CN102807803A - Method for preparing organic and inorganic composite super-hydrophobic coatings - Google Patents
Method for preparing organic and inorganic composite super-hydrophobic coatings Download PDFInfo
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- CN102807803A CN102807803A CN2012103114151A CN201210311415A CN102807803A CN 102807803 A CN102807803 A CN 102807803A CN 2012103114151 A CN2012103114151 A CN 2012103114151A CN 201210311415 A CN201210311415 A CN 201210311415A CN 102807803 A CN102807803 A CN 102807803A
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Abstract
The invention discloses a method for preparing organic and inorganic composite super-hydrophobic coatings. The method comprises the following steps of: preparing modified silicon dioxide nano particles, preparing coating sol and coating the surface of a substrate material. The method is simple in process, readily available in raw materials and low in cost and is suitable for large-scale production and application; and the prepared coatings have high super-hydrophobic property, self-cleaning performance and freezing resistance.
Description
Technical field
The present invention relates to a kind of super-hydrophobic surface coating and preparation method thereof, belong to the organic/inorganic composite material technical field.
Background technology
Surface properties is one of most important physico-chemical property of solid material, and wellability is a main aspect of material surface character.In recent years, super hydrophobic surface has caused people's extensive concern.Super hydrophobic surface is meant that contact angle with water is greater than 150
o, and roll angle is less than 10
oThe surface.Because the contact area of super hydrophobic surface and water droplet is less; Water droplet is very easily from surperficial landing; Therefore super hydrophobic surface not only has self-cleaning function, and at microfluidic device, anti-conduction of current, anticorrosion, antifog, mildew-resistant, snow defence, frost prevention, frost protection, freezing, antiseizedly echo antifouling or the like many fields and be with a wide range of applications.Research shows that super hydrophobic surface has low surface energy and high surface roughness, can obtain super hydrophobic surface through the regulation and control to chemical constitution and surface tissue form.
The method and the approach that prepare at present super hydrophobic surface mainly contain: chemical etching method, phase separation method, electrodeposition method, template, sol-gel method, plasma treatment and self-assembly etc.; But defectives such as these technological ubiquity complex steps; And all relate in the preparation process of most of super hydrophobic surfaces and use expensive low surface energy material; Compound like fluorine-containing or silane reduces surface energy; And many methods relate to special devices, exacting terms and long cycle, are difficult to realize the preparation of big area super-hydrophobic coat, have limited its practical application to a certain extent.Therefore significant through simple and easy method large-area preparation super-hydrophobic surface coating.Patent of invention CN 101575478 B disclose a kind of preparation method of epoxy resin super-hydrophobic coat.Make coating solution through silica dioxide granule, silane coupling agent, epoxy resin, the stirring of hydrophobizing agent Hybrid Heating, film, make epoxy resin cure crosslinked, get epoxy resin super-hydrophobic coat through heating at substrate material surface.Though this method has overcome some defectives of conventional art, still has room for improvement.
Summary of the invention
For overcoming the deficiency of prior art, the present invention proposes the preparation method of the compound super-hydrophobic coat of a kind of organic-inorganic.
The preparation method of the compound super-hydrophobic coat of organic-inorganic according to the invention; Step comprises that the preparation of improved silica nanoparticle, coating colloidal sol prepare and substrate material surface is filmed; It is characterized in that: said improved silica nanometer particle process method is: nano silicon is dissolved in the solvent orange 2 A; Add the long-chain alkoxy base silane as properties-correcting agent, the heated and stirred back flow reaction makes the improved silica nanoparticle; Wherein the mass ratio of nano silicon, long-chain alkoxy base silane properties-correcting agent and solvent orange 2 A materials is 0.1～5:0.1～2.5:1～50, and solvent orange 2 A is toluene, N, the mixture of a kind of or its arbitrary volume ratio in dinethylformamide, the DMSO 99.8MIN.; The preparation method of said coating colloidal sol is: is the mixed of 0.1～5:0.1～5:0.1～2.5:1～50 with the improved silica nanoparticle that makes, epoxy resin, solidifying agent and solvent B by mass ratio, and ultrasonic mixing makes coating colloidal sol; Wherein solidifying agent is epoxy curing agent T31 (Tianjin three produces with chemical ltd), and solvent B is the mixture of a kind of or its arbitrary volume ratio in toluene, the acetone; The method that said substrate material surface is filmed is: with brushing or dip coating the coating colloidal sol that makes evenly is applied in substrate surface, drying at room temperature 24～48h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: said nano silicon is a fumed silica, and particle diameter is 50～100nm.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: said long-chain alkoxy base silane is dodecyl Trimethoxy silane, dodecyl triethoxyl silane, hexadecyl Trimethoxy silane, hexadecyl triethoxyl silane, octadecyl Trimethoxy silane or octadecyltriethoxy silane.
