CN110760274A - Nano metal heat insulation film with low light reflection rate and low light transmittance and preparation method thereof - Google Patents
Nano metal heat insulation film with low light reflection rate and low light transmittance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano metal heat insulation film with low light reflection rate and low light transmittance and a preparation method thereof, the heat insulation film sequentially comprises an anti-scraping layer formed by coating an ultraviolet curing coating, a base film with two surfaces respectively pretreated, a nickel-chromium layer, an installation glue layer and a release film from top to bottom, the visible light transmittance of the nickel-chromium layer is 30-60%, the ultraviolet curing coating comprises a nano inorganic pigment slurry, an ultraviolet curing resin, a photosensitizer, a leveling agent and a solvent, the nano inorganic pigment slurry at least comprises a carbon black slurry and a silicon titanium nitride slurry, the installation glue layer is formed by coating an installation glue coating, and the installation glue coating comprises a carbon black slurry, an ultraviolet absorbent, a pressure sensitive adhesive and a solvent. The invention realizes the heat insulation film with low visible light transmittance through the nano carbon black, the nano silicon titanium nitride, the nickel-chromium layer and the nano carbon black in the mounting glue layer in the scratch resistant layer, thereby not only ensuring the weather resistance stability of the heat insulation film, but also completely solving the problem of light pollution of the low-transmittance metal film, namely the internal and external reflectivity of the heat insulation film is less than 10 percent.
Description
Technical Field
The invention relates to a nano metal heat insulation film, in particular to a nano metal heat insulation film with high weather resistance, high definition, low light reflection rate and low light transmittance and a preparation method thereof, belonging to the technical field of heat insulation sticking films.
Background
The heat insulation film has the function of adjusting the sunlight energy entering the room or the vehicle, so that the comfort level can be improved while the energy consumption of the air conditioner in summer is reduced. The visible portion of the sunlight energy can be adjusted to the ratio of entering the room or the vehicle by dye, pigment, metal or a combination of the three. The dye can be added into the composite glue to form a composite dyeing film by coating, or added into PET to form a PET primary color film by biaxial tension, and the PET primary color film is easy to match with the composite glue or PET resin, so that the film has high definition, but has poor weather resistance and infrared blocking effect. Pigments are generally much more weather resistant than dyes. The pigments are divided into organic pigments and inorganic pigments, the organic pigments basically have no infrared blocking capability, and the inorganic pigments have a certain infrared blocking effect. To ensure clarity, either organic or inorganic pigments, must be reasonably dispersed and form a good match with the chosen resin without agglomeration to ensure that the pigment thermal barrier film does not produce a hazy visual effect under sunlight.
Chinese patent document CN106965518A discloses a heat insulating film formed by compounding carbon black and an organic pigment, which has the advantage of good weather resistance, but when the visible light transmittance is less than 20%, the color uniformity and the sharpness of the coating are difficult to continuously and stably mass-produce. Chinese patent document CN104789110A discloses a heat insulation film prepared from a non-solvent type ultraviolet curing coating material combining carbon black and an organic pigment, which solves the problem of weather resistance, but has the problems of low infrared blocking rate and low definition of the film, i.e. the haze is about 2%, the requirement for ultraviolet curing energy is high, it is difficult to ensure that the base film is not deformed and the color uniformity is achieved when the visible light transmittance is less than 20%.
The metal film has the advantages of high definition, good heat insulation effect and the like, the preparation method is also multiple, the metal film can be prepared by thermally evaporating aluminum or magnetron sputtering titanium, iron or nickel-chromium, wherein the nickel-chromium metal film also has the advantage of long service life, but the metal film can cause serious light pollution due to the reflection problem when the transmittance is low. Chinese patent document CN204296154U discloses a heat insulating film made of a single-layer metal film, but when the visible light transmittance is lower than 35%, the visible light reflectance is greater than 20%, which causes serious light pollution and discomfort, and does not meet the national standards. Chinese patent CN102774111A discloses a technical scheme for reducing the visible light reflectivity by using two magnetron sputtering nickel-chromium films to be laminated and compounded, but the reflectivity is still very high, and when the visible light transmittance is approximately equal to 23%, the reflectivity is more than 15%. Chinese patent document CN103121315A discloses a technical scheme of using a low-reflection magnetron sputtering titanium nitride film and a magnetron sputtering nickel-chromium film to be attached to each other to reduce the internal reflection rate of visible light, but the external reflection rate is higher than 10%.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a nano metal heat insulation film with low light reflection rate and low light transmittance and a preparation method thereof. The nanometer metal heat insulation film realizes the heat insulation film with low visible light transmittance through the nanometer carbon black in the scratch resistant layer and the nanometer carbon black in the nanometer silicon titanium nitride layer, the nickel-chromium layer and the mounting glue layer, effectively reduces the internal and external reflectivity of the metal film, ensures the performances of the film such as weather resistance, definition and the like, simultaneously overcomes the problems of non-uniformity of coating color, deformation of a base film and the like in production, and better solves the defects in the prior art.
The purpose of the invention is realized by the following technical scheme:
the utility model provides a have nanometer metal heat insulating film of low luminousness of low reflectance concurrently, heat insulating film is from last to including in proper order down carrying out the base film of preliminary treatment, nickel chromium layer, installation glue film and the lamellar structure that forms from the type membrane respectively by anti scraping layer, the two-sided of ultraviolet curing coating formation, the haze value of base film <1%, the visible light transmissivity on nickel chromium layer is 30% ~ 60%, ultraviolet curing coating includes nanometer inorganic pigment thick liquids, ultraviolet curing resin, photosensitizer, flatting agent and solvent, nanometer inorganic pigment thick liquids include carbon black thick liquids and silicon nitride titanium thick liquids at least, the installation glue film is formed by the coating of installation glue coating, the installation glue coating includes carbon black thick liquids, ultraviolet absorbent, pressure sensitive adhesive and solvent, the solvent includes ethyl acetate at least.
