CN108912395B - Nanoparticle mixture, polymer, adhesive film and heat-insulating film - Google Patents

Nanoparticle mixture, polymer, adhesive film and heat-insulating film Download PDF

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CN108912395B
CN108912395B CN201710226939.3A CN201710226939A CN108912395B CN 108912395 B CN108912395 B CN 108912395B CN 201710226939 A CN201710226939 A CN 201710226939A CN 108912395 B CN108912395 B CN 108912395B
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metal oxide
composite metal
polymer
nanoparticle mixture
film
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CN108912395A (en
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贺俊卿
陈雪花
李永捷
甘宏宇
朱东伟
杨宇
金舟
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3M Speciality Materials Shanghai Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
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    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K3/2279—Oxides; Hydroxides of metals of antimony
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • 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
    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • 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
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00—Presence of polyester
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2475/00—Presence of polyurethane

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Abstract

The invention provides a nanoparticle mixture, which comprises at least any two of first composite metal oxide nanoparticles, carbon black nanoparticles and second composite metal oxide nanoparticles. The invention also provides a polymer comprising a mixture of nanoparticles, wherein the ratio of the weight of the mixture of nanoparticles to the weight of the polymer particles is less than 0.85. The invention also provides a film containing the polymer and a heat insulation film containing the nano-particle mixture. The nanoparticle mixture, the polymer, the film and the heat insulation film provided by the invention can be applied to automobile glass, building windows or other products needing to block infrared light, so that the automobile glass, the building windows and the products needing to block infrared light not only have excellent infrared blocking performance, but also can adjust the performances such as color tone, optical performance (such as visible light transmittance), haze and the like according to needs.

Description

Nanoparticle mixture, polymer, adhesive film and heat-insulating film
Technical Field
The invention relates to a nanoparticle mixture and a polymer, and also relates to a film and a heat insulation film which can be applied to automobile glass and building windows.
Background
The heat insulation film is widely applied to automobile glass and building windows, is used for blocking ultraviolet rays and heat in sunlight, improving the comfort level in an automobile and a room, adjusting the color of a vehicle window, protecting privacy, preventing glass from splashing after being broken, and the like. Typical heat insulating films are dyed films, metal heat insulating films and ceramic films. The production process of these films is generally complicated, and may involve multilayer sputtering, dip dyeing, copolymerization extrusion and other techniques, so that it is difficult to adjust the color, light transmittance and the like of the heat insulation film. Although the color of the heat insulating film may be adjusted by using a colored adhesive or a colored hard coat layer, the stability and the anti-aging property of the heat insulating film may be deteriorated and the infrared blocking effect and the light transmittance may be not good.
Chinese patent application (CN102625786A) discloses an interlayer film for laminated glass, which is useful for automobiles, buildings, and the like to improve the heat insulation of laminated glass, and which comprises a heat-insulating layer and a1 st ultraviolet-shielding layer, wherein the heat-insulating layer contains at least one component selected from a phthalocyanine compound, a naphthalocyanine compound, and an anthracyanine compound, a thermoplastic resin, and heat-insulating particles, and the 1 st ultraviolet-shielding layer contains a thermoplastic resin and an ultraviolet-shielding agent.
The Chinese patent application (CN103481564A) discloses a window film capable of automatically adjusting light transmittance, which automatically adjusts the light transmittance through the color change of added photochromic dyes under different light intensities, changes the window film from colorless to colored under a strong light environment, automatically reduces the light transmittance, and automatically recovers under a weak light environment.
US patent (US7883777B2) discloses a solar shading window film laminate having a light transmission of 5-80%, comprising at least two polyester fiber layers; at least one adhesive layer positioned between the two polyester fiber layers, wherein the at least one adhesive layer comprises polyurethane substrate laminated adhesive dispersed with solar particles; the solar particles comprise a composite metal oxide selected from the group consisting essentially of Cu-Cr, Cu-Fe-Mn, Cu-Mn, Cu-Cr-Mn, Cu-Cr-Mn-Ni, Co-Cr-Fe, and combinations thereof.
US patent (US7057805B2) discloses a solar energy adjusting film comprising an adhesive layer for bonding the solar energy adjusting film and a substrate, a metal layer and a scratch-resistant layer in which carbon black particles are dispersed, wherein the metal layer is located between the adhesive layer and the scratch-resistant layer; meanwhile, the patent also discloses a preparation method of the solar energy adjusting film, which comprises the following steps: carbon black particles are dispersed in a nitro resin polymer material to form a coating, and the coating is applied to a solar energy adjusting film to form a scratch-resistant layer dispersed with the carbon black particles.
