CN108641419A - A kind of super-hydrophilic coating colloidal sol and its preparation and application - Google Patents
A kind of super-hydrophilic coating colloidal sol and its preparation and application Download PDFInfo
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- CN108641419A CN108641419A CN201810422840.5A CN201810422840A CN108641419A CN 108641419 A CN108641419 A CN 108641419A CN 201810422840 A CN201810422840 A CN 201810422840A CN 108641419 A CN108641419 A CN 108641419A
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a kind of silica super-hydrophilic coating colloidal sol of normal temperature solidified strong cohesive property and its preparation and application；For silica super-hydrophilic coating colloidal sol after film forming, coating has Superhydrophilic.The present invention is using nano silicon dioxide as main matrix, and using inorganic polysilazane as binder, by the compound super hydrophilic colloidal sol for preparing normal temperature solidified strong cohesive property, prepared coating has stable Superhydrophilic；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 Durability 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 coating colloidal sols and its preparation method and application, and in particular to a kind of to use nanometer two
The super-hydrophilic coating colloidal sol and its preparation method and application that silica and inorganic polysilazane are 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.Currently, generally use organic coating and inorganic coating two ways, wherein organic painting
Layer is usually in a large amount of hydrophilic functional groups of substrate surface chemical modification；Inorganic coating is usually silica or coating of titanium dioxide.
Since titanium dioxide needs just to easily cause photic hydrophily under ultraviolet light or stronger radiation of visible light, in no light or light
According to this effect is extremely difficult in weaker environment, which greatly limits the application ranges of the self-cleaning net material of titanium dioxide.
Silica due on surface texture there are many hydroxyl group thus have preferable hydrophily.But simple silica is thin
The contact angle of film and water is about 20 °, reaches the Superhydrophilic that contact angle is less than 5 ° far away.It is super close so that silica coating has
It is aqueous, it needs to construct certain microcosmic structure on silica coating.Patent CN200910042039.9 reports pass through rotation
Cladding process prepares mesoporous silicon oxide films in glass baseplate surface, and the contact angle of film and water obtained is 0 °, shows excess of export
Hydrophily；The reports of patent CN 201310349597.6 obtain self-cleaning coating using SiO2 colloidal sols and pore-foaming agent mixed number, will be above-mentioned
Then self-cleaning coating even application carries out curing process on the surface of cleaned glass, it is micro- to remove the acquisition of coat inside pore-foaming agent
Structure is seen, to obtain automatically cleaning cladding glass.
It can be seen that, the preparation method of current super hydrophilic silica coating mostly exists and needs height from existing technology
Warm curing mode, caking property of the raising silica in base material；In addition to this, prior art prepares the method for super-hydrophilic coating more
It is complicated, of high cost, and special coating process is used, be not suitable for large-scale production and processing.
Invention content
The technical problem to be solved in the present invention is, in the prior art the shortcomings that, provide a kind of normal temperature solidified strong
The silica super-hydrophilic coating colloidal sol of caking property；
The further technical problems to be solved of the present invention are, it is super close to provide a kind of silica of normal temperature solidified strong cohesive property
The preparation and application of water coating sol；
For silica super-hydrophilic coating colloidal sol provided by the invention after film forming, coating has Superhydrophilic.
