Infrared barrier layer and preparation method thereof, and infrared barrier composite film and preparation method thereof

Abstract

The invention relates to the technical field of high polymer materials, in particular to an infrared barrier layer, a preparation method of the infrared barrier layer, an infrared barrier composite film and a preparation method of the infrared barrier composite film. The infrared blocking layer is mainly prepared from the following raw materials: 50-70 parts of a soft monomer, 0-10 parts of a hard monomer, 1-5 parts of a curing agent, 10-15 parts of a functional monomer, 1-5 parts of an infrared blocking agent and 50-100 parts of a solvent. The infrared barrier layer disclosed by the invention is prepared from the soft monomer, the hard monomer, the curing agent, the functional monomer, the infrared barrier agent and the solvent in a proper dosage ratio, and the raw materials are matched, so that the obtained infrared barrier composite film has the characteristic of high temperature resistance, still maintains the stripping force in a high-temperature environment in summer, and is good in infrared absorption performance; the high-transmittance effect is realized.

Description

Technical Field

[0001] The present invention relates to the technical field of polymer materials, and in particular to an infrared blocking layer and a preparation method thereof, an infrared blocking composite film and a preparation method thereof. Background Art

[0002] With the continuous development of science and technology, infrared radiation is used more and more widely in daily life and industrial fields, but it also brings some problems. For example, in the hot summer, the interior of the car will heat up rapidly due to the penetration of infrared rays, increasing the load and energy consumption of the air conditioner. At the same time, it will also cause the electronic equipment inside the car to be unable to work properly due to interference with sensitive components due to infrared radiation.

[0003] Therefore, it is of great significance to develop a protective film that can effectively block infrared rays and has high transparency.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] An object of the present invention is to provide an infrared blocking layer having high transmittance, excellent high temperature resistance and infrared blocking performance.

[0006] Another object of the present invention is to provide a method for preparing an infrared blocking layer, which is simple and easy to implement. Through the coordination of various steps, a composite film with high transmittance, excellent high temperature resistance and infrared blocking performance can be obtained.

[0007] Another object of the present invention is to provide an infrared blocking composite film with high transmittance, high temperature resistance and good infrared blocking performance.

[0008] Another object of the present invention is to provide a method for preparing the infrared blocking composite film, which is simple and easy to implement.

[0009] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted:

[0010] An infrared blocking layer, wherein the infrared blocking layer is mainly prepared from the following raw materials:

[0011] 50-70 parts of soft monomer, 0-10 parts of hard monomer, 1-5 parts of curing agent, 10-15 parts of functional monomer, 1-5 parts of infrared blocking agent and 50-100 parts of solvent.

[0012] In some embodiments, the infrared blocking layer is mainly prepared from the following raw materials, by weight:

[0013] 54-68 parts of soft monomer, 5-9 parts of hard monomer, 2-4 parts of curing agent, 12-14 parts of functional monomer, 2-4 parts of infrared blocking agent and 60-90 parts of solvent.

[0014] In some implementations, a mass ratio M1 of the soft monomer to the hard monomer satisfies: M1≥7.

[0015] In some implementations, a mass ratio M2 of the functional monomer to the infrared blocking agent satisfies: 3≤M2≤12.

[0016] In some embodiments, the soft monomer includes at least one of butyl acrylate, isooctyl acrylate, n-octyl acrylate and dodecyl methacrylate.

[0017] In some embodiments, the hard monomer includes at least one of methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, vinyl acetate, and styrene.

[0018] In some embodiments, the functional monomer includes at least one of hydroxypropyl methacrylate, glycidyl methacrylate, ethylene glycol dimethacrylate, maleic acid and dicumyl peroxide.

[0019] In some embodiments, the infrared blocking agent includes at least one of nano zinc oxide, nano indium tin oxide, and nano titanium dioxide.

[0020] In some embodiments, the curing agent includes at least one of diethylenetriamine, ethylenediamine, N-aminoethylpiperazine, meta-xylylenediamine, and meta-phenylenediamine.

[0021] In some embodiments, the solvent includes at least one of ethyl acetate, anhydrous ethanol, toluene and acetone.

