CN103031008B - A kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer - Google Patents

A kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer Download PDF

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CN103031008B
CN103031008B CN201210529272.1A CN201210529272A CN103031008B CN 103031008 B CN103031008 B CN 103031008B CN 201210529272 A CN201210529272 A CN 201210529272A CN 103031008 B CN103031008 B CN 103031008B
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colloidal sol
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CN103031008A (en
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吴国阳
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Caihong Group New Energy Co ltd
Shaanxi Rainbow New Materials Co ltd
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Irico Group Electronics Co Ltd
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Abstract

A kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer, the alfol colloidal sol adopting organoaluminum to be hydrolyzed into and organoalkoxysilane mix with the colloidal sol of nano silicon dispersion liquid cohydrolysis under acidic catalyst, after mixing, make silica particles be coated with one deck sial alcohol glue, the coating process such as recycling roller coat, spraying, dip-coating method are coated with one deck TiO on the silicon-aluminum sol antireflective coating having cured film forming 2colloidal sol rete, due to TiO 2film has photochemical catalysis and photic Superhydrophilic, is adsorbed on TiO 2the organic pollutant of film surface can be degraded under solar light irradiation, and pollutent and dust can be fallen by rain-out, make TiO 2coatings has self-cleaning function, and because silanol glue and substrate glass surface have good cementability, alumina sol has excellent wear resistance, and the dispersiveness of silica dioxide granule, makes plated film rete have multi-pore structure, improve the transmitance of coating.

Description

A kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer
Technical field
The present invention relates to the preparing technical field of nano-coating colloidal sol, be specifically related to a kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer.
Background technology
One of reason of solar energy converting loss in efficiency is that glass surface exists the reflection loss of about 10% to incident sunlight, and therefore reducing the reflection of glass surface sunlight is the effective ways improving solar energy converting efficiency.The most simple effective method of one making glass have anti-reflection performance plates one or more layers film at glass surface exactly, utilizes the interference of film to disappear to reduce unnecessary reflection mutually, thus reaches antireflective effect.Compared with non-coated photovoltaic glass, the transmittance of coated glass can be anti-reflection in 380-2500nm broadband range, and transmittance is increased to 98% by original 91%.Traditional method adopts sol-gel method to prepare TiO respectively 2colloidal sol and SiO 2colloidal sol, then by TiO 2colloidal sol and SiO 2colloidal sol mixes plated film, although have self-cleaning function with film prepared by the method, optical transmittance is poor, does not have good anti-reflection performance.With Nano-meter SiO_2 prepared by this traditional method 2film porosity is large, surface energy is high, and the suspended substance easily in absorption surrounding environment, after using for some time, transmittance obviously declines, thus limits its practical application.Or adopt sol-gel method to be coated with one deck Nano-meter SiO_2 respectively at photovoltaic glass surface 2film and one deck nano-TiO 2film and obtain double-layer reflection-decreasing film, has self-cleaning function with double-layer reflection-decreasing film prepared by the method and antireflective effect is better, but coatings physical strength is lower, and burnish resistance is poor, and weathering resistance is poor, is not suitable for the application of field environment.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of antireflective plated film colloidal sol of self-cleaning high permeability bilayer, compared with the existing technology, the antireflective plated film sol-process of a kind of self-cleaning high permeability bilayer prepared with present method is simple, cost is low, structure-controllable, specific refractory power continuously adjustabe, have high transmitance at photovoltaic glass surface to visible ray, infrared light, coatings has excellent rub resistance, weathering resistance and self-cleaning function.
