CN107083168B - A kind of glass nano transparent insulating coating and its application - Google Patents
A kind of glass nano transparent insulating coating and its application Download PDFInfo
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- CN107083168B CN107083168B CN201710324372.3A CN201710324372A CN107083168B CN 107083168 B CN107083168 B CN 107083168B CN 201710324372 A CN201710324372 A CN 201710324372A CN 107083168 B CN107083168 B CN 107083168B
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- 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
-
- 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
- C08K3/2279—Oxides; Hydroxides of metals of antimony
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/476—Tin oxide or doped tin oxide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/118—Deposition methods from solutions or suspensions by roller-coating
-
- 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
- C08K2003/2231—Oxides; Hydroxides of metals of tin
Abstract
The present invention relates to a kind of coating, in particular to a kind of glass nano transparent insulating coating and its application.The present invention promotes Sb using the oxidisability of hydrogen peroxide5+Doping, there is the Properties Control tin ion of chelating agent and the hydrolysis rate of antimony ion using organic acid, nano ATO crystal gelinite is prepared using hydrothermal synthesis method, after the processing of ATO crystal, it is mixed with aqueous polyurethane, using physical dispersion method, is prepared into nano transparent insulating coating, using coating processes coated glass surface, it is prepared into nano insulating glass.Glass nano transparent insulating coating has the advantages that absorb and reflection infrared wavelength and high visible light transmittance.
Description
Technical field
The present invention relates to a kind of coating, in particular to a kind of glass nano transparent insulating coating and its application.
Background technique
With the development and progress of society, for commercial floor gradually toward high-rise development, glass architecture curtain wall obtains widespread adoption,
But the energy consumption problem of glass architecture curtain wall also attracts extensive attention, the main method of energy consumption for solving glass curtain wall at present is choosing
With LOW-E hollow glass structure, reduce thermal convection and heat transfer by LOW-E layers of reduction heat radiation, by hollow structure.
The structure of hollow glass is mainly LOW-E glass Jia Baibo at present, and white glass is generally common soda lime glass, does not have
To infrared external reflection and absorption, it is easy to cause the loss of energy, needs to carry out at functionalization white glass to solve this problem
Reason, make glass have the function of absorbing with reflect it is infrared play insulation, reduce heat and consume.
Summary of the invention
The purpose of the present invention is to provide a kind of glass nano transparent insulating coating, which has absorption and reflection red
The advantages of outer wavelength and high visible light transmittance.
The present invention also provides a kind of preparation method of glass nano transparent insulating coating, this method equipment is simple, puts into
Less, it is easily formed product.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of preparation method of glass nano transparent heat-insulating, this method comprises the following steps:
(1) tin tetrachloride is dissolved in a solvent with antimony trichloride, wherein n (Sn4+) and n (Sb3+) molar ratio be 100:
(15-1) is added hydrolysis inhibitor and inhibits the hydrolysis and condensation of antimony ion, and hydrogenperoxide steam generator is added dropwise into mixed system, stirs
It mixes uniformly；
(2) alkaline aqueous solution is added dropwise in the solution obtained to step (1) and adjusts pH value of solution to 4-5, obtains gelatinous precipitate,
To precipitate it is still aging, promote metal ion be fully hydrolyzed；Eccentric cleaning is carried out to the precipitating after ageing, the chlorine in removal precipitating
Ion；
(3) precipitating for obtaining step (2) is added in 50-80 DEG C of temperature of organic acid soln, and stirring keeps precipitating complete
Dissolution, appropriate solvent is added into the solution, make system be heated to 50-80 DEG C and stir make solvent volatilize after obtain colloidal sol；It will
Colloidal sol is transferred in reaction kettle, carries out hydro-thermal reaction processing, promotes colloidal sol crystallization, and the blue oxide tin antimony being separated by solid-liquid separation is brilliant
Body gel；
(4) tin-antiomony oxide crystal gel is cleaned, removes gelinite impurity；
(5) the tin-antiomony oxide crystal gel that step (4) obtains is mixed with suitable quantity of water to adjust viscosity, regulation system pH is extremely
8-9, is added aqueous polyurethane, and ultrasonic vibration dispersion obtains glass nano transparent insulating coating.
Preferably, n (Sn4+) and n (Sb3+) molar ratio optimum value be 100:11, Sb3+Fully doped it can arrive dioxy
Change in tin crystal, and there are good infrared absorption and reflecting properties.