[0022] The method for preparing the infrared blocking layer as described above comprises the following steps:

[0023] heat-treating a mixture of a soft monomer, a hard monomer and a solvent to obtain a first system;

[0024] The first system is subjected to a first reaction with a mixture of a functional monomer and an infrared blocking agent at a first temperature T1, and then subjected to a second reaction at a second temperature T2, T2>T1, to obtain a second system;

[0025] Mixing the second system with a curing agent to obtain a coating rubber material;

[0026] The coating rubber is applied to the surface of the substrate layer, and after drying, an infrared blocking layer is obtained.

[0027] In some embodiments, the constant temperature of the heat treatment is 55 to 75° C., and the constant temperature time of the heat treatment is 20 to 40 minutes.

[0028] In some embodiments, the heat treatment is performed under protective gas conditions.

[0029] In some embodiments, the first temperature T1 is 55-75° C., and the first reaction time is 2-5 hours.

[0030] In some implementations, the difference between the second temperature T2 and the first temperature T1 satisfies: 8°C ≤ T2-T1 ≤ 15°C.

[0031] In some embodiments, the second reaction time is 30 to 60 minutes.

[0032] In some embodiments, the drying temperature is 90-105°C.

[0033] An infrared blocking composite film comprises a substrate layer and an infrared blocking layer located on the surface of the substrate layer; the infrared blocking layer is an infrared blocking layer prepared by the preparation method of the infrared blocking layer.

[0034] In some embodiments, the substrate layer has a thickness of 25 to 100 μm.

[0035] In some embodiments, the infrared blocking layer has a thickness of 10 to 40 μm.

[0036] In some embodiments, the infrared blocking composite film further includes a release film, and the release film is located on a surface of the infrared blocking layer away from the substrate layer; the thickness of the release film is 40 to 60 μm.

[0037] In some embodiments, the infrared blocking composite film has a near infrared transmittance of 38% to 60%, a mid infrared transmittance of 12% to 40%, and a far infrared transmittance of 7% to 30%.

[0038] In some embodiments, the light transmittance of the infrared blocking composite film is 91% to 94%.

[0039] In some embodiments, the haze of the infrared blocking composite film is 1.5-3.1%.

[0040] In some embodiments, the peel strength of the infrared blocking composite film is 800 to 1550 g / 25 mm.

[0041] A method for preparing an infrared blocking composite film comprises the following steps:

[0042] An infrared blocking layer is prepared according to the above method to obtain an infrared blocking composite film;

[0043] Optionally, a release film is compounded on the surface of the infrared blocking layer away from the substrate layer.

[0044] Compared with the prior art, the present invention has the following beneficial effects:

[0045] (1) The infrared blocking layer of the present invention is prepared by using soft monomers, hard monomers, curing agents, functional monomers, infrared blocking agents and solvents in appropriate dosage ratios. By combining the raw materials, the obtained infrared blocking composite film has the characteristics of high temperature resistance, can still maintain its peeling force in the high temperature environment in summer, has good infrared absorption performance, and has a high transmittance effect.

[0046] (2) The preparation method of the infrared blocking layer of the present invention is simple and easy. Through the coordination of various steps, it is more conducive to ensuring the high temperature resistance, high transmittance and excellent infrared blocking performance of the infrared blocking layer.

[0047] (3) The infrared blocking layer of the infrared blocking composite film of the present invention is prepared from soft monomers, hard monomers, curing agents, functional monomers, infrared blocking agents and solvents in appropriate dosage ratios, so that the obtained infrared blocking composite film has the characteristics of high temperature resistance and can still maintain its peeling strength in the high temperature environment in summer; the appropriate infrared blocking agent can improve the infrared absorption performance and can prevent irreversible damage to electronic products in a high temperature environment during production and use; the composite film can improve the problem of aging of automotive glass due to high temperature during use, the finished product is low-cost and easy to operate, and can greatly improve the product yield.

[0048] (4) The preparation method of the infrared blocking composite film of the present invention is simple and easy, and a composite film with high transmittance, excellent high temperature resistance and excellent infrared blocking performance can be obtained. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0050] Figure 1 A schematic structural diagram of the infrared blocking composite film of the present invention. DETAILED DESCRIPTION

[0051] The embodiments of the present invention will be described in detail below in conjunction with the examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. If no specific conditions are specified in the examples, the conditions are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be obtained commercially.

