CN104745045A - Super-hydrophobic and oleophobic composite coating and preparation method thereof - Google Patents
Super-hydrophobic and oleophobic composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a super-hydrophobic and oleophobic composite coating which comprises a super-hydrophobic and oleophobic primer coat layer and a super-hydrophobic and oleophobic finishing coat layer. The coating is characterized in that the super-hydrophobic and oleophobic finishing coat layer is located on the super-hydrophobic and oleophobic primer coat layer; the super-hydrophobic and oleophobic primer coat layer is coated by a super-hydrophobic and oleophobic primer coat which is a composition containing epoxy resin, an auxiliary A, extinction powder and a solvent; the super-hydrophobic and oleophobic finishing coat layer is coated by a super-hydrophobic and oleophobic finishing coat which is a composition containing fumed silica, an auxiliary B, an auxiliary C, a mixed solution A and a mixed solution B. Compared with the prior art, the super-hydrophobic and oleophobic composite coating disclosed by the invention not only has a super-hydrophobic performance, but also can resist greasy dirt and has a super-oleophobic performance as well as good wear resistance and stability; the preparation process is simple, and realization of industrialized production is facilitated.
Description
Technical field
The present invention relates to hydrophobic material field, specifically, relate to a kind of super-hydrophobic oleophobic compound coating and preparation method thereof.
Background technology
Super-hydrophobic phenomenon comes from the understanding of the mankind to lotus leaf effect in the Nature etc.Super hydrophobic surface refers to and is greater than 150 ° with water contact angle, and roll angle is lower than the surface of 10 °.Because water droplet keeps spherical on surface, and can Free-rolling landing when tilting small angle, take away the hydrophilic substances such as the dust on surface and earth, therefore super hydrophobic surface has excellent self-cleaning function.
The special surface wettability of super hydrophobic surface makes it be with a wide range of applications in automatically cleaning, waterproof, ice-covering-proof, the field such as protection against corrosion and fluid transport.Research shows, the formation of super hydrophobic surface is mainly determined by two factors: low-surface-energy material and micro-nano geometry roughness.Low-surface-energy material can give surface good hydrophobicity, and multi-level micro-nano geometry roughness can catch one deck air bag in solid-liquid interface, contributes to improving the contact angle of surface to water.Therefore, construct roughness or hydrophobization process is carried out to uneven surface can construct super hydrophobic surface at hydrophobic surface.But there is special micro nano structure due to super hydrophobic surface, when running into slight friction, these micro-nano structures are easily destroyed, and cause surface to lose ultra-hydrophobicity.Therefore the difficult point that good stability, wear-resisting super-hydrophobic coat or surface become research is prepared.Chinese invention patent application CN 104327703 A discloses a kind of preparation method of wear-resistant compound super-hydrophobic coat.By composite to urethane, epoxy resin and amido silicon oil, phase disengagement method is utilized to prepare the compound super-hydrophobic coat with the porous of micro-convex structure.But the method needs synthesis of polyurethane colloidal sol, and technique is more loaded down with trivial details, need set time long.And this coating oil-proofness is poor, easily by oil pollution, ultra-hydrophobicity is caused to be destroyed.
Summary of the invention
For prior art super hydrophobic material poor stability, not wear-resistant and not resistance to wet goods defect, the invention provides a kind of good stability, oil resistant and super-hydrophobic oleophobic compound coating having excellent abrasive resistance concurrently and preparation method thereof.
The present invention is achieved through the following technical solutions: a kind of super-hydrophobic oleophobic compound coating, comprise super-hydrophobic oleophobic prime coat and super-hydrophobic oleophobic top coat layer, it is characterized in that, described super-hydrophobic oleophobic top coat layer is positioned at super-hydrophobic oleophobic primer layer, described super-hydrophobic oleophobic prime coat is coated with by super-hydrophobic oleophobic priming paint to form, super-hydrophobic oleophobic priming paint comprises 5wt% ~ 20wt% epoxy resin, 0.2wt% ~ 2wt% auxiliary agent A, 0.5wt% ~ 10wt% flatting silica, the composition of 70wt% ~ 90wt% solvent, described super-hydrophobic oleophobic top coat layer is coated with by super-hydrophobic oleophobic finish paint and forms, super-hydrophobic oleophobic finish paint comprises 0.5wt% ~ 5wt% aerosil, 0.05wt% ~ 5wt% auxiliary agent B, 0.2wt% ~ 2wt% auxiliary agent C, 80wt% ~ 98wt% mixed solution A, the composition of 0.5wt% ~ 10wt% mixing solutions B.
