CN101265374A - Intelligent heat-insulating film and its preparing process - Google Patents
Intelligent heat-insulating film and its preparing process Download PDFInfo
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- CN101265374A CN101265374A CNA2008100330326A CN200810033032A CN101265374A CN 101265374 A CN101265374 A CN 101265374A CN A2008100330326 A CNA2008100330326 A CN A2008100330326A CN 200810033032 A CN200810033032 A CN 200810033032A CN 101265374 A CN101265374 A CN 101265374A
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Abstract
The invention relates to an intelligent heat-insulating film and a preparation method thereof. The invention adopts the mixture of phase transition intelligent nanometer powder in the rutile crystal structure and vanadium dioxide V1-X<MX>O2(X is more than 0 and less than 0.06) to uniformly disperse on a material which can be formed into films, thus preparing the intelligent heat-insulating film with the phase transition function. The intelligent heat-insulating film is a novel energy-saving material with the phase transition temperature adjustable within -10 DEG C to 70 DEG C. The film has high infrared transmittance and low reflectivity as well as excellent heat-insulating property at low temperatures. At high temperatures, the film has low infrared transmittance and high reflectivity as well as excellent heat insulating effect. The intelligent heat-insulating film can be used for heat-insulation and decorative-protection of the surfaces such as glass, plastic, metal, wood, concrete and so on.
Description
Technical field
The present invention relates to chemical field and material field, be specifically related to adjustable intelligent heat-insulating film of a kind of transformation temperature and preparation method thereof.
Background technology
In order to reduce the radiation of sun power, reach purpose of energy saving, people adopt variety of way to changing the light transmission of material.The vehicle glass pad pasting can intercept solar irradiation, reduce the injury of ultraviolet ray to human body, reduce each temperature surperficial and the interior air of car in the car, it is aging to slow down the interior facility of car, improve frame and take advantage of personnel's environment by bus, can reduce simultaneously the oil consumption of automobile, some building energy conservation glass also reach the obstruct solar irradiation by metal-coated membrane (aluminium, silver etc.) equally, reduce the purpose of air conditioning energy consumption.
Existing studies show that, some metal oxides have good optics barrier, as tin-antiomony oxide (ATO) near infrared of wavelength 1400nm-2500nm had good barrier (as Chinese invention patent CN200710021766.8), tin indium oxide (ITO) has good barrier (as Chinese invention patent CN98100128.9, Chinese invention patent CN200610096832.3) to the near infrared of wavelength 1100nm-2500nm, can intercept the near infrared light of 900-2500nm through the tin indium oxide (as U.S. patent of invention US Patent5518810) of special processing.Part boride such as lanthanum hexaborane (LaB6) can intercept near infrared light (as U.S. patent of invention US Patent 6060154).And the titanium dioxide of superfine powder or colloidal sol, zinc oxide, ferric oxide have good UV-light barrier.
In recent years, scientist finds that vanadium dioxide has multiple crystalline structure, and wherein R is a kind of phase-change metal oxide compound mutually, in certain temperature reversible metal-semiconductor phase transformation (MST) takes place up and down, equals (T in the resistance transformation temperature
C=68 ℃) can take place from the crystal conversion of square structure to monocline, has reversible semi-conductor-metal phase change, low temperature has semiconductor property mutually, have higher infrared transmittivity and lower reflectivity, high temperature has metalline mutually, have lower infrared transmittivity and higher reflectivity, be a kind of thermochromic material, can be applied to the sun power temperature control unit, photoelectric switch material, thermistor material, optical information storage, the blinding laser weapons safety guard, big area thermo color glass curtain wall, energy-saving coating, aspect such as polarizer and variable mirror.