[0052] According to one invention of the present invention, the present invention relates to an infrared blocking layer, which is mainly prepared from the following raw materials, measured by weight: 50 to 70 parts of soft monomer, 0 to 10 parts of hard monomer, 1 to 5 parts of curing agent, 10 to 15 parts of functional monomer, 1 to 5 parts of infrared blocking agent and 50 to 100 parts of solvent.

[0053] The infrared blocking layer of the present invention is prepared by using soft monomers, hard monomers, curing agents, functional monomers, infrared blocking agents and solvents in appropriate dosage ratios. Through the coordination of the raw materials, the obtained infrared blocking composite film has the characteristics of high temperature resistance, still maintains its peeling force in the high temperature environment in summer, has good infrared absorption performance, and has a high transmittance effect.

[0054] In some embodiments, the soft monomer is, by mass, for example, 50 parts, 51 parts, 52 parts, 53 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, 60 parts, 61 parts, 62 parts, 63 parts, 64 parts, 65 parts, 66 parts, 67 parts, 68 parts, 69 parts, 70 parts, etc., or any range between two parts. In some embodiments, the soft monomer includes one or more of butyl acrylate, isooctyl acrylate, n-octyl acrylate and dodecyl methacrylate, such as a combination of butyl acrylate and isooctyl acrylate, a combination of n-octyl acrylate and dodecyl methacrylate, etc.

[0055] In some embodiments, the soft monomer is butyl acrylate and isooctyl acrylate, and the mass ratio of butyl acrylate to isooctyl acrylate is (3-5): 2. The soft monomer of the present invention is formulated with butyl acrylate and isooctyl acrylate in a suitable mass ratio, which can give the infrared blocking layer suitable flexibility and extensibility.

[0056] In some embodiments, the hard monomer is, by weight, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc., or any range between two parts. In some embodiments, the hard monomer includes at least one of methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, vinyl acetate and styrene, or a combination of several of them, such as a combination of methyl methacrylate and ethyl methacrylate, a combination of vinyl acetate and styrene, etc.

[0057] In some embodiments, the hard monomer is n-butyl methacrylate and styrene, and the mass ratio of n-butyl methacrylate to styrene is (2-3):1. The hard monomer uses n-butyl methacrylate and styrene in an appropriate ratio, which can give the infrared blocking layer suitable hardness, brittleness and strength.

[0058] In some embodiments, the curing agent is, for example, 1 part, 1.5 parts, 2 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, etc., or any range between the two parts, in parts by mass. The curing agent includes at least one of diethylenetriamine, ethylenediamine, N-aminoethylpiperazine, meta-phenylenediamine and meta-phenylenediamine, such as a combination of diethylenetriamine and ethylenediamine, a combination of ethylenediamine and N-aminoethylpiperazine, a combination of N-aminoethylpiperazine and meta-phenylenediamine, a combination of meta-phenylenediamine and meta-phenylenediamine, etc. The curing agent in a suitable amount ratio is beneficial to the curing effect and ensures the quality of the film layer.

[0059] In some embodiments, the functional monomer is, for example, 10 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, 12.5 parts, 13 parts, 13.5 parts, 14 parts, 14.5 parts, 15 parts, etc., or any range between the two parts, by weight. The functional monomer includes one or more of hydroxypropyl methacrylate, glycidyl methacrylate, ethylene glycol dimethacrylate, maleic acid, and dicumyl peroxide.

[0060] In some embodiments, the functional monomers are material A and material B, the material A is maleic acid, the material B is at least one of hydroxypropyl methacrylate, glycidyl methacrylate, ethylene glycol dimethacrylate and dicumyl peroxide, and the mass content of the material A in the functional monomer is 80% to 100%, for example, 80%, 82%, 85%, 88%, 90%, 92%, 95%, 98%, 100%, etc. Adding maleic acid to introduce benzene rings is more conducive to the high temperature performance of the composite membrane.

[0061] In some embodiments, the infrared blocking agent is 1 to 5 parts by weight, for example, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, etc.

