CN1916057A - Sunlight controlled transparent film in low radiation, prepartion method and application - Google Patents

Sunlight controlled transparent film in low radiation, prepartion method and application Download PDF

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Publication number
CN1916057A
CN1916057A CN 200510086238 CN200510086238A CN1916057A CN 1916057 A CN1916057 A CN 1916057A CN 200510086238 CN200510086238 CN 200510086238 CN 200510086238 A CN200510086238 A CN 200510086238A CN 1916057 A CN1916057 A CN 1916057A
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oxide
mixture
film
adulterated
transparent film
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CN100463935C (en
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曹新宇
韩勇
江雷
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CHANGCHUN DIGAO INDUSTRIAL CO., LTD.
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ZHONGKE NANOMETER TECHNOLOGY ENGINEERING CENTER Co Ltd
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Abstract

This invention relates to a method for preparing low-radiation heat-insulating transparent film for controlling sunlight. The film is composed of: organic polymer 70-99.9 wt. %, doping metal oxide nanoparticles 0.1-30 wt. % and adjuvant 0-29.9 wt. %. The method comprises: (1) uniformly dispersing the doping metal oxide nanoparticles into a dispersing medium, mixing with the organic polymer and the adjuvant, and drying to obtain master batches; (2) plasticizing, smelting or extruding and blowing, calendaring, stretching, extruding and casting to obtain the film. The film can be used as the coating film for architecture glass, automobile window and ship window, and has such advantages as high visible-light permeability, good sunlight obstructing effect, good anti-electrostatic effect, and good electromagnetic radiation resistance.

Description

Low radiation transparent film of sunlight control and its production and use
Technical field
The present invention relates to organic polymer and nano inorganic particulate laminated film, particularly low radiation heat preservation energy-saving transparent film of sunlight control and its production and use.
Background technology
98% its wavelength that projects solar energy on the earth surface can be divided into three parts by its wavelength, i.e. UV-light, visible light and infrared light in the scope of 0.3～2.5 μ m.UV-light (account for wherein 3%) is an invisible light, and its wavelength is less than 380nm; Its wavelength of visible light (account for wherein 45%) is 380～780nm; Infrared light (account for wherein 49%) also is sightless, and wavelength is higher than 780nm.The heat preservation and energy conservation effects of glass or form is characterized by sheltering coefficient (Sc) and heat transfer coefficient (U) value usually, and can be by the judgement of these two parameters as the glass energy-saving performance.The Sc value is low, shows that the solar radiant heat that sees through is few, and thermal insulation is good, and the U value is low, shows the less calories that it loses because of different transfer of heat, good heat preservation performance.And because the needs of building glass daylighting need glass that visible light transmissivity is preferably arranged again.
Sunlight control low emissivity glass is a kind of building and the form energy-saving material that generally adopts at present, and the preparation method mostly is that magnetron sputtering, PVD, CVD film coating method and thermal spray method plated film are on base materials such as glass.For example:
Chinese patent notification number CN2194908Y discloses a kind of solar control film glass of the individual layer TiN film that is coated with by magnetron sputtering technique on substrate of glass.
Chinese patent application publication number 1363530A discloses a kind of absorption-type low-radiation film coated glass, has been coated with metal or the metal nitride film layers that one deck has certain receptivity earlier with the vacuum sputtering method on glass substrate, and is compounded to form this glass with multilayer film.
Above-mentioned these methods need place glass special equipment to process, and preparation has the low radiating energy-saving insulating plastic film of sunlight control, pad pasting, be applied to glass or plastics form, be the convenient-to-running method that increases glass and form heat preservation energy-saving performance, and still applicable to mounted glass.For example:
United States Patent (USP) 4973511 discloses a kind of multilayer film lamination compound sunlight control/safety film material, and sunlight key-course wherein is the method preparation by metal deposition, such as forming one deck plated film with vacuum deposition method on base material.
United States Patent (USP) 6166852 discloses a kind of solar control film that is composited by two kinds of polymeric films at least, wherein a kind of polymeric film contains uv-absorbing agent, another kind of polymeric film contains optical brightener (optical brightner), composite membrane can absorb the light of 300～410nm wave band, but and not mentioned Sunshine Red is outer or far performance.
United States Patent (USP) 6514589B1 discloses the solar control film that a kind of multilayer film is formed, comprising holographic etch layer-metal deposition layer-surface protection anti-fog layer-dye layer-pressure-sensitive adhesive layer.The deposition of metal level adopts vacuum-deposited method.
Sputter and CVD, PVD plated film, vacuum-deposited method need be carried out under the condition of special equipment and vacuum or in certain atmosphere of inert gases, its equipment price costliness, disposable having high input, the cost height all has certain restriction for shape, the size of base material and base material.The plated film film that wherein contains silver layer must carry out Vacuum Package within behind the plated film 24 hours, lose heat-insulating property otherwise the silver layer meeting is destroyed.Also need adopt and be lower than 200 ℃ condition if will on organic substrate, prepare plated film, and the problem of poor adhesive force is usually arranged again.Though the method for thermal spray descends to some extent than the method cost of sputter or vacuum plating, need glass temperature under the high temperature more than 400 degree Celsius, could realize, be not suitable for organic substrate.