Disclosure of Invention
The present invention provides a nanoparticle mixture, a polymer containing the nanoparticle mixture, a film laminate containing the polymer, and a heat insulating film containing the nanoparticle mixture, which have at least satisfactory infrared blocking properties, visible light transmittance, hue, and haze, and at the same time, the visible light transmittance and color of the film laminate and the heat insulating film of the present invention can be adjusted by the nanoparticle mixture of the present invention.
Certain aspects of the present invention provide a nanoparticle mixture comprising, in 100 wt.% based on the total weight of the nanoparticle mixture: (A)0-85 wt.% of first composite metal oxide nanoparticles comprising a composite transition metal oxide; (B)0-20 wt.% of carbon black nanoparticles; (C)0-99.9 wt.% of second composite metal oxide nanoparticles selected from the group consisting of tin-containing composite metal oxides, antimony-containing composite metal oxides, tin-and antimony-containing composite metal oxides, and combinations thereof.
According to certain embodiments, the second composite metal oxide nanoparticles are present in an amount greater than 90% by weight.
According to certain embodiments, the composite transition metal oxide is selected from the group consisting of a copper-chromium (Cu-Cr) composite metal oxide, a copper-iron-manganese (Cu-Fe-Mn) composite metal oxide, a copper-manganese (Cu-Mn) composite metal oxide, a copper-chromium-manganese (Cu-Cr-Mn) composite metal oxide, a copper-chromium-manganese-nickel (Cu-Cr-Mn-Ni) composite metal oxide, a cobalt-iron (Co-Fe) composite metal oxide, and combinations thereof.
According to certain embodiments, the carbon black nanoparticles are dispersed in an organic solvent selected from the group consisting of methyl isobutyl ketone (MIBK), Methyl Ethyl Ketone (MEK).
According to certain embodiments, the second composite metal oxide nanoparticles are selected from the group consisting of antimony doped tin oxide (ATO), antimony oxide (e.g., SbO)2，Sb2O3) Tin dioxide (SnO)2) Indium Tin Oxide (ITO) and zinc doped tin oxide (ZTO), and combinations thereof.
Certain aspects of the invention provide a polymer comprising polymer particles and a nanoparticle mixture of the invention, the ratio of the weight of the nanoparticle mixture to the weight of the polymer particles being less than 0.85.
According to certain embodiments, the polymeric particles are selected from polyester resins, polyurethane resins, and combinations thereof.
In some aspects of the present invention, a film is provided, which comprises a polymer film substrate layer, wherein the polymer film substrate layer is coated with a film containing the polymer of the present invention.
Certain aspects of the present invention provide a thermal barrier film comprising a nanoparticle mixture of the present invention and at least one coating layer, said nanoparticle mixture being dispersed in at least one of said coating layers.
According to some embodiments, the heat insulation film comprises an abrasion-resistant layer, a polymer film substrate layer, a laminated adhesive layer, a polymer film substrate layer and a pressure sensitive adhesive layer from top to bottom in sequence, and the nanoparticle mixture is dispersed in at least one of the abrasion-resistant layer, the laminated adhesive layer and the pressure sensitive adhesive layer.
Preferably, the nanoparticle mixture is dispersed in the laminate glue layer.
According to certain embodiments, the abrasion resistant layer has a thickness of 2 to 4 μm, the polymeric film substrate layer has a thickness of 12 to 50 μm, the laminate adhesive layer has a thickness of 1 to 6 μm, and the pressure sensitive adhesive layer has a thickness of 6 to 9 μm.
According to some embodiments, the thermal insulation film comprises an abrasion-resistant layer, a polymer film substrate layer, a polymer coating layer and a pressure-sensitive adhesive layer from top to bottom, and the nanoparticle mixture is dispersed in at least one of the abrasion-resistant layer, the polymer coating layer and the pressure-sensitive adhesive layer.
Preferably, the nanoparticle mixture is dispersed in the polymer coating.
Preferably, the polymeric coating is selected from the group consisting of polyester resins, polyurethane resins, and combinations thereof.
According to certain embodiments, the abrasion resistant layer has a thickness of 2 to 4 μm, the polymeric film substrate layer has a thickness of 12 to 50 μm, the polymeric coating layer has a thickness of 1 to 12 μm, and the pressure sensitive adhesive layer has a thickness of 6 to 9 μm.
The nanoparticle mixture, the polymer, the film and the heat insulation film provided by the invention can be applied to automobile glass, building windows or other products needing to block infrared light, so that the automobile glass, the building windows and the products needing to block infrared light not only have excellent infrared blocking performance, but also can adjust the performances such as color tone, optical performance (such as visible light transmittance), haze and the like according to needs.
The composite transition metal oxide in the present invention means a multi-component oxide obtained by compounding two or more transition metal oxides.
Drawings
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. It will be appreciated by those skilled in the art that the drawings are intended to illustrate preferred embodiments of the invention schematically, and that the various elements in the drawings are not drawn to scale.