In the solar radiation energy 81% all comes from visible light and near infrared light wave band, and vanadium dioxide has higher room temperature transmitance and very low high temperature transmitance at these wave bands.If with VO
2Film is coated on forms surfaces such as buildings, automobile, utilizes its phase transformation front and back to cause the change of IR transmittance, can be used to regulate automatically room temp, obtains effect cool in summer and warm in winter.Common dark coating to the reflecting rate of visible light generally greater than 35%, to prevent causing coating to be broken, by use VO owing to expanding with heat and contract with cold
2Coating intercepts infrared rays, and its reflecting rate can be reduced to below 35%.The approach that preparation commonly used contains the vanadium dioxide film mainly contains: 1. vacuum plating, as magnetron sputtering, chemical vapour deposition etc., need be in vacuum chamber the heat base material, and feeding trace oxygen, make vanadium atom combine (, adopting the reactive ion sputter coating process to prepare vanadium oxide film) with Sauerstoffatom as Chinese invention patent CN200510022085.4.2. sol-gel legal system film is coated in glass surface with the colloidal sol of Vanadium Pentoxide in FLAKES and makes gel, again through the hydrogen high temperature reduction.There is more shortcoming in these methods, as: apparatus expensive, simple glass or plastics can't stand high temperature, and the valence state and the crystal formation of vanadium are restive, are difficult to make large-area film, and gel-film produces pore etc.
But because its resistance transformation temperature is higher than room temperature for 68 ℃, its application is subjected to certain limitation, therefore reduces the sudden change of resistivity temperature, by other metallic element that mixes in vanadium dioxide, can reduce transformation temperature.Reported a kind of synthetic vanadium dioxide method of mixing tungsten as U.S. Pat 6358307, but this method is not because ammonium tungstate and ammonium vanadate are not atom level mixes, might heterogeneity, and be redox processes at decomposition course, may obtain V
nO
2n+1And V
nO
2n-1Two groups of nonstoichiometric compounds, this makes VO
2Valence state not accurate enough, and powder overlaps together, and relies on NH
3Diffusion be difficult to guarantee the homogeneity of product.Chinese patent CN 1279211A has reported the preparation method of a kind of vanadium dioxide nano powder and nano ceramics, obtains nonstoichiometric compound easily, makes vanadium dioxide lose the low temperature phase change performance.
Summary of the invention
The objective of the invention is to propose adjustable intelligent heat-insulating film of a kind of transformation temperature and preparation method thereof, this intelligent heat-insulating film is to adopt to contain phase transformation intelligent nano powder doped vanadium dioxide V
1-XM
XO
2(0＜X＜0.06) but intelligent heat insulation nano slurry and film forming material blend preparation, intelligent thermal insulating coating is obtained intelligent heat-insulating film behind 0～200 ℃ of drying and forming-film, its transformation temperature is adjustable at-10 ℃～70 ℃.
But the intelligent heat insulation nano slurry that above-mentioned intelligent heat-insulating film is used and the mass ratio of film forming material are 2～50: 30～95.
The used intelligent heat insulation nano slurry of above-mentioned intelligent heat-insulating film contains doped vanadium dioxide at least, can add other powder or colloidal sol heat insulation or antiultraviolet, comprises tin-antiomony oxide (ATO), tin indium oxide (ITO), lanthanum hexaborane (LaB
6), titanium dioxide, zinc oxide, ferric oxide, silicon-dioxide or cerium oxide etc., intelligent heat insulation nano slurry solid content 2～50wt%, the size of particles of powder or colloidal sol are 10～300nm, selected nano-powder can be wherein 1～6 kind.
Doped vanadium dioxide is to have V
1-XM
XO
2The rutile-type crystal of (0＜X＜0.06) structure, the valence state of vanadium is+4 valencys, doping agent is any of tungstate, molybdate, tantalate, niobate, titanium salt, chromic salts or aluminium salt, its grain-size is less than 100nm, transformation temperature is-10～70 ℃, and doped vanadium dioxide content accounts for 2～50wt% of intelligent heat insulation nano slurry.
Above-mentioned doped vanadium dioxide is the adjustable phase transformation intelligent material of a kind of transformation temperature according to the disclosed method preparation of publication 200610024387.X.
Intelligent heat-insulating film of the present invention, but used film forming material is polyacrylic resin, urethane resin, Synolac, aminoresin, polyester, silicone resin, inorganic silicate, inorganic phosphate and their aqueous liquid dispersion or emulsion, and selected resin is wherein 1～5 kind.