Described auxiliary agent A is the one in the silane coupling agent of band epoxy group(ing).
Described flatting silica adopts micron silica, and silicon-dioxide particle diameter is 1 ~ 50 μm.
Described solvent is ketones solvent.
Described aerosil particle diameter is 10nm ~ 100nm.
Described auxiliary agent B is fluorinated silane coupling agent, and described fluorinated silane coupling agent is the one in 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane or ten difluoro heptyl propyl trimethoxy silicanes.
Described auxiliary agent C is the one in the silane coupling agent of band amino.
Described mixed solution A is ethanol water, and the mass ratio of ethanol and water is 10:1 ~ 1:1.
Described mixing solutions B is acetic acid water, and the massfraction of acetic acid aqueous solution is 0.5wt% ~ 10wt%.
The preparation method of super water water oleophobic compound coating of the present invention is as follows:
Step one, prepares super-hydrophobic oleophobic priming paint: at room temperature, and 5wt% ~ 20wt% epoxy resin, 0.2wt% ~ 2wt% auxiliary agent A, 0.5wt% ~ 10wt% flatting silica are joined in 70wt% ~ 90wt% solvent, on homogenizer, high-speed mixing is even;
Step 2, prepare super-hydrophobic oleophobic finish paint: be dispersed in by 0.5wt% ~ 5wt% aerosil in 80wt% ~ 98wt% mixed solution A, ultrasonic mix after, add 0.05wt% ~ 5wt% auxiliary agent B and 0.2wt% ~ 2wt% auxiliary agent C, drip 0.5wt% ~ 10wt% mixing solutions B again, obtain silica dispersions, silica dispersions being moved to reflection temperature is in the reactor of 40 ~ 70 DEG C, reflection 6 ~ 10h, obtains super-hydrophobic oleophobic finish paint;
Step 3, adopts spraying coating process, the super-hydrophobic oleophobic priming paint on base material obtained by spraying process one, moves to 15min ~ 20min in 120 DEG C ~ 150 DEG C baking ovens and dries; Then be cooled to room temperature, spray the finish paint of super-hydrophobic super oleophobic coating, move to 15min ~ 20min in 150 DEG C of baking ovens dry, obtain super-hydrophobic super oleophobic coating.
Described base material is stainless steel wire drawing plate or stainless steel mirror board.
Compared with prior art, tool has the following advantages in the present invention:
(1) the super-hydrophobic oleophobic compound coating that the present invention prepares gained is composited by super-hydrophobic oleophobic top coat layer and super-hydrophobic oleophobic prime coat, the combination of silane coupling agent and silicon-dioxide, the surface energy of coating can be reduced, thus significantly improve the hydrophobic oleophobic performance of coating, prepared compound coating is greater than 150 ° with the contact angle of water droplet, while with the contact angle of oil droplet at about 150 °, this compound coating not only has ultra-hydrophobicity, and energy oil rub resistance, have super oleophobic performance concurrently.
(2) the super-hydrophobic super oleophobic coating prepared by the present invention and the adhesive property between base material good, this compound coating has good wear resistance and stability simultaneously;
(3) preparation technology is simple, is conducive to realizing suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the contact angle picture of the super-hydrophobic oleophobic compound coating of the present invention and water droplet;
Fig. 2 is the contact angle picture of the super-hydrophobic oleophobic compound coating of the present invention and peanut oil oil droplet.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the present invention is further illustrated.