In order to achieve the above object, the technical solution used in the present invention is:
A preparation method for the antireflective plated film colloidal sol of self-cleaning high permeability bilayer, comprises the following steps:
The first step, prepare Alumina gel, first organoaluminum and pure water that mass percent is 5 ~ 11:89 ~ 95 is equipped with, then organoaluminum is dissolved in pure water, is warming up to 50 DEG C ~ 80 DEG C hydrolysis reaction, redistillation 0.5 ~ 2.5 hour after 1 ~ 3 hour, then 80 DEG C ~ 95 DEG C are warming up to, adjusting PH with acid is 2 ~ 5, and back flow reaction 10 ~ 24 hours, obtains Alumina gel;
Second step, prepare silicon sol, first by organoalkoxysilane and silica dispersions, alcohol mixture, pure water and stopper are equipped with according to following mass percent, organoalkoxysilane and silica dispersions: alcohol mixture: pure water: stopper is 15 ~ 30:53 ~ 83.5:0.8 ~ 6.8:0 ~ 10, wherein, the mass ratio of organoalkoxysilane and silica dispersions is 0.1 ~ 0.8:1, then part organoalkoxysilane and silica dispersions are dissolved in the mixed solvent of ethanol and glycerol, PH=2 ~ 4 are adjusted with acid, slowly pure water is added under abundant stirring, be heated to 25 DEG C ~ 80 DEG C, hydrolysis reaction 1 ~ 3 hour, add remainder organoalkoxysilane again, continue reaction and be cooled to room temperature after 4 ~ 12 hours, add the surplus materials such as stopper again and continue stirring 0.5 ~ 1 hour, obtain the silicon sol centered by nanometer silicon dioxide particle,
3rd step, preparation has the antireflective plated film colloidal sol of high permeability: the Alumina gel first the first step prepared, silicon sol prepared by second step, alcohol mixture, stopper and drying regulator are equipped with according to following mass percent, Alumina gel: silicon sol: alcohol mixture: stopper: drying regulator is 8.1 ~ 28.5:26.2 ~ 29.9:30.4 ~ 50:0.4 ~ 2.0:10 ~ 15, then after alcohol mixture adds silicon sol respectively and Alumina gel stirs 1 hour, stopper and drying regulator is added successively, stir and within 0.5 ~ 1 hour, namely obtain having the friction resistant performance of high permeability and the nano-silicon Alumina gel coating liquid of weather resistance excellence,
4th step, preparation has the TiO of self-cleaning function 2colloidal sol: first organic titanium, ethanol 1, pure water, ethanol 2, acetic acid and drying regulator are equipped with by following mass percent, organic titanium: ethanol 1: pure water: ethanol 2: acetic acid: drying is adjusted to 6 ~ 13:21 ~ 38:33 ~ 48:8 ~ 12:0.1 ~ 0.3:7 ~ 14, then organic titanium is slowly added in ethanol 1 solvent and also fully stir, slowly drip acetic acid again, fully stir to obtain solution A; Pure water is added in ethanol 2, fully stir to obtain solution B; Then solution B is slowly joined in solution A, adjust pH value to 2 ~ 5, fully stir 0.5 ~ 2 hour, be warming up to 60 DEG C ~ 90 DEG C reactions 1 ~ 2 hour, add drying regulator again after cooling to room temperature, stir room temperature after 1 ~ 2 hour and leave standstill slaking 2 ~ 5 days, obtain TiO 2colloidal sol;
Organoaluminum described in the first step is the one of aluminum chloride, aluminum isopropylate, butoxy aluminium.
Acid described in the first step, second step is one or more in nitric acid, sulfuric acid, hydrochloric acid, if multiple, is for arbitrarily than mixing.
Second step and the alcohol mixture described in the 3rd step are multiple in ethanol, Virahol, glycerol, butanols, ethylene glycol or polyoxyethylene glycol, if multiple, are for arbitrarily than mixing.
Macrobead SiO in silica dispersions described in second step 2: small-particle SiO 2mass ratio is 0.1 ~ 0.8:1.
Organoalkoxysilane described in second step is one or more of tetraethoxysilane (TEOS), tetramethoxy-silicane, Union carbide A-162, dimethyldiethoxysilane or diphenyl diethoxy silane, if multiple, be for arbitrarily than mixing.
Stopper described in 3rd step is one or more of N methyl-2-pyrrolidone, methane amide or dimethyl formamide, if multiple, is for arbitrarily than mixing.