The purpose of the present invention is realized by following proposal：
A kind of silica super-hydrophilic coating colloidal sol of normal temperature solidified strong cohesive property, including nano silicon dioxide, inorganic poly- silicon
Azane, solvent, catalyst and dispersant；
Wherein, the solvent is ethyl alcohol, methanol, isopropanol, n-butanol, toluene, n-butyl ether, dimethylbenzene, dichloromethane, tetrahydrochysene
At least one of furans, water；
In the present invention, the catalyst be 4,4'- trimethylenes bis- (1- methyl piperidines), 1- methyl piperidines, dimethylamine, acetic acid,
At least one of hydrochloric acid；
The dispersant is polyethylene glycol 200, polyethylene glycol 400, hydrolysis of polymaleic anhydride, gelatin, propylene glycol monomethyl ether, dipropyl two
At least one of alcohol methyl ether；
The nano silicon dioxide is at least one of non-porous nano silica and meso-porous nano silica；
The inorganic polysilazane includes 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 nano silicon dioxide and inorganic polysilazane mass ratio are 10:（0.01~100）；
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 0.1 ~ 50%；
A kind of preparation method of super-hydrophilic coating colloidal sol, includes the following steps：
（1）The preparation of nanosilica solution
Non-porous nano silica, meso-porous nano silica, dispersant, solvent are mixed, is uniformly dispersed, obtains under ultrasound condition
To nanosilica solution；
The size of the non-porous nano silica is 0.5 ~ 100nm；The size of the meso-porous nano silica is 0.5
~200nm；The inner void size of the meso-porous nano silica is 0.1-20 nm；The non-porous nano silica is situated between
Hole nano silicon dioxide, dispersant, solvent mass ratio be 1:（0.02~5）:（0~0.5）:（1~10000）；
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Obtained nanosilica solution is mixed with inorganic polysilazane solution, and 1 is stirred under the conditions of 0 ~ 35 DEG C
~ 40h, is sealed, and obtains super-hydrophilic coating colloidal sol；
The inorganic polysilazane solution includes inorganic polysilazane, solvent and catalyst；
The solid content of the inorganic polysilazane solution is 1 ~ 50%.
The application method of the super-hydrophilic coating colloidal sol, including：Super-hydrophilic coating colloidal sol film on base material, room temperature
Solidification 1~for 24 hours to get to super-hydrophilic coating.The thickness of the super-hydrophilic coating is 1~1000 μm；The super-hydrophilic coating
Light transmittance is 60 ~ 99.9%；
The dispersant that the present invention uses, including polyethylene glycol 200, polyethylene glycol 400, hydrolysis of polymaleic anhydride, gelatin, propylene glycol
On the one hand the compatibility between nano silicon dioxide and inorganic polysilazane can be improved in methyl ether, dipropylene glycol methyl ether etc., promote molten
Liquid homogenizes, and can avoid the unstable appearance of colloidal sol；On the other hand, dispersant is largely aqueous substance, after colloidal sol forms a film,
In conjunction with the Superhydrophilic of coating, dispersant can be dissolved to and is discharged system, formed further by certain water wetting action
The super hydrophilic film layer of full-inorganic ingredient.
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, acetic acid, hydrochloric acid.
To obtain the silica super-hydrophilic coating colloidal sol of the present invention, on the one hand, the present invention utilizes hydrophilic nano dioxy
SiClx is as main matrix, wherein hydrophilic mesoporous nano silicon dioxide contains a large amount of nano grade pore structure, for institute of the present invention
The hydrophily stability for stating coating provides microstructure basis；On the other hand, for by nano silicon dioxide, simply fixation is bonded in
Substrate surface forms coating, and does not influence the hydrophily of coating again, and the present invention uses inorganic polysilazane（The poly- silicon nitrogen of perhydrogenating
Alkane）As binder, by being centainly formulated and process control, it is allowed to be combined with nano silicon 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, the inorganic polysilazane as binder turns
Hydrophilic silicon oxides are turned to, are collectively formed with non-porous nano silica and meso-porous nano silica of the present invention super
Hydrophilic coating.The coating hard and compact, and the nano-pore structure that meso-porous nano silica can be kept to provide, coating are super hydrophilic
Performance is stablized, and is firmly combined with base material, has excellent weatherability.