FIGS. 1-2 are schematic illustrations of a thermal barrier film according to certain embodiments of the present invention;
FIG. 3 is a light transmittance spectrum of example 19 and comparative examples 3 to 5;
FIG. 4 is a light transmittance spectrum of example 22 and comparative examples 6 to 7;
FIG. 5 is a light transmittance spectrum of examples 26 to 30.
Description of the main elements
1 nanoparticle mixture
2 and 2' Heat insulating film
21 wear layer 22 polymer film substrate layer
23 laminating adhesive layer 24 pressure sensitive adhesive layer 25 Polymer coating
Detailed Description
Some embodiments according to the invention will be described in more detail below with reference to the accompanying drawings. It is to be understood that other various embodiments can be devised and modifications can be made by those skilled in the art based on the teachings of this specification without departing from the scope or spirit of the present disclosure. The following detailed description is, therefore, to be regarded in an illustrative rather than a restrictive sense.
Unless otherwise indicated, all numbers expressing feature sizes, quantities, and physical characteristics used in the specification and claims are to be understood as being modified by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the specification and attached claims are approximations that can be suitably varied by those skilled in the art to obtain the desired properties in light of the teachings of the present invention. The recitation of numerical ranges by endpoints includes all numbers subsumed within that range, e.g. 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4, and 5, etc.
Unless otherwise indicated, the starting materials used in the examples are all commercially available and are commercially available.
Nanoparticle mixture
Certain aspects of the present invention provide a nanoparticle mixture comprising at least any two of the following components: (A) first composite metal oxide nanoparticles, (B) carbon black nanoparticles, (C) second composite metal oxide nanoparticles.
The first composite metal oxide nanoparticles are mainly used to provide an infrared blocking effect and to adjust color and light transmittance of the adhesive film and the heat insulating film, and may be selected from composite transition metal oxides such as copper-chromium (Cu-Cr) composite metal oxide, copper-iron-manganese (Cu-Fe-Mn) composite metal oxide, copper-manganese (Cu-Mn) composite metal oxide, copper-chromium-manganese (Cu-Cr-Mn) composite metal oxide, copper-chromium-manganese-nickel (Cu-Cr-Mn-Ni) composite metal oxide, cobalt-iron (Co-Fe) composite metal oxide, and combinations thereof.
The carbon black nanoparticles are used for providing a certain degree of infrared blocking effect and adjusting the color and light transmittance of the adhesive film and the heat insulation film. After the intensive research of the inventor, the compounding of the first composite metal oxide nanoparticles and the carbon black nanoparticles is found to further improve the infrared barrier property, so that the adhesive film has good heat insulation property.
The second composite metal oxide is used for providing infrared blocking effect, and can be selected from tin-containing composite metal oxide, such as tin dioxide (SnO)2) Indium Tin Oxide (ITO), zinc doped tin oxide (ZTO); it may also be selected from antimony-containing composite metal oxides, such as antimony trioxide (Sb)2O3) Antimony (SbO)2) (ii) a Composite metal oxides containing tin and antimony, such as antimony doped tin oxide (ATO), may also be selected; combinations of tin-containing, antimony-containing, and tin and antimony-containing composite metal oxides may also be selected, such as tin dioxide (SnO)2) And antimony doped tin oxide (ATO). After intensive research and repeated experiments, the addition of the second composite metal oxide has little influence on the visible light transmittance and the color tone of the adhesive film and the heat insulating film,but the infrared blocking performance can be significantly improved. In fact, the infrared blocking performance of the nanoparticle mixture increases as the content of the second composite metal oxide increases.
The total weight of the nanoparticle mixture, in 100 wt.%, comprises: 0-85 wt.% of the first composite metal oxide nanoparticles, 0-20 wt.% of the carbon black nanoparticles, 0-99.9 wt.% of the second composite metal oxide nanoparticles.
According to certain embodiments, the nanoparticle mixture may be comprised of the first composite metal oxide nanoparticles and the carbon black nanoparticles. The first composite metal oxide nanoparticles are present in an amount greater than 80 weight percent.
According to certain embodiments, the nanoparticle mixture may be comprised of the carbon black nanoparticles and the second composite metal oxide nanoparticles. The second composite metal oxide nanoparticles are present in an amount greater than 95% by weight.
According to certain embodiments, the nanoparticle mixture may be comprised of the first composite metal oxide nanoparticles and the second composite metal oxide nanoparticles. The second composite metal oxide nanoparticles are present in an amount greater than 99% by weight.
According to certain embodiments, the nanoparticle mixture may be comprised of the first composite metal oxide nanoparticles, the carbon black nanoparticles, and the second composite metal oxide nanoparticles. The second composite metal oxide nanoparticles are present in an amount greater than 90% by weight.
Method for preparing nanoparticle mixture
The components of the nanoparticle mixture provided according to the present invention are mixed to obtain a nanoparticle mixture.