The present invention promotes Sb using the oxidisability of hydrogen peroxide5+Doping, using organic acid have chelating agent performance control
The hydrolysis rate of tin ion and antimony ion processed prepares nano ATO crystal gelinite using hydrothermal synthesis method, to the processing of ATO crystal
Afterwards, it is mixed with aqueous polyurethane, using physical dispersion method, is prepared into nano transparent insulating coating, is coated using coating processes
Glass surface is prepared into nano insulating glass.
Preferably, in step (1), the mass concentration of the hydrogenperoxide steam generator is 20-30%, hydrogenperoxide steam generator with
The mass ratio of tin tetrachloride is (1-10): 30.As a further preference, the mass ratio of hydrogenperoxide steam generator and tin tetrachloride is
7:30, under hydrothermal conditions, hydrogen peroxide can be good at Sb the mixed proportion3+It is oxidized to Sb5+, promote mixing for antimony ion
It is miscellaneous.
Preferably, the hydrolysis inhibitor is selected from the mixing of one or more of hydrochloric acid, nitric acid or sulfuric acid, it is described
Solvent is selected from dehydrated alcohol, methanol or isopropanol.
Preferably, the alkaline aqueous solution is the mixed of one or more of sodium hydroxide, potassium hydroxide, ammonium hydroxide
It closes；The still aging time is 12-24 hours.
Preferably, the organic acid is the mixing of one or more of oxalic acid, citric acid, tartaric acid, organic acid
Molar ratio with tin tetrachloride is n (Sn4+):n(H+)=1:(1-3).As further preferred, organic acid and tin tetrachloride rub
You are than being n (Sn4+):n(H+)=1:2, organic acid pass through coordinate bond and Sn4+、Sb3+Chelating, is effectively controlled metal ion water
The speed of solution and condensation, ensure that the uniformity of doping.
Preferably, the hydro-thermal reaction treatment temperature is 180-220 DEG C, and the reaction time, 8-20 was small in step (3)
When.
Preferably, the aqueous polyurethane be selected from solid content be 30%-40% PUA-608A, PUA-608B,
The mass ratio of one or more of mixing in PUA-2011 or PU-303A, aqueous polyurethane and tin-antiomony oxide crystal is 1-2:1.
As further preferred, aqueous polyurethane is selected from the PUA-608A that solid content is 40%, aqueous polyurethane tin-antiomony oxide crystal
Mass ratio is 1:1, and the thermal isolation film of mixed proportion preparation has preferable translucency and preferable heat-proof quality.
Glass nano transparent insulating coating made from method described in a kind of.
A method of glass being manufactured with nano transparent insulating coating using the glass, this method is: by heat-insulated painting
Material is coated in glass surface using the method for roller coating or showering, after curing and drying 10-20 minutes, is prepared into nanometer through 90-120 DEG C
Transparent heat insulating glass.Further, the glass passes through surface grinding purified treatment before coated with nano transparent heat insulating dope,
Remove glass surface pollutant.
The beneficial effects of the present invention are:
(1) tin ion and antimony hydrolysis, condensation rates are effectively controlled using organic acid sequestering agent, promotes Uniform Doped；
(2) nanoparticle agglomerates using the coating of hydro-thermal process preparation are small, and dispersion energy consumption is small；
(3) promote nano particle to disperse using the high some surface active property of aqueous polyurethane, while being also used as into
Film.
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.It should be appreciated that this hair
Bright implementation is not limited by the following examples, and the accommodation in any form made to the present invention and/or changed will all be fallen
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
Hydrogenperoxide steam generator, commercial product, concentration are about AR30%；
Concentrated hydrochloric acid, commercial product, concentration are about AR36.5%.
Embodiment 1:
24 grams of tin tetrachlorides are weighed respectively and 2.4 grams of antimony trichlorides are dissolved in dehydrated alcohol, 9 grams of concentrated hydrochloric acids are added, and are added
2.8 grams of hydrogenperoxide steam generators stir evenly, and sodium hydroxide solution is slowly added dropwise into solution and adjusts pH to 4, generates white gels
Shape precipitating, by white precipitate still aging 15 hours, removes removing chloride with deionized water eccentric cleaning white precipitate.