The invention provides the preparation method of above-mentioned intelligent heat-insulating film.Be about to intelligent thermal insulating coating and be coated on the base material, obtain behind 0～200 ℃ of drying and forming-film, wherein the composition of intelligent thermal insulating coating and weight ratio are as follows:
But film forming material 30～95
Intelligence heat insulation nano slurry 2～50
Thinner 0～60
Among the intelligent heat-insulating film preparation method of the present invention, but used film forming material is polyacrylic resin, urethane resin, Synolac, aminoresin, polyester, silicone resin, inorganic silicate, inorganic phosphate and their aqueous liquid dispersion or emulsion, selected resin is wherein 1～5 kind, preferred good polyacrylic resin, urethane resin, aminoresin and silicone resin and aqueous dispersions or the emulsion of weathering resistance.
Among the intelligent heat-insulating film preparation method of the present invention, the nano-powder or the colloidal sol of used intelligent heat insulation nano slurry, but its dispersion medium according to selected film forming material system, for coating with conventional organic solvent or water or alcohol/water mixed solvent.
Among the intelligent heat-insulating film preparation method of the present invention, but used solidifying agent is selected conventional coating solidifying agent for use according to selected film forming material system, and consumption is 0～30wt%.
Among the intelligent heat-insulating film preparation method of the present invention, but used thinner according to selected film forming material system, for coating with conventional organic solvent or water or alcohol/water mixed solvent, consumption is 0～60wt%.
Among the intelligent heat-insulating film preparation method of the present invention, used auxiliary agent comprises coating 1～10 kind with conventional dispersion agent, flow agent, defoamer, film coalescence aid, wetting agent, thickening material at least, and consumption is 1～10wt%.
Among the intelligent heat-insulating film preparation method of the present invention, adopt the method for showering, spraying or brushing that intelligent thermal insulating coating evenly is coated on the base material.
Among the intelligent heat-insulating film preparation method of the present invention, select glass, plastics (as PMMA, PVC, PP, PE, PET, PC, POM), metal, timber, concrete etc. for use.
Among the intelligent heat-insulating film preparation method of the present invention, coating is obtained intelligent heat-insulating film behind 0～200 ℃ of drying and forming-film.
The adjustable intelligent heat-insulating film of transformation temperature that the present invention obtains can be used as the application of thermochromism film, temperature control unit, thermo color glass curtain wall or energy-saving coating.
The intelligent heat-insulating film transparency that the transformation temperature that the present invention obtains is adjustable is good, can reduce seeing through and ultraviolet injury to human body of solar energy.
The adjustable intelligent heat-insulating film of transformation temperature that the present invention obtains, heat insulation and anti-ultraviolet effect can be according to the requirement to visible light transmissivity, sun power transmitance, uv transmittance, adjust the kind of powder in the intelligent heat insulation nano slurry or colloidal sol, and the consumption of slurry reaches necessary requirement.
The adjustable intelligent heat-insulating film of transformation temperature that the present invention obtains can rise with envrionment temperature and increase infrared reflectance automatically, can possess the advantage of smart window again as common coating convenient construction, reaches energy-saving heat-insulating, reduces the effect of air conditioning energy consumption.
The adjustable intelligent heat-insulating film of transformation temperature that the present invention obtains, be the adjustable vanadium dioxide phase transformation intelligent material of a kind of transformation temperature, can be applied to fields such as sun power temperature control unit, photoelectric switch material, thermistor material, optical information storage, blinding laser weapons safety guard, big area thermo color glass curtain wall, energy-saving coating, polarizer and variable mirror.
The intelligent heat-insulating film performance characterization that transformation temperature of the present invention is adjustable is as follows: adopt DSC (DSC2910, TAInstruments, differential scanning calorimeter) to characterize the low temperature phase change performance of vanadium dioxide, test condition is nitrogen atmosphere, 10 ℃/min of temperature rise rate; Adopt Philips XL30apparatus scanning electron microscope (SEM) to characterize the pattern of vanadium dioxide; Adopt the particle diameter of BeckmanCoulter N4plus dynamic laser scattering (DLS) particle size analyzer test heat insulation nano slurry; The visible-near-infrared spectrum of heat-insulating film (Vis-NIR) adopts the test of Varian Cary500 UV, visible light near infrared spectrometer, wavelength is from 400～2500nm, to be coated with membrane prepare on slide glass, and slide glass placed on the add in-place thermic devices, the add in-place hot charging is changed to self-control, temperature-controlled precision ± 0.1 ℃.