United States Patent (USP) 6107360 discloses a kind of compound sunshade coating of resin that needs the fellatio light absorber of ultraviolet light polymerization.Preparing sunlight control low-emissivity coating with the method for solution coating is a method that relative cost is low, but the dispersion medium of its solution is the bigger organic solvent of toxicity, has limited the application of this method.
Summary of the invention
A purpose of the present invention provides the low radiation heat preservation energy-saving transparent film of sunlight control that has good visible transparent, can cover infrared, ultraviolet light.
Another order of the present invention provides a kind of method for preparing the low radiation heat preservation energy-saving film of sunlight control.
An also purpose of the present invention provides the purposes of the low radiation heat preservation energy-saving film of sunlight control.
The low radiation heat preservation energy-saving film of sunlight control of the present invention is the dispersion liquid that obtains adulterated metal oxide nanoparticles earlier by sanded, and with organic polymer and auxiliary agent thorough mixing, drying obtains master batch again; Master batch by common extrusion-blown modling, calendering, stretching or extruding to water to mould prepares the low radiation heat preservation energy-saving film of sunlight control.
The component of the low radiation heat preservation energy-saving transparent film of sunlight control of the present invention comprises the organic polymer of 70～99.9wt%, the adulterated metal oxide nanoparticles of 0.1～30wt% and the auxiliary agent of 0～29.9wt%.
Film thickness of the present invention is 5 microns～1 millimeter, preferred 5 microns～150 microns.
The preparation method of the low radiation heat preservation energy-saving transparent film of sunlight control of the present invention may further comprise the steps:
(1). the preparation of the dispersion liquid of adulterated metal oxide nanoparticles:
The thick product of adulterated metallic oxide nano powder is dispersed in the dispersion medium, (the adulterated metal oxide nanoparticles in the adulterated metallic oxide nano powder crude product here is an aggregating state, can not be dispersed in the medium with nano-scale, be referred to as thick product.This thick product can be bought from the market or know by everybody: coprecipitation method, hydrothermal method, colloid method, spray pyrolysis, the parcel precipitator method, alcohol-water salts solution heating method prepare.See document " inorganic fine chemistry industry technology " Chemical Industry Press, 2002) and add dispersion agent anabolic reaction system, the thick product of adulterated metal-oxide powder is 5～40wt% in the system, and dispersion medium is 59.5～94.5wt%, and dispersion agent is 0.5～5wt%.In the presence of sand milling medium (such as the zirconium white microballon), method by sand milling, obtain median size and be dispersed in adulterated metal oxide system in the dispersion medium, the i.e. dispersion liquid of adulterated metal oxide nanoparticles smaller or equal to 200nm (preferable particle size is 50nm or following).
(2). add organic polymer and auxiliary agent in the dispersion liquid of the adulterated metal oxide nanoparticles that step (1) is prepared, after fully stirring, mixing, drying under reduced pressure obtains master batch;
Contain the organic polymer of 70～99.9wt%, the adulterated metal oxide nanoparticles of 0.1～30wt% and the auxiliary agent of 0～29.9wt% in the described master batch.
(3). the master batch that step (2) is obtained by common extrusion-blown modling, calendering well known in the art, stretch or extrude and water the method and the processing condition of moulding, prepare the low radiation heat preservation energy-saving film of sunlight control.
This adulterated metal oxide nanoparticles has good consistency through after the sanded with described organic polymer material, and above-mentioned master batch is through plasticizing or banburying, and its adulterated metal oxide can be dispersed in the macromolecular material.The optical property of the particle diameter of contained nanoparticle, kind and film thickness and the prepared film of combined adjustable.
Described adulterated metal oxide nanoparticles has the effect to infrared Absorption and reflection, described metal oxide be Indium sesquioxide, stannic oxide, zinc oxide, Cadmium oxide, titanium oxide, vanadium oxide or similarly mix after have absorb and the metal oxide of reflected infrared in one or more mixture.
Adulterated metal is selected from one or more the mixture etc. in tin, gallium, antimony, titanium, tungsten, copper, iron, the zirconium in the described Indium sesquioxide.The mol ratio of indium is 0.1～20: 100 in doping metals and the Indium sesquioxide.
Adulterated metal is selected from one or more the mixture etc. in antimony, fluorine, phosphorus, titanium, cobalt, zinc, tungsten, manganese, cerium, tellurium, iron, gold and silver, the platinum in the described stannic oxide.The mol ratio of tin is 0.1～20: 100 in doping metals and the stannic oxide.