According to certain embodiments, (a) the first composite metal oxide nanoparticles and (B) the carbon black nanoparticles are mixed to obtain a nanoparticle mixture.
According to certain embodiments, (B) carbon black nanoparticles and (C) second composite metal oxide nanoparticles are mixed to obtain a nanoparticle mixture.
According to certain embodiments, (a) the first composite metal oxide nanoparticles and (C) the second composite metal oxide nanoparticles are mixed to obtain a nanoparticle mixture.
According to certain embodiments, (a) the first composite metal oxide nanoparticles, (B) the carbon black nanoparticles, and (C) the second composite metal oxide nanoparticles are mixed to obtain a nanoparticle mixture.
Polymer and method of making same
Certain aspects of the invention provide a polymer comprising polymer particles and a nanoparticle mixture provided herein, the ratio of the weight of the nanoparticle mixture to the weight of the polymer particles being less than 0.85. The polymeric particles may be selected from polyester resins, polyurethane resins, and combinations thereof.
The inventors have intensively studied and found that the visible light transmittance can be adjusted by adjusting the ratio of the weight of the nanoparticle mixture to the weight of the polymer particles while the formulation of the nanoparticle mixture is unchanged. The larger the ratio, the smaller the visible light transmittance.
Process for the preparation of polymers
At least any two of (A) a first composite metal oxide nanoparticle dispersion liquid, (B) a carbon black nanoparticle dispersion liquid, and (C) a second composite metal oxide nanoparticle dispersion liquid are sequentially added into a dispersion liquid containing polymer particles according to a certain proportion, and the mixture is uniformly stirred to obtain a liquid polymer solution of the invention. The polymer solution obtained above may be further dried to obtain the polymer of the present invention in a solid form.
Adhesive film
In some aspects of the present invention, a film is provided, which comprises a polymer film substrate layer, wherein the polymer film substrate layer is coated with a film containing the polymer of the present invention.
Thermal insulationFilm
Certain aspects of the present disclosure provide a thermal barrier film. As shown in fig. 1, which shows a heat insulation film 2 according to an embodiment of the present invention, the heat insulation film 2 comprises an abrasion resistant layer 21, a polymer film substrate layer 22, a lamination adhesive layer 23, a polymer film substrate layer 22 and a pressure sensitive adhesive layer 24 from top to bottom, and the nanoparticle mixture 1 of the present invention can be dispersed in at least one of the abrasion resistant layer 21, the lamination adhesive layer 23 and the pressure sensitive adhesive layer 24.
As shown in fig. 1, the nanoparticle mixture 1 of the present invention is dispersed in the lamination glue layer 23. It will be understood by those skilled in the art that the nanoparticle mixture 1 of the present invention may also be dispersed in the abrasion resistant layer 21, or in both the laminate adhesive layer 23 and the pressure sensitive adhesive layer 24, or in both the laminate adhesive layer 23, the abrasion resistant layer 21 and the pressure sensitive adhesive layer 24. Not all possible solutions are listed here.
As shown in fig. 2, which shows a heat insulation film 2 'according to another embodiment of the present invention, the heat insulation film 2' comprises an abrasion resistant layer 21, a polymer film base material layer 22, a polymer coating layer 25 and a pressure sensitive adhesive layer 24 from top to bottom, and the nanoparticle mixture 1 of the present invention can be dispersed in at least one of the abrasion resistant layer 21, the polymer coating layer 25 and the pressure sensitive adhesive layer 24.
As shown in fig. 2, the nanoparticle mixture 1 of the present invention is dispersed in a polymer coating 25. It will be understood by those skilled in the art that the nanoparticle mixture 1 of the present invention may also be dispersed in the pressure sensitive adhesive layer 24, or in both the polymer coating layer 25 and the pressure sensitive adhesive layer 24, or in both the polymer coating layer 25, the abrasion resistant layer 21 and the pressure sensitive adhesive layer 24. Not all possible solutions are listed here.
The material constituting the above-mentioned wear-resistant layer 21 may be selected from the following materials: the thickness of the silicon-containing resin, the acrylic resin and the acrylate copolymer is preferably 2 to 4 μm.
The material constituting the polymer film base material layer 22 may be selected from the following materials: polyester resins, polyolefin resins, polystyrene resins, polycarbonate resins, polyamide resins, among which polyester resins such as polyethylene terephthalate resins (PET) are most commonly used. The thickness thereof is preferably 12 to 50 μm.
The material constituting the polymer coating layer 25 may be selected from a coating layer formed of a polyester resin solution, a polyurethane resin solution, or a combination thereof. Preferably, the polymer coating is a coating formed from a polyester resin solution. The thickness thereof is preferably 1 to 12 μm.
