CN117106215A - Film for reducing heat radiation rate, composite film and preparation method thereof - Google Patents
Film for reducing heat radiation rate, composite film and preparation method thereof Download PDFInfo
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- CN117106215A CN117106215A CN202310836847.2A CN202310836847A CN117106215A CN 117106215 A CN117106215 A CN 117106215A CN 202310836847 A CN202310836847 A CN 202310836847A CN 117106215 A CN117106215 A CN 117106215A
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- 239000002131 composite material Substances 0.000 title claims abstract description 116
- 230000005855 radiation Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 23
- 238000002834 transmittance Methods 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims description 81
- 239000011347 resin Substances 0.000 claims description 79
- 229920005989 resin Polymers 0.000 claims description 79
- 229920002367 Polyisobutene Polymers 0.000 claims description 77
- 239000000463 material Substances 0.000 claims description 76
- 229910044991 metal oxide Inorganic materials 0.000 claims description 73
- 150000004706 metal oxides Chemical class 0.000 claims description 73
- 239000004698 Polyethylene Substances 0.000 claims description 67
- 229920000573 polyethylene Polymers 0.000 claims description 67
- -1 polyethylene Polymers 0.000 claims description 63
- 238000000034 method Methods 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 36
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 24
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 23
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 229910003437 indium oxide Inorganic materials 0.000 claims description 10
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 8
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 239000004417 polycarbonate Substances 0.000 claims description 5
- 229920000515 polycarbonate Polymers 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims description 4
- 229910001887 tin oxide Inorganic materials 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
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- 239000010408 film Substances 0.000 description 245
- 239000010410 layer Substances 0.000 description 175
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 63
- 239000002585 base Substances 0.000 description 50
- 239000011521 glass Substances 0.000 description 36
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- 229910052709 silver Inorganic materials 0.000 description 7
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 6
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- 239000007888 film coating Substances 0.000 description 6
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- 238000001755 magnetron sputter deposition Methods 0.000 description 6
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- 239000007789 gas Substances 0.000 description 5
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 5
- 238000010030 laminating Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 5
- 238000011160 research Methods 0.000 description 5
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- 238000010008 shearing Methods 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- OAMZXMDZZWGPMH-UHFFFAOYSA-N ethyl acetate;toluene Chemical compound CCOC(C)=O.CC1=CC=CC=C1 OAMZXMDZZWGPMH-UHFFFAOYSA-N 0.000 description 3
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000004134 energy conservation Methods 0.000 description 2
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
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- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical group CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- 229920010126 Linear Low Density Polyethylene (LLDPE) Polymers 0.000 description 1
- 206010051246 Photodermatosis Diseases 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
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- 238000010538 cationic polymerization reaction Methods 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005949 ozonolysis reaction Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/06—Polyethene
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2333/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2333/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/06—Polyethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08J2423/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention discloses a film for reducing heat radiation rate, a composite film and a preparation method thereof, wherein the film has the transmittance of sunlight in a wave band of 350-2500 nanometers not lower than 80 percent, the heat radiation rate of sunlight in a wave band of 2.5-100 micrometers not higher than 0.15 and the heat conductivity coefficient not higher than 0.35 w/m.k.
Description
Technical Field
The invention relates to a film for reducing heat emissivity, a composite film and a preparation method thereof.
Background
The energy consumption in the building industry is more than 26% of the primary energy. In hot and humid areas, the consumption of building energy is more remarkable, accounting for about 1/3 to 1/2 of the total national power. The electricity consumption of the unit building area in the residence year is 10-20kwh, the electricity consumption of the public building is much higher, the electricity consumption of the unit building area in the whole year can exceed 350kwh, and 60% of the building energy consumption is dissipated through glass doors and windows.
According to the energy transmitted through the glass formula (1):
Q ＝630 * Sc+ U *(T inner part －T Outer part ) (1)；
Q: heat transferred through the glass;
sc: a shading coefficient reflecting a shading effect on sunlight;
u: the heat transfer coefficient, W/. Multidot.K, is related to the test conditions.
U represents the thermal conductivity, with smaller values indicating less blackbody radiation heat exchange through the glass. With the increasing energy saving requirements of buildings, the less heat is required to be exchanged through the glass, the better the lower the U or K value of the glass. And the heat conduction coefficient of the single glass in unit square meter area is about 5.6-6.4w/m.K, the heat conduction coefficient of air is as low as 0.0244w/m.K, and the heat conduction coefficient of argon inert gas is as low as 0.0173w/m.K. Based on the above, vacuum glass, hollow glass, or even three-glass two-cavity and four-glass three-cavity hollow glass becomes a common means for reducing heat transfer of door and window glass. The energy transfer of the hollow glass is three modes, namely: radiation transfer, convection transfer, and conduction transfer.
Wherein, formula (2) of radiant heat transfer: h is a T ＝4σx(1/ε 1 +1/ε 2 -1) -1 xT m 3 ；
h T : radiation heat transfer;
ε 1 epsilon 2 : emissivity of the glass surface.
Based on the above, it can be seen that the heat radiation coefficient ε 1 Epsilon 2 The larger the radiation heat transfer, the larger the glass heat transfer, and the lower the heat radiation coefficient of the hollow glass cavity surface, the larger the influence on the reduction of U value is. The emissivity of common glass is 0.84, while the emissivity of the surface of the three-silver low glass can be as low as 0.05. For a 6 mm glass, a hollow glass with a cavity of 12 mm is prepared, for exampleIf the heat radiation value of the inner surface of one glass sheet is reduced from 0.84 to 0.1, the heat transfer coefficient of the hollow glass sheet is reduced from 2.8w/m.K to 1.762.8w/m.K.
The introduction of one or more low emissivity thermal shields between the two surfaces of the glass is an important way to reduce the radiative heat transfer of the gas.
Introducing a resin film between two glass sheets, then the radiation heat transfer formula (3) of the gas:
h T ＝4σx(1/ε 1 +1/ε 2 +2/ε 3 -1) -1 xT m 3 (3)；
ε 3 is the emissivity of the resin film.
Similarly, the surface emissivity of the common glass is 0.84, and based on the above formula, it can be seen that if a transparent heat shielding film with a surface emissivity of 0.1 is introduced between the glass, the radiation heat transfer of the gas is reduced to 6%, and the surface emissivity of the visible heat shielding resin film has a great influence on the radiation heat transfer of the gas.
Common optical resins have a emissivity epsilon 3 About 0.9, the surface emissivity of metallic silver is 0.02 and the surface emissivity of aluminum is 0.05. Therefore, metallic silver, gold or aluminum with nanometer thickness is commonly evaporated or magnetron sputtered on the surface of glass or resin films such as (PET) to reduce the emissivity of the material, so as to prepare low-e glass or low-e functional films (as shown in FIG. 3). However, metals such as silver and aluminum are not stable and are easily oxidized by air, and other metal oxides are often required to protect the silver layer.
Alternatively, the low emissivity product prepared by evaporating or magnetron sputtering indium tin oxide, zinc oxide and zinc doped aluminum oxide with nanometer thickness on the surface of glass or optical film in the prior art, however, the preparation by the method needs to be carried out under vacuum condition and needs high-temperature post-treatment, so the method for preparing low-e glass or functional film has complex process,
the equipment is expensive, inefficient and difficult to produce to scale (products with film widths exceeding 3 meters).
Therefore, the composite functional film with low emissivity and high solar transmittance, which is prepared by the functional polymer and the nano material, has the advantages of simple processing technology, low energy consumption, easy mass production, low price and great significance for building energy conservation.
Disclosure of Invention
1. Problems to be solved
A first object of the present invention is to provide a film and a composite film which can reduce the emissivity of heat and have high solar transmittance.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
based on the first object of the present invention, it is a further object to provide a simple method for producing a membrane.
In accordance with a first object of the present invention, a film for reducing emissivity of heat, the film comprising a layer a,
the layer a includes a resin material and metal oxide particles;
wherein,
the thickness of the layer a is 0.5-10 microns, preferably 1-5 microns, most preferably 1-2 microns;
the resin material of the layer a contains metal oxide particles.
The heat emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the ratio of the resin material to the metal oxide, calculated as weight ratio, is a: b= (2-4): 1-3; preferably, the ratio of the resin material to the metal oxide is A:B= (2.2-3.5): 1.5-2.8.
The heat emissivity-reducing film according to any one of the embodiments of the first aspect of the invention has a mass density of 2.1 to 6.1g/m, calculated as layer a having a thickness of 1.0 micron 2 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the film has a mass density of 3.0 to 5.5g/m 2 。
The heat emissivity-reducing film according to any embodiment of the first aspect of the invention, the metal oxide comprises 40 to 80wt%.
The heat emissivity reducing film according to any one of the embodiments of the first aspect of the invention, the metal oxide comprises 45 to 60wt%.
The heat emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the resin material comprises 20 to 60wt%.
The heat emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the resin material comprises 25 to 40wt%.
The heat emissivity reducing film according to any embodiment of the first aspect of the invention, the resin comprises polyethylene.
According to any embodiment of the first aspect of the present invention, the heat emissivity reducing film, the resin comprises polyisobutylene.
The heat emissivity reducing film according to any one of the embodiments of the first aspect of the invention, the resin comprises polyethylene and polyisobutylene, and the mass ratio of polyethylene to polyisobutylene is C: d= (16-19): (1-4); preferably, the mass ratio of the polyethylene to the polyisobutene is C:D= (18-15): 2-5.