Adulterated metal is selected from one or more the mixture etc. in aluminium, antimony, bismuth, tin, titanium, indium, copper, iron, cadmium, tungsten, lithium, manganese, magnesium, gallium, cerium, the silver in the described zinc oxide.The mol ratio of doping metals and zinc in zinc oxide is 0.1～20: 100.
Adulterated metal is selected from one or more the mixture etc. in tin, lanthanum, bismuth, fluorine, tungsten, the copper in the described Cadmium oxide.The mol ratio of cadmium is 0.1～20: 100 in doping metals and the Cadmium oxide.
Adulterated metal is selected from one or more the mixture etc. in niobium, tin, zinc, the lanthanum in the described titanium oxide.The mol ratio of titanium is 0.1～20: 100 in doping metals and the titanium oxide.
Metal in the described doping vanadium oxide is selected from one or more the mixture etc. in tin, titanium, fluorine, tungsten, the copper.The mol ratio of vanadium is 0.1～20: 100 in doping metals and the vanadium oxide.
Described auxiliary agent is selected from one or more the mixture in softening agent, coupling agent, the stablizer.
Described softening agent is selected from one or more the mixture in dibutyl phthalate, dioctyl phthalate (DOP), di-sec-octyl phthalate, Dinonylphthalate, dimixo-octyl phthalate, DID Su, Octyl adipate, trioctyl phosphate, n-butyl stearate, polypropylene adipate (PPA), octyl epoxy stearate, the epoxy soybean oil.
Described coupling agent is selected from titanium ethanolate, butyl (tetra) titanate, isopropyl titanate, tin tetraethoxide, the stannous octoate ester, positive silane ethyl ester, methyl triacetoxysilane, methyltrimethoxy silane, diethylenetriamine base propyl trimethoxy silicane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-glycidyl ether oxygen base propyl group methyl dimethoxysilane, diethylenetriamine base propyl group methyl dimethoxysilane, N-methyl-3-aminopropyl trimethoxysilane, N, N-diethyl-3-aminopropyl trimethoxysilane, 3-aminopropyl methyl dimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, 3-(2-hydroxyethyl aminoethyl)-aminopropyl methyl dimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, vinyltrimethoxy silane, the 3-mercaptopropyl trimethoxysilane, 3-sulfydryl propyl group methyl dimethoxysilane, the acryloxy propyl trimethoxy silicane, methacryloxypropyl trimethoxy silane, methoxyl group is by in the displaced silane of Ethoxysilane one or both in the silane of tetramethoxy-silicane or the above-mentioned type.
Described stablizer is selected from benzotriazole, 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole, 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole, Octabenzone, 2-hydroxyl-4-methoxy benzophenone, N-(second-phenyl methyl ether, 2-hydroxyl-4-methoxy benzophenone, 2, the 4-dihydroxy benzophenone, 2-hydroxyl-4-methoxyl group oxygen base carbonyl phenyl)-N '-methyl-N '-phenyl methyl ether, N-(ethoxy carbonyl phenyl)-N '-ethyl-N '-5-sulfonic acid benzophenone, 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole, 1,1,3-three (2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane (antioxidant CA), triphenyl phosphite (TPP), a kind of in dibutyl tin laurate or the similar compounds, the mixture of two kinds or three kinds stablizers.
It is the commodity polymer material of transparent film that but described organic polymer comprises thermoplastic machine-shaping, for example: a kind of in polystyrene, polyethylene, polypropylene, polybutene, polymethacrylate, polycarbonate, polyvinyl acetate (PVA), polyethylene terephthalate, the polyvinyl chloride, or any 2～3 kinds of high molecular copolymerization, intermingling material in these macromolecular materials.
Described dispersion medium is a solvent, is selected from one or more the mixture etc. in ethanol, Virahol, glycerol, propyl carbinol, dimethylbenzene, dioxane, tetrahydrofuran (THF) (THF), dimethyl formamide (DMF), hexanaphthene, pimelinketone, chloroform, sherwood oil, ethyl acetate, N-BUTYL ACETATE, white oil, liquid paraffin, the polyvinyl alcohol.
Described dispersion agent is selected from one or more the mixture in organic acid, organic amino, the hydroxyl tensio-active agent.
Described organic acid is selected from one or more the mixture in caproic acid, laurostearic acid, TETRADECONIC ACID, phenylformic acid, the tartrate.
Described organic amino is selected from one or more the mixture in trolamine, triethylamine, diethanolamine, diethylamine, thanomin, diisopropanolamine (DIPA), butylamine, the dibutylamine.
Described hydroxyl tensio-active agent is selected from polyvinyl alcohol, polysorbate60, tween 80, Si Pan (SPAN) 60, the mixture of one or more in Si Pan (SPAN) 80, special polyoxyethylene octylphenol ether (Tritonx-100), the polyoxyethylene glycol.
