CN104745052A - Preparation method of high-adhesive-force nanometer self-cleaning coating material - Google Patents
Preparation method of high-adhesive-force nanometer self-cleaning coating material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000004140 cleaning Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title abstract description 21
- 239000011248 coating agent Substances 0.000 title abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 230000032683 aging Effects 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims abstract description 9
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 9
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 9
- 239000008117 stearic acid Substances 0.000 claims abstract description 9
- -1 methane amide Chemical class 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 230000035484 reaction time Effects 0.000 claims description 16
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 239000013543 active substance Substances 0.000 claims description 8
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract 3
- 239000000243 solution Substances 0.000 abstract 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 abstract 2
- 235000019441 ethanol Nutrition 0.000 abstract 2
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract 1
- 229940043237 diethanolamine Drugs 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 239000004626 polylactic acid Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- PRPAGESBURMWTI-UHFFFAOYSA-N [C].[F] Chemical compound [C].[F] PRPAGESBURMWTI-UHFFFAOYSA-N 0.000 description 2
- 230000003749 cleanliness Effects 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
- C09D171/02—Polyalkylene oxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Landscapes
- Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a preparation method of a high-adhesive-force nanometer self-cleaning coating material and belongs to the technical field of coating materials. The method comprises the following steps: uniformly mixing ethyl alcohol, deionized water, formamide, tetraethoxysilane and butyl titanate to obtain a solution; adjusting the pH of the solution with acid to 1-2, performing reaction, performing aging after the reaction is over, drying the solution after the aging is over so as to obtain powder; enabling the powder to react in a sodium hydroxide aqueous solution, filtering out solid after the reaction is over, drying the solid, uniformly mixing the solid, stearic acid, glycerol and an ethylene-ethenol copolymer, and performing ball milling; and mixing the material obtained in the third step, ethyl alcohol, deionized water, N,N-dimethyl formamide, polyethylene glycol, polylactic acid, diethanol amine, aluminum sol and a surfactant, and then performing high-speed dispersion to obtain the coating material.
Description
Technical field
The present invention discloses a kind of preparation method of Nano self-cleaning coated material of high adhesive force, belongs to technical field of coatings.
Background technology
The curtain wall materials such as fluorine carbon aluminium sheet, glass curtain wall, because it is ornamental by force, factorial praluction, in-site installation are convenient, easily change the advantages such as recovery, obtains and apply more and more widely in decorating outer wall of building.But along with the aggravation of city environmental pollution, the pollution of decorative curtain wall material also aggravates thereupon.In order to ensure the ornamental of curtain wall material, the cost needed for cleaning building curtain wall also constantly increases, as needed to consume a large amount of water and human cost.Meanwhile, building maintain cleanliness industry is an emerging multi-disciplinary technical field, and it contains the application (as Dry ice cleaning, laser cleaning, vacuum cleaned, anhydrous cleaning etc.) of the subject knowledges such as chemistry, physics, machinery, biology.Along with the reach of science, New Building Materials constantly come out in recent years, and are widely used on the decoration of exterior wall of building, thus add cleaning difficulty, propose new challenge to traditional maintain cleanliness, maintenance process.Nano-titanium oxide coating layer not only has self-cleaning, and effectively can block ultraviolet and directly act on the Color paints such as exposure curtain wall in the sun, billboard, slows down it and to fade and long-term not easily aging, allow buildings keep pure and fresh beautiful.
Automatic cleaning coating itself is transparent, can support the use with fluorine carbon, glass, ceramic coating etc., adopt online production mode, self-cleaning coating is sprayed at outside surface, stable coatings will be formed on curtain wall surface after elevated cure, the coating formed under normal circumstances is water white stealthy coating, can not have an impact to the color of lower floor's decorative paint.For also can in-situ spraying time supporting with marble, emulsion paint, normal temperature self-drying.
Invention CN102898875A discloses a kind of nano self-cleaning antimicrobial coating liquid and application, and this coating solution is a kind of ethanolic soln, includes the TiO that particle diameter is less than 50nm
2particle, and the new element such as V, Cr, can be converted into TiO visible ray, infrared rays
2exciting light, reach nano-antibacterial film with or without the object that all can work under light conditions.Invention CN103922802A relates to super hydrophilic Zinc oxide/titanium dioxide composite nanostructure automatic cleaning coating of a kind of transmission increasing and preparation method thereof.The present invention adopts the method for hydro-thermal to grow the ZnO nanowire array structural membrane of one deck 300-800 nanometer at substrate surface, then at surface growth one deck TiO of ZnO
2nano flake.Owing to there is a large amount of space between nano wire dot matrix, thus this film has certain anti-reflection characteristic.Its transmitance brings up to more than 85% from 80% of substrate.The introducing of titanium dioxide layer causes the contact angle of zinc oxide nano-wire array to be reduced to about 10 ° from original 60 °.But some problems that above-mentioned coating exists are that the sticking power between coating and glass baseplate is not high, there will be the problem of coating shedding after life-time service.
