteristic of inorganic polysilazane, this
The colloidal sol of invention can form coating on different substrate materials surface, and other than hydrophily and self-cleaning characteristic, coating can provide the coating
To product or article with following characteristic, such as wearability, soil resistance, chemical-resistant, rub resistance, anticorrosive property, inoxidizability,
Physical barrier, fire resistance etc..In addition, by type of solvent, amount of compound material etc. in formula, this coating sol application just can be made
In very extensive purposes.
The present invention can obtain the super-hydrophilic coating that light transmittance is 60 ~ 99.9%, be applicable in by being centainly formulated and process control
In glass super-hydrophilic coating.
The coating sol of the present invention is liquid form in application, therefore coating sol can be easily by spraying, use cloth
Or method of sponge film etc. is coated on base material.In view of the preferable bonding characteristic of inorganic polysilazane, colloidal sol of the invention can
Coating is formed on different substrate materials surface, for the coating other than hydrophily, coating is provided to product or article with following characteristic,
Such as wearability, soil resistance, chemical-resistant, rub resistance, anticorrosive property, inoxidizability, physical barrier, fire resistance etc..In addition,
By type of solvent, amount of compound material etc. in formula, this coating sol just can be made to be applied to very extensive purposes.
Compared with the existing technology, the invention has the advantages that and advantageous effect：
The present invention by nano-titanium dioxide and inorganic polysilazane it is compound prepare can the super-hydrophilic self-cleaning that bonds by force of self-curing apply
Layer colloidal sol, the Superhydrophilic that prepared coating has photocatalytic activity and stablizes；Preparation process of the present invention is simple, it is of low cost,
It is environmentally protective, operating condition is easily-controllable, efficiently solve that existing coating photocatalytic activity is poor at present and preparation process be complicated
Problem may advantageously facilitate the application and development of super hydrophilic technology.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of anatase-type nanometer titanium dioxide in embodiment 1.
Fig. 2 is the water droplet contact angle test pictures of super-hydrophilic self-cleaning coating in embodiment 1.
Specific implementation mode
Specific embodiments of the present invention will be described in further detail for son with reference to the accompanying drawings and examples, but this hair
Bright embodiment is without being limited thereto.
Embodiment 1
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 10nm）, 0.1g modifying agent, 1000g isopropanols mixing, ultrasound
Under the conditions of be uniformly dispersed, obtain nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 5000g solid contents are 10%, dimethylbenzene are mixed
It closes, stirs 20h under the conditions of 5 DEG C, be sealed, obtain the super-hydrophilic self-cleaning coating sol that solid content is 3%.Used nothing
Machine polysilazane solution includes inorganic polysilazane, n-butyl ether and catalyst 4, and 4'- trimethylenes are bis- (1- methyl piperidines), wherein
The mass ratio of inorganic polysilazane and catalyst is 10:0.01.
Prepared super-hydrophilic self-cleaning coating sol film on base material, cure under the conditions of 80 DEG C for 24 hours to get to thickness
For 200 μm of super-hydrophilic coating.
Embodiment 2
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 2nm）, 1g modifying agent, the mixing of 800g ethyl alcohol, under ultrasound condition
It is uniformly dispersed, obtains nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 1000g solid contents are 10%, methanol are mixed
It closes, stirs 10h under the conditions of 25 DEG C, be sealed, obtain the super-hydrophilic self-cleaning coating sol that solid content is 3%.Used nothing
Machine polysilazane solution includes inorganic polysilazane, dimethylbenzene and catalyst 1- methyl piperidines, wherein inorganic polysilazane and is urged
The mass ratio of agent is 10:0.001.
Cure 4h prepared super-hydrophilic self-cleaning coating sol film on base material, under the conditions of 60 DEG C to get to thickness
For 200 μm of super-hydrophilic coating.
Embodiment 3
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 5nm）, 0.8g modifying agent, 1000g isopropanols mixing, ultrasound
Under the conditions of be uniformly dispersed, obtain nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 10000g solid contents are 2%, n-butanol are mixed
It closes, stirs 40h under the conditions of 35 DEG C, be sealed, obtain the super-hydrophilic self-cleaning coating sol that solid content is 1%.Used nothing
Machine polysilazane solution includes inorganic polysilazane, n-butyl ether and catalyst 4, and 4'- trimethylenes are bis- (1- methyl piperidines), wherein
The mass ratio of inorganic polysilazane and catalyst is 10:1.