[0062] Or any range between the two. The infrared blocking agent includes at least one of nano zinc oxide, nano indium tin oxide and nano titanium dioxide. The present invention uses an infrared blocking agent of appropriate quality to improve the infrared blocking effect.

[0063] In some implementations, the infrared blocking agent is material c and material d, wherein material c is nano zinc oxide and / or nano titanium dioxide, and material d is nano indium tin oxide. The mass content of material c in the infrared blocking agent is 75% to 100%.

[0064] In some embodiments, the solvent is 50 parts, 60 parts, 70 parts, 80 parts, 90 parts or 100 parts by weight. The solvent includes at least one of ethyl acetate, anhydrous ethanol, toluene and acetone, such as ethyl acetate and anhydrous ethanol, anhydrous ethanol and toluene, anhydrous ethanol, toluene and acetone.

[0065] In some embodiments, the infrared blocking layer is mainly prepared from the following raw materials:

[0066] 54-68 parts of soft monomer, 5-9 parts of hard monomer, 2-4 parts of curing agent, 12-14 parts of functional monomer, 2-4 parts of infrared blocking agent and 60-90 parts of solvent. The infrared blocking layer of the present invention further optimizes the proportion of each component, which can further coordinate and play a role to improve the high temperature resistance, high transmittance and infrared blocking performance of the infrared blocking composite film.

[0067] In some embodiments, the mass ratio M1 of the soft monomer to the hard monomer satisfies: M1 ≥ 7, such as 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 25, etc. In some embodiments, M1 is 7 to 25. The mass ratio M1 of the soft monomer to the hard monomer satisfies an appropriate range, which can be beneficial to ensuring the performance of the final composite film.

[0068] In some embodiments, the mass ratio M2 of the functional monomer to the infrared blocking agent satisfies: 3≤M2≤12, such as 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc. The mass ratio M2 of the functional monomer to the infrared blocking agent satisfies an appropriate range, which is more conducive to improving the high temperature resistance and infrared blocking performance of the composite film.

[0069] According to another aspect of the present invention, the present invention also relates to a method for preparing the infrared blocking composite film as described above, comprising the following steps:

[0070] The mixture of soft monomer, hard monomer and solvent is heat treated to obtain a first system. The first system is subjected to a first reaction with a mixture of functional monomer and infrared blocking agent at a first temperature T1, and then a second reaction is carried out at a second temperature T2, T2>T1, to obtain a second system. The second system is mixed with a curing agent to obtain a coating rubber. The coating rubber is applied to the surface of the substrate layer, and the infrared blocking layer is obtained after drying.

[0071] The preparation method of the infrared blocking layer of the present invention is simple and easy, and the coordination of various steps is more conducive to ensuring the high temperature resistance, high transmittance and excellent infrared blocking performance of the layer.

[0072] In some embodiments, the constant temperature of the heat treatment is 55-75°C, such as 55°C, 60°C, 65°C, 70°C, 75°C, etc., or any range between the two. The constant temperature time of the heat treatment is 20-40min, such as 20min, 25min, 30min, 35min, 40min, etc. The heat treatment is carried out under protective gas conditions, such as nitrogen, helium, etc.

[0073] In some embodiments, the first temperature T1 is 55-75° C., such as 55° C., 60° C., 70° C., 75° C., 75° C., etc. The first reaction time is 2-5 h, such as 2 h, 2.5 h, 3 h, 4 h, 5 h, etc. Appropriate first reaction conditions can facilitate the reaction of the material.

[0074] In some embodiments, the difference between the second temperature T2 and the first temperature T1 satisfies: 8°C ≤ T2-T1 ≤ 15°C, such as 8°C, 10°C, 11°C, 12°C, 13°C, 15°C, etc. The time of the second reaction is 30 to 60 minutes, such as 30 minutes, 40 minutes, 50 minutes or 60 minutes, etc. The appropriate second reaction conditions are conducive to further sufficient reaction of the materials and ensure the performance of the rubber compound.

[0075] The present invention can further improve the performance of the rubber material and the high temperature resistance and infrared barrier performance of the composite film by adopting the appropriate combination of the first reaction condition and the second reaction condition.

[0076] In some embodiments, the drying temperature is 90-105°C, for example, 90°C, 95°C, 100°C, 105°C, etc.