3rd step and the drying regulator described in the 4th step are propylene glycol monomethyl ether, butyl glycol ether, ethylene glycol ethyl ether, dipropylene glycol methyl ether, glycol ether ether, 1, one or more of 2 hexylene glycols, if multiple, are for arbitrarily than mixing.
Organic titanium described in 4th step is the one of butyl (tetra) titanate (four titanium butoxide) or titanium isopropylate.
The invention has the beneficial effects as follows that point 2 steps carry out plated film:
Step one: organoaluminum is hydrolyzed one step ahead and forms alfol colloidal sol, then, organoalkoxysilane and nano silicon dispersion liquid cohydrolysis under acidic catalyst.After two kinds of colloidal sol mixing, silica particles is made to be coated with one deck sial alcohol glue.The technique such as rolling method, dip-coating method is adopted first to be coated with one deck nano-silicon Alumina gel coatings at glass surface.Because silanol glue and base material (glass) surface have good cementability, alumina sol has excellent wear resistance, therefore, silica dioxide granule and the existing good cementability of coated base material (glass), have again good wear resistance.Meanwhile, due to the dispersiveness of silica dioxide granule, make plated film rete have multi-pore structure, improve the transmitance of coating.
Step 2: the coating process such as recycling roller coat, spraying, dip-coating method are coated with one deck TiO on the silicon-aluminum sol antireflective coating having cured film forming 2colloidal sol rete.TiO 2the self-cleaning function of film derives from two aspects: photochemical catalysis and photic Superhydrophilic, be namely adsorbed on TiO 2the organic pollutant of film surface can be degraded under solar light irradiation, subsequently, due to TiO 2the photic Superhydrophilic of film, pollutent and dust can be fallen by rain-out, make TiO 2coatings has self-cleaning function.
Embodiment
With specific embodiment, present method is further described below.
Embodiment one:
1. Alumina gel preparation
Sequence number Component W％
1 AlCl 3 10.19
2 Pure water 89.81
In there-necked flask, add 2 and 1 respectively, be warming up to 55 DEG C after fully stirring, react after 1 hour uncovered distillation again 1 hour, be warming up to 85 DEG C, slowly drip acid, make PH=2 ~ 5, back flow reaction 12 hours must Alumina gel;
2. silicon sol preparation
Sequence number Component Weight
1 Tetraethoxysilane 1.17
2 Dimethyldiethoxysilane 0.83
3 10～30nmSiO 2Dispersion liquid 7.40
4 30～80nmSiO 2Dispersion liquid 5.92
5 Pure water 0.81
6 Ethanol 56.67
7 Glycerol 2.00
8 Virahol 21.70
9 Polyoxyethylene glycol 3.00
10 Dimethyl formamide 0.5
Add in the mixed solvent of 6 and 7 by 1, stir, then add 3 and 4 lentamente respectively, abundant stirring, adjusts PH=2 ~ 4, fully stirs and slowly drips 5, react at 80 DEG C after 2 hours and add 2 again, continue stirring reaction at 80 DEG C 8 hours, under room temperature, add 8,9 and 10, stir 30 minutes to obtain silicon sol;
3. there is the antireflective plated film colloidal sol preparation of high permeability
Sequence number Component W％
1 Silicon sol 26.15
2 Alumina gel 28.41
3 Ethanol 9.80
4 Virahol 17.64
5 Butanols 3.00
6 Propylene glycol monomethyl ether 4.20
7 1,2-hexylene glycol 3.60
8 Ethylene glycol ethyl ether 3.30
9 Dipropylene glycol methyl ether 3.50
10 N methyl-2-pyrrolidone 0.40
In 3 and 4, add 1, after stirring, slowly add 2, stir and add 5,6,7,8,9,10 successively after 1 hour and stir, the two component high permeability coating liquid of concrete dynamic modulus must be had;
4. there is the TiO of self-cleaning function 2prepared by colloidal sol