The heat emissivity-reducing film according to any one of the embodiments of the first aspect of the invention, ignoring impurities, the resin consists of polyethylene and polyisobutylene, and the mass ratio of polyethylene to polyisobutylene is C: d= (16-19): (1-4); preferably, the mass ratio of the polyethylene to the polyisobutene is C:D= (18-15): 2-5.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the metal oxide comprising: one or two or more of tin-containing indium oxide, aluminum-containing zinc oxide, and fluorine-containing tin oxide.
The heat emissivity-reducing film according to any of the embodiments of the first aspect of the invention, the metal oxide having a particle size of no more than 120 nm.
The heat emissivity reducing film according to any one of the embodiments of the first aspect of the invention, the metal oxide having a particle size of 5-120 nm.
The heat emissivity reducing film according to any one of the embodiments of the first aspect of the invention, the metal oxide having a particle size of 10-50 nm.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the a layer comprising a base structure layer, and metal oxide particles;
The base structure layer contains a resin material, and the metal oxide particles are present inside the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the a layer comprising a base structure layer, and metal oxide particles;
the base structure layer contains a resin material, and the metal oxide particles are present in the interior of the base structure layer and the surface of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyethylene; the amount of polyethylene is not less than 15wt% of the total amount of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyethylene; the amount of polyethylene is not more than 57% of the total amount of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyisobutylene; the amount of polyisobutene is not less than 1% of the total amount of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyisobutylene; the amount of polyisobutene is not more than 5% of the total amount of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyethylene and polyisobutylene; the sum of the amounts of polyethylene and polyisobutylene is not less than 20wt% of the total amount of the base structure layer.
A heat emissivity reducing film in accordance with any one of the embodiments of the first aspect of the invention, the base structure layer comprising polyethylene and polyisobutylene; the sum of the amounts of polyethylene and polyisobutylene does not exceed 60wt% of the total amount of the base structure layer.
A heat-emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the film having a solar light transmittance of not less than 80% in the 350-2500 nm wavelength band.
A heat emissivity reducing film according to any embodiment of the first aspect of the invention, the film having a heat emissivity in the 2.5 to 100 micron band of no more than 0.15.
A reduced emissivity film of any of the embodiments of the first aspect of the invention, the film having a thermal conductivity of no more than 0.35 w/m.k.
A heat-radiation rate-reducing film according to any one of the embodiments of the first aspect of the present invention, which has a transmittance of sunlight in the wavelength band of 350 to 2500 nm of not less than 80%; and the film has a emissivity of heat in the 2.5-100 micron band of no more than 0.15.
A heat-radiation rate-reducing film according to any one of the embodiments of the first aspect of the present invention, which has a transmittance of sunlight in the wavelength band of 350 to 2500 nm of not less than 80%; and the film has a thermal conductivity of no more than 0.35 w/m.k.
A heat emissivity-reducing film according to any embodiment of the first aspect of the invention, the film having a heat emissivity in the 2.5-100 micron band of no more than 0.15; and the film has a thermal conductivity of no more than 0.35 w/m.k.
A heat-radiation rate-reducing film according to any one of the embodiments of the first aspect of the present invention, which has a transmittance of sunlight in the wavelength band of 350 to 2500 nm of not less than 80%; and the film has a emissivity of heat in the 2.5-100 micron band of no more than 0.15; and the film has a thermal conductivity of no more than 0.35 w/m.k.
A heat-emissivity-reducing film according to any one of the embodiments of the first aspect of the invention, the film having a solar light transmittance of not less than 84% in the 350-2500 nm wavelength band.
A heat-emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the film having a solar light transmittance of not less than 85% in the 350-2500 nm wavelength band.
A heat-emissivity-reducing film according to any one of the embodiments of the first aspect of the present invention, the film having a solar light transmittance of not less than 90% in the 350-2500 nm wavelength band.
A reduced emissivity film of any of the embodiments of the first aspect of the invention, the film having a thermal conductivity of no more than 0.3 w/m.k.
Based on the first object of the present invention, a second aspect of the present invention provides a method for producing a film containing a reduced emissivity to heat as described in any one of the above, comprising the steps of:
1) Preparing a mixture containing a resin material and metal oxide particles;
2) The mixture is prepared into a film.
Based on a second object of the present invention, a first aspect of the present invention provides a composite film comprising a reduced emissivity film of any one of the above, comprising a B layer;
the layer B includes a resin material;
wherein,
the thickness of the layer B is 20-1000 micrometers.
A heat emissivity reducing composite film according to any one of the first aspects of the second aspect of the invention, the composite film comprising a layer a, a layer B
The a layer comprises the composite film comprising any of the heat emissivity-reducing films described above;
the layer B includes a resin material and has a light transmittance of not less than 80% and a thickness of 20 to 1000 μm.
The heat radiation rate reducing composite film according to any one of the embodiments of the second aspect of the present invention, the resin material includes one, or two, or more of polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polymethyl methacrylate (PMMA), polyurethane (PU), polystyrene (PS), polycarbonate (PC).
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film comprising a layer a and a layer B;
the combination mode of the A layer and the B layer comprises a combination mode of forming an AB structure.
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film comprising a layer a and a layer B;
the bonding means of the A layer and the B layer comprises bonding means forming an ABA structure.
The ABA structure according to the first aspect of the second object of the present invention, wherein the ABA structure has one a layer of the same type.
The composite film for reducing emissivity of heat according to any one of the first aspect of the second object of the present invention, in which the ABA structure has two a layers of different types, a 1 BA 2 . Wherein A is 1 Layer a in one particular form; a is that 2 Is different from A 1 In another specific form of layer a.
A heat-emissivity-reducing composite film according to any one of the first aspects of the second object of the present invention has a solar light transmittance of not less than 80% in a wavelength band of 350 to 2500 nm.
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film having a heat emissivity in the 2.5-100 micron band of no more than 0.15.
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film having a thermal conductivity of not more than 0.35 w/m.k.
According to the first aspect of the second object of the present invention, the composite film having a heat emissivity reduced, the composite film having a solar light transmittance of not less than 80% in the 350-2500 nm wavelength band, and a heat emissivity of not more than 0.15 in the 2.5-100 μm wavelength band.
A heat-emissivity-reducing composite film according to any one of the embodiments of the second aspect of the present invention, the composite film having a solar light transmittance of not less than 80% in the 350-2500 nm wavelength band, and the composite film having a thermal conductivity of not more than 0.35 w/m.k.
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film having a heat emissivity of no more than 0.15 at a wavelength band of 2.5 to 100 microns, and the composite film having a thermal conductivity of no more than 0.35 w/m.k.
A heat-emissivity-reducing composite film according to any one of the first aspects of the second object of the present invention has a solar light transmittance of not less than 85% in a wavelength band of 350 to 2500 nm.
A heat emissivity reducing composite film according to any one of the embodiments of the first aspect of the second object of the invention, the composite film having a thermal conductivity of not more than 0.3 w/m.k.
Based on the second object of the present invention, a second aspect of the present invention provides a method for producing a composite film comprising a reduced emissivity to heat as described in any one of the above, comprising the steps of:
1) Preparing a layer B;
2) Preparing a material required for forming the layer a, the material including a mixture containing a resin material, metal oxide particles;
2) And coating the mixture on the surface of the layer B to prepare a film.
The method for preparing a composite film for reducing emissivity of heat according to any one of the embodiments of the second aspect of the second object of the present invention, if the resin material contains both polyethylene and polyisobutylene, the step 2) includes:
mixing polyisobutylene with metal oxide particles, adding an organic solvent to properly adjust the viscosity of the mixture, and uniformly mixing the mixture;
toluene removal treatment is carried out, and polyethylene is added to obtain an initial composite material;
finally, extruding and granulating by a double-screw extruder;
the step 3) includes: and (3) carrying out film coating on the final composite material obtained by granulation through an extrusion film coating compound machine, and forming a film (layer A) for reducing the heat emissivity on the surface of the layer B.
The method for preparing a composite film for reducing emissivity of heat according to any one of the embodiments of the second aspect of the second object of the present invention, if the resin material contains both polyethylene and polyisobutylene, the step 2) includes:
mixing polyisobutylene with metal oxide particles, adding an organic solvent to properly adjust the viscosity of the mixture, and uniformly mixing the mixture;
adding polyethylene for uniformly mixing to obtain an initial composite material;
the step 3) includes: the initial composite material was printed by inkjet printing to form a film (layer a) on the surface of layer B that reduced the emissivity of heat.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The present invention provides a novel film capable of reducing emissivity of heat, the film comprising: under the synergistic effect of the functional polymer material resin with low emissivity and specific metal oxide particles, the solar light transmittance of the film in the solar light 350-2500 nanometer wave band is not lower than 80 percent, and the heat conductivity coefficient is not higher than 0.35w/m.K; the emissivity of heat in the 2.5-100 micron band is not more than 0.15.
(2) The invention provides a novel composite film capable of reducing heat emissivity, which comprises a layer A and a layer B;
The A layer has low-emissivity functional polymer material resin and specific metal oxide particles, under the synergistic effect of the functional polymer material resin and the specific metal oxide particles, the solar light transmittance of the A layer in a solar light 350-2500 nanometer wave band is not lower than 80%, the heat conductivity coefficient is not more than 0.35w/m.K, and the heat emissivity in a 2.5-100 micrometer wave band is not more than 0.15;
the B layer is made of a high solar transmittance resin and it helps to improve mechanical strength, thermal stability, dimensional stability, and environmental aging properties and weatherability provided by the composite film.