Cure 10h prepared super-hydrophilic self-cleaning coating sol film on base material, under the conditions of 50 DEG C to get to thickness
For 300 μm of super-hydrophilic coating.
Embodiment 4
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 50nm）, 0.01g modifying agent, 10g toluene mixing, ultrasonic item
It is uniformly dispersed under part, obtains nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 1000g solid contents are 1%, n-butanol are mixed
It closes, stirs 40h under the conditions of 0 DEG C, be sealed, obtain the super-hydrophilic self-cleaning coating sol that solid content is 0.2%.It is used
Inorganic polysilazane solution includes inorganic polysilazane, dichloromethane and catalyst 1- methyl piperidines, wherein inorganic polysilazane
Mass ratio with catalyst is 10:0.5.
Cure 3h prepared super-hydrophilic self-cleaning coating sol film on base material, under the conditions of 70 DEG C to get to thickness
For 1 μm of super-hydrophilic coating.
Embodiment 5
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 6nm）, 1g modifying agent, 100g dimethylbenzene mixing, ultrasound condition
Under be uniformly dispersed, obtain nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 1000g solid contents are 50%, ethyl alcohol are mixed
It closes, stirs 30h under the conditions of 25 DEG C, be sealed, obtain the super-hydrophilic self-cleaning coating sol that solid content is 40%.It is used
Inorganic polysilazane solution includes inorganic polysilazane, n-butyl ether and catalyst 4, and 4'- trimethylenes are bis- (1- methyl piperidines),
The mass ratio of middle inorganic polysilazane and catalyst is 10:0.1.
Cure 1h prepared super-hydrophilic self-cleaning coating sol film on base material, under the conditions of 100 DEG C to get to thickness
The super-hydrophilic coating that degree is 1~1000 μm.
Embodiment 6
（1）The preparation of nanometer titanium dioxide titanium solution
By 10g anatase-type nanometer titanium dioxides（Average grain diameter is 8nm）, 0.01g modifying agent, 100g n-butyl ethers mixing, ultrasound
Under the conditions of be uniformly dispersed, obtain nanometer titanium dioxide titanium solution；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, the machine polysilazane solution that 10g solid contents are 1%, toluene mixing,
10h is stirred under the conditions of 5 DEG C, is sealed, the super-hydrophilic self-cleaning coating sol that solid content is 1% is obtained.Used inorganic poly- silicon
Azane solution includes inorganic polysilazane, dichloromethane and catalyst dimethylamine, the wherein matter of inorganic polysilazane and catalyst
Amount is than being 10:1.
Prepared super-hydrophilic self-cleaning coating sol film on base material, cure under the conditions of 0 DEG C for 24 hours to get to thickness
For 1000 μm of super-hydrophilic coating.
Performance test：
The coating that embodiment 1 ~ 6 provides is tested for the property, test method is as shown in table 1, the performance test results such as 2 institute of table
Show.
1 performance detection method therefor of table and instrument list
The performance test results of 2 embodiment 1 ~ 6 of table
As can be seen from Table 2, coating provided by the invention has Superhydrophilic, and Superhydrophilic can be maintained for a long time, in nothing
After being stored 2 months under the conditions of light, coating can still keep water droplet contact angle to be less than 5 °, and coating still has after 12 months
There is preferable hydrophily.In addition to this, coating has preferable case hardness, adhesive force, resistance to salt water and resistance to acid and alkali.Pass through
The regulation and control of inventive formulation and technique can get hydrophilic coating of the light transmittance 60 ~ 99.9.
Photocatalysis performance is tested：
The present invention obtains super-hydrophilic self-cleaning coating using anatase titanium dioxide crystal form titanium dioxide and inorganic polysilazane are compound, therefore has light and urge
Change efficiency.Prepared super-hydrophilic self-cleaning coating sol film is prepared into photocatalysis coating by embodiment 1 ~ 6 on glass slide.
Prepare 8mg/L rhodamine B aqueous solution, in photochemical reactor be added 100ml rhodamine B aqueous solution, 5 pieces
Two-sided film has 1 ~ 6 super-hydrophilic self-cleaning coating of embodiment, dark reaction 30 minutes that photocatalysis coating is made to reach adsorption equilibrium；Reach
After adsorption equilibrium, the xenon lamp of ultraviolet lamp or simulated visible light is opened, time segment sampling is measured using ultraviolet specrophotometer and inhaled
Shading value determines rhodamine B aqueous solution by the complete time that will degrade.The experimental results are shown inthe following table：
The photocatalysis performance testing result of 2 embodiment 1 ~ 6 of table
It can be seen that, the present invention, which does the super-hydrophilic self-cleaning coating prepared, has preferable photocatalytic activity from table.Repeat
Photocatalysis performance detects, and experimental result is found, after 8 cycles, the photocatalytic degradation effect of coating is almost unchanged, explanation
Coating of the present invention has excellent photocatalysis stability.