Summary of the invention
Technical problem to be solved by this invention is: the sticking power between titanium oxide self-stip coating and glass baseplate is not high, mainly realizes by carrying out improvement to the sol gel process in preparation process.
Technical scheme:
A preparation method for the Nano self-cleaning coated material of high adhesive force, comprises the steps:
1st step, by weight, ethanol 20 ~ 40 parts, deionized water 5 ~ 10 parts, methane amide 2 ~ 4 parts, tetraethyl orthosilicate 5 ~ 10 parts, butyl (tetra) titanate 5 ~ 10 parts to be mixed;
2nd step, with acid the pH of solution is adjusted to 1 ~ 2, reaction, after reaction terminates, ageing, after ageing terminates, by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 50 ~ 90 parts in powder, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 10 ~ 15 parts, glycerine 5 ~ 10 parts, ethylene-vinyl alcohol copolymer 1 ~ 3 part, carry out ball milling;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 30 ~ 40 parts, deionized water 15 ~ 25 parts, N, dinethylformamide 6 ~ 12 parts, polyoxyethylene glycol 7 ~ 14 parts, poly(lactic acid) 4 ~ 7 parts, diethanolamine 5 ~ 10 parts, Alumina gel 7 ~ 10 parts, the mixing of 2 ~ 4 parts, tensio-active agent, and then carry out high speed dispersion, obtain coated material.
In the 2nd described step, the reaction times is 12 ~ 36 hours, and temperature of reaction is 40 ~ 60 DEG C.
In the 2nd described step, the temperature of ageing is 20 ~ 30 DEG C, and the time of ageing is 100 ~ 200 hours.
In the 3rd described step, the concentration of aqueous sodium hydroxide solution is 25 ~ 30wt%, and the reaction times is 1 ~ 2 hour, and temperature of reaction is 30 ~ 45 DEG C.
In the 3rd described step, ball milling step carries out in planetary ball mill, rotating speed 180 ~ 220r/min, ball milling 20 ~ 30h.
In the 4th described step, the stirring velocity in the step of high speed dispersion is 2000 ~ 2500r/min.
In the 4th described step, the solid content of Alumina gel is 20%.
beneficial effect
The present invention by introducing monox nanometer particle in the preparation process of titanium oxide sol, make silicon oxide particle can form good network structure with titan oxide particles, next, again by corroding in sodium hydroxide solution titanium oxide/silicon oxide particle, micropore is formed on the surface of silicon oxide, by the process of ball milling, titan oxide particles is embedded in the surface imperfection of silicon oxide again, and then improves the sticking power of coating and base material.
Embodiment
Embodiment 1
1st step, ethanol 20g, deionized water 5g, methane amide 2g, tetraethyl orthosilicate 5g, butyl (tetra) titanate 5g to be mixed;
2nd step, with acid the pH of solution is adjusted to 1, reaction, the reaction times is 12 hours, and temperature of reaction is 40 DEG C, after reaction terminates, ageing, the temperature of ageing is 20 DEG C, and the time of ageing is 100 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 50g in powder, the concentration of aqueous sodium hydroxide solution is 25wt%, and the reaction times is 1 hour, and temperature of reaction is 30 DEG C, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 10g, glycerine 5g, ethylene-vinyl alcohol copolymer 1g, carry out ball milling, ball milling step carries out in planetary ball mill, rotating speed 180r/min, ball milling 20h;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 30g, deionized water 15g, N, dinethylformamide 6g, polyoxyethylene glycol 7g, poly(lactic acid) 4g, diethanolamine 5g, solid content be 20% Alumina gel 7g, tensio-active agent 2g mix, and then carry out 2000r/min high speed dispersion, obtain coated material.
Embodiment 2
1st step, ethanol 40g, deionized water 10g, methane amide 4g, tetraethyl orthosilicate 10g, butyl (tetra) titanate 10g to be mixed;
2nd step, with acid the pH of solution is adjusted to 2, reaction, the reaction times is 36 hours, and temperature of reaction is 60 DEG C, after reaction terminates, ageing, the temperature of ageing is 30 DEG C, and the time of ageing is 200 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 90g in powder, the concentration of aqueous sodium hydroxide solution is 30wt%, and the reaction times is 2 hours, and temperature of reaction is 45 DEG C, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 15g, glycerine 10g, ethylene-vinyl alcohol copolymer 3g, carry out ball milling, ball milling step carries out in planetary ball mill, rotating speed 220r/min, ball milling 30h;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 40g, deionized water 25g, N, dinethylformamide 12g, polyoxyethylene glycol 14g, poly(lactic acid) 7g, diethanolamine 10g, solid content be 20% Alumina gel 10g, tensio-active agent 4g mix, and then carry out 2500r/min high speed dispersion, obtain coated material.