[0077] According to another aspect of the present invention, the present invention also relates to an infrared blocking composite film, comprising a substrate layer and an infrared blocking layer located on the surface of the substrate layer; the infrared blocking layer is prepared by the infrared blocking layer preparation method described in the infrared blocking layer.

[0078] The infrared blocking composite film of the present invention comprises an infrared blocking layer which is prepared from soft monomers, hard monomers, curing agents, functional monomers, infrared blocking agents and solvents in suitable dosage ratios. By combining the raw materials, the obtained infrared blocking composite film has the characteristic of high temperature resistance and can still maintain its peeling force in a high temperature environment in summer. The suitable infrared blocking agent can improve the infrared absorption performance and can prevent irreversible damage to electronic products in a high temperature environment during production and use. The composite film can improve the problem of aging of automobile glass due to high temperature during use. The finished product is low-cost and easy to operate, and can greatly improve the product yield.

[0079] In some embodiments, the material of the substrate layer includes polyethylene terephthalate (PET). The thickness of the substrate layer is 25 to 100 μm, for example, 25 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, or any range between the two. The thickness of the infrared blocking layer is 10 to 40 μm, for example, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm or 40 μm. An infrared blocking layer of appropriate thickness can ensure the high temperature resistance, high transmittance and infrared blocking effect of the composite film.

[0080] In some embodiments, a release film is further included, and its material includes polyethylene terephthalate; the release film is located on the surface of the infrared blocking layer away from the substrate layer; the thickness of the release film is 40 to 60 μm, for example 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, etc.

[0081] In some embodiments, the near-infrared transmittance of the infrared blocking composite film is 38% to 60%, for example, 38%, 40%, 45%, 50%, 55%, 60%, etc.; the infrared transmittance is 12% to 40%, for example, 12%, 15%, 20%, 25%, 30%, 35% or 40%, etc.; the far-infrared transmittance is 7% to 30%, for example, 7%, 10%, 15%, 20%, 25%, 30%, etc.

[0082] In some embodiments, the light transmittance of the infrared blocking composite film is 91% to 94%, for example, 91%, 92%, 93% or 94%.

[0083] In some embodiments, the haze of the infrared blocking composite film is 1.5-3.1%, for example, 1.5%, 2%, 2.5%, 3%, 3.1%, etc.

[0084] In some embodiments, the peel strength of the infrared blocking composite film is 800-1550 g / 25 mm, for example, 800 g / 25 mm, 1000 g / 25 mm, 1050 g / 25 mm, 1100 g / 25 mm, 1150 g / 25 mm or 1550 g / 25 mm.

[0085] According to another aspect of the present invention, the present invention also relates to a method for preparing an infrared blocking composite film, comprising the following steps:

[0086] The infrared blocking layer is prepared according to the preparation method of the infrared blocking layer to obtain an infrared blocking composite film. Optionally, a release film is compounded on the surface of the infrared blocking layer away from the substrate layer.

[0087] In some embodiments, the structure diagram of the infrared blocking composite film is as follows Figure 1 As shown, it includes a substrate layer 1, an infrared blocking layer 2 and a release film 3 which are arranged in sequence.

[0088] The following is further explained in conjunction with specific embodiments and comparative examples.

[0089] Example 1

[0090] A method for preparing an infrared blocking composite film comprises the following steps:

[0091] (1) 60 parts of monomer, 8 parts of hard monomer and 80 parts of solvent are mixed and poured into a three-necked bottle; wherein the soft monomer is butyl acrylate and isooctyl acrylate, the mass ratio of butyl acrylate and isooctyl acrylate is 3:2, the hard monomer is butyl methacrylate and styrene, the mass ratio of butyl methacrylate and styrene is 3:1; the solvent is ethyl acetate. Nitrogen is introduced to deoxygenate for 10 minutes, and heat treatment is performed: the temperature is raised to 60°C and kept constant for 30 minutes to obtain the first system.

[0092] (2) Under the first temperature (T1=60°C), 12 parts of functional monomer and 2 parts of infrared blocking agent were added to the first system and reacted for 4 hours to obtain the second system, wherein the functional monomer was maleic acid and the infrared blocking agent was nano zinc oxide.