A kind of super-hydrophobic oleophobic compound coating, comprise super-hydrophobic oleophobic prime coat and super-hydrophobic oleophobic top coat layer, described super-hydrophobic oleophobic top coat layer is positioned at super-hydrophobic oleophobic primer layer, described super-hydrophobic oleophobic prime coat is coated with by super-hydrophobic oleophobic priming paint to form, super-hydrophobic oleophobic priming paint comprises 5wt% ~ 20wt% epoxy resin, 0.2wt% ~ 2wt% epoxy silane coupling, 0.5wt% ~ 10wt% flatting silica, the composition of 70wt% ~ 90wt% ketones solvent, described super-hydrophobic oleophobic top coat layer is coated with by super-hydrophobic oleophobic finish paint and forms, super-hydrophobic oleophobic finish paint comprises 0.5wt% ~ 5wt% aerosil, 0.05wt% ~ 5wt% fluorinated silane coupling agent, 0.2wt% ~ 2wt% amino silicane coupling agent, 80wt% ~ 98wt% aqueous ethanolic solution, the composition of 0.5wt% ~ 10wt% acetic acid aqueous solution.
Described epoxy silane coupling adopts the one in 3-glycydoxy Trimethoxy silane, 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane.
Described fluorinated silane coupling agent adopts the one in 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane, ten difluoro heptyl propyl trimethoxy silicanes.
Described amino silicane coupling agent adopts the one in γ-aminopropyl triethoxysilane, diethylenetriamine base propyl trimethoxy silicane, N-(2-aminoethyl)-3-aminopropyl triethoxysilane.
A kind of preparation method of super-hydrophobic oleophobic compound coating is as follows:
Embodiment 1
The preparation of the super-hydrophobic oleophobic priming paint of step (1): under room temperature, the flatting silica being 3 μm by 10g epoxy resin, 1g 3-glycydoxy Trimethoxy silane and 2g particle diameter joins in 100g butanone, homogenizer adopt 1500r/min stir 30min, after mixing, obtain super-hydrophobic oleophobic priming paint;
The preparation of the super-hydrophobic oleophobic finish paint of step (2): after 90g ethanol is mixed with 10g water, add aerosil, 1g 17 fluorine decyl Trimethoxy silane, 1g γ-aminopropyl triethoxysilane that 1g particle diameter is 16nm, homogenizer adopt 1500r/min stir 30min, drip 10wt% acetic acid aqueous solution 2g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 8h that temperature is 65 DEG C, obtain super-hydrophobic oleophobic finish paint;
Step (3) adopts spraying coating process, and stainless steel wire drawing plate sprays super-hydrophobic oleophobic priming paint, and thickness is 6 ~ 10 μm, moves to 15min in 150 DEG C of baking ovens and dries; Then be cooled to room temperature, spray super-hydrophobic oleophobic finish paint, move to 15min in 150 DEG C of baking ovens dry, obtain super-hydrophobic oleophobic compound coating.
As shown in Figure 1 and Figure 2, water droplet and oil droplet keep spherical on compound coating surface, the surface of compound coating can not be soaked, by test, the contact angle of water droplet on compound coating surface is 156 °, the contact angle of oil droplet on compound coating surface is 150 °, illustrates that the compound coating prepared by the present invention has super-hydrophobic super oleophobic performance thus.
Embodiment 2
The preparation of the super-hydrophobic oleophobic priming paint of step (1): under room temperature, the flatting silica being 3 μm by 10g epoxy resin, 1g 3-glycydoxy Trimethoxy silane and 4g particle diameter joins in 100g butanone, homogenizer adopt 1500r/min stir 30min, after mixing, obtain super-hydrophobic oleophobic priming paint;
The preparation of the super-hydrophobic oleophobic finish paint of step (2): after 90g ethanol is mixed with 10g water, add aerosil, 2g 17 fluorine decyl Trimethoxy silane, 1g γ-aminopropyl triethoxysilane that 2g particle diameter is 16nm, homogenizer adopt 1500r/min stir 30min, drip 10wt% acetic acid aqueous solution 2g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 8h that temperature is 65 DEG C, obtain super-hydrophobic oleophobic finish paint;
Step (3) is with embodiment 1.
Prepared by the present embodiment, the contact angle of super-hydrophobic oleophobic compound coating and water is 154 °, is 151 ° with the contact angle of sesame oil.