Embodiment 3
1st step, ethanol 30g, deionized water 7g, methane amide 3g, tetraethyl orthosilicate 8g, butyl (tetra) titanate 8g to be mixed;
2nd step, with acid the pH of solution is adjusted to 1, reaction, the reaction times is 20 hours, and temperature of reaction is 50 DEG C, after reaction terminates, ageing, the temperature of ageing is 25 DEG C, and the time of ageing is 150 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 70g in powder, the concentration of aqueous sodium hydroxide solution is 28wt%, and the reaction times is 2 hours, and temperature of reaction is 40 DEG C, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 12g, glycerine 8g, ethylene-vinyl alcohol copolymer 2g, carry out ball milling, ball milling step carries out in planetary ball mill, rotating speed 200r/min, ball milling 25h;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 35g, deionized water 20g, N, dinethylformamide 7g, polyoxyethylene glycol 11g, poly(lactic acid) 5g, diethanolamine 7g, solid content be 20% Alumina gel 8g, tensio-active agent 3g mix, and then carry out 2000 ~ 2500r/min high speed dispersion, obtain coated material.
Reference examples 1
Be with the difference of embodiment 3: in the 3rd step, do not carry out ball-milling processing.
1st step, ethanol 30g, deionized water 7g, methane amide 3g, tetraethyl orthosilicate 8g, butyl (tetra) titanate 8g to be mixed;
2nd step, with acid the pH of solution is adjusted to 1, reaction, the reaction times is 20 hours, and temperature of reaction is 50 DEG C, after reaction terminates, ageing, the temperature of ageing is 25 DEG C, and the time of ageing is 150 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 70g in powder, the concentration of aqueous sodium hydroxide solution is 28wt%, reaction times is 2 hours, temperature of reaction is 40 DEG C, after reaction terminates, leach solid, carry out drying, after mixing with stearic acid 12g, glycerine 8g, ethylene-vinyl alcohol copolymer 2g again, obtain mixture;
4th step, the mixture that the 3rd step is obtained and ethanol 35g, deionized water 20g, N, dinethylformamide 7g, polyoxyethylene glycol 11g, poly(lactic acid) 5g, diethanolamine 7g, solid content be 20% Alumina gel 8g, tensio-active agent 3g mix, and then carry out 2000 ~ 2500r/min high speed dispersion, obtain coated material.
Reference examples 2
Be with the difference of embodiment 3: do not add Alumina gel.
1st step, ethanol 30g, deionized water 7g, methane amide 3g, tetraethyl orthosilicate 8g, butyl (tetra) titanate 8g to be mixed;
2nd step, with acid the pH of solution is adjusted to 1, reaction, the reaction times is 20 hours, and temperature of reaction is 50 DEG C, after reaction terminates, ageing, the temperature of ageing is 25 DEG C, and the time of ageing is 150 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 70g in powder, the concentration of aqueous sodium hydroxide solution is 28wt%, and the reaction times is 2 hours, and temperature of reaction is 40 DEG C, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 12g, glycerine 8g, ethylene-vinyl alcohol copolymer 2g, carry out ball milling, ball milling step carries out in planetary ball mill, rotating speed 200r/min, ball milling 25h;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 35g, deionized water 20g, N, dinethylformamide 7g, polyoxyethylene glycol 11g, poly(lactic acid) 5g, diethanolamine 7g, tensio-active agent 3g mix, and then carry out 2000 ~ 2500r/min high speed dispersion, obtain coated material.
Reference examples 3
Be with the difference of embodiment 3:: do not add ethylene-vinyl alcohol copolymer in the 3rd step.
1st step, ethanol 30g, deionized water 7g, methane amide 3g, tetraethyl orthosilicate 8g, butyl (tetra) titanate 8g to be mixed;
2nd step, with acid the pH of solution is adjusted to 1, reaction, the reaction times is 20 hours, and temperature of reaction is 50 DEG C, after reaction terminates, ageing, the temperature of ageing is 25 DEG C, and the time of ageing is 150 hours, after ageing terminates, and by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 70g in powder, the concentration of aqueous sodium hydroxide solution is 28wt%, and the reaction times is 2 hours, and temperature of reaction is 40 DEG C, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 12g, glycerine 8g, carry out ball milling, ball milling step carries out in planetary ball mill, rotating speed 200r/min, ball milling 25h;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 35g, deionized water 20g, N, dinethylformamide 7g, polyoxyethylene glycol 11g, poly(lactic acid) 5g, diethanolamine 7g, solid content be 20% Alumina gel 8g, tensio-active agent 3g mix, and then carry out 2000 ~ 2500r/min high speed dispersion, obtain coated material.