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 is using nano silicon dioxide as main matrix, can be normal by compound prepare using inorganic polysilazane as binder
The super hydrophilic colloidal sol of temperature solidification strong cohesive property, prepared coating have stable Superhydrophilic；Preparation process of the present invention is simple, at
This is cheap, environmentally protective, operating condition is easily-controllable, efficiently solves that existing Coating Durability at present is poor and preparation process complexity
The problem of, it may advantageously facilitate the application and development of super hydrophilic technology.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of non-porous nano silica in embodiment 1；
Fig. 2 is the transmission electron microscope picture of 1 intermediary hole nanometer titanium dioxide silicon nano of embodiment；
Fig. 3 is the water droplet contact angle test pictures of super-hydrophilic 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 nanosilica solution
By 10g non-porous nano silica (average grain diameter 10nm), 0.2 g meso-porous nano silica（Average grain diameter is 50nm,
Inner void average-size is 10 nm）, 0.1g polyethylene glycol 200s, the mixing of 500g ethyl alcohol, be uniformly dispersed under ultrasound condition, obtain
Nanosilica solution.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution that obtained nanosilica solution is 5% with 20g solid contents, methanol are mixed
It closes, sealing stirring 20h, is sealed under the conditions of 20 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 2%.Used nothing
Machine polysilazane solution include inorganic polysilazane, toluene and catalyst 4,4'- trimethylenes are bis- (1- methyl piperidines), wherein without
The mass ratio of machine polysilazane and catalyst is 10:0.01.
Prepared super-hydrophilic coating colloidal sol film on base material, normal temperature cure is for 24 hours to get to super-hydrophilic coating.Institute
The thickness of the super-hydrophilic coating of preparation is 50 μm.
Embodiment 2
（1）The preparation of nanosilica solution
By 10g non-porous nano silica (average grain diameter 100nm), 50g meso-porous nano silica（Average grain diameter is 100nm,
Inner void average-size is 1 nm, 5g polyethylene glycol 400, the mixing of 100000g methanol, is uniformly dispersed, obtains under ultrasound condition
Nanosilica solution.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution, methanol of the obtained nanosilica solution with 50000g solid contents for 1%
Mixing, sealing stirring 30h, is sealed under the conditions of 0 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 0.1%.It is used
Inorganic polysilazane solution include inorganic polysilazane, tetrahydrofuran and catalyst 1- methyl piperidines, wherein inorganic poly- silicon nitrogen
The mass ratio of alkane and catalyst is 10:0.001.
Prepared super-hydrophilic coating colloidal sol film on base material, normal temperature cure is for 24 hours to get to super-hydrophilic coating.Institute
The thickness of the super-hydrophilic coating of preparation is 5 μm.
Embodiment 3
（1）The preparation of nanosilica solution
By 10g non-porous nano silica (average grain diameter 0.5nm), 10g meso-porous nano silica（Average grain diameter is 80nm,
Inner void average-size is 3 nm）, 0.1g hydrolysis of polymaleic anhydride, the mixing of 2000g isopropanols, disperse under ultrasound condition equal
It is even, obtain nanosilica solution.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution that obtained nanosilica solution is 10% with 10000g solid contents, positive fourth
Alcohol mixes, and sealing stirring 20h, is sealed under the conditions of 25 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 0.5%.Made
Inorganic polysilazane solution includes inorganic polysilazane, toluene 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 coating colloidal sol film on base material, normal temperature cure 12h is to get to super-hydrophilic coating.Institute
The thickness of the super-hydrophilic coating of preparation is 200 μm.
Embodiment 4
（1）The preparation of nanosilica solution
By 10g non-porous nano silica (average grain diameter 50nm), 40g meso-porous nano silica（Average grain diameter is 90nm, interior
Portion's hole average-size is 10nm）, the mixing of 8000g isopropanols, be uniformly dispersed under ultrasound condition, it is molten to obtain nano silicon dioxide
Liquid.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution that obtained nanosilica solution is 2% with 100g solid contents, ethyl alcohol are mixed
It closes, sealing stirring 10h, is sealed under the conditions of 15 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 1%.Used nothing
Machine polysilazane solution includes inorganic polysilazane, dichloromethane and catalyst 4, and 4'- trimethylenes are bis- (1- methyl piperidines),
The mass ratio of middle inorganic polysilazane and catalyst is 10:0.1.