Wherein: the preferred dodecyl Trimethoxy silane of said long-chain alkoxy base silane, dodecyl triethoxyl silane or hexadecyl Trimethoxy silane.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: the mass ratio of said nano silicon, long-chain alkoxy base silane properties-correcting agent and solvent orange 2 A materials is preferably 1～3:0.5～1.5:15～35.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: preferred toluene of said solvent orange 2 A or N, dinethylformamide.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: said improved silica nanoparticle, epoxy resin, solidifying agent and solvent B are preferably 2～4:0.5～3:0.5～1.5:15～35 by mass ratio.
Among the preparation method of the compound super-hydrophobic coat of above-mentioned organic-inorganic: preferred toluene of said solvent B and acetone are the mixture of 2:1 by volume.
The present invention has made full use of the advantage of inorganic nano compound and polymkeric substance, multiple function such as that the coating of preparation has is super-hydrophobic, self-cleaning and freezing performance.Simultaneously, the preparation method is simple, practical, cost is low and convenience.Be suitable for enterprise implement and large-scale production and application, have social benefit and economic worth widely.
Embodiment
For being easy to further understand the present invention, the following example will be done further elaboration to the present invention.
Embodiment 1
(1) preparation of improved silica nanoparticle: the 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol: with the mixed solvent (toluene: acetone=2:1 of 0.4g improved silica nanoparticle, 0.4g epoxy resin, 0.2g epoxy curing agent T31 (Tianjin three produces with chemical ltd) and 8mL toluene and acetone; Volume ratio); Ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed: with brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Embodiment 2
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.Mixed solvent (toluene: acetone=2:1 with 0.4g improved silica nanoparticle, 0.2g epoxy resin, 0.1g epoxy curing agent T31 (Tianjin three produces with chemical ltd) and 8mL toluene and acetone; Volume ratio); Ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Embodiment 3
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.Mixed solvent (toluene: acetone=2:1 with 0.4g improved silica nanoparticle, 0.1g epoxy resin, 0.05g epoxy curing agent T31 (Tianjin three produces with chemical ltd) and 8mL toluene and acetone; Volume ratio); Ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Embodiment 4
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.Mixed solvent (toluene: acetone=2:1 with 0.4g improved silica nanoparticle, 0.067g epoxy resin, 0.033g epoxy curing agent T31 (Tianjin three produces with chemical ltd) and 8mL toluene and acetone; Volume ratio); Ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Embodiment 5
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.With the mixed solvent (toluene: acetone=2:1, volume ratio) of 0.4g improved silica nanoparticle, 0.05g epoxy resin, 0.025g epoxy curing agent T31 and 8mL toluene and acetone, ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Comparative example 1
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.With the mixed solvent (toluene: acetone=2:1, volume ratio) of 0.4g epoxy resin, 0.2g epoxy curing agent T31 and 8mL toluene and acetone, ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 24h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
Comparative example 2
(1) preparation of improved silica nanoparticle.The 5g nanometer silicon dioxide particle is dissolved in the 50mL toluene, adds 2.5g hexadecyl Trimethoxy silane as properties-correcting agent, the heated and stirred back flow reaction makes improved silica.
(2) preparation of coating colloidal sol.With the mixed solvent (toluene: acetone=2:1, volume ratio) of 0.1g epoxy resin, 0.05g epoxy curing agent T31 and 8mL toluene and acetone, ultrasonic mixing makes coating colloidal sol.