Sequence number Component W％
1 Butyl (tetra) titanate 6.39
2 Pure water 33.80
3 Ethanol 1 8.65
4 Ethanol 2 33.06
5 1,2 hexylene glycols 4.00
6 Propylene glycol monomethyl ether 8.00
7 Ethylene glycol ethyl ether 6.00
8 Acetic acid 0.10
In Erlenmeyer flask, put into 3, then add 1, fully stir, then slowly drip 8 and obtain solution A; In another Erlenmeyer flask, add 2 and 4, stir to obtain solution B.Adjust PH=2 ~ 5 with acid, in solution A, slowly add solution B under fully stirring, stir after 0.5 hour, be warming up to 65 DEG C, stirring reaction 2 hours, adds 5,6,7 under room temperature successively, stirs and leaves standstill the TiO must for 3 days with self-cleaning function again in 1.5 hours 2colloidal sol;
5. result of implementation:
Viscosity Transmitance % Salt spray resistance Scratch resistance Self-cleaning function
2.08 2.03％ Qualified ≥3H Good
Embodiment two:
1. Alumina gel preparation
Sequence number Component W％
1 Aluminum isopropylate 7.03
2 Pure water 92.97
In there-necked flask, add 2 and 1 respectively, be warming up to 80 DEG C after fully stirring, react after 2 hours uncovered distillation again 2 hours, be warming up to 92 DEG C, slowly drip acid, make PH=2 ~ 5, back flow reaction 20 hours must Alumina gel;
2. silicon sol preparation
Sequence number Component Weight
1 Tetraethoxysilane 3.89
2 Dimethyldiethoxysilane 2.77
3 10～30nmSiO 2Dispersion liquid 8.87
4 30～80nmSiO 2Dispersion liquid 4.44
5 Pure water 2.69
6 Ethanol 45.83
7 Glycerol 2.00
8 Virahol 21.52
9 Polyoxyethylene glycol 3.00
10 N methyl-2-pyrrolidone 3.07
11 Dimethyl formamide 1.93
First add 1 in the mixed solvent of 6 and 7, stir, then add 3 and 4 lentamente respectively, abundant stirring, adjusts PH=2 ~ 4, fully stirs and slowly drips 5, react at 70 DEG C after 2 hours and add 2 again, continue stirring reaction at 70 DEG C 10 hours, under room temperature, add 8,9,10 and 11, stir 30 minutes to obtain silicon sol;
3. there is the antireflective plated film colloidal sol preparation of high permeability
Sequence number Component W％
1 Silicon sol 28.53
2 Alumina gel 15.50
3 Ethanol 14.20
4 Virahol 24.97
5 Butanols 3.00
6 Propylene glycol monomethyl ether 3.80
7 1,2-hexylene glycol 3.20
8 Ethylene glycol ethyl ether 2.80
9 Dipropylene glycol methyl ether 3.0
10 Dimethyl formamide 0.40
11 N methyl-2-pyrrolidone 0.60
In 3 and 4, add 1, after stirring, slowly add 2, stir and add 5,6,7,8,9,10,11 successively after 1 hour and stir, the two component high permeability coating liquid of concrete dynamic modulus must be had;
4. there is the TiO of self-cleaning function 2prepared by colloidal sol
In Erlenmeyer flask, put into 3, then add 1, fully stir, then slowly drip 8 and obtain solution A; In another Erlenmeyer flask, add 2 and 4, stir to obtain solution B.Adjust PH=2 ~ 5 with acid, in solution A, slowly add solution B under fully stirring, stir after 0.5 hour, be warming up to 80 DEG C, stirring reaction 2 hours, adds 5,6,7 under room temperature successively, stirs and leaves standstill the TiO must for 3 days with self-cleaning function again in 1 hour 2colloidal sol;
5. result of implementation:
Viscosity Transmitance % Salt spray resistance Scratch resistance Self-cleaning function
2.24 2.46％ Qualified ≥3H Good
Embodiment three:
1. Alumina gel preparation
Sequence number Component W％
1 Aluminum isopropylate 5.37
2 Pure water 93.47
In there-necked flask, add 2 and 1 respectively, be warming up to 80 DEG C after fully stirring, react after 2 hours uncovered distillation again 2 hours, be warming up to 95 DEG C, slowly drip acid, make PH=2 ~ 5, back flow reaction 24 hours must Alumina gel.
