CN107057549B - A kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning - Google Patents
A kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning Download PDFInfo
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- CN107057549B CN107057549B CN201710393289.1A CN201710393289A CN107057549B CN 107057549 B CN107057549 B CN 107057549B CN 201710393289 A CN201710393289 A CN 201710393289A CN 107057549 B CN107057549 B CN 107057549B
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- 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
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- C08K2003/2241—Titanium dioxide
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Abstract
A kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning of the invention is raw material with titanium tetrachloride, tin oxide, antimony chloride, hydrogen peroxide is oxidant, citric acid is auxiliary agent, and dodecyl sodium sulfate is surfactant, and TiO is prepared using the method for co-precipitation and hydro-thermal2/ ATO compound function nano powder, using aqueous polyurethane as film forming matter, pass through silane coupling agent, it is aided with chelating dispersing agent dispersion, in conjunction with high speed shear dispersion and ultrasonic disperse, coating obtained not only has good filming performance, and there are also higher infrared barrier performance, visible light transmittance and superhydrophilic self-cleaning performances.
Description
Technical field
The present invention relates to insulating moulding coating technical fields, heat-insulated more particularly to a kind of high-transparent glass of superhydrophilic self-cleaning
The preparation method of coating.
Background technique
Currently, the energy-saving heat-insulating product for comparing mainstream has a membrane plating heat-reflection glass, and vacuum glass, hollow glass etc., but this
A little insulation products fail to solve glass surface heat-insulating problem very well all there is different problems.In recent years, insulating moulding coating is because of it
The performance of higher visible light transmittance and selectively masking infrared light and ultraviolet light and be concerned.Authorization Notice No. is CN
The Chinese invention patent of 102876197 B discloses a kind of glass coating with thermal-insulation, self-cleaning function, mainly by forming a film
The groups such as resin, nanometer antimony-doped stannic oxide (ATO) powder, nano TiO 2 powder, dispersing agent, coalescing agent are grouped as.Wherein receive
Rice ATO ~ TiO2The preparation method of composite mortar is to take prior art routine operation, by nano ATO powder, titanium dioxide powder
Grain, distilled water and dispersing agent carry out grinding distribution, further disperse after then reconciling pH value, this method is by nano antimony doped two
Tin oxide (ATO) powder and nano-TiO2Powder is directly simply mixed, the ATO ~ TiO manufactured2Composite mortar because of ATO and
TiO2It cannot stablize and closely uniformly get along and be easy to generate precipitating, it is uneven so as to cause coating, influence the heat insulation of coating
And other effects.
Therefore, in the prior art there are problem, it is urgent to provide one kind not to allow precipitating easily generated, robust consistent
Effective removing insulating moulding coating technology is particularly important.
Summary of the invention
It is an object of the invention to avoid shortcoming in the prior art and providing that precipitating easily generated, performance is not allowed to stablize
The persistently preparation method of the high transparency removing insulating moulding coating of effective superhydrophilic self-cleaning.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning, includes following steps:
(1) TiO is prepared2/ ATO complex function nanopowder particles
Tin oxide and antimony chloride are added in the concentrated sulfuric acid and stir into jelly by 1.1；
1.2 are slowly added to hydrogen peroxide, continue to stir；
1.3 are added titanium tetrachloride, continue to stir；
1.4 are added citric acid and dodecyl sodium sulfate, and stirring is transferred to after a certain period of time in polytetrafluoroethylene (PTFE) water heating kettle
Reaction；
1.5 will dry after the product progress centrifugal treating in water heating kettle；
(2) TiO is prepared2/ ATO composite water soluble slurry
2.1 by TiO2/ ATO complex function nanopowder particles, silane coupling agent and deionized water ball milling；
(3) glass heat-insulating coating is prepared
3.1 by TiO2/ ATO composite water soluble slurry is aided with the dispersion of chelating dispersing agent high speed shear and ultrasonic disperse is made.
Preferably, it calculates in parts by mass, step (1) raw material dosage is as follows:
10 ~ 15 parts of tin oxide
6 ~ 8 parts of antimony chloride
6 ~ 8 parts of the concentrated sulfuric acid
30% 25 ~ 30 parts of hydrogen peroxide
10 ~ 15 parts of titanium tetrachloride
2 ~ 4 parts of citric acid
1 ~ 2 part of dodecyl sodium sulfate.
Preferably, in step 1.4, reaction kettle is warming up to 170 DEG C ~ 200 DEG C, reacts 12 ~ 16 hours.