The adjustable intelligent heat-insulating film of a kind of transformation temperature that the present invention proposes has the following advantages: adopt liquid-phase precipitation method to prepare the doped vanadium dioxide presoma, after filtration, washing, drying, heating, crystallization, obtain having the V of rutile-type crystalline structure
1-XM
XO
2(0＜X＜0.06) phase transformation intelligent material, the phase transformation intelligent material grain-size of acquisition is less than 100 nanometers, and the valence state of vanadium equals+4 valencys, both can avoid occurring nonstoichiometric compound, can mix by homogeneous phase again, and transformation temperature can be regulated at-10 ℃-70 ℃.By having the phase change material of temperature effective---dopen Nano VO
2Introducing is filmed, and class coating material is had from temperature adjustment function with about room temperature infra-red heat is reflected the function of controlling, and when temperature is higher than a certain design temperature as 25 ℃, can effectively stop the infrared rays in the sunlight to be absorbed; And when temperature is lower than design temperature, can guarantee that the infrared rays in the sunlight is absorbed.Make it to stop indoor intensification at energy usable reflection infrared rays in the summer of sweltering heat, then help infrared ray absorption and see through cold winter, improves room temp.Intelligent heat-insulating film can be with simple brushing or spraying coating process at complex surface with can not stand pyritous surface system film, do not need thermal treatment and other subsequent disposal, have broad application prospects, can be applicable to stadiums, the building, the airport, the station, track traffic, automobile, train, aircraft, oil tank, petroleum pipe line, shell, spacecraft, the naval vessel, commander's shelter, tank, panzer, the energy-saving coating and the big area thermo color glass curtain wall on surface such as tent also can be applicable to the sun power temperature control unit, photoelectric switch material, thermistor material, optical information storage, the blinding laser weapons safety guard, field such as polarizer and variable mirror.
Description of drawings
Fig. 1 is doped vanadium dioxide particulate pattern (SEM figure), and powder is agglomerating particles, but there is a large amount of holes in intercrystalline.
Fig. 2 is the dsc analysis figure of pure vanadium dioxide (a) and doped vanadium dioxide (b, c, d).As can be seen from the figure, the transformation temperature of pure vanadium dioxide (a) is 66 ℃, and doped vanadium dioxide (b, c, d) transformation temperature is respectively 42 ℃, 36 ℃, 15 ℃.
Fig. 3 is the Visible-to-Near InfaRed transmitted spectrum of intelligent heat-insulating film, can calculate visible light transmissivity, ultraviolet permeability and the near infrared light average transmittances of membrane from figure.Wherein visible light transmissivity high temperature is 71%, low temperature is 65%, and ultraviolet permeability high temperature is 38%, low temperature is 36%, and near infrared light transmitance high temperature is 29%, low temperature is 50%.
Embodiment
Embodiment 1-embodiment 6 is the preparation of doped vanadium dioxide.
Embodiment 1:
In beaker, 50 ℃ of controlled temperature, under the 500rpm rotating speed, prepare the potassium molybdate aqueous solution of 0.5mol/L of 4mol/L sodium bicarbonate aqueous solution, the 30ml of the 0.5mol/L vanadylic sulfate aqueous solution, the 100ml of 100ml respectively, in the reactor that agitator, dropping funnel, condenser are housed, under the 500rpm rotating speed, controlled temperature 40-50 ℃, the vanadylic sulfate aqueous solution and potassium molybdate aqueous solution were stirred 20 minutes, keep 40-50 ℃ of temperature, after dripping sodium bicarbonate aqueous solution in 3-4 hour, obtain the hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, with Methyl amyl ketone washing 1-2 time, in nitrogen atmosphere, will obtain adulterated amorphous presoma and place retort furnace then, be warming up to 400-500 ℃ of following high temperature sintering 10 hours, obtain doped vanadium dioxide.
