CN114316127B - Thermosensitive adhesive main resin, thermosensitive adhesive for solar film and preparation method of thermosensitive adhesive main resin - Google Patents
Thermosensitive adhesive main resin, thermosensitive adhesive for solar film and preparation method of thermosensitive adhesive main resin Download PDFInfo
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- CN114316127B CN114316127B CN202111653736.5A CN202111653736A CN114316127B CN 114316127 B CN114316127 B CN 114316127B CN 202111653736 A CN202111653736 A CN 202111653736A CN 114316127 B CN114316127 B CN 114316127B
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Abstract
The invention provides a thermosensitive adhesive main body resin, a thermosensitive adhesive for a solar film and a preparation method thereof, wherein the thermosensitive adhesive main body resin comprises the combination of four different types of acrylate monomers, an initiator and a chain transfer agent in specific parts, and the thermosensitive adhesive main body resin can be used as a solar film interlayer adhesive by selecting the combination of four different types of acrylate monomers with different performances and adding the specific parts of the chain transfer agent and the initiator in a matching way, so that the adhesive performance of the thermosensitive adhesive main body resin is greatly improved, and the thermosensitive adhesive main body resin, an auxiliary agent and a filler have excellent compatibility, so that the transparency, the heat insulation performance and the ultraviolet light resistance of the thermosensitive adhesive are improved.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a thermosensitive adhesive main resin, a thermosensitive adhesive for a solar film and a preparation method of the thermosensitive adhesive.
Background
The adhesive for automobile film is generally divided into interlayer adhesive and mounting adhesive, and the adhesive for automobile film is required to have the characteristics of no color, heat insulation, ultraviolet resistance, no smell, no corrosiveness, easy dissolution in organic solvents, easy coating on PET film and other base materials, and the like. The interlayer adhesive has the advantages of high peeling force and capability of being matched with pigment or inorganic nanometer heat insulation materials.
At present, the solar film interlayer adhesive mainly adopts thermosensitive adhesive (TSA type), and also adopts polyurethane or polyester laminating adhesive in a small part. CN104232004a discloses a polyurethane thermosensitive adhesive composition, a preparation method and application. The polyurethane thermosensitive adhesive composition comprises polyurethane main adhesive and additive composition, wherein the polyurethane main adhesive is prepolymer with-NCO groups formed by polycondensation of diisocyanate and polyester diol and/or polyether diol, and high molecular weight polyurethane main adhesive with-OH groups blocked is obtained by chain extension and crosslinking. CN105482751a discloses a high-performance polyurethane thermosensitive adhesive, which comprises the following raw materials in parts by weight: 70-90 parts of neoprene, 60-80 parts of methyl methacrylate, 60-80 parts of hydroxyl polysiloxane, 30-50 parts of xylene resin, 30-50 parts of polyisocyanate, 20-40 parts of carbon fiber, 20-40 parts of alkene resin, 10-18 parts of azo compound foaming agent, 10-18 parts of rosin resin, 5-10 parts of triethylamine, 5-10 parts of methylpentanethinyl alcohol, 5-10 parts of polybutadiene, 4-8 parts of triethylamine, 1-2 parts of dibutyltin dilaurate and 0.5-1 part of N-methylol acrylamide; the preparation method comprises the following steps: 70-90 parts of neoprene, 60-80 parts of methyl methacrylate, 60-80 parts of hydroxyl polysiloxane, 30-50 parts of xylene resin and 30-50 parts of polyisocyanate are weighed according to the weight ratio, added into a reaction kettle, the temperature of the reaction kettle is raised to 60-80 ℃, and fully stirred. The preparation method is simple, and the prepared polyurethane thermosensitive adhesive has high performance, is environment-friendly and is suitable for large-scale production.
However, heat-sensitive adhesives have a problem of deterioration in weather resistance and adhesion, while polyurethane or polyester adhesives have a problem of incompatibility with pigments or fillers.