The thickness of the above-mentioned laminate adhesive layer 23 is preferably 1 to 6 μm, and the thickness of the above-mentioned pressure-sensitive adhesive layer 24 is preferably 6 to 9 μm.
While the thermal barrier film structures shown in fig. 1 and 2 illustrate certain aspects of the present invention by way of example and not limitation, those skilled in the art will appreciate that the thermal barrier film structures may be provided in other multi-layer structures. Not all possible solutions are exhaustive here.
Examples
The following examples and comparative examples are provided to aid in understanding the present invention, and are provided for illustrative purposes only and should not be construed as limiting the scope of the present invention. All parts and percentages are by weight unless otherwise indicated.
The raw materials used in the examples of the present invention and the comparative examples are shown in table 1.
TABLE 1
Figure BDA0001264734370000091
The apparatus used to prepare and test the inventive and comparative examples is shown in Table 2.
TABLE 2
Figure BDA0001264734370000101
Preparation method of adhesive film
The film samples in the examples and comparative examples of the present invention were prepared by the following preparation methods.
A sheet of PET film (7211) was spread on a bench coater, and a prepared polymer solution (e.g., a laminating adhesive solution, a polyester resin solution) was applied to one side of the PET film (7211) using a 3# wire bar (wet coating thickness about 25 μm), and then dried in an oven at 70 ℃ to prepare a film sample.
Preparation method of heat insulation film
The heat insulating film samples in the examples and comparative examples of the present invention were prepared by the following preparation methods.
The method comprises the following steps: a film sample was prepared according to the film preparation method of the present invention, and a PET film (BH216) was applied to the surface of the film sample (the side coated with the nanoparticle mixture) using a heat laminator. The surface of the adhesive film (one surface of the PET film (7211)) is coated with an abrasion-resistant coating solution, and the adhesive film is cured and formed by ultraviolet light emitted by an ultraviolet curing machine. And (3) coating a pressure-sensitive adhesive solution on the surface of the other side (one side of the PET film (BH 216)) of the laminating film, drying, and laminating with a release film to prepare a heat insulation film sample.
The method 2 comprises the following steps: according to the preparation method of the film, the film sample is prepared, the wear-resistant coating solution is coated on the surface of the film sample (the surface which is not coated with the nano-particle mixture), and the film sample is cured and formed through ultraviolet light emitted by an ultraviolet curing machine. And (3) coating a pressure-sensitive adhesive solution on the surface of the film sample (the surface coated with the nanoparticle mixture), drying, and laminating with a release film to prepare the heat-insulating film sample.
Test method
According to the invention, the infrared barrier performance of the adhesive film and the heat insulation film is evaluated through a total solar barrier test, the color adjusting performance of the nanoparticle mixture on the adhesive film and the heat insulation film is evaluated through a color tone test, the optical performance of the adhesive film and the heat insulation film is evaluated through a visible light transmittance test, and the haze performance of the adhesive film and the heat insulation film is evaluated through a haze test.
Total solar energy rejection test
The spectrum data of the sample is measured by a spectrometer according to the ASTM E903 standard, and then the total solar energy blocking rate is calculated according to the ISO9050 standard. Total solar energy includes visible light, infrared light, ultraviolet light, and the like. The greater the total solar energy blocking rate of the sample at the same visible light transmittance level, the better the infrared blocking performance of the sample is considered. In addition, a light transmittance spectrogram of the sample can be obtained according to the spectral data, wherein the lower the light transmittance value in the infrared region is, the better the infrared blocking effect is.
Color tone testing
Color tone of the sample (Ta) according to ASTM E308 Standard using a colorimeter＊，Tb＊) And (6) carrying out testing. Ta＊The larger the value, the darker the red, if Ta＊The value is within the range of-3 to 0, and the value is considered to be in accordance with the requirement; tb＊The larger the value, the darker the yellow, if Tb＊Values in the range of 0 to 4 are considered satisfactory.
Visible light transmittance test
The samples were tested using a spectrometer according to ASTM E903 standard. The optical properties of the samples were considered satisfactory if the visible transmission of the samples ranged from 5% to 85%.
Haze test
The samples were tested using a transmission hazemeter according to ASTM D1003. The haze properties of the sample are considered good if the haze value of the sample is less than 3.5, and excellent if the haze value is less than 2.5.
Film sample
Example 1
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA20), and 1.60g of the composite nano metal oxide dispersion (VH-805) and 0.55g of the nano carbon black dispersion (AY-813C) were added under stirring to give a clear and transparent blue-black solution.
According to the film preparation method of the present invention, the film sample of example 1 was prepared.
The samples of example 1 were tested according to the test method of the present invention and the results of each test are recorded in table 4.
Examples 2 to 3
The preparation method and the raw material components are the same as example 1, and the weight of the raw materials is shown in Table 3.
The samples of examples 2-3 were tested according to the test method of the present invention and the results of each test are reported in table 4.