Film thickness of the present invention is 5 microns～1 millimeter, preferred 5 microns～150 microns, has good visible transparent, and screening performance infrared, ultraviolet: visible light transmissivity is 20～95%, simultaneously can prevent that the infrared light more than 30% sees through in the sunlight, far-infrared light is also had reflection and control action kou.Film of the present invention can be compound with pressure sensitive adhesive, heat-sensitive glue, as the pad pasting of building glass, vehicle, steamer form, increases its sunlight control low radiance; For the double glazing assembly, can place between the layer glass, or attach to the one side of glass surface to hollow layer, increase the effect of its heat preservation energy-saving.Can to mounted glass and form be transformed and site operation, be subjected to place, weather, environmental limit little.
Film of the present invention also has static resistance and anti-electromagnetic-radiation performance.
Film of the present invention can the effect of compound other transparent film to obtain better sunlight control and to hang down the radiation heat preservation energy-saving.
The present invention has the advantage of face, site operation greatly, and it is limited many to overcome environmental pollution, construction that solution methods may have, and the relatively poor shortcoming of solution stability in storage; Overcome various sputtering methods, vacuum coating method disposable input height when preparation sunlight control low radiation film simultaneously, the cost height is to the restriction of substrate material, size.
The optical property of film is according to GB/T 2680-94, and GB/T18915.1-18915.29 measures by UV-4100 HITACHI SPECTROPHOTMETER; Pencil hardness is measured by the regulation of GB 6739; Sheltering coefficient is measured according to GB/T2680-94, and the U value is measured according to GB/T8484-2002.
Below in conjunction with embodiment technical scheme of the present invention is described in detail.
Description of drawings
Fig. 1. blank glass sample and the embodiment of the invention 5 film samples 0～2700nm Optical transmission spectrum figure.
Embodiment
Embodiment 1
(1) the thick product of Indium sesquioxide nano powder with the 3wt% tin dope bought mixes by the weight percent of showing 1-1 with DMF, pimelinketone, butylamine, tween 80, and to add diameter be that 0.8 millimeter zirconium white microballon carries out sand milling, isolate zirconium oxide bead, obtaining median size is the Indium sesquioxide uniform particles dispersive solution system of 25 nanometer tin dopes.
Table 1-1:
Form Weight percent (%)
The thick product of Indium sesquioxide nano powder of 3wt% tin dope 32.47
DMF 32.46
Pimelinketone 32.47
Butylamine 1.3
Tween 80 1.3
With the homodisperse solution system of the Indium sesquioxide of above-mentioned tin dope, polyvinyl chloride, vinyltrimethoxy silane, dioctyl phthalate (DOP), 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole, antioxidant CA and TPP are 2: 100: 2 according to weight ratio: 25: 1.5: 1.3: 0.5 mixed, and in vacuum drying oven, remove volatile small molecules solvent, obtain master batch, form as table 1-2.Weight percent among the table 1-2 refers to the shared ratio of each component in the master batch.
Table 1-2:
Form Weight percent (%)
Polyvinyl chloride 76.05
The Indium sesquioxide nano powder of tin dope 0.5
Vinyltrimethoxy silane 1.51
Dioctyl phthalate (DOP) 19.01
2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole 1.11
Antioxidant CA 0.91
TPP 0.91
(2) with master batch through twin screw 170～180 ℃ of plasticizings, 190～200 ℃ of T type heads are extruded, four-roll calendaring, the cylinder surface temperature is 165～175 ℃, rolling press operating line speed is 45～70m/min, obtains the film that thickness is 120 μ m.The film performance test result is as table 1-3, and the gained film can be compound with building glass, obtains sunlight control energy-saving glass.
Table 1-3
Visible light transmissivity (@550nm) (%) Sunshine Red external shield (%) Ultraviolet shielded (%) Pencil hardness
75 38 99 2H
Embodiment 2
(1) with the thick product of Indium sesquioxide nano powder of the 18wt% tin dope bought and dispersion medium and dispersion agent to show the 2-1 mixed, and fit diameter is that 0.8 millimeter zirconium white microballon carries out sand milling, isolate zirconium oxide bead, the Indium sesquioxide particle median size that obtains tin dope is the homodisperse solution systems of 80 nanometers.
Table 2-1:
Form Weight percent (%)
The thick product of the Indium sesquioxide of 18wt% tin dope 31.85
Pimelinketone 31.85
Chloroform 31.85
Laurostearic acid 1.27
This Pan 80 3.18
The homodisperse solution of Indium sesquioxide nanoparticle with above-mentioned tin dope, polyvinyl chloride, vinyltrimethoxy silane, dioctyl phthalate (DOP), 2-hydroxyl-4-methoxy benzophenone, antioxidant CA, TPP is 6: 100: 2 according to weight ratio: 30: 1.5: 1: 0.5 mixed, and in vacuum drying oven, remove volatile small molecules solvent, and obtain master batch, form as table 2-2.Weight percent among the table 2-2 refers to the shared ratio of each component in the master batch.