Therefore, development of a main resin of a thermosensitive adhesive, and further obtaining a thermosensitive adhesive for solar films with excellent weather resistance and adhesion fastness, is an urgent problem to be solved in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a thermosensitive adhesive main body resin, a thermosensitive adhesive for a solar film and a preparation method thereof, wherein the thermosensitive adhesive main body resin is prepared by combining four types and functions of acrylate monomers and matching with an initiator and a chain transfer agent, so that the thermosensitive adhesive for the solar film, which has excellent adhesive property, high transparency, heat insulation and ultraviolet light prevention effect, is obtained.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a heat-sensitive adhesive main body resin, which comprises the following components in parts by weight:
40 to 60 weight portions of acrylic monomer
Initiator 0.5-1 weight portions
0.05 to 0.15 weight portion of chain transfer agent;
the acrylic ester monomer comprises the following components in parts by weight:
the acrylic monomer may be 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50 parts by weight, 52 parts by weight, 54 parts by weight, 56 parts by weight, 58 parts by weight, or the like.
The initiator may be 0.55, 0.6, 0.65, 0.7, 0.75, 0.8, 0.85, 0.9, or 0.95 parts by weight, etc.
The chain transfer agent may be 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, or 0.14 parts by weight, etc.
The isobornyl methacrylate and/or isobornyl acrylate may be 13.5 parts by weight, 14 parts by weight, 14.5 parts by weight, 15 parts by weight, 15.5 parts by weight, 16 parts by weight, 16.5 parts by weight, or the like.
The methyl methacrylate and/or methyl acrylate may be 13.5 parts by weight, 14 parts by weight, 14.5 parts by weight, 15 parts by weight, 15.5 parts by weight, 16 parts by weight, 16.5 parts by weight, or the like.
The ethyl acrylate may be 58.5 parts by weight, 59 parts by weight, 59.5 parts by weight, 60 parts by weight, 60.5 parts by weight, 61 parts by weight, 61.5 parts by weight, or the like.
The hydroxyethyl acrylate and/or hydroxyethyl methacrylate may be 9.2 parts by weight, 9.4 parts by weight, 9.6 parts by weight, 9.8 parts by weight, 10 parts by weight, 10.2 parts by weight, 10.4 parts by weight, 10.6 parts by weight, 10.8 parts by weight, or the like.
The main resin of the thermosensitive adhesive provided by the invention comprises a combination of a specific part of acrylic ester monomers, an initiator and a chain transfer agent, wherein the acrylic ester monomers comprise the combination of four different acrylic ester monomers; the four acrylic monomers with different performances are selected, and the specific parts of chain transfer agent and initiator are matched, so that the comprehensive performance of the thermosensitive adhesive containing the thermosensitive adhesive main body resin is greatly improved, wherein the comprehensive performance comprises adhesive performance, weather resistance, elasticity, hardness degree and the like, and the thermosensitive adhesive main body resin also has excellent compatibility with pigment and filler, so that the transparency, heat insulation and ultraviolet light resistance of the thermosensitive adhesive are improved, and the thermosensitive adhesive can be applied as solar film interlayer adhesive.
Preferably, the initiator comprises azobisisobutyronitrile.
Preferably, the chain transfer agent comprises tertiary dodecyl mercaptan and/or the chain transfer agent AMSD.
Preferably, the thermosensitive gum main resin also comprises a solvent and/or an auxiliary agent.
Preferably, the auxiliary agent comprises an ultraviolet light absorber and/or an epoxy resin.
Preferably, the content of the ultraviolet absorber in the heat-sensitive adhesive main resin is 0.2 to 0.3 parts by weight, for example, 0.21 parts by weight, 0.22 parts by weight, 0.23 parts by weight, 0.24 parts by weight, 0.25 parts by weight, 0.26 parts by weight, 0.27 parts by weight, 0.28 parts by weight, 0.29 parts by weight, or the like.
Preferably, the content of the epoxy resin in the heat-sensitive adhesive main resin is 1 to 3 parts by weight, for example, 1.2 parts by weight, 1.4 parts by weight, 1.6 parts by weight, 1.8 parts by weight, 2 parts by weight, 2.2 parts by weight, 2.4 parts by weight, 2.6 parts by weight, 2.8 parts by weight, or the like.
Preferably, the solvent comprises ethyl acetate and/or butanone.
Preferably, the content of the solvent in the heat-sensitive adhesive main resin is 40 to 60 parts by weight, for example, 42 parts by weight, 44 parts by weight, 46 parts by weight, 48 parts by weight, 50 parts by weight, 52 parts by weight, 54 parts by weight, 56 parts by weight, 58 parts by weight, or the like.
Preferably, the solid content of the heat-sensitive adhesive main resin is 49-51%, such as 49.2%, 49.4%, 49.6%, 49.8%, 50.1%, 50.3%, 50.5%, 50.7% or 50.9%, etc.