Embodiment 2:
In beaker, controlled temperature 10-20 ℃, under the 200rpm rotating speed, prepare the 0.1mol/L vanadylic sulfate aqueous solution of 100ml respectively, the 0.01mol/L aqueous sodium hydroxide solution of 200ml, the 0.1mol/L tantalic acid ammonium of 40ml, the 0.01mol/L aluminum chloride aqueous solution of 40ml, agitator is being housed, dropping funnel, in the reactor of condenser, under the 500rpm rotating speed, controlled temperature 10-20 ℃, with the vanadylic sulfate aqueous solution and tantalic acid aqueous ammonium, aluminum chloride aqueous solution mixes stirring 20 minutes, keep 10-20 ℃ of temperature, behind 5-6 hour dropping sodium aqueous solution, obtain the hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, use washing with alcohol 1-2 time then, will obtain adulterated amorphous presoma and place 40 ℃ of vacuum drying ovens dry 6 hours, in nitrogen atmosphere, place retort furnace, be warming up to 1000-1200 ℃ of following high temperature sintering 2 hours, obtain doped vanadium dioxide.
Embodiment 3:
In beaker, controlled temperature 10-20 ℃, under the 1000rpm rotating speed, prepare the 5mol/L vanadylic sulfate aqueous solution of 100ml respectively, the 10mol/L sodium acetate aqueous solution of 100ml, the 1mol/L ammonia aqueous solution of 20ml, the 0.5mol/L potassium wolframate of 1ml, the 0.5mol/L chlorination oxygen titanium aqueous solution of 1ml, the 0.1mol/L ammonium molybdate aqueous solution of 1ml, agitator is being housed, dropping funnel, in the reactor of condenser, under the 500rpm rotating speed, controlled temperature 70-80 ℃, with the vanadylic sulfate aqueous solution and the potassium wolframate aqueous solution, the chlorination oxygen titanium aqueous solution, ammonium molybdate aqueous solution mixes stirring 20 minutes, keep 70-80 ℃ of temperature, dripped the mixed solution of sodium acetate aqueous solution and ammonia aqueous solution at 1-2 hour, obtain the hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, will obtain adulterated amorphous presoma and place 80 ℃ of baking ovens dry 1 hour, in nitrogen atmosphere, place retort furnace, be warming up to 700-900 ℃ of following high temperature sintering 5 hours, obtain doped vanadium dioxide.
Embodiment 4:
In beaker, controlled temperature 30-40 ℃, under the 500rpm rotating speed, prepare the 0.05mol/L vanadylic sulfate aqueous solution of 100ml respectively, the 0.1mol/L wet chemical of 200ml, the 0.05mol/L potassium niobate aqueous solution of 20ml, the 0.05mol/L chromium chloride solution of 20ml, agitator is being housed, dropping funnel, in the reactor of condenser, under the 500rpm rotating speed, controlled temperature 30-40 ℃, with the vanadylic sulfate aqueous solution and the potassium niobate aqueous solution, chromium chloride solution mixes stirring 60 minutes, keep 30-40 ℃ of temperature, drip wet chemical at 8-9 hour, obtain the hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, use washing with acetone 1-2 time then, will obtain adulterated amorphous presoma and place 50 ℃ of baking ovens dry 5 hours, in nitrogen atmosphere, place retort furnace, be warming up to 400-500 ℃ of following high temperature sintering 10 hours, be warming up to 600-800 ℃ of following high temperature sintering again 5 hours, and obtained doped vanadium dioxide.