Table 2-2:
Form Weight percent (%)
Polyvinyl chloride 72.89
The Indium sesquioxide nano powder of tin dope 1.58
Vinyltrimethoxy silane 1.47
Dioctyl phthalate (DOP) 21.87
2-hydroxyl-4-methoxy benzophenone 1.09
Antioxidant CA 0.74
TPP 0.36
(2) with above-mentioned master batch through twin screw 170～190 ℃ of plasticizings, extrude at 190～200 ℃ of T type heads, four-roll calendaring, the cylinder surface temperature is 175～185 ℃, rolling press operating line speed is 30～40m/min, obtaining film thickness is 35 μ m.The gained film can be compound with building glass, obtains sunlight control energy-saving glass, and this glass properties test result is as table 2-3.
Table 2-3
Visible light transmissivity (@550nm) (%) Sunshine Red external shield (%) Ultraviolet shielded (%)
68 53 98
Embodiment 3
(1) makes the thick product of the adulterated tin oxide nano powder of 7wt% antimony certainly by aforementioned documents, mixed shown in this thick product is pressed with other composition of table 3-1, and be that 0.8 millimeter zirconium oxide bead is that the sand milling medium carries out sand milling with diameter, isolate zirconium oxide bead afterwards, obtain the adulterated tin oxide nano uniform particles of 7wt% antimony dispersion liquid, wherein the adulterated granules of stannic oxide median size of antimony is 50 nanometers.With the homodisperse solution of the adulterated tin oxide nano particulate of above-mentioned antimony, polystyrene, vinyltrimethoxy silane, epoxy soybean oil is 15: 100: 2 according to weight ratio: 2: 1.5 mixed, in vacuum drying oven, remove volatile small molecules solvent afterwards, obtain master batch, form as table 3-2.Weight percent among the table 3-2 refers to the shared ratio of each component in the master batch.
Table 3-1
Form Weight percent (%)
The thick product of the adulterated granules of stannic oxide nanometer of 7wt% antimony 24.15
THF 72.46
White oil 2.42
Butylamine 0.97
Table 3-2
Form Weight percent (%)
Polystyrene 91.52
The antimony-doped tin oxide nano powder 3.45
Vinyltriethoxysilane 1.83
Benzotriazole 1.83
Epoxy soybean oil 1.37
(2) with the master batch that obtains by 120～140 ℃ plasticate, 180～200 ℃ extrude (100MPa), adopt flat once step stretching method, 100～130 ℃ of draft temperatures make the film that thickness is 30 μ m.
A composite hot melt pressure sensitive adhesive at film, and be applied to building doors and windows glass, for being located in the room that BeiJing, China, 40 square metres of floor area of building, glass door and window area are 18 square metres independent heating (being single glass door and window), winter, indoor design temperature was not less than 20 ℃, saved heating energy consumption 15%; Summer, indoor design temperature was not higher than 28 ℃, saved electric power changes of air conditioners 27%.
This film is affixed on the white glass of 3mm, its The performance test results such as table 5.
Table 5
Visible light transmissivity (@550nm) (%) Sunshine Red external shield (%) Ultraviolet shielded (%) Pencil hardness
81 32 99 3H
Embodiment 4
(1) makes the thick product of the adulterated vanadium oxide nano powder of 3wt% tungsten certainly by aforementioned documents, with itself and dispersion medium and dispersion agent composition and mixed by table 4-1, fit diameter is that 0.8 millimeter zirconium oxide bead mixes, through sand milling, isolate zirconium oxide bead, obtaining median size is the homodisperse solution of the adulterated vanadium oxide nano particle of tungsten of 30nm.With this dispersion liquid, polystyrene, vinyltriethoxysilane, benzotriazole and epoxy soybean oil are 15: 100: 2 according to weight ratio: 2: 1.5 mixed, and drying under reduced pressure, obtain master batch, form as table 4-2.Weight percent among the table 4-2 refers to the shared ratio of each component in the master batch.
Table 4-1
Form Weight percent (%)
The thick product of the adulterated vanadium oxide nano powder of 3wt% tungsten 20.33
Hexanaphthene 60.98
Sherwood oil 16.26
Butylamine 0.41
Special polyoxyethylene octylphenol ether 2.02
Table 4-2
Form Weight percent (%)
Polystyrene 91.83
Tungsten doping vanadium oxide nano powder 2.97
Vinyltriethoxysilane 1.84
Benzotriazole 1.84
Epoxy soybean oil 1.52
(2) above-mentioned master batch by 120～140 ℃ plasticate, 180～200 ℃ extrude (100MPa), adopt flat once step stretching method, 100～130 ℃ of draft temperatures make the film that thickness is 20 μ m.The film performance test result is as table 4-3.