Preferably, the viscosity of the heat sensitive adhesive body resin is 3500-4500 cps, for example 3600cps, 3700cps, 3800cps, 3900cps, 4000cps, 4100cps, 4200cps, 4300cps or 4400cps, etc.
In a second aspect, the present invention provides a method for preparing the heat-sensitive adhesive main body resin according to the first aspect, the method comprising: and adding an acrylic monomer, an initiator and a chain transfer agent into a solvent for reaction to obtain the heat-sensitive adhesive main resin.
Preferably, the reaction further comprises the step of adding an auxiliary agent for mixing after the reaction is finished.
Preferably, the preparation method specifically comprises the following steps:
(1) 8 to 12 weight parts of acrylic ester monomer, 0.2 to 0.4 weight part of initiator and 2 to 3 weight parts of solvent are mixed to obtain a first mixed solution; mixing 32-48 parts by weight of acrylic monomer, 24-36 parts by weight of solvent, 0.05-0.15 part by weight of chain transfer agent and 0.25-0.5 part by weight of initiator to obtain a second mixed solution; heating 8-12 parts by weight of solvent to obtain a heated solvent;
(2) Adding the first mixed solution obtained in the step (1) into the heated solvent obtained in the step (1), carrying out heat preservation for the first time, adding the second mixed solution obtained in the step (1), carrying out heat preservation for the second time, finally adding 6-9 parts by weight of solvent and 0.05-0.1 part by weight of initiator, carrying out heat preservation for the third time, and adding optional auxiliary agents for mixing to obtain the heat-sensitive adhesive main resin.
Preferably, the temperature of the first incubation is 75 to 80 ℃, e.g., 75.5 ℃, 76 ℃, 76.5 ℃, 77 ℃, 77.5 ℃, 78 ℃, 78.5 ℃, 79 ℃, 79.5 ℃, or the like.
Preferably, the time of the first heat preservation is 20-40 min, for example 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min or 38min, etc.
Preferably, the temperature of the second incubation is 75-80 ℃, e.g., 75.5 ℃, 76 ℃, 76.5 ℃, 77 ℃, 77.5 ℃, 78 ℃, 78.5 ℃, 79 ℃, 79.5 ℃, or the like.
Preferably, the time of the second incubation is 1.5-2.5 h, for example 1.6h, 1.7h, 1.8h, 1.9h, 2h, 2.1h, 2.2h, 2.3h or 2.4h, etc.
Preferably, the temperature of the third incubation is 75 to 80 ℃, e.g., 75.5 ℃, 76 ℃, 76.5 ℃, 77 ℃, 77.5 ℃, 78 ℃, 78.5 ℃, 79 ℃, 79.5 ℃, or the like.
Preferably, the time of the third heat preservation is 20-40 min, for example 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min or 38min, etc.
In a third aspect, the present invention provides a thermosensitive adhesive for solar film, which comprises the combination of the thermosensitive adhesive main resin and the curing agent according to the first aspect.
Preferably, the mass ratio of the heat-sensitive adhesive main resin to the curing agent is 5 (2-4), such as 5:2.2, 5:2.4, 5:2.6, 5:2.8, 5:3, 5:3.2, 5:3.4, 5:3.6 or 5:3.8.
Preferably, the curing agent is prepared from a combination of isocyanate and polyether polyol.
Preferably, the isocyanate comprises toluene diisocyanate and/or hexamethylene diisocyanate;
preferably, the molar ratio of isocyanate to polyether polyol is 1 (0.33 to 0.75), such as 1:0.35, 1:0.4, 1:0.45, 1:0.5, 1:0.55, 1:0.6, 1:0.65, or 1:0.7, etc.
Preferably, the solids content of the curing agent is 40-60%, such as 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56% or 58%, etc.
Preferably, the preparation raw materials of the thermosensitive adhesive for the solar film further comprise any one or a combination of at least two of nano heat insulation slurry, nano pigment or coupling agent.
Preferably, the mass of the coupling agent is 0.3 to 0.5g, for example, 0.32g, 0.34g, 0.36g, 0.38g, 0.4g, 0.42g, 0.44g, 0.46g, 0.48g, or the like, based on 1000g of the acrylic resin for a solar film.
In a fourth aspect, the present invention provides a method for preparing the hot-press adhesive for solar films according to the third aspect, the method comprising: mixing the heat-sensitive adhesive main body resin and the curing agent, adding an optional solvent for dilution, adding an optional nano heat-insulating slurry and an optional nano pigment for stirring, and finally adding an optional coupling agent for mixing to obtain the hot-press adhesive for the solar film.