Applicant states that the present invention illustrates the method detailed of the present invention, but the present invention not office by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalent substitution and auxiliary element to each raw material of product of the present invention
Addition, the selection etc. of concrete mode, all fall within protection scope of the present invention and the open scope.
Claims (5)
1. a kind of super-hydrophilic self-cleaning coating sol, which is characterized in that the super-hydrophilic self-cleaning coating sol includes nanometer titanium dioxide
Titanium, inorganic polysilazane, solvent, catalyst.
2. a kind of super-hydrophilic coating colloidal sol according to claim 1, it is characterised in that：
The solvent be ethyl alcohol, methanol, isopropanol, n-butanol, toluene, n-butyl ether, dimethylbenzene, dichloromethane, water at least
It is a kind of；
The catalyst is at least one of 4,4'- trimethylenes bis- (1- methyl piperidines), 1- methyl piperidines, dimethylamine；
The nano-titanium dioxide is anatase-type nanometer titanium dioxide；
The average grain diameter of the nano-titanium dioxide is 0.1 ~ 50nm；
The inorganic polysilazane is perhydrogenating polysilazane, and structural formula is：
, wherein n is 1 ~ 3000；
The mass ratio of the nano-titanium dioxide and inorganic polysilazane is 10:（0.1~5）；
The mass ratio of the inorganic polysilazane and catalyst is 10:（0.001~1）；
The solid content of the super-hydrophilic self-cleaning coating sol is 1 ~ 70%.
3. according to a kind of preparation method of super-hydrophilic self-cleaning coating sol described in claim 1 ~ 2, which is characterized in that including with
Lower step：
（1）The preparation of nanometer titanium dioxide titanium solution
Anatase-type nanometer titanium dioxide, modifying agent, solvent are mixed, is uniformly dispersed under ultrasound condition, obtains nanometer titanium dioxide
Titanium solution solution；
The modifying agent is hexamethyldisilazane, hexamethyldisiloxane, at least one of methyltriethoxysilane；
The anatase-type nanometer titanium dioxide, modifying agent, solvent mass ratio be 1:（0.001~0.1）：（1~1000）；
（2）The preparation of super-hydrophilic self-cleaning coating sol
By step（1）Obtained nanometer titanium dioxide titanium solution, inorganic polysilazane solution, solvent mixes, under the conditions of 0 ~ 35 DEG C
1 ~ 40h is stirred, is sealed, obtains super-hydrophilic self-cleaning coating sol；
The inorganic polysilazane solution includes inorganic polysilazane, solvent and catalyst；
The solid content of the inorganic polysilazane solution is 1 ~ 60%.
4. according to the application method of claims 1 to 3 any one of them super-hydrophilic self-cleaning coating sol, it is characterised in that：
Super-hydrophilic self-cleaning coating sol film cures 1 on base material, under the conditions of 0 ~ 100 DEG C~for 24 hours to get to super-hydrophilic coating.
5. the application method of super-hydrophilic self-cleaning coating sol according to claim 4, it is characterised in that：The super hydrophilic painting
The thickness of layer is 1~1000 μm.
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| CN110028900A (en) * | 2019-03-12 | 2019-07-19 | 南京尚易环保科技有限公司 | A kind of automobile finish brilliant liquid of plating and preparation method thereof |
| CN110862703A (en) * | 2019-11-29 | 2020-03-06 | 苏燕辉 | Nano fireproof heat-insulating anticorrosive paint and preparation method thereof |
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| CN110862703B (en) * | 2019-11-29 | 2021-08-03 | 苏燕辉 | Nano fireproof heat-insulating anticorrosive paint and preparation method thereof |
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| CN112391112A (en) * | 2020-11-03 | 2021-02-23 | 江苏皇冠新材料科技有限公司 | Antifogging coating, antifogging film and preparation method thereof |
| WO2022148287A1 (en) * | 2021-01-08 | 2022-07-14 | 杭州三花研究院有限公司 | Heat exchanger, and preparation method therefor and thermal management system thereof |
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