(3) The method for preparing the glass or the film with low emissivity in the prior art is to prepare silver, gold, copper, aluminum or indium tin oxide with nanometer thickness on the surface of the glass or the resin film by magnetron sputtering or vacuum evaporation; the film layer prepared by magnetron sputtering or vacuum evaporation needs to be treated at high temperature to obtain the functional film layer with high compactness and smooth surface. The prepared film is usually required to be subjected to heat treatment at a high temperature of 400-600 ℃, the method has high energy consumption, large equipment investment, high equipment requirements, complex process and low production efficiency, and the wide-width product exceeding 1.5 meters is difficult to prepare; particularly, for vapor deposition to polymer films such as (PET) products, the temperature resistance of the polymer is difficult to exceed 150 ℃ in general, and thus, it is difficult to prepare high-performance low-radiation films;
The preparation method of the film (or composite film) capable of reducing the heat emissivity provided by the invention has the advantages of simpler processing technology, low equipment investment, easiness in continuous and efficient mass production, low energy consumption in the production process, and capability of preparing films (or composite films) with the width of more than 3 meters, which is difficult to reach by the traditional magnetron sputtering method.
Drawings
FIG. 1 is a solar spectrum and a blackbody radiation thermal spectrum;
FIG. 2 is a graph showing solar transmittance of a pure PE film (thickness 10 μm) and a pure PET film (thickness 10 μm) prepared from the low-density polyethylene and polyisobutylene respectively in example 1;
fig. 3 is a graph of solar transmittance of low emissivity silver coated glass.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
As used herein, the term "about" is used to provide the flexibility and inaccuracy associated with a given term, metric or value. The degree of flexibility of a particular variable can be readily determined by one skilled in the art.
Concentrations, amounts, percentages, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of about 1 to about 4.5 should be interpreted to include not only the explicitly recited limits of 1 to about 4.5, but also include individual numbers (such as 2, 3, 4) and subranges (such as 1 to 3, 2 to 4, etc.). The same principle applies to ranges reciting only one numerical value, such as "less than about 4.5," which should be construed to include all such values and ranges. Moreover, such an interpretation should apply regardless of the breadth of the range or the characteristics being described.
[ film for reducing emissivity of Heat ]
The film for reducing the heat radiation rate comprises an A layer, wherein the A layer comprises a resin material and metal oxide particles, the resin material of the A layer contains the metal oxide particles, and the thickness of the A layer is 0.5-10 microns; the film comprising the layer A has a transmittance of not less than 80%, a emissivity of not more than 0.15, and a thermal conductivity of not more than 0.35w/m.k under the condition of sunlight in a wavelength band of 350 to 2500 nm.
As used herein, "300-2500 nm sunlight" is classified as ultraviolet, visible, and near infrared. The wavelength is 300-380 nm, ultraviolet light, visible light and near infrared light, respectively, and the wavelength is 380-760 nm, 760-2500 nm. When the solar light irradiates the object surface, as in fig. 1, it is converted into blackbody radiation heat by the object coefficient, and all the objects radiate outward. Taking room temperature of 25 degrees as an example, the maximum value of the blackbody radiation peak is 10 microns, so that the building energy conservation requires materials with low radiation rate of 8-20 microns.
As described above, as the resin material participating in the a layer constituting the film of the present invention, polyethylene is included; alternatively, the resin comprises polyisobutylene; alternatively, the resin includes polyethylene and polyisobutylene.
If the resin comprises both polyethylene and polyisobutylene, the ratio of the two can be defined as C: d= (16-19) in terms of mass ratio: (1-4); preferably, the ratio of the two can be defined as C and D= (18-15) and (2-5).
As the ratio C:D of the polyethylene to the polyisobutene:
the magnitude of the C value may be any value taken from any of the following sets of value ranges: 16-19, 16-18.5, 16-18, 16-17.5, 16-17, 16-16.5, 16.5-19, 16.5-18.5, 16.5-18, 16.5-17.5, 16.5-17, 17-19, 17-18.5, 17-18, 17-17.5, 17.5-19, 17.5-18.5, 17.5-18, 18-19, 18-18.5, 18.9-19.
The D value may be any value from any of the following sets of value ranges: 1-4, 1-3.8, 1-3.5, 1-3.2, 1-3, 1-2.8, 1-2.5, 1-2.2, 1-2, 1-1.8, 1-1.5, 1-1.2;1.2-4, 1.2-3.8, 1.2-3.5, 1.2-3.2, 1.2-3, 1.2-2.8, 1.2-2.5, 1.2-2.2, 1.2-2, 1.2-1.8, 1.2-1.5;1.5-4, 1.5-3.8, 1.5-3.5, 1.5-3.2, 1.5-3, 1.5-2.8, 1.5-2.5, 1.5-2.2, 1.5-2, 1.5-1.8;1.8-4, 1.8-3.8, 1.8-3.5, 1.8-3.2, 1.8-3, 1.8-2.8, 1.8-2.5, 1.8-2.2, 1.8-2;2-4, 2-3.8, 2-3.5, 2-3.2, 2-3, 2-2.8, 2-2.5, 2-2.2;2.2-4, 2.2-3.8, 2.2-3.5, 2.2-3.2, 2.2-3, 2.2-2.8, 2.2-2.5;2.5-4, 2.5-3.8, 2.5-3.5, 2.5-3.2, 2.5-3, 2.5-2.8, 2.8-4, 2.8-3.8, 2.8-3.5, 2.8-3.2, 2.8-3.3; 3-4, 3-3.8, 3-3.5, 3-3.2;3.2-4, 3.2-3.8, 3.2-3.5;3.5-4, 3.5-3.8;3.8-4.
"Polyethylene (PE)", as described herein, is a thermoplastic resin made by the polymerization of ethylene. Polyethylene is classified into High Density Polyethylene (HDPE), low Density Polyethylene (LDPE) and Linear Low Density Polyethylene (LLDPE) depending on the polymerization method, molecular weight, and chain structure. The heat emissivity of the PE host material, such as a particle board, is 0.9. The research of the invention shows that the radiation rate of the prepared film can be as low as 0.1 by precisely controlling the processing conditions, strictly controlling the thickness of the film, the transparency, the crystallinity and the crystallization size of the film and the coarse superness of the surface of the film. In addition, the film prepared from the high-density polyethylene as a raw material has lower transparency than the film prepared from the low-density polyethylene as a raw material because of higher crystallinity under the same processing conditions, and the low-density polyethylene is preferable from the viewpoint of improving the transparency of the film.
"Polyisobutylene (PIB)" as described herein is a polymer made from the cationic polymerization of isobutylene, and can have a molecular weight ranging from several hundred to millions. Polyisobutenes are a typical saturated linear polymer. The main body of the molecular chain does not contain double bonds, long-chain branches do not exist, and asymmetric carbon atoms do not exist. Polyisobutene is a colorless, odorless and nontoxic viscous liquid or semisolid substance, and has the properties of heat resistance, oxygen resistance, ultraviolet resistance, acid and alkali resistance and other chemicals. Polyisobutene molecules containing CH only 3 ，C-C，CH 2 Functional groups have very weak absorption in the 8-20 μm band, so polyisobutene can also produce low-emissivity optical films. The polyisobutene has very good light transmittance and good adhesion. Polyisobutenes are based on the molecular weights low-molecular weight, medium-molecular weight and high-molecular weight polyisobutenes. In general, materials having molecular weights between 350 and 3500 are referred to as low molecular weight polyisobutenes, medium molecular weight products having molecular weights between one hundred thousand and one hundred thousand, and high molecular weight products having molecular weights between one hundred thousand and one hundred thousand. In addition, the polyisobutene with the molecular weight below thirty thousand is usually in a liquid state, and if the polyisobutene in the liquid state is used as a raw material for preparing the film, the preparation and processing of the film can be greatly improved, and the use is influenced by the softer performance of the prepared film; the higher the molecular weight, the more difficult it is to process in the course of processing and use, the higher the processing requirements are, and on the basis of this, the polyisobutene according to the invention has a molecular weight of 3W to 100W, preferably 10W to 100W higher than 100W.
The metal oxide involved in the a layer constituting the film of the present invention is not particularly limited, and examples thereof include: ITO, AZO, FTO.
"AZO", as described herein, is aluminum doped zinc oxide, also known as aluminum doped zinc oxide (ZnO: al, AZO);
as described herein, "ITO" is tin-doped indium oxide, also known as tin-doped indium oxide (In 2 O 3 :Sn，ITO)；
As described herein, "FTO" is fluorine doped tin oxide, also known as fluorine doped tin oxide (SnO 2 :F，FTO)；
The 'AZO, ITO, FTO' has good conductivity and light transmittance, and is widely applied to the fields of solar cells, gas sensors, liquid crystal display screens, low-radiation glass and the like; the existing preparation methods mainly comprise a physical method and a chemical method. Physical methods include magnetron sputtering, pulsed laser deposition, vacuum evaporation, spraying, and the like; the chemical preparation method comprises chemical vapor deposition, atomic layer epitaxy, sol-gel method, spray thermal decomposition, etc. (see, document 1: nature, preparation method of ITO transparent conductive film and research progress [ J ]. Development and application of materials 2010,25 (4): 68-71.; document 2: yu Jianyuan, wang Likun, wang Li, etc. FTO film preparation technical research progress [ J ]. Artificial lens theory, 2016,45 (11): 2645-2649.; document 3: yellow steady, yu Zhou, zhang Yong, etc. AZO film preparation process and performance research [ J ]. Material guide, 2012,26 (1): 35-39).
The metal oxide particles may be used alone or in combination.