Embodiment 5:
In beaker, controlled temperature 30-40 ℃, under the 100rpm rotating speed, prepare the 0.01mol/L vanadylic sulfate aqueous solution of 100ml, the 0.01mol/L ammonium carbonate solution of 400ml, the 0.01mol/L niobic acid aqueous ammonium of 5ml respectively, in the reactor that agitator, dropping funnel, condenser are housed, under the 100rpm rotating speed, controlled temperature 80-90 ℃, the vanadylic sulfate aqueous solution and niobic acid aqueous ammonium are mixed stirring 10 minutes, keep 80-90 ℃ of temperature, drip ammonium carbonate solution at 1-2 hour, obtain the hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, use washing with alcohol 1-2 time then, in nitrogen atmosphere, will obtain adulterated amorphous presoma and place retort furnace, be warming up to 400-600 ℃ of following high temperature sintering 18 hours, obtain doped vanadium dioxide.
Embodiment 6:
In beaker, controlled temperature 50-60 ℃, under the 800rpm rotating speed, prepare the 10mol/L vanadylic sulfate aqueous solution of 100ml, the 2mol/L potassium hydroxide aqueous solution of 10ml, the 8mol/L ammonium tungstate aqueous solution of 3ml respectively, in the reactor that agitator, dropping funnel, condenser are housed, under the 800rpm rotating speed, controlled temperature 50-60 ℃, the vanadylic sulfate aqueous solution and ammonium tungstate aqueous solution are mixed stirring 20 minutes, keep 50-60 ℃ of temperature, in 2 hours, drip potassium hydroxide aqueous solution, obtain hydroxide hydrate precipitation, sedimentation and filtration, be washed to no SO
4 2-, use washing with acetone 1-2 time then, will obtain adulterated amorphous presoma and place 30 ℃ of vacuum drying ovens dry 1 hour, in nitrogen atmosphere, place retort furnace, be warming up to 800-1000 ℃ of following high temperature sintering 8 hours, obtain doped vanadium dioxide.
Embodiment 7-embodiment 10 is the preparation of intelligent heat-insulating film.
Embodiment 7:
(1) preparation of water-based intelligence heat insulation nano slurry:
Tin indium oxide (ITO) 2
Doping titanium dioxide alum 16
Nano zine oxide 4
Wetting dispersing agent (Disperbyk-190) 0.6
Hyper-dispersant (Hyperdisper-5410) 2.0
Water 75
Wetting dispersing agent and hyper-dispersant are added to the water earlier, under the 500rpm rotating speed, stirred 5 minutes, under the 1500rpm rotating speed, add above-mentioned powder, under the 500rpm rotating speed, stirred 5 minutes, sand milling is 36 hours in sand mill, obtains the intelligent heat insulation nano slurry about median size 80 nanometers.
(2) preparation of intelligent heat-insulating film:
Water soluble acrylic acid/polyurethane dispersing liquid 80
Dipropylene glycol monomethyl ether 6
Water 11
Defoamer (BYK-019) 0.9
Thickening material (RM-8W) 1.5
Wetting agent (H-140) 0.6
Above-mentioned materials is added by the prescription consumption, stirred 50 minutes under the 1500rpm rotating speed with dispersion machine, add 30 parts of water-based intelligence heat insulation nano slurries, under the 200rpm rotating speed, stirred 10 minutes, be coated on the glass baseplate, can obtain the transparent intelligent heat-insulating film of ultraviolet permeability 18%, visible light transmissivity 65%, solar energy transmitance 42%.
Embodiment 8:
(1) preparation of intelligent heat insulation nano slurry:
Doping titanium dioxide alum 7
Transparent ferric oxide 3
Wetting dispersing agent PEG 6,000 0.6
Hyper-dispersant (Hyperdisper-5410) 1.5
Ethanol 88
Join wetting dispersing agent PEG6000 and hyper-dispersant in the ethanol earlier, after stirring 10 minutes under the 1500rpm rotating speed, under the 3000rpm rotating speed, add above-mentioned powder, under the 1000rpm rotating speed, stirred 10 minutes, sand milling is 50 hours in sand mill, obtains the intelligent heat insulation nano slurry about median size 100 nanometers.
(2) preparation of intelligent heat-insulating film
Alcohol dissolubility silicone resin 80
Nano pulp 8
Ethanol 11
Defoamer (BYK-028) 0.4
This coating is coated on the base material, dried by the fire 30 minutes down at 80 ℃～120 ℃, hardness reaches more than the 5H, the transparent intelligent heat-insulating film of ultraviolet permeability 15%, visible light transmissivity 60%, solar energy transmitance 40%.
