CN110205019A - The preparation of micro-nano decorating liquid and super-hydrophobic surface coating - Google Patents

The preparation of micro-nano decorating liquid and super-hydrophobic surface coating Download PDF

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Publication number
CN110205019A
CN110205019A CN201910314273.6A CN201910314273A CN110205019A CN 110205019 A CN110205019 A CN 110205019A CN 201910314273 A CN201910314273 A CN 201910314273A CN 110205019 A CN110205019 A CN 110205019A
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solution
added
nano
micro
preparation
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胡征宇
蒋义锋
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Runner Xiamen Corp
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Runner Xiamen Corp
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04Polysiloxanes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention discloses the preparation method of micro-nano decorating liquid and super-hydrophobic surface coating, the preparation step of the super-hydrophobic surface coating is as follows: preparing micro-nano decorating liquid;Prepare low-surface-energy modification liquid;The modification of micro/nano level surface texture is carried out on product after cleaning;It is modified that low-surface-energy finally is carried out to the product after modification.Then the present invention is modified drop low-surface-energy to micro/nano level surface, so that product has super-hydrophobicity, so that its surface is easy to clean, and extends the decorative effect of product by constructing micro/nano level surface texture in product surface.

Description

The preparation of micro-nano decorating liquid and super-hydrophobic surface coating
Technical field
The present invention relates to the preparations of micro-nano decorating liquid and super-hydrophobic surface coating.
Background technique
The metallic luster for having product after plating or physical vapour deposition (PVD) is the promotion common technique of decorative effect, but Since product surface hydrophobicity is poor, spot is becomed easily infected by, surface is dirty after a period of use and is difficult to clean, while can send out Raw different degrees of corrosion, causes decorative effect to decline.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide micro-nano decorating liquid and super-hydrophobic surface coatings Preparation.
The present invention is achieved through the following technical solutions: a kind of preparation method of micro-nano decorating liquid, which is characterized in that step It is rapid as follows:
Step a: bridging property esters solvent and dehydrated alcohol are mixed, and obtain solution A;
Step b: by water, dense HNO3 is added in dehydrated alcohol, obtains solution B, wherein the water, dense HNO3 and anhydrous The volume ratio of ethyl alcohol is 0.4:0.25:5.8;
Step c: nano-oxide is added in solution B, obtains solution C, and the nano-oxide is TIO2 or SIO2
Step d: solution C and solution A are mixed, and obtain solution D;
Step e: being added dispersed alcoholic solvent in solution D, and sealing stirring obtains solution E;
Step f: dehydrated alcohol is added in solution E, obtains decorating liquid after mixing.
Preferably, the nanometer TIO2Or nanometer SIO2Diameter be 5~20 nanometers.
Preferably, the bridging property esters solvent includes tetra-n-butyl titanate and acrylate.
Preferably, the dispersibility alcoholic solvent includes polyethylene glycol and poly- propyl alcohol.
The present invention also provides a kind of preparation methods of super-hydrophobic surface coating, and steps are as follows:
Step 1: the product after cleaning being immersed in micro-nano decorating liquid prepared by above-mentioned steps, slow draw is carried out and modifies;
Step 2: later should treated product immerse in low-surface-energy modification liquid, taking-up is dried.
Preferably, it is modified to obtain the low-surface-energy by carrying out ultrasonic dissolution after silicon fluoride is added in ethanol solution Liquid.
Preferably, the silicon fluoride is triethoxy -1H, 13 fluoro n-octyl silane of 1H, 2H-.
Then the present invention is modified drop to micro/nano level surface by constructing micro/nano level surface texture in product surface Low-surface-energy so that its surface is easy to clean, and extends the decorative effect of product so that product has super-hydrophobicity.