Prepared super-hydrophilic coating colloidal sol film on base material, normal temperature cure 1h is to get to super-hydrophilic coating.It is made
The thickness of standby super-hydrophilic coating is 800 μm.
Embodiment 5
（1）The preparation of nanosilica solution
By 10g non-porous nano silica (average grain diameter 30nm), 50g meso-porous nano silica（Average grain diameter is 200nm,
Inner void average-size is 10 nm）, 0.1g gelatin, the mixing of 6000g toluene, be uniformly dispersed under ultrasound condition, obtain nanometer two
Silica solution.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution that obtained nanosilica solution is 50% with 1000g solid contents, positive fourth
Alcohol mixes, and sealing stirring 40h, is sealed under the conditions of 0 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 2%.It is used
Inorganic polysilazane solution include inorganic polysilazane, dimethylbenzene and catalyst dimethylamine, wherein inorganic polysilazane and urge
The mass ratio of agent is 10:1.
Prepared super-hydrophilic coating colloidal sol film on base material, normal temperature cure is for 24 hours to get to super-hydrophilic coating.Institute
The thickness of the super-hydrophilic coating of preparation is 1000 μm.
Embodiment 6
（1）The preparation of nanosilica solution
By 10g non-porous nano silica (average grain diameter 10nm), 30g meso-porous nano silica（Average grain diameter is 100nm,
Inner void average-size is 10 nm）, 2g dipropylene glycol methyl ethers, the mixing of 10000g methanol, be uniformly dispersed under ultrasound condition, obtain
To nanosilica solution.
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Inorganic polysilazane solution that obtained nanosilica solution is 1% with 2000g solid contents, ethyl alcohol are mixed
It closes, sealing stirring 30h, is sealed under the conditions of 35 DEG C, obtains the super-hydrophilic coating colloidal sol that solid content is 0.4%.It is used
Inorganic polysilazane solution include inorganic polysilazane, n-butyl ether and catalyst 1- methyl piperidines, wherein inorganic polysilazane and
The mass ratio of catalyst is 10:0.01.
Prepared super-hydrophilic coating colloidal sol film on base material, normal temperature cure 12h is to get to super-hydrophilic coating.Institute
The thickness of the super-hydrophilic coating of preparation is 1000 μm；.
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, 12
After a month, still there is preferable hydrophily；And coating has preferable case hardness, adhesive force, resistance to salt water and acid and alkali-resistance
Property.In addition to this, the regulation and control of formula and technique through the invention, can get hydrophilic coating of the light transmittance 60 ~ 99.9.
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 coating colloidal sol, which is characterized in that the super-hydrophilic coating colloidal sol includes nano silicon dioxide, inorganic poly-
Silazane, solvent, catalyst and dispersant；
Wherein, the solvent is ethyl alcohol, methanol, isopropanol, n-butanol, n-butyl ether, dimethylbenzene, dichloromethane, toluene, tetrahydrochysene
At least one of furans, water；
The catalyst be 4,4'- trimethylenes bis- (1- methyl piperidines), 1- methyl piperidines, dimethylamine, acetic acid, hydrochloric acid at least
It is a kind of；
The dispersant is polyethylene glycol 200, polyethylene glycol 400, hydrolysis of polymaleic anhydride, gelatin, propylene glycol monomethyl ether, dipropyl two
At least one of alcohol methyl ether.
2. a kind of super-hydrophilic coating colloidal sol according to claim 1, which is characterized in that
The nano silicon dioxide is at least one of non-porous nano silica and meso-porous nano silica；
The inorganic polysilazane is perhydrogenating polysilazane, and structural formula is：
, wherein n is 1 ~ 3000；
The nano silicon dioxide and inorganic polysilazane mass ratio are 10:（0.01~100）；
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 0.1 ~ 50%.