Example 4
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA10), and 0.97g of the composite nano metal oxide dispersion (VH-805) and 0.33g of the nano carbon black dispersion (AY-813C) were added under stirring to give a clear and transparent blue-black solution.
According to the film preparation method of the present invention, the film sample of example 4 was prepared.
The sample of example 4 was tested according to the test method of the present invention and the results of each test are recorded in table 4.
Examples 5 to 7
The preparation method and the raw material components are the same as example 4, and the weight of the raw materials is shown in Table 3.
The samples of examples 5-7 were tested according to the test method of the present invention and the results of each test are reported in table 4.
Example 8
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA10), and 1.033g of the composite nano metal oxide dispersion (VH-805) and 0.248g of the nano carbon black dispersion (VH-803) were added under stirring to obtain a clear and transparent blue-black solution.
According to the film preparation method of the present invention, the film sample of example 8 was prepared.
The sample of example 8 was tested according to the test method of the present invention and the results of each test are recorded in table 4.
Example 9
10g of the laminating adhesive solution (LA10) was charged in a 50ml glass bottle, and 0.058g of the composite nano-metal oxide dispersion (VH-805) and 2.0g of SbO were added under stirring2Dispersion (CX-Z410K) gave a clear, transparent black solution.
According to the film preparation method of the present invention, the film sample of example 9 was prepared.
The sample of example 9 was tested according to the test method of the present invention and the results of each test are recorded in table 4.
Example 10
20g of laminating adhesive solution (LA10) was put into a 50ml glass bottle, and 1.212g of antimony-doped oxide dispersion (ATO-8230-MEK) was added under stirring to prepare a mixed solution I; 8g of the mixed solution I was charged into a 50ml glass bottle, and 0.044g of the composite nano-metal oxide dispersion (VH-805) was added under stirring to obtain a clear and transparent black solution.
According to the film preparation method of the present invention, the film sample of example 10 was prepared.
The sample of example 10 was tested according to the test method of the present invention and the results of each test are recorded in table 4.
Examples 11 to 12
The preparation method and the raw material components are the same as in example 10, and the weight of the raw materials is shown in Table 3.
The samples of examples 11-12 were tested according to the test method of the present invention and the results of each test are reported in table 4.
Example 13
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA10), and 0.056g of the composite nano metal oxide dispersion (VH-805) and 0.019g of the nano carbon black dispersion (AY-813C) were added under stirring to obtain a clear and transparent black solution.
According to the film preparation method of the present invention, a film sample of example 13 was prepared.
The sample of example 13 was tested according to the test method of the present invention and the results of each test are recorded in table 4.
Example 14
10g of the laminating adhesive solution (LA10) was put into a 50ml glass bottle, 0.056g of the composite nano metal oxide dispersion (VH-805) and 0.019g of the nano carbon black dispersion (AY-813C) were added under stirring to obtain a clear and transparent black solution, and 0.25g of SbO was added to the black solution2The dispersion (CX-Z410K) gave a mixed solution.
According to the film preparation method of the present invention, the film sample of example 14 was prepared.
The samples of example 14 were tested according to the test method of the present invention and the results of each test are recorded in table 4.
Examples 15 to 17
The preparation method and the raw material components are the same as in example 14, and the weight of the raw materials is shown in Table 3.
The samples of examples 15-17 were tested according to the test method of the present invention and the results of each test are reported in table 4.
Comparative example 1
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA20), and 1.60g of the composite nano-metal oxide dispersion (VH-805) was added thereto with stirring to obtain a clear and transparent solution.
According to the film preparation method of the present invention, the film sample of comparative example 1 was prepared.
The samples of comparative example 1 were tested according to the test method of the present invention, and the results of each test are recorded in table 4.
Comparative example 2
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA20), and 0.55g of the nano-carbon black dispersion (AY-813C) was added under stirring to give a clear and transparent black solution.
According to the film preparation method of the present invention, a film sample of comparative example 2 was prepared.
The samples of comparative example 2 were tested according to the test method of the present invention, and the results of each test are recorded in table 4.
Heat insulation film sample
Example 18
A50 ml glass bottle was charged with 10g of the polyester resin solution, and 0.03g of the nano carbon black dispersion (ZKBLACK4) and 0.75g of the ATO dispersion (ATO-8230-MEK) were added with stirring to give a clear and transparent black solution. After stirring for 15 minutes, 0.15g of isocyanate NCO (L75) was added.
According to the heat insulating film production method 2 of the present invention, a heat insulating film sample was produced.
The sample of example 18 was tested according to the test method of the present invention and the results of each test are recorded in table 5.