Preferably, in step 2.1, at room temperature, by TiO240 ~ 50 mass parts of/ATO complex function nanopowder particles, KH570 silicon
The deionized water of 1 ~ 2 mass parts of alkane coupling agent and 40 ~ 50 mass parts, which is put into ball mill, carries out ball milling, revolving speed be 5000 ~
6000r/min, Ball-milling Time are 4 ~ 12 hours.
Preferably, in step 3.1, TiO2The WPU8340 of 40 ~ 50 mass parts of/ATO composite water soluble slurry, 10 ~ 30 mass parts
Be added to the ethylene bis stearic acid amide of 2 ~ 4 mass parts in the deionized water of 20 ~ 30 mass parts, in the case where stirring be added 2 ~
The thickener CA908 of 4 mass parts, the coalescing agent SG-505 of 2 ~ 5 mass parts and the levelling agent TB-120 of 2 ~ 3 mass parts, use ammonia
Water adjusts pH value to 7 ~ 9, and the high-transparent glass of first high speed dispersion re-ultrasonic dispersion, the obtained superhydrophilic self-cleaning that is uniformly dispersed is heat-insulated
Coating.
It is furthermore preferred that dispersing 60 ~ 120min, re-ultrasonic dispersion with after ammonium hydroxide adjusting pH value with 1000 ~ 2500r/min revolving speed
20~40min。
It is furthermore preferred that defoaming agent is added dropwise when dispersion.
Beneficial effects of the present invention:
Direct mixing by nano-titanium dioxide powder and tin-antiomony oxide in the solution compared with the existing technology, the present invention with
Titanium tetrachloride, tin oxide and antimony chloride are raw material, and the concentrated sulfuric acid and hydrogen peroxide are oxidant, and citric acid is auxiliary agent, dodecyl sulphur
Sour sodium is surfactant, and the compound function nano composite powder of TiO2/ATO is prepared using the method for co-precipitation and hydro-thermal
Grain, uses TiO2The TiO that/ATO complex function nanopowder particles, silane coupling agent and deionized water ball milling obtain2/ ATO composite water soluble
Stability of Slurry is good, and precipitating not easily generated persistently keeps good thermal insulation, hydrophily and light transmission.Wherein, TiO2/ATO
Composite water soluble slurry is aided with chelating dispersing agent dispersion using aqueous polyurethane as film forming matter, in conjunction with high speed shear dispersion and ultrasound
Dispersing coating obtained not only has good filming performance, and there are also higher infrared barrier performances, and infrared barrier rate is up to 80%
More than, it is seen that light transmission rate has superhydrophilic self-cleaning up to 70% or more, and water droplet angle is less than 10.
Detailed description of the invention
Using attached drawing, the present invention will be further described, but the content in attached drawing does not constitute any limitation of the invention.
Fig. 1 is TiO obtained by embodiment 12The X-ray diffraction (XRD) figure of/ATO complex function nanoparticle；
Fig. 2 is TiO obtained by embodiment 12Transmission electron microscope (TEM) electronic chart of/ATO composite water soluble slurry
Picture；
Fig. 3 is the optics spectrogram that transparent heat insulating dope obtained by embodiment 1 is coated on glass by czochralski method, wherein
A is the glass of original uncoated coating, and b is the glass coated with transparent heat insulating dope；
Fig. 4 is the water droplet angle test that transparent heat insulating dope obtained by embodiment 1 is coated on glass by czochralski method,
Middle a is the glass of original uncoated coating, and b is the glass coated with transparent heat insulating dope.
Specific embodiment
The invention will be further described with the following Examples.
Embodiment 1
A kind of insulating mold coating for high-transparent glass of the superhydrophilic self-cleaning of the present embodiment the preparation method is as follows:
(1) by the tin oxide of 10 mass parts, the concentrated sulfuric acid of 6 mass parts is first added in the antimony chloride of 6 mass parts, stirs plastic
Object is filled, 30% hydrogen peroxide for being slowly added to 25 mass parts continues to stir, and one timing of titanium tetrachloride stirring of 10 mass parts is then added
Between after, add 2 mass parts citric acid and 1 mass parts dodecyl sodium sulfate stirring mixture is shifted after a certain period of time
Into polytetrafluoroethylene (PTFE) water heating kettle, after being warming up to 170 DEG C, reaction 12 hours, obtained product is passed through into centrifugation and drying
Obtain TiO2/ ATO complex function nanopowder particles.
(2) at room temperature, by TiO240 mass parts of/ATO complex function nanopowder particles, 1 mass parts of KH570 silane coupling agent and
The deionized water of 40 mass parts, which is put into ball mill, carries out ball milling, revolving speed 5000r/min, and Ball-milling Time is 4 hours, obtains
TiO2/ ATO composite water soluble slurry.