[0093] (3) The temperature is raised to the second temperature (T2 = 70°C) and the reaction is carried out for 50 minutes to obtain a highly transparent rubber compound.

[0094] (4) Add 2 parts of curing agent (diethylenetriamine) to the prepared rubber to obtain a coating slurry; the alkali-coated rubber is coated on a 50 μm PET substrate layer, and dried at 100° C. to obtain a high-transparency infrared blocking composite film, wherein the thickness of the infrared blocking layer is 10 μm.

[0095] Example 2

[0096] A method for preparing an infrared blocking composite film comprises the following steps:

[0097] (1) 60 parts of soft monomer, 8 parts of hard monomer and 80 parts of solvent are uniformly mixed and poured into a three-necked bottle; wherein the soft monomer is butyl acrylate and isooctyl acrylate, and the mass ratio of butyl acrylate and isooctyl acrylate is 3:2; the hard monomer is butyl methacrylate and styrene, and the mass ratio of butyl methacrylate and styrene is 3:1; and the solvent is ethyl acetate; nitrogen is introduced for deoxygenation for 10 minutes, and then heat treatment is performed: the temperature is increased to 60°C and kept constant for 30 minutes.

[0098] (2) 14 parts of a functional monomer and 3 parts of an infrared blocking agent were added under a first temperature (T1 = 60°C) environment and reacted for 4 hours to obtain a second system; wherein the functional monomer was maleic acid; and the infrared blocking agent was nano-titanium dioxide.

[0099] (3) The second system is heated to a second temperature (T2 = 70°C) and reacted for 50 minutes to obtain a highly transparent rubber compound.

[0100] (4) Add 2 parts of curing agent (diethylenetriamine) to the prepared rubber compound and mix to obtain a coating rubber compound; apply the coating rubber compound on a 50 μm PET substrate layer, and dry it at 100° C. to obtain a high-transparency infrared blocking composite film, wherein the thickness of the infrared blocking layer is 10 μm.

[0101] Example 3

[0102] A method for preparing an infrared blocking composite film comprises the following steps:

[0103] (1) 60 parts of a soft monomer, 8 parts of a hard monomer and 60 parts of a solvent are uniformly mixed and poured into a three-necked bottle; wherein the soft monomer is butyl acrylate and isooctyl acrylate, and the mass ratio of butyl acrylate to isooctyl acrylate is 3:2; the hard monomer is butyl methacrylate and styrene, and the mass ratio of butyl methacrylate to styrene is 3:1; nitrogen is introduced to deoxygenate for 10 minutes, and then heat treatment is performed: the temperature is increased to 60° C. and maintained at this temperature for 30 minutes to obtain a first system.

[0104] (2) Add 12 parts of functional monomer and 3 parts of infrared blocking agent to the first system at a first temperature of 60° C. and react for 4 hours; the functional monomer is maleic acid; the infrared blocking agent is nano titanium dioxide.

[0105] (3) The first system is heated to a first temperature (T1 = 70°C) and reacted for 50 minutes to obtain a rubber compound.

[0106] (4) Add 2 parts of curing agent (diethylenetriamine) to the prepared rubber compound and mix to obtain a coating rubber compound; apply the coating rubber compound on a 50 μm PET substrate layer, and dry it at 100° C. to obtain a high-transparency infrared blocking composite film, wherein the thickness of the infrared blocking layer is 10 μm.

[0107] Example 4

[0108] A method for preparing an infrared blocking composite film, which differs from Example 3 in that:

[0109] The infrared blocking agent is nano zinc oxide, nano indium tin oxide and nano titanium dioxide, and the mass ratio of nano zinc oxide, nano indium tin oxide and nano titanium dioxide is 5:1:4;

[0110] The functional monomers are maleic acid and ethylene glycol dimethacrylate, and the mass content of maleic acid in the functional monomers is 85%.

[0111] Example 5

[0112] A method for preparing an infrared blocking composite film comprises the following steps:

[0113] (1) 50 parts of a soft monomer, 2 parts of a hard monomer, and 50 parts of a solvent are uniformly mixed and poured into a three-necked flask; wherein the soft monomer is butyl acrylate and isooctyl acrylate, and the mass ratio of butyl acrylate to isooctyl acrylate is 3:2; the hard monomer is butyl methacrylate and styrene, and the mass ratio of butyl methacrylate to styrene is 3:1; nitrogen is introduced to deoxygenate for 10 minutes, and then heat treatment is performed: the temperature is increased to 55° C. and maintained at a constant temperature for 40 minutes to obtain a first system.