In a fifth aspect, the present invention provides a method for using the hot-press adhesive for solar film according to the third aspect, the method comprising: and (3) coating the solar film on the surface of the base film by using a hot-pressing adhesive, drying, attaching another base film, rolling and curing.
Preferably, the coating is performed by a micro-gravure coater.
Preferably, the coating amount of the coating is 3 to 5g/m 3 For example 3.2g/m 3 、3.4g/m 3 、3.6g/m 3 、3.8g/m 3 、4g/m 3 、4.2g/m 3 、4.4g/m 3 、4.6g/m 3 Or 4.8g/m 3 Etc.
Preferably, the drying temperature is 100 to 130 ℃, for example 103 ℃, 106 ℃, 109 ℃, 112 ℃, 115 ℃, 118 ℃, 121 ℃, 124 ℃, 127 ℃, or the like.
Preferably, the temperature of the rolling is 70 to 90 ℃, for example 72 ℃, 74 ℃, 76 ℃, 78 ℃,80 ℃, 82 ℃, 84 ℃, 86 ℃, 88 ℃, or the like.
Preferably, the curing temperature is 50 to 60 ℃, for example, 51 ℃, 52 ℃, 53 ℃, 54 ℃,55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, or the like.
Preferably, the curing time is 48 to 72 hours, for example 50 hours, 52 hours, 54 hours, 56 hours, 58 hours, 60 hours, 62 hours, 64 hours, 66 hours, 68 hours or 70 hours, etc.
Compared with the prior art, the invention has the following beneficial effects:
the heat-sensitive glue main body resin provided by the invention comprises the combination of four different types of acrylic ester monomers, an initiator and a chain transfer agent in a specific part, wherein the heat-sensitive glue main body resin is prepared by selecting the four different types of acrylic ester monomers with different performances to be mutually combined and adding the specific part of the chain transfer agent and the initiator in a matching way, so that the adhesive property of the heat-sensitive glue containing the heat-sensitive glue main body resin is greatly improved, and the heat-sensitive glue main body resin also has excellent compatibility with pigments and fillers, so that the transparency, the heat insulation and the ultraviolet light resistance of the heat-sensitive glue are improved, and the heat-sensitive glue main body resin can be applied as a solar film interlayer glue.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Example 1
The heat-sensitive adhesive main resin comprises the following components in parts by weight:
the acrylic ester monomer comprises the following components in parts by weight:
the preparation method of the thermosensitive gum main resin provided by the embodiment comprises the following steps:
(1) Mixing 10 parts by weight of acrylic monomer, 0.3 part by weight of azobisisobutyronitrile and 2.5 parts by weight of ethyl acetate to obtain a first mixed solution; mixing 40 parts by weight of acrylic monomer, 30 parts by weight of ethyl acetate, 0.1 part by weight of chain transfer agent and 0.375 part by weight of azobisisobutyronitrile to obtain a second mixed solution; heating 10 parts by weight of ethyl acetate to obtain a heating solvent;
(2) Dropwise adding the first mixed solution obtained in the step (1) into the heating solvent obtained in the step (1), carrying out first heat preservation for 30min at 75 ℃, dropwise adding the second mixed solution obtained in the step (1), carrying out second heat preservation for h at 75 ℃, finally dropwise adding 7.5 parts by weight of ethyl acetate and 0.075 part by weight of azodiisobutyronitrile, carrying out third heat preservation for 30min at 75 ℃, and adding 2 parts by weight of epoxy resin (EPON 58006, guangzhou pickaxe chemical industry Co., ltd.) and 0.25 part by weight of ultraviolet absorber (ultraviolet absorber UV-0), thereby obtaining the heat sensitive glue main resin.