(3) under room temperature condition and magnetic agitation, TiO240 mass parts of/ATO complex function nanoparticle aqueous slurry, 10
One of WPU8340(aqueous polyurethane of mass parts) and the ethylene bis stearic acid amide (EBS) of 2 mass parts be added to 20 matter
In the deionized water for measuring part, the thickener CA908 of 2 mass parts, the coalescing agent SG- of 2 mass parts are added in the case where stirring
The levelling agent TB-120 of 505,2 mass parts adjusts pH value to 7 using ammonium hydroxide, disperses 60min, then ultrasound with 1000r/min revolving speed
Disperse 20min, defoaming agent is added dropwise, is uniformly dispersed and the polyurethane transparent insulating glass coating with super hydrophilic effect is made.
Wherein, tin oxide, antimony chloride, the concentrated sulfuric acid, 30% hydrogen peroxide, titanium tetrachloride, citric acid, dodecyl sodium sulfate,
KH570 silane coupling agent, WPU8340, ethylene bis stearic acid amide, thickener CA908, coalescing agent SG-505, levelling agent TB-
120, ammonium hydroxide and defoaming agent can be obtained from purchase on the market.
Embodiment 2
The main technical schemes of the present embodiment are substantially the same manner as Example 1, and the feature not laid down a definition in the present embodiment is adopted
With the explanation in embodiment 1, no longer repeated herein.The present embodiment is unlike the first embodiment:
(1) it is calculated by quality point, 15 parts of tin oxide, 8 parts of antimony chloride, 8 parts of the concentrated sulfuric acid, 30 parts of hydrogen peroxide, titanium tetrachloride 15
Part, 4 parts and 2 parts of dodecyl sodium sulfate of citric acid.
In water heating kettle, after being warming up to 200 DEG C, reaction 16 hours.
(2) TiO250 parts of/ATO complex function nanopowder particles, 2 parts of KH570 silane coupling agent, 50 parts of deionized water put, and turn
Speed is 6000r/min, and Ball-milling Time is 12 hours, obtains TiO2/ATO composite water soluble slurry.
(3) TiO250 parts, 30 parts WPU8340 of/ATO composite water soluble slurry, 4 parts of ethylene bis stearic acid amide (EBS), 30
Part deionized water, 4 parts of thickener CA908,5 parts of coalescing agent SG-505,3 parts of levelling agent TB-120, pH value are adjusted to 9, with
2500r/min revolving speed disperses 120min, re-ultrasonic dispersion 40min, and defoaming agent is added dropwise.
Embodiment 3
The main technical schemes of the present embodiment are substantially the same manner as Example 1, and the feature not laid down a definition in the present embodiment is adopted
With the explanation in embodiment 1, no longer repeated herein.The present embodiment is unlike the first embodiment:
(1) it calculates in parts by mass, 12 parts of tin oxide, 7 parts of antimony chloride, (30%) 27 part of hydrogen peroxide, 12 parts of titanium tetrachloride, lemon
3 parts, 2 parts of dodecyl sodium sulfate of lemon acid；
In water heating kettle, after being warming up to 185 DEG C, reaction 14 hours, obtained product can be obtained by centrifugation and drying
TiO2/ ATO complex function nanopowder particles；
(2) 45 mass parts of TiO2/ATO complex function nanoparticle, KH570 silane coupling agent 2 mass parts, 45 mass parts
Deionized water, rotational speed of ball-mill 5500r/min, Ball-milling Time are 8 hours, obtain TiO2/ ATO complex function nanoparticle slurry
Material；
(3) under room temperature condition and magnetic agitation, TiO2/ ATO composite water soluble slurry 45 mass parts, 20 mass parts
WPU8340, the ethylene bis stearic acid amide (EBS) of 3 mass parts, the deionized water of 25 mass parts, 3 mass parts thickener
The levelling agent TB-120 of CA908, the coalescing agent SG-505 of 3 mass parts and 3 mass parts, pH value are adjusted to 8, are turned with 2000r/min
Speed dispersion 90min, re-ultrasonic dispersion 30min, are added dropwise defoaming agent, are uniformly dispersed and the polyurethane transparent with super hydrophilic effect is made
Insulating glass coating.
Finally it should be noted that the above examples are only used to illustrate the technical scheme of the present invention explanation rather than right is wanted
Ask the limitation of protection scope.Those skilled in the art should be appreciated that referring to preferred embodiment and can be to of the invention
Technical solution is modified or replaced equivalently, but belongs to the substantially identical and protection scope of technical solution of the present invention.