The solar light transmittance and emissivity of the layer a are greatly affected by the polymer compound such as the resin material used in the layer a. Taking polyethylene as an example of a high molecular compound:
in the first aspect, in the case of polyethylene itself, since its segment is compliant, it is easy to crystallize, and crystallization, particularly large-sized crystals, are key factors affecting the transparency and emissivity of the a layer. The mixing of the metal oxide particles can control the crystallization degree and the crystal size of the high molecular compound polyethylene, so that the solar light transmittance of the obtained film is improved, and the emissivity is reduced;
in the second aspect, in the case of using metal oxide particles such as ITO and AZO as a film for improving solar transmittance, emissivity and the like of a glass surface, a continuous coating layer is generally adopted by a coating or a direct current magnetron sputtering method, and a usable film is generally formed finally after high-temperature aging (> 400 ℃) is generally required, otherwise, gaps exist among the metal oxide particles such as ITO and AZO, which results in an undensified film layer, a rough surface layer and serious inhibition of conductivity of the film layer, which results in an improvement of emissivity, and the method has high equipment requirements, complex process and low production efficiency, and is difficult to prepare a product with a width exceeding 1.5 m. In the research of the invention, it is found that metal oxide particles such as ITO, AZO and the like are directly mixed into a high polymer compound such as polyethylene and the like, and the polyethylene can be used as a continuous phase to enable the metal oxide particles to be closely packed, so that even if the film is not subjected to high-temperature treatment as described above, a film with a flat surface can be obtained, and the emissivity of the film is greatly reduced.
From the viewpoint of further improving the mechanical strength of the film, the resin used in the a layer includes both polyethylene and polyisobutylene. Polyethylene has the characteristics of easy photooxidation, thermal oxidation, ozonolysis and the like, and is easy to degrade under the action of ultraviolet rays, and then can undergo reactions such as crosslinking, chain scission, unsaturated group formation and the like. The addition of the polyisobutylene polymer can increase the compatibility of metal oxide particles such as ITO, AZO and the like and PE polymer, and can improve the oxygen resistance, photo-aging capability and adhesion of the A layer.
As the metal oxide participating in the a layer constituting the film of the present invention, it is necessary to control the particle size of the metal oxide particles, and it is generally required to have a particle size of not more than 120 nm; in this regard, the particle size of the metal oxide may be any value selected from the following group of value ranges, unless otherwise specified: 5-120nm, 5-115nm, 5-110nm, 5-105nm, 5-100nm, 5-95nm, 5-90nm, 5-85nm, 5-80nm, 5-75nm, 5-70nm, 5-65nm, 5-60nm, 5-55nm, 5-50nm, 5-45nm, 5-40nm, 5-35nm, 5-30nm, 5-25nm, 5-20nm, 5-15nm, 5-10nm;10-120nm, 10-115nm, 10-110nm, 10-105nm, 10-100nm, 10-95nm, 10-90nm, 10-85nm, 10-80nm, 10-75nm, 10-70nm, 10-65nm, 10-60nm, 10-55nm, 10-50nm, 10-45nm, 10-40nm, 10-35nm, 10-30nm, 10-25nm, 10-20nm, 10-15nm;15-120nm, 15-115nm, 15-110nm, 15-105nm, 15-100nm, 15-95nm, 15-90nm, 15-85nm, 15-80nm, 15-75nm, 15-70nm, 15-65nm, 15-60nm, 15-55nm, 15-50nm, 15-45nm, 15-40nm, 15-35nm, 15-30nm, 15-25nm, 15-20nm;20-120nm, 20-115nm, 20-110nm, 20-105nm, 20-100nm, 20-95nm, 20-90nm, 20-85nm, 20-80nm, 20-75nm, 20-70nm, 20-65nm, 20-60nm, 20-55nm, 20-50nm, 20-45nm, 20-40nm, 20-35nm, 20-30nm, 20-25nm;25-120nm, 25-115nm, 25-110nm, 25-105nm, 25-100nm, 25-95nm, 25-90nm, 25-85nm, 25-80nm, 25-75nm, 25-70nm, 25-65nm, 25-60nm, 25-55nm, 25-50nm, 25-45nm, 25-40nm, 25-35nm, 25-30nm;30-120nm, 30-115nm, 30-110nm, 30-105nm, 30-100nm, 30-95nm, 30-90nm, 30-85nm, 30-80nm, 30-75nm, 30-70nm, 30-65nm, 30-60nm, 30-55nm, 30-50nm, 30-45nm, 30-40nm, 30-35nm;35-120nm, 35-115nm, 35-110nm, 35-105nm, 35-100nm, 35-95nm, 35-90nm, 35-85nm, 35-80nm, 35-75nm, 35-70nm, 35-65nm, 35-60nm, 35-55nm, 35-50nm, 35-45nm, 35-40nm;40-120nm, 40-115nm, 40-110nm, 40-105nm, 40-100nm, 40-95nm, 40-90nm, 40-85nm, 40-80nm, 40-75nm, 40-70nm, 40-65nm, 40-60nm, 40-55nm, 40-50nm, 40-45nm;45-120nm, 45-115nm, 45-110nm, 45-105nm, 45-100nm, 45-95nm, 45-90nm, 45-85nm, 45-80nm, 45-75nm, 45-70nm, 45-65nm, 45-60nm, 45-55nm, 45-50nm;50-120nm, 50-115nm, 50-110nm, 50-105nm, 50-100nm, 50-95nm, 50-90nm, 50-85nm, 50-80nm, 50-75nm, 50-70nm, 50-65nm, 50-60nm, 50-55nm;55-120nm, 55-115nm, 55-110nm, 55-105nm, 55-100nm, 55-95nm, 55-90nm, 55-85nm, 55-80nm, 55-75nm, 55-70nm, 55-65nm, 55-60nm;60-120nm, 60-115nm, 60-110nm, 60-105nm, 60-100nm, 60-95nm, 60-90nm, 60-85nm, 60-80nm, 60-75nm, 60-70nm, 60-65nm;65-120nm, 65-115nm, 65-110nm, 65-105nm, 65-100nm, 65-95nm, 65-90nm, 65-85nm, 65-80nm, 65-75nm, 65-70nm;70-120nm, 70-115nm, 70-110nm, 70-105nm, 70-100nm, 70-95nm, 70-90nm, 70-85nm, 70-80nm, 70-75nm;75-120nm, 75-115nm, 75-110nm, 75-105nm, 75-100nm, 75-95nm, 75-90nm, 75-85nm, 75-80nm;80-120nm, 80-115nm, 80-110nm, 80-105nm, 80-100nm, 80-95nm, 80-90nm, 80-85nm;85-120nm, 85-115nm, 85-110nm, 85-105nm, 85-100nm, 85-95nm, 85-90nm;90-120nm, 90-115nm, 90-110nm, 90-105nm, 90-100nm, 90-95nm;95-120nm, 95-115nm, 95-110nm, 95-105nm, 95-100nm;100-120nm, 100-115nm, 100-110nm, 100-105nm;105-120nm, 105-115nm, 105-110nm;110-120nm, 110-115nm;115-120nm.
The "particle size" of the metal oxide particles has a large influence on the crystallinity of PE, and in turn on the solar light transmittance and haze of the a layer, and therefore, from the viewpoint of pursuing the effect in this respect, it is preferable that the metal oxide particles have a particle size of 10 to 50 nm.
The term "particle size" in the context of the present invention mainly refers to the maximum particle size that the particles have.
In addition, it is necessary to control the amount of the metal oxide and the resin material used as the a layer that participates in the formation of the film of the present invention, specifically, the amount of the metal oxide and the resin material used may satisfy any one or more of the following conditions (i) to (ii):
(i) The ratio of the resin material to the metal oxide is A:B= (2-4): 1-3;
the ratio A of the resin material to the metal oxide is not particularly limited, and in the ratio A:B:
the magnitude of the a value may be any value taken from any of the following sets of value ranges: 2-4, 2-3.8, 2-3.5, 2-3.2, 2-3, 2-2.8, 2-2.5, 2-2.2, 2.2-4, 2.2-3.8, 2.2-3.5, 2.2-3.2, 2.2-3.3, 2.2-2.8, 2.2-2.5, 2.5-4, 2.5-3.8, 2.5-3.5, 2.5-3.2, 2.5-3, 2.5-2.8, 3-4, 3-3.8, 3-3.5, 3-3.2, 3.2-4, 3.2-3.8, 3.2-3.5, 3.5-4, 3.5-3.8, 3.8-4;
The magnitude of the B value may be any value taken from any of the following sets of value ranges: 1-3, 1-2.8, 1-2.5, 1-2.2, 1-2, 1-1.8, 1-1.5, 1-1.2;1.2-3, 1.2-2.8, 1.2-2.5, 1.2-2.2, 1.2-2, 1.2-1.8, 1.2-1.5;1.5-3, 1.5-2.8, 1.5-2.5, 1.5-2.2, 1.5-2, 1.5-1.8;1.8-3, 1.8-2.8, 1.8-2.5, 1.8-2.2, 1.8-2;2-3, 2-2.8, 2-2.5, 2-2.2;2.2-3, 2.2-2.8, 2.2-2.5;2.5-3, 2.5-2.8 and 2.8-3;
(ii) The metal oxide accounts for 40-80wt%;
the size of the ratio of the metal oxide may be any value selected from any of the following numerical ranges, if not particularly limited: 40-80wt%, 40-75wt%, 40-70wt%, 40-65wt%, 40-60wt%, 40-55wt%, 40-50wt%, 40-45wt%, 45-80wt%, 45-75wt%, 45-70wt%, 45-65wt%, 45-60wt%, 45-55wt%, 45-50wt%, 50-80wt%, 50-75wt%, 50-70wt%, 50-65wt%, 50-60wt%, 50-55wt%, 55-80wt%, 55-75wt%, 55-70wt%, 55-65wt%, 55-60wt%, 60-80wt%, 60-75wt%, 60-70wt%, 60-65wt%, 65-80wt%, 65-75wt%, 65-70wt%, 70-80wt%, 70-75wt%, 75-80 wt%.