[0114] (2) Add 10 parts of functional monomer and 2 parts of infrared blocking agent to the first system at a first temperature of 55° C. and react for 5 hours; the functional monomer is maleic acid; the infrared blocking agent is nano titanium dioxide.

[0115] (3) The first system is heated to a first temperature (T1 = 60°C) and reacted for 63 minutes to obtain a rubber compound.

[0116] (4) Add 1 part of curing agent (diethylenetriamine) to the prepared rubber compound and mix to obtain a coating rubber compound; apply the coating rubber compound on a 50 μm PET substrate layer, and dry it at 100° C. to obtain a high-transparency infrared blocking composite film, wherein the thickness of the infrared blocking layer is 10 μm.

[0117] Example 6

[0118] A method for preparing an infrared blocking composite film comprises the following steps:

[0119] (1) 70 parts of a soft monomer, 10 parts of a hard monomer and 100 parts of a solvent are uniformly mixed and poured into a three-necked flask; wherein the soft monomer is butyl acrylate and isooctyl acrylate, and the mass ratio of butyl acrylate to isooctyl acrylate is 3:2; the hard monomer is butyl methacrylate and styrene, and the mass ratio of butyl methacrylate to styrene is 3:1; nitrogen is introduced to deoxygenate for 10 minutes, and then heat treatment is performed: the temperature is increased to 75° C. and maintained at this temperature for 20 minutes to obtain a first system.

[0120] (2) Add 15 parts of functional monomer and 5 parts of infrared blocking agent to the first system at a first temperature of 75° C. and react for 2 hours; the functional monomer is maleic acid; the infrared blocking agent is nano-titanium dioxide.

[0121] (3) The first system is heated to a first temperature (T1 = 80°C) and reacted for 50 minutes to obtain a rubber compound.

[0122] (4) Add 5 parts of curing agent (diethylenetriamine) to the prepared rubber compound and mix to obtain a coating rubber compound; apply the coating rubber compound on a 50 μm PET substrate layer, and dry it at 100° C. to obtain a high-transparency infrared blocking composite film, wherein the thickness of the infrared blocking layer is 10 μm.

[0123] Comparative Example 1

[0124] A method for preparing an infrared blocking composite film, which differs from Example 1 in that:

[0125] No functional monomer maleic acid is added; no nano zinc oxide infrared blocking agent is added;

[0126] Experimental example

[0127] The infrared blocking composite films of the above-mentioned embodiments and comparative examples were tested for performance, as follows:

[0128] The test was conducted according to the national standard for high temperature resistance (GB / T2792-1998) and the national standard for peel strength (GB / T2792-1998). The test results are shown in Table 1. The test results for infrared blocking rate, light transmittance, and haze are shown in Table 2.

[0129] Table 1 Peel force test results

[0130]

[0131] Table 2 Test results of infrared blocking rate, light transmittance and haze

[0132]

[0133]

[0134] It can be seen from Tables 1 and 2 that the infrared blocking composite film obtained by the invention of the present invention has high transmittance, excellent high temperature resistance and infrared blocking performance, the PET protective film with a total thickness of 58 to 62 μm has a 180° peel strength of 800 to 1550 g / 25 mm, and there is no residual glue after hot tearing and cold tearing after high-temperature baking at 280°C and 300°C, and after adding an appropriate proportion of infrared blocking agent, the infrared blocking performance is significantly improved.

[0135] The protective film obtained in Comparative Example 1 has poor high temperature resistance and poor infrared blocking effect.

[0136] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An infrared blocking layer, characterized in that: The infrared blocking layer is mainly prepared from the following raw materials: 50-70 parts of soft monomer, 0-10 parts of hard monomer, 1-5 parts of curing agent, 10-15 parts of functional monomer, 1-5 parts of infrared blocking agent and 50-100 parts of solvent.