(3) substrate material surface is filmed.With brushing or dip coating the coating colloidal sol that makes in (2) evenly is applied in substrate surface, drying at room temperature 48h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.Test its water contact angle, the result sees table 1.
The compound super-hydrophobic coat water contact angle of table 1 test result
Annotate: the German Data Physics product OCAAO of company type full-automatic video contact angle measurement, useful range 0～180 are adopted in the contact angle test
o, tolerance range is 0.1
o, the row of making even is tested three times MV.
Can find out that by table 1 water contact angle of single epoxy coating is 100
oAbout, and the water contact angle of improved silica/epoxy resin compound coating is all 150
oAbout, can reach super-hydrophobic effect, the toughness of following coating and rigidity be coordination principle mutually, and the super-hydrophobic coat of preparation has ideal effect during improved silica/epoxy resin=6:1 (mass ratio).
Super-hydrophobic coat provided by the invention is expected to be used widely in fields such as waterproof and dampproof, automatically cleaning, freezings.
Claims (8)
1. the preparation method of the compound super-hydrophobic coat of organic-inorganic; Step comprises that the preparation of improved silica nanoparticle, coating colloidal sol prepare and substrate material surface is filmed; It is characterized in that: said improved silica nanometer particle process method is: nano silicon is dissolved in the solvent orange 2 A; Add the long-chain alkoxy base silane as properties-correcting agent, the heated and stirred back flow reaction makes the improved silica nanoparticle; Wherein the mass ratio of nano silicon, long-chain alkoxy base silane properties-correcting agent and solvent orange 2 A materials is 0.1～5:0.1～2.5:1～50, and solvent orange 2 A is toluene, N, the mixture of a kind of or its arbitrary volume ratio in dinethylformamide, the DMSO 99.8MIN.; The preparation method of said coating colloidal sol is: is the mixed of 0.1～5:0.1～5:0.1～2.5:1～50 with the improved silica nanoparticle that makes, epoxy resin, solidifying agent and solvent B by mass ratio, and ultrasonic mixing makes coating colloidal sol; Wherein solidifying agent is epoxy curing agent T31, and solvent B is the mixture of a kind of or its arbitrary volume ratio in toluene, the acetone; The method that said substrate material surface is filmed is: with brushing or dip coating the coating colloidal sol that makes evenly is applied in substrate surface, drying at room temperature 24～48h promptly forms the compound super-hydrophobic coat of one deck organic-inorganic at substrate surface.
2. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: said nano silicon is a fumed silica, particle diameter is 50～100nm.
3. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: said long-chain alkoxy base silane is dodecyl Trimethoxy silane, dodecyl triethoxyl silane, hexadecyl Trimethoxy silane, hexadecyl triethoxyl silane, octadecyl Trimethoxy silane or octadecyltriethoxy silane.
4. like the preparation method of the compound super-hydrophobic coat of the said organic-inorganic of claim 3, it is characterized in that: said long-chain alkoxy base silane is dodecyl Trimethoxy silane, dodecyl triethoxyl silane or hexadecyl Trimethoxy silane.
5. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: the mass ratio of said nano silicon, long-chain alkoxy base silane properties-correcting agent and solvent orange 2 A materials is 1～3:0.5～1.5:15～35.
6. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: said solvent orange 2 A is toluene or N, dinethylformamide.
7. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: said improved silica nanoparticle, epoxy resin, solidifying agent and solvent B are 2～4:0.5～3:0.5～1.5:15～35 by mass ratio.
8. the preparation method of the compound super-hydrophobic coat of organic-inorganic according to claim 1, it is characterized in that: said solvent B is that toluene and acetone are the mixture of 2:1 by volume.
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| CN115651437A (en) * | 2022-11-04 | 2023-01-31 | 中国长江三峡集团有限公司 | Super-hydrophobic material, preparation method thereof and application thereof in drainage pipeline |
| CN116120808A (en) * | 2023-01-03 | 2023-05-16 | 国家石油天然气管网集团有限公司 | Durable super-hydrophobic anti-corrosion coating and preparation method thereof |
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