(iii) The resin material accounts for 20-60wt%;
the size of the ratio of the resin material may be any value taken from any one of the following sets of value ranges: 20-60wt%, 20-55wt%, 20-50wt%, 20-45wt%, 20-40wt%, 20-35wt%, 20-30wt%, 20-25wt%, 25-60wt%, 25-55wt%, 25-50wt%, 25-45wt%, 25-40wt%, 25-35wt%, 25-30wt%, 30-60wt%, 30-55wt%, 30-50wt%, 30-45wt%, 30-40wt%, 30-35wt%, 35-60wt%, 35-55wt%, 35-50wt%, 35-45wt%, 35-40wt%, 40-60wt%, 40-55wt%, 40-50wt%, 40-45wt%, 45-60wt%, 45-55wt%, 45-50wt%, 50-60wt%, 50-55wt%, 55-60wt%.
(iv) The film has a mass density of 2.1 to 6.1g/m, calculated as layer A having a thickness of 1.0 μm 2 The method comprises the steps of carrying out a first treatment on the surface of the Preferably, the film has a mass density of 3.0 to 5.5g/m 2 。
Based on the above, as the film for reducing emissivity of heat provided by the present invention, one specific case of the a layer included in the film is as follows: the layer a comprises a base structure layer and metal oxide particles; the base structure layer contains a resin material, and the metal oxide particles are present inside the base structure layer; alternatively, the metal oxide particles are present within the base structure layer and on the surface of the base structure layer.
On the basis of the foregoing "specific case of layer a", the foundation structure layer may satisfy any one or more of the following conditions (i) to (iii):
(i) The base structure layer comprises polyethylene; the amount of polyethylene is not less than 15wt% of the total amount of the base structure layer.
(ii) The base structure layer comprises polyethylene; the amount of polyethylene is not more than 57% of the total amount of the base structure layer.
(iii) The amount of polyethylene in the base structure layer may be any value selected from any of the following groups of values, if not particularly limited: 15-57%, 15-55%, 15-50%, 15-45%, 15-40%, 15-35%, 15-30%, 15-25%, 15-20%;20-57%, 20-55%, 20-50%, 20-45%, 20-40%, 20-35%, 20-30%, 20-25%;25-57%, 25-55%, 25-50%, 25-45%, 25-40%, 25-35%, 25-30%;30-57%, 30-55%, 30-50%, 30-45%, 30-40%, 30-35%;35-57%, 35-55%, 35-50%, 35-45%, 35-40%;40-57%, 40-55%, 40-50%, 40-45%;45-57%, 45-55%, 45-50%;50-57%, 50-55%;55-57%.
(iv) The base structure layer comprises polyisobutylene; the amount of polyisobutene is not less than 1% of the total amount of the base structure layer.
(v) The base structure layer comprises polyisobutylene; the amount of polyisobutene is not more than 5% of the total amount of the base structure layer.
(vi) The amount of polyisobutylene in the base structure layer may be any value within any one of the following sets of values, if not particularly limited: 1-5%, 1-4%, 1-3%, 1-2%, 2-5%, 2-4%, 2-3%, 3-5%, 3-4%, 4-5%.
(vii) The base structure layer comprises polyethylene and polyisobutylene; the sum of the amounts of polyethylene and polyisobutylene is not less than 20wt% of the total amount of the base structure layer.
(viii) The base structure layer comprises polyethylene and polyisobutylene; the sum of the amounts of polyethylene and polyisobutylene does not exceed 60wt% of the total amount of the base structure layer.
(ix) The base structure layer is composed of polyethylene and polyisobutylene, and the sum of the amounts of the polyethylene and the polyisobutylene is not less than 20wt% of the total amount of the base structure layer.
(x) The base structure layer is comprised of polyethylene and polyisobutylene, the sum of the amounts of which is no more than 60wt% of the total base structure layer.
(xi) The ratio of the sum of the amounts of polyethylene and polyisobutylene in the base structure layer may be any value within any one of the following sets of values, if not particularly limited: 20-60%, 20-55%, 20-50%, 20-45%, 20-40%, 20-35%, 20-30%, 20-25%;25-60%, 25-55%, 25-50%, 25-45%, 25-40%, 25-35%, 25-30%;30-60%, 30-55%, 30-50%, 30-45%, 30-40%, 30-35%;35-60%, 35-55%, 35-50%, 35-45%, 35-40%;40-60%, 40-55%, 40-50%, 40-45%;45-60%, 45-55% and 45-50%;50-60% and 50-55%;55-60%.
[ method for producing Heat emissivity-reducing film ]
A method of preparing a film for reducing emissivity of heat as claimed in any one of the preceding claims, comprising the steps of:
1) Preparing a mixture containing a resin material and metal oxide particles;
3) The mixture is prepared into a film.
Step 1) preparing a mixture containing a resin material and metal oxide particles;
the usual operating procedures for the heat treatment for reference of this procedure 1) are: the resin material and the metal oxide particles are mixed, the viscosity of the resin material and the metal oxide particles can be properly adjusted by adding an organic solvent, and then the resin material and the metal oxide particles are uniformly mixed so as to ensure that the metal oxide particles are uniformly dispersed to the greatest extent and avoid agglomeration.
The mixing treatment can be carried out by adopting the prior known means, such as a sand mill or a high-speed dispersing machine, or a combination of the sand mill and the high-speed dispersing machine;
wherein, the technological parameters for reference when adopting the sand mill to carry out the treatment are as follows: treating for 20-30 minutes, and keeping the temperature at 30-40 ℃;
the parameters that can be referred to when high-speed dispersion is performed by using the high-speed dispersing machine are as follows: stirring at high speed for 8-12 hr at 90-100 deg.C.
In addition to the step 1), the method preferably further comprises the step 2):
Firstly, toluene removal operation, namely toluene removal treatment is carried out on a sand mill treatment product to obtain an initial composite material; of course, the resin material can also be added again at this step to obtain the initial composite material
Wherein, the toluene removal treatment is carried out by the prior known means, such as natural evaporation, oven drying, reduced pressure distillation treatment and the like; preference is given to using distillation under reduced pressure, the parameters which can be referenced being as follows: 90-110 ℃, 90-110 Pa and 0.5-3 h.
Then adding materials comprising the initial composite material into a hopper, extruding and granulating by a double-screw extruder to obtain a final composite material;
the temperatures of the feed cylinders which can be used for reference during extrusion granulation of the double-screw extruder are as follows:
the temperature of the feeding section is 40-50 ℃;
the temperature of the shearing section is 80-100 ℃;
the temperature of the plasticizing section is 100-110 ℃;
the temperature of the die head is 90-110 ℃.
Taking the film with reduced heat emissivity as an example, the resin material of the film contains polyethylene and polyisobutylene at the same time, the film is prepared byWorking procedures 1) and 2)The more detailed operation steps are as follows:
firstly, mixing polyisobutene and metal oxide particles in an organic solvent (such as toluene) to obtain a blend, and then uniformly mixing the blend;
Then, toluene removal treatment is carried out, and then polyethylene is added to obtain an initial composite material;
finally, extruding and granulating by a double-screw extruder to obtain the final composite material.
Based on the steps 1) and 2), the step 3) at this time can select an extrusion coating method to prepare the film, the specific reference steps are as follows:spraying the final composite material obtained by granulation through an extrusion film-spraying compound machine, and obtaining a film (A layer) with the corresponding heat radiation rate reduced on a substrate film;
in addition, the processing temperature of the laminating extruder, the die temperature, the advancing speed of the substrate membrane and the temperature of the cooling roller can all influence the thickness of the obtained membrane (A layer) with reduced heat emissivity; based on this, the parameters of lamination that can be referenced are as follows:
the plasticizing temperature of the laminating extruder is controlled to be 220-250 ℃;
the die temperature is controlled to be 250-280 ℃;
the advancing speed of the base membrane is not 80-100 m/min;
the temperature of the cooling roller is 10-20 ℃.
Alternatively, on the basis of the aforementioned step 1), the procedure included in step 2) for reference is as follows:
mixing the mixture obtained in the step 1) with other resin materials to obtain a final composite material mixed solution;
The mixing treatment can be carried out by adopting the prior known means, such as a sand mill or a high-speed dispersing machine, or a combination of the sand mill and the high-speed dispersing machine;
wherein, the technological parameters for reference when adopting the sand mill to carry out the treatment are as follows: treating for 20-30 minutes, and keeping the temperature at 30-40 ℃;
the parameters that can be referred to when high-speed dispersion is performed by using the high-speed dispersing machine are as follows: stirring at high speed for 8-12 hr at 90-100 deg.C.
In step 3) in the above steps 1) and 2), spraying may be selectedThe ink printing method is used for the preparation of films,
the specific reference steps are as follows:
the final composite material mixed solution obtained by the high-speed stirring treatment is subjected to viscosity adjustment by using an organic solvent such as toluene ethyl acetate, the viscosity is adjusted to 4000-6000 centipoises, a corresponding film (A layer) for reducing the heat emissivity is obtained on a substrate film by ink-jet printing, and the obtained film (A layer) for reducing the heat emissivity can be controlled to have different thicknesses by controlling the viscosity of the mixed solution and the control of the printing layer number.