Table 4-3
Visible light transmissivity (@550nm) (%) Sunshine Red external shield (%) Ultraviolet shielded (%) Pencil hardness
67 41 42 2H
Embodiment 5
(1) the thick product of the adulterated tin oxide nano powder of 11wt% antimony is mixed with forming in the ratio of table 5-1 with dispersion medium and dispersion agent, fit diameter is that 0.8 millimeter zirconium oxide bead carries out sand milling, isolate zirconium oxide bead, obtaining median size is the adulterated tin oxide nano uniform particles of the antimony dispersive solution of 20nm.
Table 5-1
Form Weight percent (%)
The thick product of the adulterated tin oxide nano powder of 11wt% antimony 13.89
Dioxane 69.44
THF 13.89
Diethylamide 2.78
Dispersion liquid with above-mentioned nanoparticle, new LDPE (film grade), polystyrene, Octabenzone and 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole is 60: 100: 50 according to weight ratio: 2: 2 mixed, in vacuum drying oven, remove volatile small molecules solvent, obtain master batch, form as table 5-2.Weight percent among the table 5-2 refers to the shared ratio of each component in the master batch.
Table 5-2
Form Weight percent (%)
Polyethylene 60.98
Polystyrene 30.48
The adulterated tin oxide nano powder of antimony * 5.08
Octabenzone 1.73
2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole 1.73
(2) master batch is plasticated by 140～180 ℃, the method that adopts T type head to extrude curtain coating prepares film, and extrusion temperature is 200～220 ℃, makes the film of thickness 20 μ m.
The optics spectrogram as shown in Figure 1.Can be applicable to vehicle glass, save the fuel cost of automative air conditioning.Be affixed on 5mm individual layer white glass by polyester hot-melt adhesive, the sunlight sheltering coefficient is 0.67, and the U value is 5.1, and pencil hardness is 4H.
Embodiment 6
(1) with the 2.1wt% antimony of the buying thick product of adulterated tin oxide nano powder and dispersion medium and dispersion agent mixed by table 6-1, fit diameter is that 1.2 millimeters zirconium oxide bead carries out sand milling, isolate zirconium oxide bead, obtaining median size is the antimony-doped tin oxide uniform particles dispersive solution of 100 nanometers.With this dispersion liquid, new LDPE (film grade), Octabenzone, benzotriazole is 100: 100: 4 according to weight ratio: 2 mixed, and drying under reduced pressure, obtain master batch, form as table 6-2.Weight percent among the table 6-2 refers to the shared ratio of each component in the master batch.
Table 6-1
Form Weight percent (%)
The thick product of the adulterated tin oxide nano powder of 2.1wt% antimony 31.75
Dimethylbenzene 63.49
Dibutylamine 1.59
Polyvinyl alcohol 3.17
Table 6-2
Form Weight percent (%)
Polyethylene 73.16
The adulterated tin oxide nano powder of antimony 22.63
Octabenzone 2.81
Benzotriazole 1.4
(2) master batch is plasticated by 140～180 ℃, and the method that adopts T type head to extrude curtain coating prepares film, and extrusion temperature is 200～220 ℃, makes the film of thickness 5 μ m, is used for the low radiation insulation film made of sunlight control.
Embodiment 7
Embodiment 5 resulting films are compound with the polyester film and the heat-sensitive glue that are coated with the thick aluminium film of 10nm with magnetically controlled sputter method, can be as the low radiation pad pasting of sunlight control and the energy-conservation pad pastings of automobile heat insulation of building glass, and energy-saving effect can increase about 10%.
Embodiment 8
(1) with the 9wt% fluorine of the buying thick product of adulterated tin oxide nano powder and dispersion medium and dispersion agent composition and mixed by table 8-1, fit diameter is that 0.8 millimeter zirconium oxide bead carries out sand milling, isolate zirconium oxide bead then, obtaining median size is the adulterated tin oxide nano dispersion liquid of 9wt% fluorine of 20 nanometers.With this fluorine-doped tin oxide uniform particles dispersive solution, new LDPE (film grade), polypropylene, Octabenzone, 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole is 100: 20: 100 according to weight ratio: 2: 2 mixed, drying under reduced pressure obtains master batch, forms as table 8-2.Weight percent among the table 8-2 refers to the shared ratio of each component in the master batch.
Table 8-1
Form Weight percent (%)
The thick product of the adulterated tin oxide nano powder of 9wt% fluorine 10.63
Dimethylbenzene 85.11
Dibutylamine 2.13
Polyvinyl alcohol 2.13
Table 8-2
Form Weight percent (%)
Polypropylene 72
Polyethylene 16.8
The adulterated tin oxide nano powder of fluorine 7.84
Octabenzone 1.68
2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole 1.68
(2) master batch is plasticated by 140～180 ℃, and the method that adopts T type head to extrude curtain coating prepares film, and extrusion temperature is 200～220 ℃, and the sunlight that makes thickness 50 μ m is controlled energy-conservation film.