It takes 15 grams of tartaric acid to be dissolved in 400ml deionized water and obtains tartaric acid solution, the white after chloride ion will be gone to sink
Shallow lake is slowly dissolve into 60 DEG C of tartaric acid solution, is stirring evenly and then adding into 8 grams of dehydrated alcohols, so that system is heated to 80 DEG C and stir
Mixing makes solvent volatilize, and when the volume concentration of system is to 120ml, solution is placed in reaction kettle hydro-thermal reaction under the conditions of 190 DEG C
12 hours, after the reaction was completed, the cleaning of ATO crystal gelinite, centrifugation to acquisition took 100ml deionized water to be added clear after centrifugation
ATO gelinite after washing adjusts pH to 9 using ammonium hydroxide, the PUA-608A that 50 grams of solid contents are 30% is added, under agitation
Ultrasonic wave 1 hour, obtain black-and-blue clear dope.
Embodiment 2:
24 grams of tin tetrachlorides are weighed respectively and 2 grams of antimony trichlorides are dissolved in dehydrated alcohol, 9 grams of concentrated hydrochloric acids are added, and are added 3.8
Gram hydrogenperoxide steam generator stirs evenly, and sodium hydroxide solution is slowly added dropwise into solution and adjusts pH to 4, it is heavy to generate white gels shape
It forms sediment, by white precipitate still aging 17 hours, removes removing chloride with deionized water eccentric cleaning white precipitate.
It takes 6 grams of dissolving oxalic acids to obtain oxalic acid solution in 100ml deionized water, the white precipitate after chloride ion will be gone slow
Be dissolved into 50 DEG C of oxalic acid solution, be stirring evenly and then adding into 3 grams of ethyl alcohol, make system be heated to 60 DEG C and stir wave solvent
Hair, when the volume concentration of system is to 25ml, solution is placed in reaction kettle hydro-thermal reaction 9 hours under the conditions of 200 DEG C, is reacted
After the completion, to the cleaning of ATO crystal gelinite, the centrifugation of acquisition, take 10ml deionized water that the ATO gel after cleaning is added after centrifugation
Body adjusts pH to 9, the PUA-608B that 50 grams of solid contents are 35% using ammonium hydroxide, and ultrasonic wave 1 hour, obtains under agitation
Blue-tinted transparent coating.
Embodiment 3:
24 grams of tin tetrachlorides are weighed respectively and 1.5 grams of antimony trichlorides are dissolved in dehydrated alcohol, 8 grams of concentrated hydrochloric acids are added, and are added
3.5 grams of hydrogenperoxide steam generators stir evenly, and sodium hydroxide solution is slowly added dropwise into solution, adjust pH to 4, generate white gels
Shape precipitating, by white precipitate still aging 16 hours, removes removing chloride with deionized water eccentric cleaning white precipitate.
It takes 7 grams of citric acids to be dissolved in 200ml deionized water and obtains citric acid solution, the white precipitate after chloride ion will be removed
Be slowly dissolve into 80 DEG C of citric acid solution, be stirring evenly and then adding into 4 grams of ethyl alcohol, make system be heated to 70 DEG C and stir make it is molten
Agent volatilization, when the volume concentration of system is to 35ml, solution is placed in reaction kettle hydro-thermal reaction 9 hours under the conditions of 220 DEG C,
After the reaction was completed, to the cleaning of ATO crystal gelinite, the centrifugation of acquisition, take 20ml deionized water that the ATO after cleaning is added after centrifugation
Gelinite adjusts pH to 8 using ammonium hydroxide, and 60 grams of solid contents are 35%PUA-2011, and supersonic oscillations 0.5 are small under agitation
When obtain blue-tinted transparent coating.
The manufacture of nano transparent heat-insulating glass is carried out using coating made from above-described embodiment, specific method is: will be heat-insulated
Coating is coated in glass surface using the method for roller coating or showering, after curing and drying 10-20 minutes, is prepared into and receives through 90-120 DEG C
Rice transparent heat insulating glass.Gained glass is compared with the performance of existing product, obtains the data of table 1.