2. The infrared blocking layer according to claim 1, characterized in that: The infrared blocking layer is mainly prepared from the following raw materials in parts by mass: 54-68 parts of soft monomer, 5-9 parts of hard monomer, 2-4 parts of curing agent, 12-14 parts of functional monomer, 2-4 parts of infrared blocking agent and 60-90 parts of solvent.

3. The infrared blocking layer according to claim 1, characterized in that: Contains at least one of the following features (1) to (3): (1) The mass ratio M1 of the soft monomer to the hard monomer satisfies: M1 ≥ 7; (2) The mass ratio M2 of the functional monomer to the infrared blocking agent satisfies: 3≤M2≤12.

4. The infrared blocking layer according to claim 1, characterized in that: The invention comprises at least one of the following features (1) to (6): (1) The soft monomer comprises at least one of butyl acrylate, isooctyl acrylate, n-octyl acrylate and dodecyl methacrylate; (2) the hard monomer comprises at least one of methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, vinyl acetate and styrene; (3) the functional monomer comprises at least one of hydroxypropyl methacrylate, glycidyl methacrylate, ethylene glycol dimethacrylate, maleic acid and dicumyl peroxide; (4) The infrared blocking agent includes at least one of nano zinc oxide, nano indium tin oxide and nano titanium dioxide; (5) The curing agent includes at least one of diethylenetriamine, ethylenediamine, N-aminoethylpiperazine, m-xylylenediamine and m-phenylenediamine; (6) The solvent includes at least one of ethyl acetate, anhydrous ethanol, toluene and acetone.

5. The method for preparing an infrared blocking layer according to any one of claims 1 to 4, characterized in that: The following steps are involved: heat-treating a mixture of a soft monomer, a hard monomer and a solvent to obtain a first system; The first system is subjected to a first reaction with a mixture of a functional monomer and an infrared blocking agent at a first temperature T1, and then subjected to a second reaction at a second temperature T2, T2>T1, to obtain a second system; Mixing the second system with a curing agent to obtain a coating rubber material; The coating rubber is applied to the surface of the substrate layer, and after drying, an infrared blocking layer is obtained.

6. The method for preparing the infrared blocking layer according to claim 5, characterized in that: Contains at least one of the following features (1) to (6): (1) The constant temperature of the heat treatment is 55 to 75° C., and the constant temperature time of the heat treatment is 20 to 40 minutes; (2) The heat treatment is carried out under protective gas conditions; (3) The first temperature T1 is 55 to 75° C., and the first reaction time is 2 to 5 hours; (4) The difference between the second temperature T2 and the first temperature T1 satisfies: 8°C ≤ T2-T1 ≤ 15°C; (5) The second reaction time is 30 to 60 minutes; (6) The drying temperature is 90-105°C.

7. An infrared blocking composite film, characterized in that: It comprises a substrate layer and an infrared blocking layer located on the surface of the substrate layer; the infrared blocking layer is the infrared blocking layer described in any one of claims 1 to 4, or an infrared blocking layer prepared by the preparation method of the infrared blocking layer described in claim 5 or 6.

8. The infrared blocking composite film according to claim 7, characterized in that: Contains at least one of the following features (1) to (3): (1) The thickness of the substrate layer is 25 to 100 μm; (2) The thickness of the infrared blocking layer is 10 to 40 μm; (3) The infrared blocking composite film further comprises a release film, and the release film is located on a surface of the infrared blocking layer away from the substrate layer; the thickness of the release film is 40 to 60 μm.

9. The infrared blocking composite film according to claim 7, characterized in that: Contains at least one of the following features (1) to (4): (1) The infrared blocking composite film has a near infrared transmittance of 38% to 60%, a mid infrared transmittance of 12% to 40%, and a far infrared transmittance of 7% to 30%; (2) The light transmittance of the infrared blocking composite film is 91% to 94%; (3) The haze of the infrared blocking composite film is 1.5 to 3.1%; (4) The peel strength of the infrared blocking composite film is 800 to 1550 g / 25 mm.

10. A method for preparing an infrared blocking composite film, characterized in that: The following steps are involved: An infrared blocking layer is prepared according to the method of claim 5 or 6 to obtain an infrared blocking composite film; Optionally, a release film is compounded on the surface of the infrared blocking layer away from the substrate layer.

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