[ composite film for reducing emissivity of Heat ]
The present invention provides a composite film for reducing emissivity of heat, the composite film comprising any one of the above layers a, and B; the B layer comprises a resin material, and the thickness of the B layer is 20-1000 micrometers. The transmittance of sunlight of the composite film in a wave band of 350-2500 nanometers is not lower than 85 percent, the emissivity is not more than 0.15, and the heat conductivity coefficient is not more than 0.35w/m.k.
The thickness of the B layer may be any value selected from any of the following ranges of values, if not particularly limited: 20-1000 microns, 20-900 microns, 20-800 microns, 20-700 microns, 20-600 microns, 20-500 microns, 20-400 microns, 20-300 microns, 20-200 microns, 20-100 microns, 100-1000 microns, 100-900 microns, 100-800 microns, 100-700 microns, 100-600 microns, 100-500 microns, 100-400 microns, 100-300 microns, 100-200 microns, 200-1000 microns, 200-900 microns, 200-800 microns, 200-700 microns, 200-600 microns, 200-500 microns, 200-400 microns, 200-300 microns, 20-1000 microns 300-900 microns, 300-800 microns, 300-700 microns, 300-600 microns, 300-500 microns, 300-400 microns, 400-1000 microns, 400-900 microns, 400-800 microns, 400-700 microns, 400-600 microns, 400-500 microns, 500-1000 microns, 500-900 microns, 500-800 microns, 500-700 microns, 500-600 microns, 600-1000 microns, 600-900 microns, 600-800 microns, 600-700 microns, 700-1000 microns, 700-900 microns, 700-800 microns, 800-1000 microns, 800-900 microns, 900-1000 microns.
Examples of the resin material participating in the formation of the layer B used in the present invention include: polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polymethyl methacrylate (PMMA), polyurethane (PU), polystyrene (PS), polycarbonate (PC). The resin material may be used alone or in combination of 2 or more.
The specific form of the composite film for reducing the emissivity of heat may be any one of the following (i) to (ii):
the composite film comprises a layer A and a layer B; the combination mode of the A layer and the B layer comprises a combination mode of forming An (AB) n structure; wherein n is an integer greater than or equal to 1; if the value of n is greater than 1, a plurality of layers A in the (AB) n structure can be the same or different, and a plurality of layers B can be the same or different;
examples thereof include: a is that 1 B 1 -A 1 B 1 -(A 1 B 1 ) n, or (A) 1 B 1 )n-(A 2 B 1 ) n, or (A) 1 B 1 )n-(A 1 B 2 ) n, or (A) 1 B 1 )n-(A 2 B 2 )n；
(ii) the composite film comprises a layer a and a layer B; the bonding mode of the A layer and the B layer comprises a bonding mode of forming an (ABA) n structure; wherein n is an integer greater than or equal to 1; if a plurality of A layers or a plurality of B layers exist, the plurality of A layers can be the same or different, and the plurality of B layers can be the same or different;
examples thereof include: a is that 1 B 1 A 1 -A 1 B 1 A 1 -(A 1 B 1 A 1 ) n, or (A) 1 B 1 A 1 )n-(A 2 B 1 A 1 ) n, or (A) 1 B 1 A 1 )n-(A 1 B 2 A 1 ) n, or (A) 1 B 1 A 1 )n-(A 2 B 2 A 1 ) n, or (A) 1 B 1 A 1 )n-(A 2 B 2 A 2 ) n, etc.
[ method for producing composite film for reducing emissivity of heat ]
The method for preparing a composite film for reducing emissivity of heat according to any one of the above, comprising the steps of:
1) Preparing a layer B;
2) Preparing a material required for forming the layer a, the material including a mixture containing a resin material, metal oxide particles;
4) And coating the mixture on the surface of the layer B to prepare a film.
Step 1) preparation of layer B:the B layer is preferably an optical B layer of a resin material having a different thickness, which is subjected to double-sided corona treatment, so that a composite film having a reduced emissivity to heat can be finally obtained.
As the double-sided corona treatment, the following key parameters were set: corona voltage 5000v/m, travelling speed of B layer film 50m/min.
Step 2) preparation of a material required for A layer formation, the material including a resin material, metal oxide particles Mixture:the usual operating procedures for the heat treatment for reference of this procedure 2) are:
the resin material and the metal oxide particles are mixed, the viscosity of the resin material and the metal oxide particles can be properly adjusted by adding an organic solvent, and then the resin material and the metal oxide particles are uniformly mixed so as to ensure that the metal oxide particles are uniformly dispersed to the greatest extent and avoid agglomeration.
The mixing treatment can be carried out by adopting the prior known means, such as a sand mill or a high-speed dispersing machine, or a combination of the sand mill and the high-speed dispersing machine;
wherein, the technological parameters for reference when adopting the sand mill to carry out the treatment are as follows: treating for 20-30 minutes, and keeping the temperature at 30-40 ℃;
The parameters that can be referred to when high-speed dispersion is performed by using the high-speed dispersing machine are as follows: stirring at high speed for 8-12 hr at 90-100 deg.C.
In addition to the steps 1) and 2), the method preferably further comprises the steps of3)：
Firstly, toluene removal operation, namely toluene removal treatment is carried out on a sand mill treatment product to obtain an initial composite material; of course, the resin material can also be added again at this step to obtain the initial composite material
Wherein, the toluene removal treatment is carried out by the prior known means, such as natural evaporation, oven drying, reduced pressure distillation treatment and the like; preference is given to using distillation under reduced pressure, the parameters which can be referenced being as follows: 90-110 ℃, 90-110 Pa and 0.5-3 h.
Then adding materials comprising the initial composite material into a hopper, extruding and granulating by a double-screw extruder to obtain a final composite material;
the temperatures of the feed cylinders which can be used for reference during extrusion granulation of the double-screw extruder are as follows:
the temperature of the feeding section is 40-50 ℃;
the temperature of the shearing section is 80-100 ℃;
the temperature of the plasticizing section is 100-110 ℃;
the temperature of the die head is 90-110 ℃.
Taking the film with reduced heat emissivity as an example, the resin material of the film contains polyethylene and polyisobutylene at the same time, the film is prepared by Working procedures 1) and 2)The more detailed operation steps are as follows:
firstly, mixing polyisobutene and metal oxide particles in an organic solvent (such as toluene) to obtain a blend, and then uniformly mixing the blend;
then, toluene removal treatment is carried out, and then polyethylene is added to obtain an initial composite material;
finally, extruding and granulating by a double-screw extruder to obtain a final composite material;
based on the steps 1), 2) and 3), the step 4) at this time can select an extrusion coating method to carry out the composite film
Specifically, the preparation method comprises the following steps of:
spraying the final composite material obtained by granulation through an extrusion film-spraying compound machine, and obtaining a corresponding film (a layer) for reducing the heat radiation rate on a base film (a layer B film);
in addition, the processing temperature of the laminating extruder, the die temperature, the travelling speed of the base film sheet (B layer film) and the temperature of the cooling roller can all influence the thickness of the obtained film (A layer) with reduced heat emissivity; based on this, the parameters of lamination that can be referenced are as follows:
the plasticizing temperature of the laminating extruder is controlled to be 220-250 ℃;
the die temperature is controlled to be 250-280 ℃;
the advancing speed of the base film sheet (B layer film) is not 80-100 m/min;
The temperature of the cooling roller is 10-20 ℃.
Alternatively, on the basis of the aforementioned steps 1), 2), the operations included in step 3) for reference are as follows:
mixing the mixture obtained in the step 1) with other resin materials to obtain a final composite material mixed solution;
the mixing treatment can be carried out by adopting the prior known means, such as a sand mill or a high-speed dispersing machine, or a combination of the sand mill and the high-speed dispersing machine;
wherein, the technological parameters for reference when adopting the sand mill to carry out the treatment are as follows: treating for 20-30 minutes, and keeping the temperature at 30-40 ℃;
the parameters that can be referred to when high-speed dispersion is performed by using the high-speed dispersing machine are as follows: stirring at high speed for 8-12 hr at 90-100 deg.C.
Step 4) in this case may be selected based on the above steps 1), 2) and 3)The preparation of the film by the inkjet printing method can be specifically referred to as follows:
and (3) carrying out high-speed stirring treatment to obtain a final composite material mixed solution, regulating the viscosity to 4000-6000 centipoises by utilizing an organic solvent such as toluene ethyl acetate, and carrying out ink-jet printing on the layer B to form a layer A, so as to obtain the composite film comprising the layer A and the layer B and capable of reducing the heat emissivity. The resulting heat radiation rate-reduced film (a layer) can be controlled to have different thicknesses by controlling the viscosity of the mixed liquid and the number of printing layers.
The invention is further described below in connection with specific embodiments. The experimental procedures, which do not address the specific conditions in the examples below, are generally carried out under conventional conditions or under conditions recommended by the manufacturer.
Transmittance test
The freshly prepared AB composite film was cut to the size required for the sample. In the experiment, the visible light transmittance of the film is tested by using a Lambda 750s, perkinelmer ultraviolet-visible spectrophotometer manufactured by the United states, and the wavelength range of detection is set between 300nm and 2500 nm. The light source is a light beam emitter, and can emit light beams with corresponding wave bands according to test requirements; a monochromator is a filter for a light beam whose spectral effect is such that the light emitted by a light source is converted into monochromatic light which is then applied to a sample. The light after the sample is applied is received by the detector and the signal is converted to a display output. The ratio of transmitted light intensity It to incident light intensity I0 is instantaneous the visible light transmittance of the sample. The absorptivity of the sample to light can be determined by: a% = 1-R% -T%, where a% is the absorbance of the sample for light; r% is the reflectivity of the sample to light; t% is the transmittance of the sample to light.