Table 1
Conclusion: as known from Table 1, coating of the invention, which has, to be absorbed and reflects the excellent of infrared wavelength and high visible light transmittance
Point.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (8)
1. a kind of preparation method of glass nano transparent insulating coating, it is characterised in that this method comprises the following steps:
(1) tin tetrachloride is dissolved in a solvent with antimony trichloride, wherein n (Sn4+) and n (Sb3+) molar ratio be 100:(15-
1) hydrolysis inhibitor, is added and inhibits the hydrolysis and condensation of antimony ion, and hydrogenperoxide steam generator is added dropwise into mixed system, stirring is equal
It is even；The mass concentration of the hydrogenperoxide steam generator is 20-30%, and the mass ratio of hydrogenperoxide steam generator and tin tetrachloride is (1-10):
30；
(2) alkaline aqueous solution is added dropwise in the solution obtained to step (1) and adjusts pH value of solution to 4-5, obtains gelatinous precipitate, will sink
It forms sediment still aging；Eccentric cleaning is carried out to the precipitating after ageing；
(3) precipitating for obtaining step (2) is added in 50-80 DEG C of temperature of organic acid soln, and stirring is completely dissolved precipitating,
Appropriate solvent is added into the solution, make system be heated to 50-80 DEG C and stir make solvent volatilize after obtain colloidal sol；Colloidal sol is turned
It moves in reaction kettle, carries out hydro-thermal reaction processing, promote colloidal sol crystallization, the blue oxide tin antimony crystal being separated by solid-liquid separation is solidifying
Glue；The organic acid is the mixing of one or more of oxalic acid, citric acid, tartaric acid, and organic acid and tin tetrachloride rub
You are than being n (Sn4+):n(H+)=1:(1-3)；
(4) tin-antiomony oxide crystal gel is cleaned；
(5) tin-antiomony oxide crystal gel that step (4) obtains is mixed with suitable quantity of water to adjust viscosity, regulation system pH to 8-9,
Aqueous polyurethane is added, ultrasonic vibration dispersion obtains glass nano transparent insulating coating.
2. preparation method according to claim 1, it is characterised in that: the hydrolysis inhibitor is selected from hydrochloric acid, nitric acid or sulphur
The mixing of one or more of acid, solvent described in step (1) and (3) are selected from dehydrated alcohol, methanol or isopropanol.
3. preparation method according to claim 1, it is characterised in that: the alkaline aqueous solution is sodium hydroxide, hydrogen-oxygen
Change the mixing of one or more of potassium, ammonium hydroxide；The still aging time is 12-24 hours.
4. preparation method according to claim 1, it is characterised in that: in step (3), the hydro-thermal reaction treatment temperature
It is 180-220 DEG C, reaction time 8-20 hour.
5. preparation method according to claim 1, it is characterised in that: it is 30%- that the aqueous polyurethane, which is selected from solid content,
One or more of mixing, aqueous polyurethane and tin oxide in 40% PUA-608A, PUA-608B, PUA-2011 or PU-303A
The mass ratio of antimony crystal gel is (1-5): 1.
6. glass nano transparent insulating coating made from a kind of method described in claim 1.
7. a kind of method for manufacturing glass with nano transparent insulating coating using glass as claimed in claim 6, it is characterised in that
This method is: insulating moulding coating being coated in glass surface using the method for roller coating or showering, through 90-120 DEG C of curing and drying 10-20
After minute, it is prepared into nano transparent heat-insulating glass.
8. according to the method described in claim 7, it is characterized by: the glass is passed through before coated with nano transparent heat insulating dope
Surface grinding purified treatment is crossed, glass surface pollutant is removed.
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| CN109005611A (en) * | 2018-06-13 | 2018-12-14 | 浙江西溪玻璃有限公司 | A kind of Dual-layer electrothermal membrane electrically heated glass |
| CN111960690A (en) * | 2020-07-10 | 2020-11-20 | 江苏科技大学 | High-dispersity tin antimony oxide high-molecular film and preparation method thereof |
| CN114059736A (en) * | 2020-08-10 | 2022-02-18 | 江西省颐冠涂料有限公司 | Granite soft ceramic chip and preparation method thereof |
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| CN104925853B (en) * | 2015-06-04 | 2016-07-06 | 天津市职业大学 | A kind of stability nanometer antimony-doped stannic oxide hydrosol and preparation method thereof |
| CN105694574B (en) * | 2016-03-16 | 2018-06-26 | 浙江凯色丽科技发展有限公司 | Platelet-like reflective heat-insulating powder and preparation method thereof |
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