Specific embodiment
The technical solution in inventive embodiments is clearly and completely described below, it is clear that described embodiment is only It is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, ordinary skill people Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
The step of surface covering of product of the invention, is as follows: preparing micro-nano decorating liquid;Prepare low-surface-energy modification liquid; The modification of micro/nano level surface texture is carried out on product after cleaning;Finally low-surface-energy is carried out to the product after modification to change Property.Wherein, which can be by being added 1~5 gram of silicon fluoride dissolution in 100~500 milliliters of ethanol solutions It is prepared.
Wherein, the bridging property esters solvent in following embodiment of the present invention includes but is not limited to tetra-n-butyl titanate, propylene Other bridging property esters such as acid esters;Dispersed alcoholic solvent includes but is not limited to other alcohols solvents such as polyethylene glycol, poly- propyl alcohol;It produces Product may include plastic material or metal material etc. other carry out the product decorated of surface treatment.In addition, the present invention is real Apply the nanometer TIO in example2With nanometer SIO2Diameter be preferably 5~20 nanometers.
Embodiment 1
One, the preparation step of micro-nano decorating liquid is as follows:
1) 8.2 milliliters of tetra-n-butyl titanate is added in 5.8 milliliters of dehydrated alcohol, obtains solution by ultrasonic treatment A;
2) by 0.4 milliliter of water, 0.25 milliliter of dense HNO3It is added in 5.8 milliliters of dehydrated alcohols, obtains solution B, wherein should Dense HNO3Refer to that mass fraction is 68% nitric acid;
3) by 0.98 gram of nanometer TIO2It is added in solution B, ultrasonic disperse obtains solution C;
4) solution C and solution A are mixed and stirred for 30 minutes, obtain solution D;
5) 0.3 gram of polyethylene glycol is added in solution D and obtains solution E after sealing stirring 24 hours;
6) add dehydrated alcohol to 200 milliliters in solution E, micro-nano decorating liquid is obtained after ultrasonic mixing.
Two, low-surface-energy modification liquid preparation step is as follows:
After 2 grams of 13 fluoro n-octyl silane of triethoxy -1H, 1H, 2H- are added in 200 milliliters of ethanol solutions, carry out Ultrasonic dissolution obtains the low-surface-energy modification liquid.
Three, the preparation of super-hydrophobic surface coating, steps are as follows:
1) treated that product immerses in above-mentioned micro-nano decorating liquid by clean, carry out it is slow draw modification, spontaneously dry, repeat 3 times;
2) will be immersed in low-surface-energy modification liquid through step 1 treated product after, in 1 point after take out and spontaneously dry.
Embodiment 2
One, the preparation step of micro-nano decorating liquid is as follows:
1) 6 milliliters of tetra-n-butyl titanate is added in 5 milliliters of dehydrated alcohol, obtains solution A by ultrasonic treatment;
2) by 0.4 milliliter of water, 0.25 milliliter of dense HNO3It is added in 5.8 milliliters of dehydrated alcohols, obtains solution B, wherein should Dense HNO3Refer to that mass fraction is 68% nitric acid;
3) by 0.7 gram of nanometer TIO2It is added in solution B, ultrasonic disperse obtains solution C;
4) solution C and solution A are mixed and stirred for 30 minutes, obtain solution D;
5) 0.3 gram of polyethylene glycol is added in solution D and obtains solution E after sealing stirring 24 hours;
6) add dehydrated alcohol to 200 milliliters in solution E, micro-nano decorating liquid is obtained after ultrasonic mixing.
Two, low-surface-energy modification liquid preparation step is as follows:
After 2 grams of 13 fluoro n-octyl silane of triethoxy -1H, 1H, 2H- are added in 200 milliliters of ethanol solutions, carry out Ultrasonic dissolution obtains the low-surface-energy modification liquid.
Three, the preparation of super-hydrophobic surface coating, steps are as follows:
1) treated that product immerses in above-mentioned micro-nano decorating liquid by clean, carry out it is slow draw modification, spontaneously dry, repeat 3 times;
2) will be immersed in low-surface-energy modification liquid through step 1 treated product after, in 1 point after take out and spontaneously dry.
Embodiment 3
One, the preparation step of micro-nano decorating liquid is as follows:
1) 8.2 milliliters of tetra-n-butyl titanate is added in 5.8 milliliters of dehydrated alcohol, obtains solution by ultrasonic treatment A;
2) by 0.4 milliliter of water, 0.25 milliliter of dense HNO3It is added in 5.8 milliliters of dehydrated alcohols, obtains solution B, wherein should Dense HNO3Refer to that mass fraction is 68% nitric acid;
3) by 0.64 gram of nanometer SIO2It is added in solution B, ultrasonic disperse obtains solution C;
4) solution C and solution A are mixed and stirred for 30 minutes, obtain solution D;
5) 0.3 gram of polyethylene glycol is added in solution D and obtains solution E after sealing stirring 24 hours;
6) add dehydrated alcohol to 600 milliliters in solution E, micro-nano decorating liquid is obtained after ultrasonic mixing.
Two, low-surface-energy modification liquid preparation step is as follows:
After 2 grams of 13 fluoro n-octyl silane of triethoxy -1H, 1H, 2H- are added in 200 milliliters of ethanol solutions, carry out Ultrasonic dissolution obtains the low-surface-energy modification liquid.
Three, the preparation of super-hydrophobic surface coating, steps are as follows:
1) treated that product immerses in above-mentioned micro-nano decorating liquid by clean, carry out it is slow draw modification, spontaneously dry, repeat 3 times;
2) will be immersed in low-surface-energy modification liquid through step 1 treated product after, in 1 point after take out and spontaneously dry.
Embodiment 4
One, the preparation step of micro-nano decorating liquid is as follows:
1) 6 milliliters of tetra-n-butyl titanate is added in 5 milliliters of dehydrated alcohol, obtains solution A by ultrasonic treatment;
2) by 0.4 milliliter of water, 0.25 milliliter of dense HNO3It is added in 5.8 milliliters of dehydrated alcohols, obtains solution B, wherein should Dense HNO3Refer to that mass fraction is 68% nitric acid;
3) by 0.5 gram of nanometer SIO2It is added in solution B, ultrasonic disperse obtains solution C;
4) solution C and solution A are mixed and stirred for 30 minutes, obtain solution D;
5) 0.3 gram of polyethylene glycol is added in solution D and obtains solution E after sealing stirring 24 hours;
6) add dehydrated alcohol to 600 milliliters in solution E, micro-nano decorating liquid is obtained after ultrasonic mixing.
Two, low-surface-energy modification liquid preparation step is as follows:
After 2 grams of 13 fluoro n-octyl silane of triethoxy -1H, 1H, 2H- are added in 200 milliliters of ethanol solutions, carry out Ultrasonic dissolution obtains the low-surface-energy modification liquid.
Three, the preparation of super-hydrophobic surface coating, steps are as follows:
1) treated that product immerses in above-mentioned micro-nano decorating liquid by clean, carry out it is slow draw modification, spontaneously dry, repeat 3 times;
2) will be immersed in low-surface-energy modification liquid through step 1 treated product after, in 1 point after take out and spontaneously dry.
By carrying out test discovery to product with super-hydrophobic surface coating of the above-described embodiment 1 into embodiment 4, pass through The water contact angle for crossing treated product can reach 152 °.Compared to product (the unmodified processing before being not handled by Product water contact angle be 91 °), the present invention is by constructing micro/nano level surface texture in product surface, then to micro-nano Grade surface is modified drop low-surface-energy, so that product has super-hydrophobicity, so that its surface is easy to clean, and extends product Decorative effect.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office Be limited to form disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations, modification and Environment, and can be changed within that scope of the inventive concept describe herein by the above teachings or related fields of technology or knowledge It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention In scope of protection of the claims.