Preferably, the pretreatment of the base film is a coating precoat layer and a corona treatment, and the precoat layer is an acrylic layer or a Polyurethane (PU) layer.
Preferably, the base film is a PET base film, the thickness of the base film is 30-100 mu m, the longitudinal thermal shrinkage rate and the transverse thermal shrinkage rate of the PET base film are respectively 1.0-1.5% and-0.1-0.5%, the nickel-chromium layer is formed on the corona surface of the PET base film through magnetron sputtering of nickel-chromium alloy, and the proportion of chromium in the nickel-chromium alloy is 10-30%.
Preferably, the carbon black slurry comprises carbon black, the silicon titanium nitride slurry comprises silicon titanium nitride, and the weight ratio of the silicon titanium nitride to the carbon black in the ultraviolet light curing coating is 1.0-5.0 times.
Preferably, the carbon black slurry comprises carbon black, a dispersing agent and a solvent, wherein the particle size of the carbon black is 10-20 nm, and the using amount of the dispersing agent is 50-80% of the weight of the carbon black; the titanium silicon nitride slurry comprises titanium silicon nitride, a dispersing agent and a solvent, wherein the particle size of the titanium silicon nitride is 15-35 nm, the silicon doping ratio in the titanium silicon nitride is 0-20%, and the using amount of the dispersing agent is 60-100% of the weight of the titanium silicon nitride; the dispersing agent comprises a micromolecular dispersing agent and a polymer dispersing agent, wherein the molecular weight of the micromolecular dispersing agent is less than 1000, the micromolecular dispersing agent is provided with an acid group, a basic group or an acid-base homologous group, the molecular weight of the polymer dispersing agent is more than 3000, the polymer dispersing agent has an amine value or an acid value of 10-100 mg KOH/g, the proportion of the micromolecular dispersing agent is 0-30%, and the proportion of the polymer dispersing agent is 70-100%.
Preferably, the nano inorganic pigment slurry further comprises cesium tungsten oxide slurry, wherein the cesium tungsten oxide doping proportion is 3-6%, and the particle size of the cesium tungsten oxide is 20-80 nm.
Preferably, the ultraviolet light curing resin is hexa-functional or higher aliphatic polyurethane acrylate with molecular weight>1000, the dosage of the ultraviolet curing resin in the scratch resistant layer is 1.8-4.5 g/m2The nano inorganic pigmentThe slurry comprises a dispersant which is compatible with the ultraviolet curing resin, and the dispersant is an acrylate copolymer dispersant.
Preferably, the photosensitizer comprises a photosensitizer capable of absorbing long-wave ultraviolet light, medium-wave ultraviolet light and short-wave ultraviolet light, wherein the photosensitizer capable of absorbing long-wave ultraviolet light accounts for 25-50% of the total amount of the photosensitizer, the photosensitizer capable of absorbing medium-wave ultraviolet light accounts for 20-30% of the total amount of the photosensitizer, and the photosensitizer capable of absorbing short-wave ultraviolet light accounts for 20-55% of the total amount of the photosensitizer.
Preferably, the photosensitizer is (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenylpropanone and benzophenone.
Preferably, the leveling agent is a silicon modified copolymer, and the leveling agent is 0.5-2% of the weight of the ultraviolet curing resin.
Preferably, the pressure-sensitive adhesive in the mounting adhesive coating is a single-component acrylate composite adhesive, the peel strength of the pressure-sensitive adhesive and the nickel-chromium layer is 600-800 g/inch, and the using amount of the pressure-sensitive adhesive in the mounting adhesive layer is 5.5-9.5 g/m2The ultraviolet absorbent in the mounting adhesive coating is hydroxyl benzene triazine, and the using amount of the ultraviolet absorbent in the mounting adhesive coating is 0.2-0.75 g/m2The amount of the carbon black in the mounting adhesive coating in the mounting adhesive layer is 0.02-0.06 g/m2The nano inorganic pigment slurry comprises a dispersing agent which is compatible with the pressure-sensitive adhesive, and the dispersing agent is an acrylate copolymer dispersing agent.
The polymer dispersant is selected under the condition that compatibility matching with aliphatic polyurethane acrylate, single-component acrylate composite adhesive, solvent ethyl acetate and the like can be realized, and the polymer dispersant is acrylate copolymer dispersant, so that high-definition performance, namely low haze value, of the heat-insulating film is ensured. When the dispersing agent layer wrapped on the surface of the nano material is thin, the ultraviolet curing resin or the single-component acrylate composite adhesive can realize compatibility matching with the dispersing agent consisting of the nano material, the small molecular dispersing agent and the polymer dispersing agent in the slurry, so that the dispersing agent layer with proper thickness is wrapped according to different nano materials, namely the proportion of the dispersing agent is at least more than 50%, and the obstacle of the nano material in the polarity matching process can be reduced.