Emissivity test
The infrared reflectivity of the prepared composite film directly determines the emissivity of the film, and is a key reference index for representing a low-emissivity film. The infrared reflectivity test of the low-emissivity film in the experiment adopts a VERTEX 70v Fourier transform infrared spectrometer manufactured by Germany, and the wavelength range of the test is set in the middle infrared region, namely the wavelength range is between 2.5 mu m and 25 mu m. Kirchhoff's law discloses the relationship between emissivity and absorptivity when an object is in thermal equilibrium with the surrounding environment. For a particular wavelength, there is ε λ ＝α λ Epsilon in λ 、α λ The emissivity and absorptivity corresponding to the wavelength lambda, respectively. The emissivity of the sample is thus e=1-R-T, R being the reflectivity of the band and T being the transmissivity of the band.
Thermal conductivity testing
Cutting and laminating the composite material into a wafer with the diameter of 10mm and the thickness of 2mm, and testing the heat conductivity of the composite film material by using a NETZSCH LFA 457Microflash instrument. The number of test pieces for different samples is two, each test is performed twice, namely four data are measured according to each proportion, and finally the average value of the four data is calculated as the value of the final heat conductivity
Example 1: extrusion lamination composite preparation of composite functional film
The specific formulation of the film (A1) for reducing the emissivity of heat is as follows:
70 parts of low-density polyethylene (LDPE for short, brand: shanghai petrochemical, model: Q281);
10 parts of polyisobutene (PIB for short, average molecular weight of 10 ten thousand);
20 parts of tin-doped indium oxide (indium tin oxide) particles (ITO for short, particle size 20-50 nm) (preparation methods are referred to Boudiar, T, sandu, C S, canut, B, blancin, M.G. Interst of Rapid Thermal Annealing (RTA) for the elaboration of SnO2: sb transparent conducting oxide by the Sol-gel technology. Journal of Sol-Gel Science and Technology,2003 (26): 1067-1070.);
50 parts of toluene.
The specific preparation process of the film (A1) for reducing the emissivity of heat is as follows:
s1, dissolving PIB in toluene, adding ITO to obtain a blend, and treating the blend at a set temperature of 35 ℃ for 20-30 minutes by a sand mill until the blend presents transparent mucus.
S2, toluene removal operation, namely performing reduced pressure distillation treatment on a sand mill treatment product under the treatment conditions of 100 ℃ and 100Pa for 1h to obtain a PIB-ITO composite material;
s3, adding the LDPE and PIB-ITO composite material into a hopper, and extruding and granulating through a double-screw extruder with the diameter of 20 mm to obtain the LDPE-PIB-ITO composite material;
the temperature of the charging barrel during extrusion granulation of the double-screw extruder is kept at the following temperature:
the temperature of the feeding section is 45 ℃;
the temperature of the shearing section is 90 ℃;
the temperature of the plasticizing section is 105 ℃;
the die temperature is 100 ℃;
s4, spraying the LDPE-PIB-ITO composite material obtained by granulation through an extrusion film-spraying compound machine, obtaining a corresponding film (A1) for reducing the heat radiation rate on a substrate film, and controlling the processing temperature, the die temperature, the advancing speed of the substrate film and the temperature of a cooling roller of the film-spraying extruder to obtain films (A1) with different thicknesses for reducing the heat radiation rate;
Wherein, if the substrate film is replaced with an optical B layer which is processed by double-sided corona treatment (corona voltage is 5000v/m, film travelling speed is 50 m/min) and is composed of corresponding resin materials and has different thicknesses, the composite film with reduced heat emissivity can be finally obtained.
Example 2: method for preparing composite functional glass by ink-jet printing method
Specific formulation of the film (A2) for reducing the emissivity of heat:
35 parts of low-density polyethylene (LDPE for short, brand: shanghai petrochemical, model: Q281);
15 parts of polyisobutene (PIB for short, average molecular weight of 10 ten thousand);
40 parts of tin-doped indium oxide particles (ITO for short, particle size of 90-100 nm) (same as in example 1);
10 parts of aluminum-doped zinc oxide particles (AZO for short, particle size of 10-20 nm) (see Rajak, sukla, ray, mina. Composite study of plasmonic resonance in transparent conducting oxides: ITO and AZO. Journal of Optics,2014 (43): 231-238.);
80 parts of toluene;
5 parts of isopropanol;
the specific preparation process of the film (A2) for reducing the emissivity of heat is as follows:
s1, dissolving PIB in 80 parts of toluene, and then adding ITO nanoparticles, AZO nanoparticles and isopropanol to mix to obtain a blend;
s2, treating the blend for 20-30 minutes by using a sand mill, wherein the treatment temperature is set to 35 ℃, and the treatment is carried out until the blend presents mucus in a transparent state.
S3, adding the product obtained by sand mill treatment and LDPE into a high-speed dispersing machine, heating to 95 ℃, and stirring at high speed for 10 hours until the blending liquid is transparent.
S4, adding the transparent blending liquid into toluene ethyl acetate organic solvent to dilute to 4000-6000 centipoises in viscosity, obtaining a corresponding film (A2) for reducing the heat emissivity on a substrate film through ink-jet printing, and controlling the number of layers through ink-jet printing to obtain films (A2) for reducing the heat emissivity with different thicknesses;
if the substrate film is replaced with an optical B layer of a corresponding resin material having a different thickness, which is subjected to double-sided corona treatment (same as in example 1), a composite film with reduced heat emissivity can be finally obtained.
The table below shows the properties of the composite film prepared in the manner of the above (A1) or (A2) with the optical B layer (i.e., the base film sheet) having different thickness composed of various types of resin materials, which was subjected to the double-sided corona treatment, as well as the solar transmittance, the film surface emissivity, the heat transfer coefficient, the haze, and the like of the composite film.
In the table:
a1 represents:the a layer was prepared using the procedure provided in example 1;
Taking A1 (10 μm) as an example, it represents a layer A having a thickness of 10 μm prepared by the method provided in example 1;
a2 represents:the a layer was prepared using the procedure provided in example 2;
taking A2 (1 μm) as an example, it represents an a layer having a thickness of 1 μm prepared by the manner provided in example 1;
PET, PEN, PC, PS, PMMA, PU respectivelyThe representation is:a B layer made of polyethylene terephthalate (PET), a B layer made of polyethylene naphthalate (PEN), a B layer made of Polycarbonate (PC), a B layer made of Polystyrene (PS), a B layer made of polymethyl methacrylate (PMMA) and a B layer made of Polyurethane (PU);
to be used forPET(100 μm) for example, which represents a layer B of polyethylene terephthalate (PET) material with a thickness of 100 μm;
taking PET+A1 as an example, it means that the composite film is composed of (left) layer B PET and (right) layer A1;
taking A1+PEN as an example, it means that the composite film is composed of (left) A layer A1 and (right) B layer PEN;
taking a1+pen+a2 as an example, it means that the composite film is composed of B-layer PEN in the middle, and (left) a-layer A1 and (right) a-layer A2 on both sides of the B-layer, respectively.
Comparative example 3
80 parts of low-density polyethylene (LDPE for short, brand: shanghai petrochemical, model: Q281);
20 parts of tin-doped indium oxide (indium tin oxide) particles (ITO for short, particle size of 20-50 nm) (same as in example 1);
50 parts of toluene.
The specific preparation process of the film for reducing the heat emissivity is as follows:
s1, 10 parts of LDPE is dissolved in toluene, then ITO is added to obtain a blend, and the blend is treated by a sand mill at a set temperature of 35 ℃ for the same time as in example 1.
S2, toluene removal operation, namely performing reduced pressure distillation treatment on a sand mill treatment product under the treatment conditions of 100 ℃ and 100Pa for 1h to obtain an LDPE-ITO composite material;
s3, adding 70 parts of LDPE and LDPE-ITO composite material into a hopper, extruding and granulating by a double-screw extruder with the diameter of 20 mm to obtain the LDPE-LDPE-ITO composite material;
the temperature of the charging barrel during extrusion granulation of the double-screw extruder is kept at the following temperature:
the temperature of the feeding section is 45 ℃;
the temperature of the shearing section is 90 ℃;
the temperature of the plasticizing section is 105 ℃;
the die temperature is 100 ℃;
s4, performing film coating on the optical PET (125 micrometers) serving as a base film piece subjected to double-sided corona treatment (same as that of the embodiment 1) by using an extrusion film coating compound machine on the LDPE-LDPE-ITO composite material obtained by granulation in the same manner as the embodiment 1 to obtain a film (calculated by PE) with the thickness of 5 micrometers and capable of reducing the heat emissivity;
Finally, the PET+PE composite film is prepared,
the test shows that the visible light transmittance of the prepared composite film is 60%, the haze is more than 10%, and the PE side emissivity epsilon is 0.3.
Comparative example 4
This example is basically the same as example 1, except that the particle diameter of the tin-doped indium oxide particles is 150 to 200nm,
in this example, the B-layer substrate film selected was optical PET (125 microns) with double sided corona treatment (as in example 1), the remainder being as in example 1.
Finally, the PET+PE composite film is prepared, and the test shows that the visible light transmittance of the prepared composite film is 53%, the haze is more than 20%, and the PE side emissivity epsilon is 0.35.