Embodiment 9:
(1) preparation of water-based intelligence heat insulation nano slurry:
Doping titanium dioxide alum 3
Wetting dispersing agent (Disperbyk-190) 0.6
Hyper-dispersant (Hyperdisper-5410) 2.0
Water 94
Wetting dispersing agent and hyper-dispersant are added to the water earlier, under the 500rpm rotating speed, stirred 20 minutes, under the 2000rpm rotating speed, add above-mentioned powder, under the 500rpm rotating speed, stirred 10 minutes, sand milling is 36 hours in sand mill, obtains the intelligent heat insulation nano slurry about median size 80 nanometers.
(2) preparation of intelligent heat-insulating film
Water soluble hydroxy acrylic resin 30
Waterborne nano slurry 46
Water 23
Flow agent (BYK380) 0.5
Defoamer (BYK-028) 0.5
Said components is mixed, add 5 parts of water-compatible amino resins during construction, mix being coated on the base material storing temperature 130-170 ℃, about 30 minutes set times, can obtain the transparent intelligent heat-insulating film of ultraviolet permeability 12%, visible light transmissivity 63%, solar energy transmitance 42%.
Embodiment 10:
(1) preparation of intelligent heat insulation nano slurry:
Nano-cerium oxide 5
Doping titanium dioxide alum 10
Nano zine oxide 4
Wetting dispersing agent (Disperbyk-161) 0.6
Hyper-dispersant (BSK 32800SH) 2.0
Dimethylbenzene 70
Join wetting dispersing agent and hyper-dispersant in the dimethylbenzene earlier, under the 1000rpm rotating speed, stirred 40 minutes, under the 4000rpm rotating speed, add above-mentioned powder, under the 1500rpm rotating speed, stirred 5 minutes, sand milling is 28 hours in sand mill, obtains the slurry about median size 80 nanometers.
(2) preparation of intelligent heat-insulating film
Nano pulp 10
Dimethylbenzene 31
Flow agent (BYK-302) 0.5
Defoamer (BYK-071) 0.5
Said components is mixed, add 30 parts of isocyanate curing agent TDI (50%) during construction, be sprayed on the base material, can obtain the transparent intelligent heat-insulating film of ultraviolet permeability 14%, visible light transmissivity 65%, solar energy transmitance 45%.
Claims (16)
1, the adjustable intelligent heat-insulating film of a kind of transformation temperature is characterized in that, this intelligent heat-insulating film is to adopt to contain phase transformation intelligent nano powder doped vanadium dioxide V
1-XM
XO
2But the intelligent heat insulation nano slurry of 0＜X＜0.06 prepares with the film forming material blend, and intelligent thermal insulating coating is obtained intelligent heat-insulating film behind 0～200 ℃ of drying and forming-film, and its transformation temperature is adjustable at-10 ℃～70 ℃; Wherein, intelligent heat insulation nano slurry contains doped vanadium dioxide at least, can add other heat insulation or antiultraviolet powder or colloidal sol, is tin-antiomony oxide ATO, tin indium oxide ITO, lanthanum hexaborane LaB
6, among titanium dioxide, zinc oxide, ferric oxide, silicon-dioxide or the cerium oxide any 1～6 kind; But film forming material is polyacrylic resin, urethane resin, Synolac, aminoresin, polyester, silicone resin, inorganic silicate, inorganic phosphate and their aqueous liquid dispersion or emulsion, and selected material is wherein 1～5 kind.
2, intelligent heat-insulating film according to claim 1 is characterized in that, intelligent heat insulation nano slurry solid content 2～50wt%, and the size of particles of powder or colloidal sol is 10～300nm.
3, intelligent heat-insulating film according to claim 1 is characterized in that, doped vanadium dioxide is to have V
1-XM
XO
2, the rutile-type crystal of 0＜X＜0.06 structure, the valence state of vanadium be+4 valencys, doping agent is any or combination of tungstate, molybdate, tantalate, niobate, titanium salt, chromic salts or aluminium salt; The doped vanadium dioxide grain-size is less than 100nm, and transformation temperature is-10～70 ℃, and its content accounts for 2～50wt% of intelligent heat insulation nano slurry.