Preferably, the preparation method of the nano metal heat insulation film with low light reflection rate and low light transmittance comprises the following steps:
s1, preparing a nickel-chromium-based film: selecting a transparent PET with two sides subjected to pre-coating and corona treatment respectively and haze less than 1% as a base film, plating a layer of nickel-chromium alloy on the corona surface of the base film through magnetron sputtering, and controlling the thickness to obtain a nickel-chromium base film with transmittance of 30-60%, wherein the two sides are a PU (polyurethane) pre-coating layer and a nickel-chromium layer respectively;
s2, preparation of nano inorganic pigment slurry: firstly, mixing and stirring a dispersant and a solvent in a premixing cylinder, then introducing the mixture into a grinding cavity of a ball mill for grinding, gradually adding carbon black or titanium silicon nitride, and respectively preparing carbon black slurry or titanium silicon nitride slurry after grinding;
s3, preparation of the ultraviolet curing coating: adding a solvent into a stirring cylinder, then respectively adding the carbon black slurry and the titanium silicon nitride slurry prepared in the step S2 into the stirring cylinder, finally gradually adding the ultraviolet curing resin, the photosensitizer and the flatting agent into the mixture, and stirring the mixture to prepare the ultraviolet curing coating;
s4, preparing a mounting adhesive coating: adding a solvent into a stirring cylinder, then respectively adding the carbon black slurry prepared in the step S2 and an ultraviolet absorbent during stirring, finally gradually adding a pressure-sensitive adhesive, and stirring to prepare the mounting adhesive coating;
s5, preparing an installation adhesive layer: coating the mounting adhesive coating prepared by S4 on the nickel-chromium-plated chromium layer surface of the nickel-chromium-based film prepared by S1 in a micro-concave coating mode, drying the coating by an oven at 100 ℃, and compounding the coating with a release film;
s6, preparing an anti-scratch layer: and (3) coating the ultraviolet curing coating prepared by the step (S3) on the other surface of the nickel-chromium base film in the semi-finished product prepared by the step (S5), namely the PU precoated surface, drying the coating in an oven at the temperature of 80 ℃, and irradiating and curing the coating by ultraviolet rays in the nitrogen atmosphere to obtain the nano metal heat insulation film.
The invention has the beneficial effects that: 1. through resistanceThe carbon black in the scraping layer, the silicon titanium nitride layer, the nickel-chromium layer and the carbon black in the mounting glue layer jointly realize low visible light transmittance, and the weather resistance stability of the heat insulation film is ensured, namely the carbon black passes through 100mW/cm at the temperature of 80 DEG C2The average visible light transmittance of the heat insulating film of the present invention is substantially unchanged after 10 hours of irradiation with ultraviolet intensity of (c).
2. Compared with the metal heat insulation films produced by patent applications CN102774111A and CN103121315A, the reflectivity of visible light inside and outside the metal heat insulation film is lower than 10 percent and is far lower than 20 percent of the reflectivity of national standard, and the problem of light pollution of the low-transmittance metal film is completely solved.
3. The scratch-resistant layer of the nano metal heat-insulating film adopts the combination of carbon black and silicon titanium nitride, particularly the silicon titanium nitride material is used, the ultraviolet transmittance of the scratch-resistant layer is far higher than that of the combination of the carbon black and the organic pigment, so that the requirement of ultraviolet curing energy is reduced, in addition, the ultraviolet absorption of the scratch-resistant layer is further reduced because the nickel-chromium layer shares a part of visible light blocking function, so that the problem of deformation of a base film caused by high ultraviolet energy requirement in the patent application CN104789110A is solved, the infrared blocking rate is improved from about 55 percent to about 75 percent, meanwhile, the clarity is also greatly improved because the combination of micromolecules and a polymer dispersant is adopted in a solvent system for matching and dispersing, namely, the haze is reduced from about 2 percent to about 0.41 percent.
4. Compared with the production methods provided by the patent applications CN102774111A, CN103121315A and CN106965518A, the invention reduces a composite process production flow, greatly improves the production efficiency and reduces the production cost. Compared with the carbon black and organic pigment combined low heat-insulating film provided by patent applications CN106965518A and CN104789110A, the production stability is easy to control.
Drawings
FIG. 1: the invention relates to a schematic diagram of a layered structure of a nano metal heat insulation film;
FIG. 2: the transmission and reflection spectra of sample 1 in example 1 of the invention;
FIG. 3: the ultraviolet aging spectrogram of the sample 1 in the example 1 of the invention, wherein the temperature of the test cavity is 80 ℃, and the ultraviolet irradiation intensity is 100mW/cm2The intensity is violet in sunlight60 times of external energy;
FIG. 4: the transmission and reflection spectra of sample 1 of comparative example 1 of the present invention;
FIG. 5: the transmission and reflection spectra of sample 2 of comparative example 2 of the present invention.
Detailed Description
The invention discloses a nano metal heat insulation film with low light reflection rate and low light transmittance, which utilizes the anti-reflection performance of nano inorganic pigment to solve the problem of light reflection in the existing metal heat insulation film product and provides the nano metal heat insulation film with good weather resistance, high definition, low light reflection rate and low light transmittance. Combine figure 1 to show, thermal-insulated membrane is from last to including in proper order down the resistant layer 201 of scraping that forms by the coating of ultraviolet curing coating, base film 202, nickel chromium layer 203, installation glue film 204 and the lamellar structure who forms from type membrane 205, the haze value of base film 202 <1%, the visible light transmittance on nickel chromium layer 203 is 30% ~ 60%, the ultraviolet curing coating includes nanometer inorganic pigment thick liquids, ultraviolet curing resin, photosensitizer, flatting agent and solvent, nanometer inorganic pigment thick liquids include carbon black thick liquids and silicon titanium nitride thick liquids at least. The mounting adhesive layer is formed by coating a mounting adhesive coating, and the mounting adhesive coating comprises carbon black slurry, an ultraviolet absorber, a pressure-sensitive adhesive and a solvent. The leveling agent is a silicon modified copolymer, and the weight of the leveling agent is 0.5-2% of that of the ultraviolet curing resin. The solvent includes at least ethyl acetate.