Embodiment 9:
The method of employing embodiment 1 and embodiment 3 obtains the Indium sesquioxide and the adulterated tin oxide nano dispersion soln of antimony of tin dope respectively, and with them and polypropylene, Octabenzone is 50: 50: 100 according to weight ratio: drying under reduced pressure behind 2 the ratio thorough mixing, obtain master batch, form as table 9-1.Weight percent among the table 9-1 refers to the shared ratio of each component in the master batch.
Table 9-1
Form Weight percent (%)
Polypropylene 76.08
Tin-doped indium oxide nano powder (among the embodiment 1) 12.88
Antimony-doped tin oxide nano powder (among the embodiment 3) 9.52
Octabenzone 1.52
Master batch is plasticated by 140～180 ℃, and the method that adopts T type head to extrude curtain coating prepares film, and extrusion temperature is 200～220 ℃, makes the film of thickness 30 μ m.The film performance test result is shown in table 9-2.
Table 9-2:
Visible light transmissivity (@500nm) (%) Sunshine Red external shield (%) Ultraviolet shielded (%) Pencil hardness
82 63 78 3H
Embodiment 10
(1) adopt the method for embodiment 4 to make the adulterated vanadium oxide nano dispersion fluid of 3wt% tungsten, and and new LDPE (film grade), Octabenzone, 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole, antioxidant CA was according to 10: 100: 2: behind 4: 0.1 the ratio thorough mixing, drying under reduced pressure obtains master batch, forms as table 10.Weight percent in the table 10 refers to the shared ratio of each component in the master batch.
Table 10
Form Weight percent (%)
Polyethylene 92.34
The adulterated vanadium oxide nano powder of tungsten (among the embodiment 4) 1.97
Octabenzone 1.89
2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole 3.71
Antioxidant CA 0.09
(2) master batch is plasticated by 140～180 ℃, and the method that adopts T type head to extrude curtain coating prepares film, and extrusion temperature is 200～220 ℃, makes the film of thickness 16 μ m.When temperature rising or sunlight grow, the ability of this thin-film barrier and the heat that flashes back the sunlight increases, and is applied on the building glass, thereby controls in the heat inlet chamber in summer, reaches the effect of saving the air-conditioning expense.

Claims (10)

1. the radiation transparent film is hanged down in a sunlight control, it is characterized in that: the component of the low radiation transparent film of described sunlight control comprises the organic polymer of 70～99.9wt%, the adulterated metal oxide nanoparticles of 0.1～30wt% and the auxiliary agent of 0～29.9wt%;
The metal oxide of described adulterated metal oxide nanoparticles is selected from one or more the mixture in Indium sesquioxide, stannic oxide, zinc oxide, Cadmium oxide, titanium oxide, the vanadium oxide;
Adulterated metal is selected from one or more the mixture in tin, gallium, antimony, titanium, tungsten, copper, iron, the zirconium in the described Indium sesquioxide; The mol ratio of indium is 0.1～20: 100 in doping metals and the Indium sesquioxide;
Adulterated metal is selected from one or more the mixture in antimony, fluorine, phosphorus, titanium, cobalt, zinc, tungsten, manganese, cerium, tellurium, iron, gold and silver, the platinum in the described stannic oxide; The mol ratio of tin is 0.1～20: 100 in doping metals and the stannic oxide;
Adulterated metal is selected from one or more the mixture in aluminium, antimony, bismuth, tin, titanium, indium, copper, iron, cadmium, tungsten, lithium, manganese, magnesium, gallium, cerium, the silver in the described zinc oxide; The mol ratio of doping metals and zinc in zinc oxide is 0.1～20: 100;
Adulterated metal is selected from one or more the mixture in tin, lanthanum, bismuth, fluorine, tungsten, the copper in the described Cadmium oxide; The mol ratio of cadmium is 0.1～20: 100 in doping metals and the Cadmium oxide;
Adulterated metal is selected from one or more the mixture in niobium, tin, zinc, the lanthanum in the described titanium oxide; The mol ratio of titanium is 0.1～20: 100 in doping metals and the titanium oxide;
Metal in the described doping vanadium oxide is selected from one or more the mixture in tin, titanium, fluorine, tungsten, the copper; The mol ratio of vanadium is 0.1～20: 100 in doping metals and the vanadium oxide;
Described auxiliary agent is selected from one or more the mixture in softening agent, coupling agent, the stablizer.
2. transparent film according to claim 1 is characterized in that: the particle diameter of described adulterated metal oxide nanoparticles is smaller or equal to 200nm.
3. transparent film according to claim 1 is characterized in that: described softening agent is selected from one or more the mixture in dibutyl phthalate, dioctyl phthalate (DOP), di-sec-octyl phthalate, Dinonylphthalate, dimixo-octyl phthalate, DID Su, Octyl adipate, trioctyl phosphate, n-butyl stearate, polypropylene adipate (PPA), octyl epoxy stearate, the epoxy soybean oil.