2. silicon sol preparation
Sequence number Component Weight
1 Tetraethoxysilane 9.74
2 Dimethyldiethoxysilane 6.93
3 10～30nmSiO 2Dispersion liquid 11.58
4 30～80nmSiO 2Dispersion liquid 1.74
5 Pure water 6.73
6 Ethanol 30.53
7 Glycerol 2.00
8 Virahol 17.75
9 Polyoxyethylene glycol 3.00
10 N methyl-2-pyrrolidone 6.40
11 Dimethyl formamide 3.60
First join 1 in the mixed solvent of 6 and 7, stir, then add 3 and 4 lentamente respectively, abundant stirring, adjusts PH=2 ~ 4, fully stirs and slowly drips 5, react at 60 DEG C after 2 hours and add 4 again, continue stirring reaction at 60 DEG C 12 hours, under room temperature, add 8,9,10 and 11, stir 30 minutes to obtain silicon sol;
3. there is the antireflective plated film colloidal sol preparation of high permeability
Sequence number Component W％
1 Silicon sol 29.89
2 Alumina gel 8.12
3 Ethanol 19.00
4 Virahol 27.99
5 Butanols 3.00
6 Propylene glycol monomethyl ether 3.20
7 1,2-hexylene glycol 2.80
8 Ethylene glycol ethyl ether 2.00
9 Dipropylene glycol methyl ether 2.00
10 Dimethyl formamide 0.80
11 N methyl-2-pyrrolidone 1.20
In 3 and 4, add 1, after stirring, slowly add 2, stir and add 5,6,7,8,9,10,11 successively after 1 hour and stir, the two component high permeability coating liquid of concrete dynamic modulus must be had;
4. there is the TiO of self-cleaning function 2prepared by colloidal sol
Sequence number Component W％
1 Titanium isopropylate 12.45
2 Pure water 47.3
3 Ethanol 1 20.18
4 Ethanol 2 8.77
1,2 hexylene glycols 4.0
5 Propylene glycol monomethyl ether 4.0
6 Ethylene glycol ethyl ether 3.0
7 Acetic acid 0.3
In Erlenmeyer flask, put into 3, then add 1, fully stir, then slowly drip 8 and obtain solution A; In another Erlenmeyer flask, add 2 and 4, stir to obtain solution B.Adjust PH=2 ~ 5 with acid, in solution A, slowly add solution B under fully stirring, stir after 0.5 hour, be warming up to 80 DEG C, stirring reaction 2 hours, adds 5,6,7 under room temperature successively, stirs and leaves standstill the TiO must for 3 days with self-cleaning function again in 1 hour 2colloidal sol;
5. result of implementation:
Viscosity Transmitance % Salt spray resistance Scratch resistance Self-cleaning function
2.56 2.32％ Qualified ≥3H Good

Claims (9)

1. a preparation method for the antireflective plated film colloidal sol of self-cleaning high permeability bilayer, is characterized in that, comprise the steps:
The first step, prepare Alumina gel, first organoaluminum and pure water that mass percent is 5 ~ 11:89 ~ 95 is equipped with, then organoaluminum is dissolved in pure water, being warming up to the redistillation 0.5 ~ 2.5 hour after 1 ~ 3 hour of 50 DEG C ~ 80 DEG C hydrolysis reaction, being then warming up to 80 DEG C ~ 95 DEG C, is 2 ~ 5 with acid adjustment PH, back flow reaction 10 ~ 24 hours, obtains Alumina gel;
Second step, prepare silicon sol: first by organoalkoxysilane and silica dispersions, alcohol mixture, pure water and stopper are equipped with according to following mass percent, organoalkoxysilane and silica dispersions: alcohol mixture: pure water: stopper is 15 ~ 30:53 ~ 83.5:0.8 ~ 6.8:0 ~ 10, wherein, the mass ratio of organoalkoxysilane and silica dispersions is 0.1 ~ 0.8:1, then part organoalkoxysilane and silica dispersions are dissolved in the mixed solvent of ethanol and glycerol, PH=2 ~ 4 are adjusted with acid, slowly pure water is added under abundant stirring, be heated to 25 DEG C ~ 80 DEG C, hydrolysis reaction 1 ~ 3 hour, add remainder organoalkoxysilane again, continue reaction and be cooled to room temperature after 4 ~ 12 hours, add the surplus materials such as stopper again and continue stirring 0.5 ~ 1 hour, obtain the silicon sol centered by nanometer silicon dioxide particle,