The base film is a PET base film, the nickel-chromium layer is formed on the surface of the PET base film through magnetron sputtering of nickel-chromium alloy, wherein the proportion of chromium in the nickel-chromium alloy is 10-30%, and the preferable proportion is that the proportion of chromium in the nickel-chromium alloy is 15-25%.
The pretreatment of the base film is to coat a precoating layer or perform corona treatment, and the precoating layer is an acrylic layer or a polyurethane layer. In order to ensure that the adhesive force between the ultraviolet curing resin and the nano inorganic slurry and the PET base film is better than 1 grade, the PET base film pretreated by Polyurethane (PU) is preferred. The heat-insulating film is easy to construct and requires that the heat shrinkage rate of the PET base film is larger, on the other hand, in the magnetron sputtering nickel-chromium process or the ultraviolet curing process, the heat shrinkage rate of the PET base film cannot be too large, otherwise, irreversible heat shrinkage deformation can be generated due to overhigh temperature, and therefore, in order to meet the requirements of the two, the longitudinal heat shrinkage rate and the transverse heat shrinkage rate of the PET base film are respectively 1.0-1.5% and-0.1-0.5%. The thickness of the PET base film is 30-100 mu m, and in order to provide good construction performance, the thickness is preferably 30-50 mu m.
The weight ratio of the titanium silicon nitride and the carbon black in the nano inorganic pigment slurry in the scratch-resistant layer or the ultraviolet curing coating is 1.0-5.0 times, and 1.8-2.5 times can be preferably adopted to ensure pure blackness of the color. By adjusting the proportion of the two components, the colors of the heat insulation film, such as yellow, yellow green, pure black, blue and the like, can be adjusted. The matching use of the titanium silicon nitride and the carbon black can not only adjust the color of the heat insulation film, but also greatly improve the weather resistance of the heat insulation film, and is superior to the stability of organic pigment. In addition, under the condition of the same visible light transmittance, the silicon titanium nitride absorbs lower ultraviolet energy than the carbon black, so that the energy requirement in the ultraviolet curing process is reduced, and the deformation problem of the PET base film caused by overhigh temperature in the curing process is further reduced.
The carbon black slurry in the nano inorganic pigment slurry comprises carbon black, a dispersing agent and a solvent, wherein the particle size of the carbon black is 10-20 nm, and the using amount of the dispersing agent is 50-80% of the weight of the carbon black; the titanium silicon nitride slurry comprises titanium silicon nitride, a dispersing agent and a solvent, wherein the particle size of the titanium silicon nitride is 15-35 nm, and the silicon doping ratio in the titanium silicon nitride is 0-20%. Silicon doping in the titanium silicon nitride can improve the dispersion performance of the material and reduce blue absorption, and the dosage of the dispersant is 60-100% of the weight of the titanium silicon nitride. The dispersing agent comprises a micromolecular dispersing agent and a polymer dispersing agent, wherein the molecular weight of the micromolecular dispersing agent is less than 1000, the micromolecular dispersing agent is provided with an acid group, a basic group or an acid-base homologous group, the molecular weight of the polymer dispersing agent is more than 3000, the polymer dispersing agent has an amine value or an acid value of 10-100 mg KOH/g, the proportion of the micromolecular dispersing agent is 0-30%, and the proportion of the polymer dispersing agent is 70-100%.
The nano inorganic pigment slurry can also comprise cesium-doped tungsten oxide heat insulation material slurry, wherein the cesium doping proportion in the cesium tungsten oxide is 3-6%, and the particle size of the cesium tungsten oxide is 20-80 nm.
The ultraviolet light curing resin is aliphatic polyurethane acrylate with molecular weight more than 1000 and more than six functional groups, and the adhesion force between the ultraviolet light curing resin and the precoating layer of the base film is superior to grade 1. The ultraviolet light curing resin and the polymer dispersant in the silicon titanium nitride and carbon black slurry form good matching, namely, the nano inorganic pigment has no obvious agglomeration in the scratch-resistant layer, thereby ensuring high definition, namely low haze value<1 percent, wherein the dispersant is acrylate copolymer dispersant. The dosage of the ultraviolet curing resin in the scratch-resistant layer is 1.8-4.5 g/m2。
The photosensitizer in the ultraviolet curing coating comprises a photosensitizer capable of absorbing long, medium and short ultraviolet light. The photosensitizer capable of absorbing long ultraviolet light accounts for 25-50% of the total amount of the photosensitizer, the photoinitiator capable of absorbing medium ultraviolet light accounts for 20-30% of the total amount of the photosensitizer, and the photosensitizer capable of absorbing short ultraviolet light accounts for 20-55% of the total amount of the photosensitizer. The photosensitizer is specifically selected from (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl acetone and benzophenone. The combination of multiple photosensitizers can fully match the absorption spectra of carbon black and titanium silicon nitride, so that the residual ultraviolet energy is well utilized to realize complete curing, the requirement of ultraviolet curing energy is reduced, and the deformation problem of a base film caused by overhigh temperature is reduced.