Claims (6)
1. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning, which is characterized in that include following step
It is rapid:
(1) TiO is prepared2/ ATO complex function nanopowder particles
Tin oxide and antimony chloride are added in the concentrated sulfuric acid and stir into jelly by 1.1；
1.2 are slowly added to hydrogen peroxide, continue to stir；
1.3 are added titanium tetrachloride, continue to stir；
1.4 are added citric acid and dodecyl sodium sulfate, and stirring is transferred in polytetrafluoroethylene (PTFE) water heating kettle anti-after a certain period of time
It answers；
1.5 will dry after the product progress centrifugal treating in water heating kettle；
(2) TiO is prepared2/ ATO composite water soluble slurry
2.1 by TiO2/ ATO complex function nanopowder particles, silane coupling agent and deionized water ball milling；
(3) glass heat-insulating coating is prepared
3.1 by TiO2/ ATO composite water soluble slurry is aided with the dispersion of chelating dispersing agent high speed shear and ultrasonic disperse is made；
Wherein, it calculates in parts by mass, step (1) raw material dosage is as follows:
10 ~ 15 parts of tin oxide
6 ~ 8 parts of antimony chloride
6 ~ 8 parts of the concentrated sulfuric acid
30% 25 ~ 30 parts of hydrogen peroxide
10 ~ 15 parts of titanium tetrachloride
2 ~ 4 parts of citric acid
1 ~ 2 part of dodecyl sodium sulfate.
2. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning according to claim 1, special
Sign is that reaction kettle is warming up to 170 DEG C ~ 200 DEG C in step 1.4, reacts 12 ~ 16 hours.
3. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning according to claim 1, special
Sign is, in step 2.1, at room temperature, by TiO240 ~ 50 mass parts of/ATO complex function nanopowder particles, KH570 silane coupling agent
The deionized water of 1 ~ 2 mass parts and 40 ~ 50 mass parts, which is put into ball mill, carries out ball milling, and revolving speed is 5000 ~ 6000r/min, ball
Time consuming is 4 ~ 12 hours.
4. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning according to claim 1, special
Sign is, in step 3.1, TiO2The WPU8340 and 2 ~ 4 matter of 40 ~ 50 mass parts of/ATO composite water soluble slurry, 10 ~ 30 mass parts
The ethylene bis stearic acid amide of amount part is added in the deionized water of 20 ~ 30 mass parts, and 2 ~ 4 mass parts are added in the case where stirring
Thickener CA908, the coalescing agent SG-505 of 2 ~ 5 mass parts and the levelling agent TB-120 of 2 ~ 3 mass parts, with ammonium hydroxide adjust pH
Value is to 7 ~ 9, first high speed dispersion re-ultrasonic dispersion, the insulating mold coating for high-transparent glass for the obtained superhydrophilic self-cleaning that is uniformly dispersed.
5. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning according to claim 4, special
Sign is, disperses 60 ~ 120min, 20 ~ 40min of re-ultrasonic dispersion with after ammonium hydroxide adjusting pH value with 1000 ~ 2500r/min revolving speed.
6. a kind of preparation method of the insulating mold coating for high-transparent glass of superhydrophilic self-cleaning according to claim 4, special
Sign is, when dispersion, defoaming agent is added dropwise.
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| CN107500564A (en) * | 2017-08-24 | 2017-12-22 | 中航百慕新材料技术工程股份有限公司 | The preparation method of glass |
| CN107903667B (en) * | 2017-10-25 | 2020-06-19 | 广州一新科技有限公司 | Multifunctional super-hydrophilic coating and preparation method thereof |
| CN108298551B (en) * | 2017-12-27 | 2020-09-18 | 佛山科学技术学院 | Preparation method of mesoporous molecular sieve nanocomposite with core-shell-core structure |
| CN108295836B (en) * | 2017-12-27 | 2020-09-18 | 佛山科学技术学院 | Preparation method of ATO/silicon dioxide/titanium dioxide composite material with core-shell structure |
| CN112521775A (en) * | 2020-12-30 | 2021-03-19 | 江南大学 | Preparation method of composite nano powder and coating for preparing anti-reflection and transparent heat-insulation coating |
| CN116102916A (en) * | 2021-09-16 | 2023-05-12 | 长沙民德消防工程涂料有限公司 | Indium tin oxide/titanium dioxide composite material and preparation method thereof, and automotive glass heat insulation coating and preparation method thereof |
| CN116063865A (en) * | 2023-01-18 | 2023-05-05 | 浙江理工大学 | Self-cleaning antistatic heat-insulating functional filler and preparation method and application thereof |
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