3rd step, prepare the nano-coating colloidal sol of high permeability: the Alumina gel first the first step prepared, silicon sol prepared by second step, alcohol mixture, stopper and drying regulator are equipped with according to following mass percent, Alumina gel: silicon sol: alcohol mixture: stopper: drying regulator is 8.1 ~ 28.5:26.2 ~ 29.9:30.4 ~ 50:0.4 ~ 2.0:10 ~ 15, then after alcohol mixture adds silicon sol respectively and Alumina gel stirs 1 hour, stopper and drying regulator is added successively, stir and within 0.5 ~ 1 hour, namely obtain having the friction resistant performance of high permeability and the nano-silicon Alumina gel coating liquid of weather resistance excellence,
4th step, preparation has the TiO of self-cleaning function 2colloidal sol: first organic titanium, ethanol 1, pure water, ethanol 2, acetic acid and drying regulator are equipped with by following mass percent, organic titanium: ethanol 1: pure water: ethanol 2: acetic acid: drying is adjusted to 6 ~ 13:21 ~ 38:33 ~ 48:8 ~ 12:0.1 ~ 0.3:7 ~ 14, then organic titanium is slowly added in ethanol 1 solvent and also fully stir, the acetic acid slowly dripped again, fully stirs to obtain solution A; Pure water is added in ethanol 2, fully stir to obtain solution B; Then solution B is slowly joined in solution A, adjust pH value to 2 ~ 5, fully stir 0.5 ~ 2 hour, be warming up to 60 DEG C ~ 90 DEG C reactions 1 ~ 2 hour, add drying regulator again after cooling to room temperature, stir room temperature after 1 ~ 2 hour and leave standstill slaking 2 ~ 5 days, obtain TiO 2colloidal sol.
2. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, is characterized in that, the organoaluminum described in the first step is the one in aluminum chloride, aluminum isopropylate, butoxy aluminium.
3. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, is characterized in that, the acid described in the first step, second step is one or more in nitric acid, sulfuric acid, hydrochloric acid, if multiple, is then arbitrarily than mixing.
4. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, it is characterized in that, second step and the alcohol mixture described in the 3rd step are multiple in ethanol, Virahol, glycerol, butanols, ethylene glycol or polyoxyethylene glycol, if multiple, be for arbitrarily than mixing.
5. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, is characterized in that, macrobead SiO in the silica dispersions described in second step 2: small-particle SiO 2mass ratio is 0.1 ~ 0.8:1.
6. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, it is characterized in that, organoalkoxysilane described in second step is one or more of tetraethoxysilane, tetramethoxy-silicane, Union carbide A-162, dimethyldiethoxysilane or diphenyl diethoxy silane, if multiple; For arbitrarily than mixing.
7. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, it is characterized in that, stopper described in 3rd step is one or more of N methyl-2-pyrrolidone, methane amide or dimethyl formamide, if multiple, is for arbitrarily than mixing.
8. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, it is characterized in that, drying regulator described in 3rd step is propylene glycol monomethyl ether, butyl glycol ether, ethylene glycol ethyl ether, dipropylene glycol methyl ether, glycol ether ether or 1, one or more of 2 hexylene glycols, if multiple, be for arbitrarily than mixing.
9. the preparation method of the antireflective plated film colloidal sol of a kind of self-cleaning high permeability bilayer according to claim 1, is characterized in that, the organic titanium described in the 4th step is the one of butyl (tetra) titanate (four titanium butoxide) or titanium isopropylate.
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