The pressure-sensitive adhesive in the mounting adhesive coating is a single-component acrylate composite adhesive, the peel strength of the pressure-sensitive adhesive and the nickel-chromium layer is 600-800 g/inch, and the using amount of the pressure-sensitive adhesive in the mounting adhesive layer is 5.5-9.5 g/m2。
The specific amount of pressure sensitive adhesive used depends on the peel strength and clarity requirements, which are related to factors such as the thickness of the base film, the amount of uv absorber used, and the amount of carbon black used. When the thickness of the base film and the amount of the ultraviolet absorber are increased, the amount of the pressure-sensitive adhesive to be used is increased, for example, in the case where the amount of the pressure-sensitive adhesive to be used is increased to a certain amount, the amount of the ultraviolet absorber to be used is increased to a certain amountAt this point, the ultraviolet absorber precipitates to cause a decrease in peel strength and deterioration in clarity. Meanwhile, in order to ensure the definition of the carbon black added with the pressure-sensitive adhesive, the dosage of the pressure-sensitive adhesive is not too large. Therefore, in consideration of the above and the construction property, the thickness of the base film is within the range of 30-50 μm, and the usage amount of the pressure-sensitive adhesive in the mounting adhesive layer is 5.5-7.5 g/m2The ultraviolet absorbent is hydroxybenzene triazine, and the using amount of the ultraviolet absorbent in the mounting adhesive layer is 0.2-0.55 g/m2The amount of the carbon black in the adhesive layer is 0.02-0.045 g/m2. The polymer dispersant in the carbon black slurry and the single-component acrylate composite adhesive form good matching so as to ensure that the heat insulation film has proper definition, and the dispersant is an acrylate copolymer dispersant.
In order to reduce the requirement of ultraviolet curing energy, at least one proper inorganic pigment, namely the inorganic pigment with low ultraviolet absorption, is selected to form the ultraviolet curing pigment film. In order to improve the definition, the surface modification, namely the dispersion treatment, of which the proportion of the dispersing agent is more than 50% is realized by using the combination of micromolecules and polymer dispersing agents in a solvent system through ball milling, so that the dispersion and the matching with ultraviolet curing resin are better realized, the definition problem caused by poor matching in the Chinese patent application CN104789110A and the deformation problem of a base film are avoided, and the infrared blocking efficiency is greatly improved.
The invention also discloses a preparation method of the nano metal heat insulation film with low light reflection rate and low light transmittance, which comprises the following steps:
s1, preparing a nickel-chromium-based film: selecting a transparent PET with two sides respectively subjected to PU precoating and corona treatment and haze less than 1% as a base film, plating a layer of nickel-chromium alloy on the corona surface of the base film through magnetron sputtering, and controlling the thickness to obtain a nickel-chromium base film with transmittance of 30-60%, wherein the two sides are respectively a PU precoating layer and a nickel-chromium layer;
s2, preparing inorganic pigment slurry: firstly, mixing and stirring a dispersant and a solvent in a premixing cylinder, then introducing the mixture into a grinding cavity of a ball mill for grinding, gradually adding carbon black or titanium silicon nitride, and respectively preparing carbon black slurry or titanium silicon nitride slurry after grinding;
s3, preparation of the ultraviolet curing coating: adding a solvent into a stirring cylinder, adding the carbon black slurry and the silicon titanium nitride slurry prepared in the step S2 while stirring, gradually adding the ultraviolet curing resin, the photosensitizer and the leveling agent, and stirring to prepare the ultraviolet curing coating;
s4, preparing a mounting adhesive coating: adding a solvent into a stirring cylinder, adding the carbon black slurry prepared in the step S2 and an ultraviolet absorbent during stirring, gradually adding a pressure-sensitive adhesive, and stirring to prepare the mounting adhesive coating;
s5, preparing an installation adhesive layer: coating the mounting adhesive coating prepared by S4 on the nickel-chromium plating surface of the nickel-chromium-based film prepared by S1 in a micro-concave coating mode, drying the coating by an oven at 100 ℃, and compounding the coating with a release film;
s6, preparing an anti-scratch layer: and (3) coating the other side of the nickel-chromium base film in the semi-finished product prepared by the S5, namely the PU precoating side, with the ultraviolet curing coating prepared by the S3 in a micro-concave coating mode, drying the coating in an oven at 80 ℃, and curing by ultraviolet irradiation in a nitrogen atmosphere to obtain the low-transmittance nano metal heat insulation film.
Example 1
Selecting a base film: a 36 μm thick PET base film having a haze of less than 1% was selected, and the heat shrinkages in the machine direction and the transverse direction were 1.2% and 0.2%, respectively. One side of the base film is processed by corona treatment, and the other side is pre-coated with a PU coating.
Preparing a nickel-chromium coating: plating a layer of nickel-chromium (chromium content is 20%) alloy on the corona surface of the selected PET base film by magnetron sputtering, and preparing the nickel-chromium base film with the visible light transmittance of about 43% by thickness control.
Preparing titanium silicon nitride slurry: weighing 10 parts of silicon titanium nitride with the particle size of 20nm (the doping ratio of silicon is 10%), 2 parts of micromolecular dispersant with the molecular weight of 800, 7 parts of polymer dispersant with the molecular weight of 5000 and 81 parts of ethyl acetate, firstly mixing and stirring the dispersant and a solvent in a premixing cylinder for 15 minutes, then gradually adding the silicon titanium nitride, stirring for 30 minutes at the rotating speed of 1000RPM, finally circularly entering a grinding cavity of an 8-liter ball mill through a pneumatic diaphragm pump, grinding for 36 hours under the condition that the online speed is 10m/s, and preparing 40kg of silicon titanium nitride slurry.