Embodiment 3
The preparation of the super-hydrophobic oleophobic priming paint of step (1): under room temperature, by 10g epoxy resin, 1g2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane and 2g particle diameter be that the flatting silica of 6 μm joins in 100g butanone, homogenizer adopt 1500r/min stir 30min, after mixing, obtain super-hydrophobic oleophobic priming paint;
The preparation of the super-hydrophobic oleophobic finish paint of step (2): after 90g ethanol is mixed with 10g water, add aerosil, 1g ten trifluoro octyltri-ethoxysilane, 1g diethylenetriamine base propyl trimethoxy silicane that 1g particle diameter is 20nm, homogenizer adopt 1500r/min stir 30min, drip 10wt% acetic acid aqueous solution 2g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 8h that temperature is 65 DEG C, obtain super-hydrophobic oleophobic finish paint;
Step (3) is with embodiment 1.
Prepared by the present embodiment, the contact angle of super-hydrophobic oleophobic compound coating and water is 154 °, is 150 ° with the contact angle of lubricating oil.
Embodiment 4
The preparation of the super-hydrophobic oleophobic priming paint of step (1): under room temperature, by 15g epoxy resin, 2g 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane and 3g particle diameter be that the flatting silica of 8 μm joins in 100g acetone, homogenizer adopt 2000r/min stir 30min, after mixing, obtain super-hydrophobic oleophobic priming paint;
The preparation of the super-hydrophobic oleophobic finish paint of step (2): after 75g ethanol is mixed with 25g water, add aerosil, 2g ten difluoro heptyl propyl trimethoxy silicane, 1g N-(2-aminoethyl)-3-aminopropyl triethoxysilane that 1.5g particle diameter is 12nm, homogenizer adopt 2000r/min stir 30min, drip 5wt% acetic acid aqueous solution 5g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 10h that temperature is 70 DEG C, obtain super-hydrophobic oleophobic finish paint;
Step (3) adopts spraying coating process, and stainless steel mirror board sprays the priming paint of super-hydrophobic super oleophobic coating, and thickness is 6 ~ 10 μm, moves to 20min in 120 DEG C of baking ovens and dries; Then be cooled to room temperature, spray the finish paint of super-hydrophobic super oleophobic coating, move to 20min in 150 DEG C of baking ovens dry, obtain super-hydrophobic super oleophobic coating.
Prepared by the present embodiment, the contact angle of super-hydrophobic oleophobic compound coating and water is 158 °, is 151 ° with the contact angle of n-Hexadecane.
Embodiment 5
The preparation of step (1) priming paint: under room temperature, by 15g epoxy resin, 2g 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane and 5g particle diameter be that the flatting silica of 8 μm joins in 100g acetone, homogenizer adopt 2000r/min stir 30min, after mixing, obtain super-hydrophobic super oleophobic coating priming paint;
The preparation of step (2) finish paint: after 75g ethanol is mixed with 25g water, add aerosil, 2.5g ten difluoro heptyl propyl trimethoxy silicane, 1g N-(2-aminoethyl)-3-aminopropyl triethoxysilane that 3g particle diameter is 12nm, homogenizer adopt 2000r/min stir 30min, drip 5wt% acetic acid aqueous solution 5g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 10h that temperature is 70 DEG C, obtain super-hydrophobic super oleophobic tricoat finish;
Step (3) is with embodiment 4.
Prepared by the present embodiment, the contact angle of super-hydrophobic oleophobic compound coating and water is 155 °, is 149 ° with the contact angle of peanut oil.
Embodiment 6
The preparation of the super-hydrophobic oleophobic priming paint of step (1): under room temperature, by 15g epoxy resin, 2g 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane and 1.5g particle diameter be that the flatting silica of 20 μm joins in 100g acetone, homogenizer adopt 2000r/min stir 30min, after mixing, obtain super-hydrophobic oleophobic priming paint;
The preparation of the super-hydrophobic oleophobic finish paint of step (2): after 75g ethanol is mixed with 25g water, add aerosil, 1.5g 17 fluorine decyl Trimethoxy silane, 1g N-(2-aminoethyl)-3-aminopropyl triethoxysilane that 1g particle diameter is 60nm, homogenizer adopt 2000r/min stir 30min, drip 5wt% acetic acid aqueous solution 5g, move in 500ml four-hole boiling flask after mixing, be placed in the water-bath reacting by heating 10h that temperature is 70 DEG C, obtain super-hydrophobic oleophobic finish paint;
Step (3) is with embodiment 4.