Comparative example 5
The film (A2) for reducing the emissivity of heat is specifically:
this example is substantially the same as example 2 except that the low density polyethylene is replaced with polyvinyl butyral (PVB for short, wall-filling riser plastic, viscosity 20-40, butyraldehyde group 68-75%, hydroxyl 17-22%);
in this example, the B-layer substrate film selected was a polyethylene terephthalate film (PET film) with a thickness of 100 μm by double sided corona treatment (same as in example 1), and the remainder was the same as in example 2.
Finally, the PET+PVB composite film is prepared, and the test proves that the visible light transmittance of the composite film is 85 percent,
Haze <2.1% and PVB side emissivity epsilon of 0.48.
Comparative example 6
Specific formulation of the film (A2) for reducing the emissivity of heat:
10 parts of low-density polyethylene (LDPE for short, brand: shanghai petrochemical, model: Q281);
5 parts of polyisobutylene (PIB for short, with average molecular weight of 10 ten thousand);
70 parts of tin-doped indium oxide particles (ITO for short, with the particle size of 90-100 nm) (same as in example 1);
15 parts of aluminum-doped zinc oxide particles (AZO for short, with the particle size of 10-20 nm) (the same as in example 2);
80 parts of toluene;
5 parts of isopropanol;
specific preparation of the film (A2) for reducing emissivity of heat while example 2,
in this example, the B-layer substrate film selected was a polyethylene terephthalate film (PET film) with a thickness of 100 μm by double sided corona treatment (same as in example 1), and the remainder was the same as in example 2.
Finally, the PET+PVB composite film is prepared, and the test shows that the visible light transmittance of the composite film is 45%, the haze is more than 25%, and the PE side emissivity epsilon is 0.38.
Comparative example 7
The specific formulation of the film (A1) for reducing the emissivity of heat is as follows:
60 parts of polyisobutene (PIB for short, average molecular weight 5100 ten thousand);
15 parts of tin-doped indium oxide (indium tin oxide) particles (ITO for short, particle size of 20-50 nm) (same as in example 1);
50 parts of toluene.
The specific preparation process of the film (A1) for reducing the emissivity of heat is as follows:
s1, the method is the same as that of the embodiment 1;
s2, the same as in the embodiment 1;
s3, adding 50 parts of PIB and PIB-ITO composite material into a hopper, and extruding and granulating through a double-screw extruder with the diameter of 20 mm to obtain the PIB-PIB-ITO composite material; the remainder is the same as in example 1;
s4, performing film coating on the optical PET (125 micrometers) serving as a base film piece subjected to double-sided corona treatment (same as that of the embodiment 1) by using a PIB-PIB-ITO composite material obtained by granulation through an extrusion film coating compound machine in the same manner as the embodiment 1 to obtain a film with the thickness of 5 micrometers (calculated by PIB) and capable of reducing the heat emissivity;
finally, the PET+PIB composite film is prepared,
the test shows that the visible light transmittance of the composite film is 85%, the haze is less than 1.1%, and the PIB side emissivity epsilon is 0.58.
The above description of the invention and its embodiments has been given by way of illustration and not limitation, and the examples shown are merely examples of embodiments of the invention, without limitation to the actual embodiments. Therefore, if one of ordinary skill in the art is informed by this disclosure, embodiments and examples similar to the technical solution are not creatively devised without departing from the gist of the present invention, and all the embodiments and examples are considered to be within the protection scope of the present invention.
Claims (13)
1. A film for reducing heat radiation rate, characterized in that,
the film comprises a layer a of the film,
the layer a includes a resin material and metal oxide particles;
wherein,
the thickness of the layer A is 0.5-10 microns, preferably 1-2 microns;
the resin material of the layer a contains metal oxide particles.
2. The film for reducing heat emissivity according to claim 1,
the resin comprises polyethylene;
or,
the resin comprises polyisobutylene;
or,
the resin comprises polyethylene and polyisobutylene, and the mass ratio of the polyethylene to the polyisobutylene is (16-19): (1-4);
and/or the number of the groups of groups,
the metal oxide includes one or two or more of indium oxide containing tin, zinc oxide containing aluminum, and tin oxide containing fluorine.
3. The emissivity-reducing film of claim 2 wherein said metal oxide has a particle size of no more than 120 nm;
preferably the metal oxide has a particle size of 5-120 nm;
it is further preferred that the metal oxide has a particle size of 10-50 nm.
4. A film for reducing heat emissivity according to any one of claim 1 to 3,
the ratio of the resin material to the metal oxide is (2-4) to (1-3) according to the weight ratio; and/or the number of the groups of groups,
The film has a mass density of 2.1 to 6.0g/m, calculated as layer A having a thickness of 1.0 μm 2 。
5. The film for reducing heat emissivity according to any one of claims 1 to 4,
the layer a comprises a base structure layer and metal oxide particles;
the base structure layer contains a resin material, and the metal oxide particles are present inside the base structure layer;
or,
the layer a comprises a base structure layer and metal oxide particles;
the base structure layer contains a resin material, and the metal oxide particles are present in the interior of the base structure layer and the surface of the base structure layer.
6. The heat radiation rate reducing film according to any one of claims 1 to 5,
the base structure layer comprises polyethylene; the amount of polyethylene is not less than 15wt% of the total amount of the base structure layer; or,
the base structure layer comprises polyisobutylene; the amount of the polyisobutene is not less than 1% of the total amount of the base structure layer; or,
the base structure layer comprises polyethylene and polyisobutylene; the sum of the amounts of polyethylene and polyisobutylene is not less than 20wt% of the total amount of the base structure layer.
7. The film for reducing heat radiation rate according to claim 6, wherein the film has a transmittance of sunlight of not less than 80% in a wavelength band of 350 to 2500 nm; and/or
The film has a emissivity of heat in the 2.5-100 micron band of no more than 0.15; and/or
The film has a thermal conductivity of no more than 0.35 w/m.k.
8. A process for producing a film for reducing heat emissivity according to any one of claim 1 to 7,
1) Preparing a mixture containing a resin material and metal oxide particles;
2) The mixture is prepared into a film.
9. A composite film for reducing heat radiation rate comprises a layer A and a layer B
The layer a comprises the film of any one of claims 1-7 or prepared by the method of claim 8;
the layer B includes a resin material and has a light transmittance of not less than 80% and a thickness of 20 to 1000 μm.
10. The composite film according to claim 9, wherein the resin material comprises one, two, or more of polyethylene terephthalate, polyethylene naphthalate, polymethyl methacrylate, polyurethane, polystyrene, and polycarbonate.
11. The composite film for reducing emissivity of claim 10, wherein,
the combination mode of the A layer and the B layer comprises a combination mode of forming an AB structure;
Or,
the bonding mode of the A layer and the B layer comprises a bonding mode of forming an ABA structure; wherein, in the ABA structure, there is one a layer of the same type;
or alternatively
The bonding mode of the A layer and the B layer comprises a bonding mode of forming an ABA structure; wherein, in the ABA structure, there are two a layers of different types.
12. The composite film for reducing heat radiation rate according to any one of claims 9 to 11, wherein the transmittance of sunlight in a wavelength band of 350 to 2500 nm is not less than 80%; and/or the number of the groups of groups,
the emissivity of the heat of the composite film in the wave band of 2.5-100 microns is not more than 0.15; and/or the number of the groups of groups,
the composite film has a thermal conductivity of no more than 0.35 w/m.k.
13. A method for producing a composite film for reducing heat emissivity according to any one of claim 9 to 12,
1) Preparing a layer B;
2) Preparing a material required for forming the layer a, the material including a mixture containing a resin material, metal oxide particles; 2) And coating the mixture on the surface of the layer B to prepare a film.
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| CN1226573A (en) * | 1997-12-22 | 1999-08-25 | 住化普拉斯技术株式会社 | Resin film |
| CN1916057A (en) * | 2005-08-17 | 2007-02-21 | 中科纳米技术工程中心有限公司 | Sunlight controlled transparent film in low radiation, prepartion method and application |
| US20080283290A1 (en) * | 2006-04-28 | 2008-11-20 | Nitto Denko Corporation | Article including sheet-like electromagnetic shielding structure |
| CN104040384A (en) * | 2011-12-28 | 2014-09-10 | 柯尼卡美能达株式会社 | Infrared shielding film, heat reflective laminated glass using same, and method for producing heat reflective laminated glass |
| CN109403808A (en) * | 2018-12-06 | 2019-03-01 | 南京睿爻新材料科技有限公司 | A kind of intelligent glass system of high-efficient single direction photo-thermal transmitting |
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2023
- 2023-07-10 CN CN202310836847.2A patent/CN117106215A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1226573A (en) * | 1997-12-22 | 1999-08-25 | 住化普拉斯技术株式会社 | Resin film |
| CN1916057A (en) * | 2005-08-17 | 2007-02-21 | 中科纳米技术工程中心有限公司 | Sunlight controlled transparent film in low radiation, prepartion method and application |
| US20080283290A1 (en) * | 2006-04-28 | 2008-11-20 | Nitto Denko Corporation | Article including sheet-like electromagnetic shielding structure |
| CN104040384A (en) * | 2011-12-28 | 2014-09-10 | 柯尼卡美能达株式会社 | Infrared shielding film, heat reflective laminated glass using same, and method for producing heat reflective laminated glass |
| CN109403808A (en) * | 2018-12-06 | 2019-03-01 | 南京睿爻新材料科技有限公司 | A kind of intelligent glass system of high-efficient single direction photo-thermal transmitting |
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