Preparation of carbon black slurry: weighing 10 parts of carbon black with the particle size of 15nm, 1 part of micromolecular dispersant with the molecular weight of 800, 6.5 parts of polymer dispersant with the molecular weight of 5000 and 82.5 parts of ethyl acetate, firstly mixing and stirring the dispersant and the solvent in a premixing cylinder for 15 minutes, then gradually adding the carbon black, stirring for 45 minutes at the rotating speed of 1000RPM, finally circularly entering a grinding cavity of an 8-liter ball mill through a pneumatic diaphragm pump, grinding for 24 hours under the condition that the linear speed is 10m/s, and preparing 35kg of carbon black slurry.
Preparing the ultraviolet curing coating: 6.72 parts of the prepared silicon titanium nitride slurry, 2.89 parts of carbon black slurry, 34.70 parts of hexafunctional aliphatic polyurethane acrylate resin with the molecular weight of 1000, 0.66 part of a leveling agent, 0.694 part of benzophenone, 0.352 part of 2-hydroxy-2-methyl-1-phenyl acetone, (0.694 part of 2,4, 6-trimethylbenzoyl) diphenylphosphine oxide and 53.29 parts of ethyl acetate are weighed. Adding a solvent ethyl acetate into a stirring cylinder, then respectively adding silicon titanium nitride slurry and carbon black slurry, stirring for 5 minutes at the rotating speed of 300RPM, and finally adding the rest materials, stirring for 30 minutes at the rotating speed of 500RPM to obtain the required ultraviolet curing coating.
Preparing a mounting adhesive coating: weighing 1.25 parts of the prepared carbon black slurry, 1.15 parts of a hydroxyphenyltriazine ultraviolet absorbent, 53.10 parts of a single-component acrylic pressure-sensitive adhesive (with the solid content of 34%), 39.70 parts of ethyl acetate and 4.80 parts of propylene glycol monomethyl ether acetate. Adding solvents of ethyl acetate and propylene glycol monomethyl ether acetate into a stirring cylinder, then adding carbon black slurry and an ultraviolet absorbent, stirring for 10 minutes at the rotating speed of 300RPM, and finally gradually adding a pressure-sensitive adhesive, and stirring for 45 minutes at the rotating speed of 500RPM to prepare the mounting adhesive coating.
Preparing a low-permeability nano metal heat insulation film: firstly, coating the mounting adhesive coating on the nickel-chromium plating surface of the nickel-chromium-based film in a micro-concave coating mode, drying the coating for 1 minute by a drying oven at 100 ℃ to form a mounting adhesive layer with the thickness of 6.3 mu m, and then compounding the mounting adhesive layer with a release film. And coating the other surface of the nickel-chromium base film, namely the PU precoated surface, in the semi-finished product with the ultraviolet curing coating in a micro-concave coating mode, drying the coating for 1 minute by using an oven at the temperature of 80 ℃ to form a scratch-resistant layer with the thickness of 3.3 mu m, and irradiating and curing by using a high-pressure mercury lamp with the coating speed of 23m/min under the nitrogen atmosphere to obtain the low-permeability nano metal heat-insulating film sample 1. The scratch resistant layer of sample 1 has an adhesion of 0 grade on the PU precoated surface of the PET base film, and has no obvious scratch on the surface after being rubbed back and forth 60 times by 0000# steel wool under the condition of 500g load.
To facilitate optical and weathering tests, sample 1 was removed from the release film and mounted on a 3mm thick glass slide. The optical properties of sample 1 are shown in table 1 and fig. 2, and the visible light transmittance is 18.29%, the visible light internal reflectance is 6.30%, the visible light external reflectance is 9.64%, and the haze is 0.41%. The UV aging performance of sample 1 is shown in FIG. 3 at a temperature of 80 deg.C under a load of 100mW/cm2After the ultraviolet intensity is irradiated for 10 hours, the optical performance of the material is basically unchanged, and the material has good weather resistance. By comparing the optical data of the example 1 and the comparative examples 1 and 2 in the table 1, when the visible light transmittance of the invention is about 20%, the internal and external reflectivity is greatly reduced, the internal reflection is lower than 8% of that of the common glass, the external reflection is close to that of the common glass and is far lower than the 20% reflectivity of the national standard, so the invention completely solves the problem of light pollution of the low-transmittance metal film.
Example 2
Example 2 is mainly different from example 1 in that a cesium tungsten oxide high thermal insulation nanomaterial is added to a scratch resistant layer, so that it is necessary to prepare a cesium tungsten oxide slurry and a uv curable coating unlike example 1, and the rest of the materials and preparation are the same as those in example 1 and will not be described again.
Preparation of cesium tungsten oxide slurry: weighing 20 parts of cesium tungsten oxide with the particle size of 50nm (the doping ratio of cesium is 5%), 10 parts of polymer dispersant with the molecular weight of 10000 and 70 parts of ethyl acetate, firstly mixing and stirring the dispersant and a solvent in a premixing cylinder for 15 minutes, then gradually adding the cesium tungsten oxide, stirring at the rotating speed of 1000RPM for 15 minutes, finally circularly entering a grinding cavity of an 8-liter ball mill through a pneumatic diaphragm pump for grinding, and grinding for 40 hours under the condition that the linear speed is 14m/s to prepare 50kg of cesium tungsten oxide slurry.