Claims (9)

1. a kind of preparation method of micro-nano decorating liquid, which is characterized in that steps are as follows:
Step a: bridging property esters solvent and dehydrated alcohol are mixed, and obtain solution A;
Step b: by water, dense HNO3It is added in dehydrated alcohol, obtains solution B, wherein the water, dense HNO3With dehydrated alcohol Volume ratio is 0.4:0.25:5.8;
Step c: nano-oxide is added in solution B, obtains solution C, and the nano-oxide is TIO2Or SIO2
Step d: solution C and solution A are mixed, and obtain solution D;
Step e: being added dispersed alcoholic solvent in solution D, and sealing stirring obtains solution E;
Step f: dehydrated alcohol is added in solution E, obtains decorating liquid after mixing.
2. the preparation method of micro-nano decorating liquid according to claim 1, which is characterized in that steps are as follows:
Step a: the bridging property esters solvent of 6~8.2 parts by volume being added in the dehydrated alcohol of 5~5.8 parts by volume, obtains solution A;
Step b: by water, dense HNO3It is added in dehydrated alcohol, obtains solution B, wherein the water, dense HNO3With dehydrated alcohol Volume ratio is 0.4:0.25:5.8;
Step c: by the nanometer TIO of 0.7~0.98 parts by weight2It is added in solution B, obtains solution C;
Step d: solution C and solution A are mixed, and obtain solution D;
Step e: being added the dispersed alcoholic solvent of 0.3 parts by weight in solution D, and sealing stirring obtains solution E;
Step f: in solution E plus dehydrated alcohol is to 200 parts by volume, obtains decorating liquid after mixing.
3. the preparation method of micro-nano decorating liquid according to claim 1, which is characterized in that steps are as follows:
Step a: the bridging property esters solvent of 6~8.2 parts by volume being added in the dehydrated alcohol of 5~5.8 parts by volume, obtains solution A;
Step b: by water, dense HNO3It is added in dehydrated alcohol, obtains solution B, wherein the water, dense HNO3With dehydrated alcohol Volume ratio is 0.4:0.25:5.8;
Step c: by the nanometer SIO of 0.5~0.64 parts by weight2It is added in solution B, obtains solution C;
Step d: solution C and solution A are mixed, and obtain solution D;
Step e: being added the dispersed alcoholic solvent of 0.3 parts by weight in solution D, and sealing stirring obtains solution E;
Step f: in solution E plus dehydrated alcohol is to 600 parts by volume, obtains decorating liquid after mixing.
4. the preparation method of micro-nano decorating liquid according to claim 1, which is characterized in that the nanometer TIO2Or nanometer SIO2Diameter be 5~20 nanometers.
5. the preparation method of micro-nano decorating liquid according to claim 1, which is characterized in that the bridging property esters solvent Including tetra-n-butyl titanate and acrylate.
6. the preparation method of micro-nano decorating liquid according to claim 1, which is characterized in that the dispersibility alcoholic solvent packet Include polyethylene glycol and poly- propyl alcohol.
7. a kind of preparation method of super-hydrophobic surface coating, which is characterized in that steps are as follows:
Step 1: the product after cleaning being immersed in any micro-nano decorating liquid of the claims 1-6, is drawn slowly Modification;
Step 2: later should treated product immerse in low-surface-energy modification liquid, taking-up is dried.
8. the preparation method of super-hydrophobic surface coating according to claim 7, which is characterized in that
By carrying out ultrasonic dissolution after silicon fluoride is added in ethanol solution, the low-surface-energy modification liquid is obtained.
9. the preparation method of super-hydrophobic surface coating according to claim 8, which is characterized in that the silicon fluoride is three second 13 fluoro n-octyl silane of Oxy-1 H, 1H, 2H-.
CN201910314273.6A 2019-04-18 2019-04-18 The preparation of micro-nano decorating liquid and super-hydrophobic surface coating Pending CN110205019A (en)

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Publication number Priority date Publication date Assignee Title
US20150072171A1 (en) * 2013-09-12 2015-03-12 Sri Lanka Institute of Nanotechnology (Pvt) Ltd. Hydrophobic surface treatment compositions comprising titanium precursors
CN104441127A (en) * 2014-11-18 2015-03-25 中南林业科技大学 Super-hydrophobic wood and preparation method thereof
CN105038439A (en) * 2015-08-18 2015-11-11 东北石油大学 Superhydrophobic composite coating with self-repair function and preparation method thereof
CN105906375A (en) * 2016-04-20 2016-08-31 长沙学院 Preparation method of transparent mesoporous titanium dioxide hydrophobic/ultra-hydrophilic functional thin film
CN107083545A (en) * 2017-05-22 2017-08-22 厦门建霖健康家居股份有限公司 One Albatra metal chromium-free passivation liquid
CN109111129A (en) * 2018-08-09 2019-01-01 华南理工大学 A kind of preparation method of super-hydrophobic automatic cleaning glass

Patent Citations (6)

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Publication number Priority date Publication date Assignee Title
US20150072171A1 (en) * 2013-09-12 2015-03-12 Sri Lanka Institute of Nanotechnology (Pvt) Ltd. Hydrophobic surface treatment compositions comprising titanium precursors
CN104441127A (en) * 2014-11-18 2015-03-25 中南林业科技大学 Super-hydrophobic wood and preparation method thereof
CN105038439A (en) * 2015-08-18 2015-11-11 东北石油大学 Superhydrophobic composite coating with self-repair function and preparation method thereof
CN105906375A (en) * 2016-04-20 2016-08-31 长沙学院 Preparation method of transparent mesoporous titanium dioxide hydrophobic/ultra-hydrophilic functional thin film
CN107083545A (en) * 2017-05-22 2017-08-22 厦门建霖健康家居股份有限公司 One Albatra metal chromium-free passivation liquid
CN109111129A (en) * 2018-08-09 2019-01-01 华南理工大学 A kind of preparation method of super-hydrophobic automatic cleaning glass

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