Performance test
Self-cleaning antireflecting coating material provided by the invention, in preparation section, leaves standstill after 24 hours, namely completes ageing, may be used for coating application.By the coated material of embodiment and reference examples gained after still aging 24 hours, adopt crystal pulling method film on K9 glass, the rate of pulling is 10cm ∕ min, can use after dry.
Table 1 transmittance test-results
| Substrate | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | Reference examples 3 | |
| Transmittance (1053 nm place) | 91.1% | 95.5% | 95.1% | 96.5% | 94.3% | 96.1% | 95.9% |
As can be seen from the table, after being applied with coated material provided by the invention, the transmittance of substrate has been improved, and due to the operation without ball milling in reference examples 1, result in transmittance and is also inferior to embodiment 3.
The sticking power of cross-hatching GB/T9286-1998 to coating is adopted to detect
Table 2 adhesion performance test-results
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | Reference examples 3 | |
| Sticking power | 0 grade | 0 grade | 0 grade | 1 grade | 0 grade | 0 grade |
As can be seen from the table, embodiment 3 adds the technique of ball milling relative to reference examples 1, improves sticking power.
The self-cleaning characteristic parameter of table 3
As can be seen from Table 3, coated material provided by the invention puts on after on substrate, and PARA FORMALDEHYDE PRILLS(91,95) has good degradation rate.In addition, after the irradiation of UV-light, the contact angle of substrate surface becomes about 1 ~ 2 DEG C from without about 72 DEG C when irradiating, and illustrates that it creates Decomposition for organism, can reduce organism remaining on surface.
Claims (7)
1. a preparation method for the Nano self-cleaning coated material of high adhesive force, is characterized in that, comprise the steps:
1st step, by weight, ethanol 20 ~ 40 parts, deionized water 5 ~ 10 parts, methane amide 2 ~ 4 parts, tetraethyl orthosilicate 5 ~ 10 parts, butyl (tetra) titanate 5 ~ 10 parts to be mixed;
2nd step, with acid the pH of solution is adjusted to 1 ~ 2, reaction, after reaction terminates, ageing, after ageing terminates, by drying materials, obtains powder;
3rd step, to react in aqueous sodium hydroxide solution 50 ~ 90 parts in powder, after reaction terminates, leach solid, carry out drying, then after mixing with stearic acid 10 ~ 15 parts, glycerine 5 ~ 10 parts, ethylene-vinyl alcohol copolymer 1 ~ 3 part, carry out ball milling;
4th step, by the material that obtains after the 3rd step ball milling and ethanol 30 ~ 40 parts, deionized water 15 ~ 25 parts, N, dinethylformamide 6 ~ 12 parts, polyoxyethylene glycol 7 ~ 14 parts, poly(lactic acid) 4 ~ 7 parts, diethanolamine 5 ~ 10 parts, Alumina gel 7 ~ 10 parts, the mixing of 2 ~ 4 parts, tensio-active agent, and then carry out high speed dispersion, obtain coated material.
2. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 2nd described step, the reaction times is 12 ~ 36 hours, and temperature of reaction is 40 ~ 60 DEG C.
3. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 2nd described step, and the temperature of ageing is 20 ~ 30 DEG C, and the time of ageing is 100 ~ 200 hours.
4. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 3rd described step, the concentration of aqueous sodium hydroxide solution is 25 ~ 30wt%, and the reaction times is 1 ~ 2 hour, and temperature of reaction is 30 ~ 45 DEG C.
5. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 3rd described step, and ball milling step carries out in planetary ball mill, rotating speed 180 ~ 220r/min, ball milling 20 ~ 30h.
6. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 4th described step, the stirring velocity in the step of high speed dispersion is 2000 ~ 2500r/min.
7. the preparation method of the Nano self-cleaning coated material of high adhesive force according to claim 1, is characterized in that: in the 4th described step, the solid content of Alumina gel is 20%.
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| CN105244768A (en) * | 2015-10-30 | 2016-01-13 | 国网山东省电力公司东营供电公司 | Waterproof power distribution cabinet for outdoor application |
| CN105885594A (en) * | 2016-06-27 | 2016-08-24 | 赵兰 | High-stability self-cleaning coating material and preparation method thereof |
| CN106594609A (en) * | 2016-12-14 | 2017-04-26 | 神州交通工程集团有限公司 | LED road lamp with self-cleaning capability |
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