Preparing the ultraviolet curing coating: weighing 4.59 parts of the prepared silicon titanium nitride slurry, 2.52 parts of carbon black slurry, 24 parts of cesium tungsten oxide slurry, 26.4 parts of octafunctional aliphatic urethane acrylate resin with the molecular weight of 1500, 0.53 part of a leveling agent, 0.54 part of benzophenone, 0.30 part of 2-hydroxy-2-methyl-1-phenyl acetone, 0.61 part of (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide and 40.51 parts of ethyl acetate. Adding ethyl acetate solvent into a stirring cylinder, respectively adding silicon titanium nitride slurry, carbon black slurry and cesium tungsten oxide slurry, stirring for 5 minutes at the rotating speed of 300RPM, finally adding the rest materials, and stirring for 30 minutes at the rotating speed of 500RPM to obtain the required ultraviolet curing coating.
Preparing a low-permeability nano metal heat insulation film: firstly, the mounting adhesive coating in the embodiment 1 is coated on the nickel-chromium plating surface of the nickel-chromium-based film selected in the embodiment 1 in a micro-concave coating mode, the coating is dried for 1 minute at 100 ℃ to form a mounting adhesive layer with the thickness of 6.3 mu m, and then the mounting adhesive layer is compounded with a release film. And coating the other surface of the nickel-chromium base film, namely the PU precoated surface, in the semi-finished product with the ultraviolet curing coating in a micro-concave coating mode, drying the coating for 1 minute in an oven at 80 ℃ to form a scratch-resistant layer with the thickness of 3.5 mu m, and irradiating and curing by a high-pressure mercury lamp with the thickness of 110W/cm under the conditions of nitrogen atmosphere and the coating speed of 20m/min to obtain a low-permeability nano metal heat-insulating film sample 2. Through tests, the heat insulation performance of the sample 2 in the embodiment is greatly improved, the infrared blocking rate of the sample is improved from 75% to more than 90%, and other performances are basically consistent with those of the sample 1 in the embodiment.
Comparative example 1
The nickel-chromium-based film prepared in example 1 was selected, firstly, a mounting adhesive coating (containing an ultraviolet absorber) without a nano pigment was coated on the surface of the nickel-chromium coating layer, and after drying, the film was compounded with a release film, then, an ultraviolet-curable coating without a nano pigment was coated on the surface of the PU coating layer, after drying, a dry film was formed by ultraviolet irradiation, and finally, the release film was removed and attached to a glass slide with a thickness of 3mm, to prepare a comparative sample 1. The optical properties of comparative sample 1 are shown in table 1 and fig. 4, with a visible light transmission of 45.67%, an internal visible light reflectance of 14.37%, and an external visible light reflectance of 18.21%.
Comparative example 2
Selecting 2 nickel-chromium-based films prepared in the example 1, firstly coating a mounting adhesive coating solution without a nano and ultraviolet absorbent on the nickel-chromium plating surface of one of the nickel-chromium-based films, drying the mounting adhesive coating solution, then compounding the dried mounting adhesive coating solution with the nickel-chromium plating surface of the other nickel-chromium-based film, then coating a mounting adhesive coating (containing an ultraviolet absorbent) without a nano pigment on any surface of the composite film, drying the mounting adhesive coating solution, then compounding the mounting adhesive coating solution with a release film, finally coating an ultraviolet curing coating without a nano pigment on the other surface of the composite film, drying the coating solution, irradiating the coating solution by ultraviolet rays to form a dry film, removing the release film, and pasting the release film on a glass slide with the thickness. The optical properties of comparative sample 2 are shown in table 1 and fig. 5, and have a visible light transmittance of 23.53%, a visible light internal reflectance of 13.87%, and a visible light external reflectance of 15.44%.
Table 1: the optical properties of the inventive sample of example 1 and the comparative sample were compared.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (12)
1. The utility model provides a have nanometer metal heat insulating film of low luminousness of low reflectance concurrently which characterized in that: the heat insulating film is from last to including in proper order down carrying on the base film of preliminary treatment respectively by anti scraping layer, the double-sided of ultraviolet curing coating formation, nickel chromium layer, installation glue film and the lamellar structure who forms from the type membrane, the haze value of base film <1%, the visible light transmissivity on nickel chromium layer is 30% ~ 60%, ultraviolet curing coating includes nanometer inorganic pigment thick liquids, ultraviolet curing resin, photosensitizer, flatting agent and solvent, nanometer inorganic pigment thick liquids include carbon black thick liquids and silicon nitride titanium thick liquids at least, the installation glue film is formed by the coating of installation glue coating, installation glue coating includes carbon black thick liquids, ultraviolet absorbent, pressure sensitive adhesive and solvent, the solvent includes ethyl acetate at least.
2. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the pretreatment of base film is for coating precoat and corona treatment, precoat is ya keli layer or polyurethane layer.
3. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 2, wherein: the base film is a PET base film, the thickness of the base film is 30-100 mu m, the longitudinal thermal shrinkage rate and the transverse thermal shrinkage rate of the PET base film are respectively 1.0-1.5% and-0.1-0.5%, the nickel-chromium layer is formed on the corona surface of the PET base film through magnetron sputtering of nickel-chromium alloy, and the proportion of chromium in the nickel-chromium alloy is 10-30%.
4. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the carbon black slurry comprises carbon black, the silicon titanium nitride slurry comprises silicon titanium nitride, and the weight ratio of the silicon titanium nitride to the carbon black in the ultraviolet curing coating is 1.0-5.0 times.
5. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 4, wherein: the carbon black slurry comprises carbon black, a dispersing agent and a solvent, wherein the particle size of the carbon black is 10-20 nm, and the using amount of the dispersing agent is 50-80% of the weight of the carbon black; the titanium silicon nitride slurry comprises titanium silicon nitride, a dispersing agent and a solvent, wherein the particle size of the titanium silicon nitride is 15-35 nm, the silicon doping ratio in the titanium silicon nitride is 0-20%, and the using amount of the dispersing agent is 60-100% of the weight of the titanium silicon nitride; the dispersing agent comprises a micromolecular dispersing agent and a polymer dispersing agent, wherein the molecular weight of the micromolecular dispersing agent is less than 1000, the micromolecular dispersing agent is provided with an acid group, a basic group or an acid-base homologous group, the molecular weight of the polymer dispersing agent is more than 3000, the polymer dispersing agent has an amine value or an acid value of 10-100 mg KOH/g, the proportion of the micromolecular dispersing agent is 0-30%, and the proportion of the polymer dispersing agent is 70-100%.
6. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 4, wherein: the nano inorganic pigment slurry also comprises cesium tungsten oxide slurry, wherein the cesium doping proportion of cesium tungsten oxide in the cesium tungsten oxide slurry is 3-6%, and the particle size of the cesium tungsten oxide is 20-80 nm.
7. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the ultraviolet light curing resin is aliphatic polyurethane acrylate with more than six functional groups and has molecular weight>1000, the dosage of the ultraviolet curing resin in the scratch resistant layer is 1.8-4.5 g/m2The nano inorganic pigment slurry comprises a dispersant which is compatible with the ultraviolet curing resin, and the dispersant is an acrylate copolymer dispersant.
8. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the photosensitizer comprises a photosensitizer capable of absorbing long-wave ultraviolet light, medium-wave ultraviolet light and short-wave ultraviolet light, wherein the photosensitizer capable of absorbing the long-wave ultraviolet light accounts for 25-50% of the total amount of the photosensitizer, the photosensitizer capable of absorbing the medium-wave ultraviolet light accounts for 20-30% of the total amount of the photosensitizer, and the photosensitizer capable of absorbing the short-wave ultraviolet light accounts for 20-55% of the total amount of the photosensitizer.
9. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 8, wherein: the photosensitizer is (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl acetone and benzophenone.
10. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the leveling agent is a silicon modified copolymer, and the weight of the leveling agent is 0.5-2% of that of the ultraviolet curing resin.
11. The nano-metal heat insulation film with low light reflectivity and low light transmittance as claimed in claim 1, wherein: the pressure-sensitive adhesive in the mounting adhesive coating is a single-component acrylate composite adhesive, the peel strength of the pressure-sensitive adhesive and the nickel-chromium layer is 600-800 g/inch, and the using amount of the pressure-sensitive adhesive in the mounting adhesive layer is 5.5-9.5 g/m2The ultraviolet absorbent in the mounting adhesive coating is hydroxyl benzene triazine, and the using amount of the ultraviolet absorbent in the mounting adhesive coating is 0.2-0.75 g/m2The amount of the carbon black in the mounting adhesive coating in the mounting adhesive layer is 0.02-0.06 g/m2The carbon black slurry comprises a dispersing agent which is compatible with the pressure-sensitive adhesive, and the dispersing agent is an acrylate copolymer dispersing agent.
12. The method for preparing the nano metal heat insulation film with low light reflection rate and low light transmittance as claimed in claim 1, which is characterized in that: the method comprises the following steps:
s1, preparing a nickel-chromium-based film: selecting a transparent PET with two sides subjected to pre-coating and corona treatment respectively and haze less than 1% as a base film, plating a layer of nickel-chromium alloy on the corona surface of the base film through magnetron sputtering, and controlling the thickness to obtain a nickel-chromium base film with transmittance of 30-60%, wherein the two sides are a PU (polyurethane) pre-coating layer and a nickel-chromium layer respectively;
s2, preparation of nano inorganic pigment slurry: firstly, mixing and stirring a dispersant and a solvent in a premixing cylinder, then introducing the mixture into a grinding cavity of a ball mill for grinding, gradually adding carbon black or titanium silicon nitride, and respectively preparing carbon black slurry or titanium silicon nitride slurry after grinding;
s3, preparation of the ultraviolet curing coating: adding a solvent into a stirring cylinder, then respectively adding the carbon black slurry and the titanium silicon nitride slurry prepared in the step S2 into the stirring cylinder, finally gradually adding the ultraviolet curing resin, the photosensitizer and the flatting agent into the mixture, and stirring the mixture to prepare the ultraviolet curing coating;
s4, preparing a mounting adhesive coating: adding a solvent into a stirring cylinder, then respectively adding the carbon black slurry prepared in the step S2 and an ultraviolet absorbent during stirring, finally gradually adding a pressure-sensitive adhesive, and stirring to prepare the mounting adhesive coating;
s5, preparing an installation adhesive layer: coating the mounting adhesive coating prepared by S4 on the nickel-chromium-plated chromium layer surface of the nickel-chromium-based film prepared by S1 in a micro-concave coating mode, drying the coating by an oven at 100 ℃, and compounding the coating with a release film;
s6, preparing an anti-scratch layer: and (3) coating the other side of the nickel-chromium-based film in the semi-finished product prepared by the S5, namely the PU precoating side, with the ultraviolet curing coating prepared by the S3 in a micro-concave coating mode, drying the coating in an oven at 80 ℃, and curing the coating by ultraviolet irradiation in a nitrogen atmosphere to obtain the nano metal heat insulation film.
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