Examples 19 to 30
Using the film attachment sample of example 1, a heat insulating film sample of example 19 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 4, a heat insulating film sample of example 20 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 5, a heat insulating film sample of example 21 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 9, a heat insulating film sample of example 22 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 10, a heat insulating film sample of example 23 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 11, a heat insulating film sample of example 24 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 12, a heat insulating film sample of example 25 was prepared according to heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 13, a heat insulating film sample of example 26 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 14, a heat insulating film sample of example 27 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 15, a heat insulating film sample of example 28 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 16, a heat insulating film sample of example 29 was prepared according to the heat insulating film production method 1 of the present invention.
Using the film attachment sample of example 17, a heat insulating film sample of example 30 was prepared according to the heat insulating film production method 1 of the present invention.
The samples of examples 19-30 were tested according to the test method of the present invention and the results are reported in Table 5
Comparative examples 3 to 4
Using the film-attached sample of comparative example 1, a heat insulating film sample of comparative example 3 was prepared according to the heat insulating film preparation method 1 of the present invention.
Using the film-attached sample of comparative example 2, a heat insulating film sample of comparative example 4 was prepared according to the heat insulating film preparation method 1 of the present invention.
The samples of comparative examples 3-4 were tested according to the test method of the present invention, and the results are reported in table 5.
Comparative example 5
The heat insulation film product with the brand of the glamour shadow produced by 3M company is selected.
The samples of comparative example 5 were tested according to the test method of the present invention, and the test results are recorded in table 5.
Comparative example 6
A50 ml glass bottle was charged with 10g of the laminating adhesive solution (LA10), and 0.058 composite nano-metal oxide dispersion (VH-805) was added under stirring to give a clear and transparent solution.
According to the heat insulating film preparation method 1 of the present invention, a heat insulating film sample of comparative example 6 was prepared.
The samples of comparative example 6 were tested according to the test method of the present invention, and the test results are recorded in table 5.
Comparative example 7
The heat insulation film product manufactured by 3M company and having a mark of smooth wind collection is selected.
The sample of comparative example 7 was tested according to the test method of the present invention, and the test results are recorded in table 5.
The components in the examples and comparative examples of the present invention are shown in table 3.
Figure BDA0001264734370000181
Figure BDA0001264734370000191
Figure BDA0001264734370000201
The test results of the examples and comparative examples of the film samples of the present invention are shown in table 4.
TABLE 4
Figure BDA0001264734370000211
The test results of examples and comparative examples of the heat insulating film sample of the present invention are shown in table 5.
TABLE 5
Figure BDA0001264734370000221
As can be seen from the test results of examples 1 to 17 in Table 4, the adhesive film according to the present invention has satisfactory color tone, visible light transmittance and haze.
As can be seen from the test results of examples 18 to 30 in Table 5, the heat insulating film according to the present invention has satisfactory color tone, visible light transmittance and haze.
FIG. 3 is a graph showing the light transmittance spectra of example 19 and comparative examples 3 to 5, in which the horizontal axis represents the wavelength range (unit: nm) and the vertical axis represents the magnitude of light transmittance (unit:%), and the infrared light transmittance of example 19 is significantly lower than that of comparative examples 3 to 5 in the infrared region (wavelength greater than 700 nm). The use of the first composite metal oxide nanoparticles and the carbon black nanoparticles, respectively, can reduce the transmittance of light in the infrared region to some extent, but the use of the first composite metal oxide nanoparticles and the carbon black nanoparticles in combination can provide infrared barrier properties that are more excellent than those achievable by using either of them alone. In addition, the first composite oxide nanoparticles and the carbon black nanoparticles are matched for use, so that the color tones of the film can be better adjusted to meet the requirements. In contrast, the use of only the first composite metal oxide nanoparticles (e.g., comparative examples 1 and 3) resulted in a patch that was less yellow and less desirable; the use of only carbon black nanoparticles (e.g., comparative examples 2 and 4) resulted in a darker red and yellow color of the film, which was not satisfactory.
FIG. 4 is a graph showing the light transmittance spectra of example 22 and comparative examples 6 to 7, in which the horizontal axis shows the wavelength range (unit: nm) and the vertical axis shows the magnitude of light transmittance (unit:%), and the infrared light transmittance of example 22 is significantly lower than that of comparative example 6 and comparative example 7 in the infrared region (wavelength of more than 700 nm).
FIG. 5 is a graph showing the light transmittance spectra of examples 26 to 30, in which the horizontal axis represents the wavelength range (unit: nm) and the vertical axis represents the light transmittance (unit:%), and it was found that the infrared light transmittance of the heat insulating film decreases as the percentage of antimony trioxide increases in the infrared light region (wavelength greater than 700nm), i.e., the infrared blocking effect of the heat insulating film becomes more remarkable.
The addition of the second composite metal oxide nanoparticles has little influence on light transmittance and color, but can further improve the infrared blocking performance, and the total solar blocking rate is continuously improved along with the increase of the second composite metal oxide.