The contact angle of the prepared super thin super oleophobic compound coating of the present embodiment and water is 152 °, is 147 ° with the contact angle of peanut oil.
The foregoing is only better embodiment of the present invention, the present invention is not limited to above-mentioned embodiment, the structural modification that local is small may be there is in implementation process, if do not depart from the spirit and scope of the present invention to various change of the present invention or modification, and belonging within claim of the present invention and equivalent technologies scope, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. a super-hydrophobic oleophobic compound coating, comprise super-hydrophobic oleophobic prime coat and super-hydrophobic oleophobic top coat layer, it is characterized in that, described super-hydrophobic oleophobic top coat layer is positioned at super-hydrophobic oleophobic primer layer, described super-hydrophobic oleophobic prime coat is coated with by super-hydrophobic oleophobic priming paint to form, super-hydrophobic oleophobic priming paint comprises 5wt% ~ 20wt% epoxy resin, 0.2wt% ~ 2wt% auxiliary agent A, 0.5wt% ~ 10wt% flatting silica, the composition of 70wt% ~ 90wt% solvent, described super-hydrophobic oleophobic top coat layer is coated with by super-hydrophobic oleophobic finish paint and forms, super-hydrophobic oleophobic finish paint comprises 0.5wt% ~ 5wt% aerosil, 0.05wt% ~ 5wt% auxiliary agent B, 0.2wt% ~ 2wt% auxiliary agent C, 80wt% ~ 98wt% mixed solution A, the composition of 0.5wt% ~ 10wt% mixing solutions B.
2. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described auxiliary agent A is the one in the silane coupling agent of band epoxy group(ing).
3. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described flatting silica adopts micron silica, and silicon-dioxide particle diameter is 1 ~ 50 μm.
4. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described solvent is ketones solvent.
5. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described aerosil particle diameter is 10nm ~ 100nm.
6. super-hydrophobic oleophobic compound coating according to claim 1, it is characterized in that: described auxiliary agent B is fluorinated silane coupling agent, described fluorinated silane coupling agent is the one in 17 fluorine decyl Trimethoxy silanes, ten trifluoro octyltri-ethoxysilane or ten difluoro heptyl propyl trimethoxy silicanes.
7. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described auxiliary agent C is the one in the silane coupling agent of band amino.
8. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described mixed solution A is ethanol water, the mass ratio of ethanol and water is 10:1 ~ 1:1.
9. super-hydrophobic oleophobic compound coating according to claim 1, is characterized in that: described mixing solutions B is acetic acid water, the massfraction of acetic acid aqueous solution is 0.5wt% ~ 10wt%.
10. the preparation method of a super water water oleophobic compound coating according to claim 1 is as follows:
Step one, prepares super-hydrophobic oleophobic priming paint: at room temperature, and 5wt% ~ 20wt% epoxy resin, 0.2wt% ~ 2wt% auxiliary agent A, 0.5wt% ~ 10wt% flatting silica are joined in 70wt% ~ 90wt% solvent, on homogenizer, high-speed mixing is even;
Step 2, prepare super-hydrophobic oleophobic finish paint: be dispersed in by 0.5wt% ~ 5wt% aerosil in 80wt% ~ 98wt% mixed solution A, ultrasonic mix after, add 0.05wt% ~ 5wt% auxiliary agent B and 0.2wt% ~ 2wt% auxiliary agent C, drip 0.5wt% ~ 10wt% mixing solutions B again, obtain silica dispersions, silica dispersions being moved to reflection temperature is in the reactor of 40 ~ 70 DEG C, reflection 6 ~ 10h, obtains super-hydrophobic oleophobic finish paint;
Step 3, adopts spraying coating process, the super-hydrophobic oleophobic priming paint on base material obtained by spraying process one, moves to 15min ~ 20min in 120 DEG C ~ 150 DEG C baking ovens and dries; Then be cooled to room temperature, spray the finish paint of super-hydrophobic super oleophobic coating, move to 15min ~ 20min in 150 DEG C of baking ovens dry, obtain super-hydrophobic super oleophobic coating.
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