4. transparent film according to claim 1, it is characterized in that: described coupling agent is selected from titanium ethanolate, butyl (tetra) titanate, isopropyl titanate, tin tetraethoxide, the stannous octoate ester, positive silane ethyl ester, methyl triacetoxysilane, methyltrimethoxy silane, diethylenetriamine base propyl trimethoxy silicane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, 3-glycidyl ether oxygen base propyl group methyl dimethoxysilane, diethylenetriamine base propyl group methyl dimethoxysilane, N-methyl-3-aminopropyl trimethoxysilane, N, N-diethyl-3-aminopropyl trimethoxysilane, 3-aminopropyl methyl dimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, 3-(2-hydroxyethyl aminoethyl)-aminopropyl methyl dimethoxysilane, 3-(2-aminoethyl)-aminopropyl trimethoxysilane, vinyltrimethoxy silane, the 3-mercaptopropyl trimethoxysilane, 3-sulfydryl propyl group methyl dimethoxysilane, the acryloxy propyl trimethoxy silicane, methacryloxypropyl trimethoxy silane, methoxyl group is by in the displaced silane of Ethoxysilane one or both in the silane of tetramethoxy-silicane or the above-mentioned type.
5. transparent film according to claim 1, it is characterized in that: described stablizer is selected from benzotriazole, 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole, 2-(2 ' hydroxyl-5 '-aminomethyl phenyl) benzotriazole, Octabenzone, 2-hydroxyl-4-methoxy benzophenone, N-(second-phenyl methyl ether, 2-hydroxyl-4-methoxy benzophenone, 2, the 4-dihydroxy benzophenone, 2-hydroxyl-4-methoxyl group oxygen base carbonyl phenyl)-N '-methyl-N '-phenyl methyl ether, N-(ethoxy carbonyl phenyl)-N '-ethyl-N '-5-sulfonic acid benzophenone, 2-(2 '-hydroxyl-the 3 '-tertiary butyl-5 '-aminomethyl phenyl)-5-chlorinated benzotriazole, 1,1,3-three (2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane, triphenyl phosphite, a kind of in the dibutyl tin laurate, the mixture of two kinds or three kinds stablizers.
6. transparent film according to claim 1, it is characterized in that: described organic polymer is selected from a kind of in polystyrene, polyethylene, polypropylene, polybutene, polymethacrylate, polycarbonate, polyvinyl acetate (PVA), polyethylene terephthalate, the polyvinyl chloride or any 2～3 kinds of high molecular copolymerization, intermingling material in these macromolecular materials.
7. preparation method according to each described transparent film of claim 1～6, it is characterized in that: this method may further comprise the steps:
(1). the thick product of adulterated metallic oxide nano powder is dispersed in the dispersion medium, and adding dispersion agent anabolic reaction system, the thick product of adulterated metal-oxide powder is 5～40wt% in the system, and dispersion medium is 59.5～94.5wt%, and dispersion agent is 0.5～5wt%; Through sand milling, obtain the dispersion liquid of adulterated metal oxide nanoparticles;
(2). add organic polymer and auxiliary agent in the dispersion liquid of the adulterated metal oxide nanoparticles that step (1) is prepared, after fully stirring, mixing, drying under reduced pressure obtains master batch;
Contain the organic polymer of 70～99.9wt%, the adulterated metal oxide nanoparticles of 0.1～30wt% and the auxiliary agent of 0～29.9wt% in the described master batch;
(3). the master batch that step (2) is obtained by extrusion-blown modling, calendering, stretch or extrude to water and mould, prepare the low radiation heat preservation energy-saving film of sunlight control.
8. method according to claim 7 is characterized in that: described dispersion medium is selected from one or more the mixture in ethanol, Virahol, glycerol, propyl carbinol, dimethylbenzene, dioxane, tetrahydrofuran (THF), dimethyl formamide, hexanaphthene, pimelinketone, chloroform, sherwood oil, ethyl acetate, N-BUTYL ACETATE, white oil, liquid paraffin, the polyvinyl alcohol;
Described dispersion agent is selected from one or more the mixture in organic acid, organic amino, the hydroxyl tensio-active agent.
9. method according to claim 8 is characterized in that: described organic acid is selected from one or more the mixture in caproic acid, laurostearic acid, TETRADECONIC ACID, phenylformic acid, the tartrate;
Described organic amino is selected from one or more the mixture in trolamine, triethylamine, diethanolamine, diethylamine, thanomin, diisopropanolamine (DIPA), butylamine, the dibutylamine;
Described hydroxyl tensio-active agent is selected from polyvinyl alcohol, polysorbate60, tween 80, this Pan 60, the mixture of one or more in this Pan 80, special polyoxyethylene octylphenol ether, the polyoxyethylene glycol.
10. a sunlight according to claim 1 is controlled the purposes of hanging down the radiation transparent film, it is characterized in that: low radiation transparent film of described sunlight control and pressure sensitive adhesive, heat-sensitive glue are compound, as the pad pasting of building glass, vehicle, steamer form, increase its sunlight control low radiance.
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