When the formula of the nanoparticle mixture is not changed, the visible light transmittance of the film can be adjusted by adjusting the ratio of the weight of the nanoparticle mixture to the weight of the polymer particles. The larger the ratio, the smaller the visible light transmittance.
In summary, according to the nanoparticle mixture of the present invention and the adhesive film and the heat insulating film containing the nanoparticle mixture of the present invention, not only the infrared blocking performance can be improved, but also the color tone, the visible light transmittance and the haze of the adhesive film can be adjusted to meet the requirements.
The above-described embodiments of the present invention are merely illustrative of the principles and effects of the present invention and are not intended to limit the present invention, and it will be apparent to those skilled in the art that any changes and modifications may be made within the scope of the present invention without departing from the spirit and scope of the invention. The protection scope of the present invention should be defined as set forth in the appended claims.

Claims (13)

1. A nanoparticle mixture comprising a combination of the following component (a) and component (C); a combination of component (B) and component (C); or a combination of component (a), component (B) and component (C):
(A) first composite metal oxide nanoparticles comprising a composite transition metal oxide selected from the group consisting of copper-chromium composite metal oxide, copper-iron-manganese composite metal oxide, copper-chromium-manganese-nickel composite metal oxide, cobalt-iron composite metal oxide, and combinations thereof;
(B) carbon black nanoparticles; and
(C) second composite metal oxide nanoparticles selected from the group consisting of antimony doped tin oxide, antimony oxide, tin dioxide, indium tin oxide, zinc doped tin oxide, and combinations thereof,
wherein:
when the nanoparticle mixture consists of the carbon black nanoparticles and the second composite metal oxide nanoparticles, the weight percent content of the second composite metal oxide nanoparticles is greater than 90% in 100 wt.% of the total weight of the nanoparticle mixture;
when the nanoparticle mixture consists of the first composite metal oxide nanoparticles and the second composite metal oxide nanoparticles, the weight percent content of the second composite metal oxide nanoparticles is greater than 90% by weight, based on 100 wt.% of the total weight of the nanoparticle mixture; and is
When the nanoparticle mixture consists of the first composite metal oxide nanoparticles, the carbon black nanoparticles, and the second composite metal oxide nanoparticles, the weight percent of the second composite metal oxide nanoparticles is greater than 90% based on 100 wt.% of the total weight of the nanoparticle mixture.
2. The nanoparticle mixture according to claim 1, wherein the carbon black nanoparticles are dispersed in an organic solvent selected from methyl isobutyl ketone, butanone.
3. A polymer comprising polymer particles and a nanoparticle mixture as claimed in claim 1 or 2, the ratio of the weight of the nanoparticle mixture to the weight of the polymer particles being less than 0.85.
4. The polymer of claim 3, wherein the polymer particles are selected from polyester resins, polyurethane resins, and combinations thereof.
5. A film comprising a polymer film base material layer, wherein the polymer according to claim 3 or 4 is coated on the surface of the polymer film base material layer.
6. A thermal barrier film comprising a nanoparticle mixture according to claim 1 or 2 and at least one coating layer in which the nanoparticle mixture is dispersed.
7. The heat insulating film according to claim 6, wherein the heat insulating film comprises an abrasion resistant layer, a polymer film substrate layer, a laminating adhesive layer, a polymer film substrate layer and a pressure sensitive adhesive layer from top to bottom, and the nanoparticle mixture is dispersed in at least one of the abrasion resistant layer, the laminating adhesive layer and the pressure sensitive adhesive layer.
8. The thermal insulating film of claim 7, wherein the nanoparticle mixture is dispersed in the laminate subbing layer.
9. The heat insulating film according to claim 7, wherein the abrasion resistant layer has a thickness of 2-4 μm, the polymer film substrate layer has a thickness of 12-50 μm, the laminate adhesive layer has a thickness of 1-6 μm, and the pressure sensitive adhesive layer has a thickness of 6-9 μm.
10. The heat insulating film according to claim 6, wherein the heat insulating film comprises an abrasion resistant layer, a polymer film substrate layer, a polymer coating layer and a pressure sensitive adhesive layer from top to bottom, and the nanoparticle mixture is dispersed in at least one of the abrasion resistant layer, the polymer coating layer and the pressure sensitive adhesive layer.
11. The thermal insulating film of claim 10, wherein the nanoparticle mixture is dispersed in the polymeric coating.
12. The thermal film of claim 10 wherein said polymeric coating is selected from the group consisting of polyester resins, polyurethane resins, and combinations thereof.
13. The insulation film according to claim 10, wherein the abrasion resistant layer has a thickness of 2-4 μm, the polymer film substrate layer has a thickness of 12-50 μm, the polymer coating layer has a thickness of 1-12 μm, and the pressure sensitive adhesive layer has a thickness of 6-9 μm.
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