3. according to a kind of preparation method of super-hydrophilic coating colloidal sol described in claim 1 ~ 2, which is characterized in that including following step
Suddenly：
（1）The preparation of nanosilica solution
Non-porous nano silica, meso-porous nano silica, dispersant, solvent are mixed, is uniformly dispersed, obtains under ultrasound condition
To nanosilica solution；
The average grain diameter of the non-porous nano silica is 0.5 ~ 100nm；The meso-porous nano silica is averaged
Grain size is 0.5 ~ 200nm；The inner void average-size of the meso-porous nano silica is 0.1-20 nm；It is described non-porous to receive
Rice silica, meso-porous nano silica, dispersant, solvent mass ratio be 1:（0.02~5）:（0~0.5）:（1~
10000）；
（2）The preparation of super-hydrophilic coating colloidal sol
By step（1）Obtained nanosilica solution is mixed with inorganic polysilazane solution, solvent, under the conditions of 0 ~ 35 DEG C
Sealing 1 ~ 40h of stirring, is sealed, obtains super-hydrophilic coating colloidal sol；
The inorganic polysilazane solution includes inorganic polysilazane, solvent and catalyst；
The solid content of the inorganic polysilazane solution is 1 ~ 50%.
4. according to the application method of claims 1 to 3 any one of them super-hydrophilic coating colloidal sol, it is characterised in that：Super close
Water coating sol film is on base material, and normal temperature cure 1~for 24 hours is to get to super-hydrophilic coating.
5. the application method of super-hydrophilic coating colloidal sol according to claim 4, it is characterised in that：
The thickness of the super-hydrophilic coating is 1~1000 μm；
The light transmittance of the super-hydrophilic coating is 60 ~ 99.9%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110076070A (en) * | 2019-03-08 | 2019-08-02 | 广州碧然环保有限公司 | A kind of coating method for the super hydrophilic plastic film of the antifouling antistatic of automatically cleaning covering inorganic coating |
| CN111548732A (en) * | 2020-04-30 | 2020-08-18 | 广州弘海化工科技有限公司 | Super-hydrophilic silicon nano-microstructure anti-reflection coating and preparation and use methods thereof |
| CN113136166A (en) * | 2021-04-01 | 2021-07-20 | 中国船舶重工集团公司第七一八研究所 | Glass antifogging agent and preparation method thereof |
| CN113372814A (en) * | 2021-05-27 | 2021-09-10 | 广州一新科技有限公司 | Cage-shaped polysilsesquioxane-based super-hydrophilic functional coating and preparation method thereof |
| CN113881252A (en) * | 2021-08-24 | 2022-01-04 | 东南大学 | Super-hydrophilic anti-fog coating with good durability and preparation method thereof |
| CN113897135A (en) * | 2021-11-29 | 2022-01-07 | 广东晟毅新材料科技有限公司 | Super-hydrophilic anti-fog coating and preparation method thereof |
| CN116041998A (en) * | 2022-12-02 | 2023-05-02 | 国家电投集团杭州新能源生产运营有限公司 | Super-hydrophilic coating composition, super-hydrophilic coating and preparation method thereof |
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| CN113136166B (en) * | 2021-04-01 | 2022-08-19 | 中国船舶重工集团公司第七一八研究所 | Glass antifogging agent and preparation method thereof |
| CN113372814A (en) * | 2021-05-27 | 2021-09-10 | 广州一新科技有限公司 | Cage-shaped polysilsesquioxane-based super-hydrophilic functional coating and preparation method thereof |
| CN113881252A (en) * | 2021-08-24 | 2022-01-04 | 东南大学 | Super-hydrophilic anti-fog coating with good durability and preparation method thereof |
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| CN116041998A (en) * | 2022-12-02 | 2023-05-02 | 国家电投集团杭州新能源生产运营有限公司 | Super-hydrophilic coating composition, super-hydrophilic coating and preparation method thereof |
| CN116041998B (en) * | 2022-12-02 | 2024-04-30 | 国家电投集团杭州新能源生产运营有限公司 | Super-hydrophilic coating composition, super-hydrophilic coating and preparation method thereof |
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