4, intelligent heat-insulating film according to claim 1, but it is characterized in that the intelligent heat insulation nano slurry and the mass ratio of film forming material are 2～50: 30～95.
5, according to the preparation method of the described intelligent heat-insulating film of claim 1, it is characterized in that intelligent thermal insulating coating is coated on the base material, behind 0～200 ℃ of drying and forming-film, obtain, wherein the composition of intelligent thermal insulating coating and weight ratio are as follows:
But film forming material 30～95
Intelligence heat insulation nano slurry 2～50
Solidifying agent 0～30
Thinner 0～60
Auxiliary agent 1～10
6, preparation method according to claim 5, it is characterized in that, but film forming material is polyacrylic resin, urethane resin, Synolac, aminoresin, polyester, silicone resin, inorganic silicate, inorganic phosphate and their aqueous liquid dispersion or emulsion, selected resin is wherein 1～5 kind, preferred good polyacrylic resin, urethane resin, aminoresin and silicone resin and aqueous dispersions or the emulsion of weathering resistance.
7, preparation method according to claim 5 is characterized in that, intelligent heat insulation nano slurry contains doped vanadium dioxide at least, can add other heat insulation or anti-ultraviolet powder or colloidal sol, is tin-antiomony oxide ATO, tin indium oxide ITO, lanthanum hexaborane LaB
6, among titanium dioxide, zinc oxide, ferric oxide, silicon-dioxide or the cerium oxide any 1～6 kind, intelligent heat insulation nano slurry solid content 2～50wt%, the size of particles of powder or colloidal sol is 10～300nm.
8, intelligent heat insulation nano slurry according to claim 7 is characterized in that doped vanadium dioxide is to have V
1-XM
XO
2The rutile-type crystal of 0＜X＜0.06 structure, the valence state of vanadium is+4 valencys, doping agent is any or combination of tungstate, molybdate, tantalate, niobate, titanium salt, chromic salts or aluminium salt, its grain-size is less than 100nm, transformation temperature is-10～70 ℃, and doped vanadium dioxide content accounts for 2～50wt% of intelligent heat insulation nano slurry.
9, intelligent heat insulation nano slurry according to claim 7, it is characterized in that, the nano-powder or the colloidal sol of intelligence heat insulation nano slurry, but its dispersion medium according to selected film forming material system, for coating with conventional organic solvent or water or alcohol/water mixed solvent.
10, preparation method according to claim 5, it is characterized in that, but film forming material is polyacrylic resin, urethane resin, Synolac, aminoresin, polyester, silicone resin, inorganic silicate, inorganic phosphate and their aqueous liquid dispersion or emulsion, selected material is wherein 1～5 kind, preferred good polyacrylic resin, urethane resin, aminoresin and silicone resin and aqueous dispersions or the emulsion of weathering resistance.
11, preparation method according to claim 5 is characterized in that, but solidifying agent is selected conventional coating solidifying agent for use according to selected film forming material system, and consumption is 0～30wt%.
12, preparation method according to claim 5 is characterized in that, but thinner according to selected film forming material system, for coating with conventional organic solvent or water or alcohol/water mixed solvent, consumption is 0～60wt%.
13, preparation method according to claim 5 is characterized in that, selected auxiliary agent comprises coating 1～10 kind with conventional dispersion agent, flow agent, defoamer, film coalescence aid, wetting agent, thickening material at least, and consumption is 1～10wt%.
14, preparation method according to claim 5 is characterized in that, adopts the method for showering, spraying or brushing that intelligent thermal insulating coating evenly is coated on the base material.
15, preparation method according to claim 5 is characterized in that, described base material selects for use glass, metal, timber, concrete or plastics to comprise PMMA, PVC, PP, PE, PET, PC, POM.
16, the adjustable intelligent heat-insulating film of the transformation temperature of each acquisition of claim 1 to 15 can be applicable to thermochromism film, temperature control unit, thermo color glass curtain wall or energy-saving coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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