Example 2
The heat-sensitive adhesive main resin comprises the following components in parts by weight:
the acrylic ester monomer comprises the following components in parts by weight:
the preparation method of the thermosensitive gum main resin provided by the embodiment comprises the following steps:
(1) Mixing 8 parts by weight of acrylic monomer, 0.2 part by weight of azobisisobutyronitrile and 1.6 parts by weight of ethyl acetate to obtain a first mixed solution; mixing 32 parts by weight of acrylic monomer, 24 parts by weight of ethyl acetate, 0.05 part by weight of chain transfer agent and 0.25 part by weight of azobisisobutyronitrile to obtain a second mixed solution; heating 8 parts by weight of ethyl acetate to obtain a heating solvent;
(2) Dropwise adding the first mixed solution obtained in the step (1) into the heating solvent obtained in the step (1), carrying out first heat preservation for 20min at 80 ℃, dropwise adding the second mixed solution obtained in the step (1), carrying out second heat preservation for 1.5h at 80 ℃, finally dropwise adding 6.4 parts by weight of ethyl acetate and 0.05 part by weight of azodiisobutyronitrile, carrying out third heat preservation for 20min at 80 ℃, and adding 2 parts by weight of epoxy resin (Guangzhou pick rhyme chemical company, EPON 58006) and 0.25 part by weight of ultraviolet absorber (ultraviolet absorber UV-0) to obtain the heat sensitive glue main resin.
Example 3
The heat-sensitive adhesive main resin comprises the following components in parts by weight:
the acrylic ester monomer comprises the following components in parts by weight:
the preparation method of the thermosensitive gum main resin provided by the embodiment comprises the following steps:
(1) Mixing 12 parts by weight of acrylic monomer, 0.4 part by weight of azobisisobutyronitrile and 3 parts by weight of ethyl acetate to obtain a first mixed solution; mixing 48 parts by weight of acrylic monomer, 36 parts by weight of ethyl acetate, 0.15 part by weight of chain transfer agent and 0.5 part by weight of azobisisobutyronitrile to obtain a second mixed solution; heating 12 parts by weight of ethyl acetate to obtain a heating solvent;
(2) Dropwise adding the first mixed solution obtained in the step (1) into the heating solvent obtained in the step (1), carrying out first heat preservation for 20min at 80 ℃, dropwise adding the second mixed solution obtained in the step (1), carrying out second heat preservation for 1.5h at 80 ℃, finally dropwise adding 9 parts by weight of ethyl acetate and 0.1 part by weight of azodiisobutyronitrile, carrying out third heat preservation for 20min at 80 ℃, and adding 2 parts by weight of epoxy resin (EPON 58006, guangzhou pickaxe chemical industry Co., ltd.) and 0.25 part by weight of ultraviolet absorber (ultraviolet absorber UV-0) to obtain the heat sensitive glue main resin.
Example 4
A heat-sensitive adhesive main body resin was different from example 1 only in that no epoxy resin was added, and other components, amounts and preparation methods were the same as those of example 1.
Comparative example 1
The heat-sensitive adhesive main body resin is different from the embodiment 1 in that the acrylic monomer comprises the following components in parts by weight:
17 parts by weight of methyl methacrylate
68 parts by weight of ethyl acrylate
12 parts by weight of hydroxyethyl acrylate;
other components, amounts and preparation methods were the same as in example 1.
Comparative example 2
The heat-sensitive adhesive main body resin is different from the embodiment 1 in that the acrylic monomer comprises the following components in parts by weight:
isobornyl methacrylate 17 parts by weight
68 parts by weight of ethyl acrylate
12 parts by weight of hydroxyethyl acrylate;
other components, amounts and preparation methods were the same as in example 1.
Comparative example 3
The heat-sensitive adhesive main body resin is different from the embodiment 1 in that the acrylic monomer comprises the following components in parts by weight:
isobornyl methacrylate 36 weight portions
Methyl methacrylate 36 parts by weight
25 parts of hydroxyethyl acrylate;
other components, amounts and preparation methods were the same as in example 1.
Comparative example 4
The heat-sensitive adhesive main body resin is different from the embodiment 1 in that the acrylic monomer comprises the following components in parts by weight:
isobornyl methacrylate 16 weight portions
Methyl methacrylate 16 parts by weight
65 parts by weight of ethyl acrylate;
other components, amounts and preparation methods were the same as in example 1.
Application example 1
A preparation method of thermosensitive adhesive for solar films comprises the following steps: mixing the main body resin (example 1) of the thermosensitive adhesive with a curing agent (comprising toluene diisocyanate and polyether polyol PTMG650 in a molar ratio of 1:0.4), adding ethyl acetate for dilution, adding nano heat-insulating slurry and pigment for stirring, and finally adding diphenyl dimethoxy silane for mixing to obtain the thermosensitive adhesive for the solar film.
Application examples 2 to 4
The heat-sensitive adhesive for solar film was different from application example 1 only in that the heat-sensitive adhesive main resins obtained in examples 2 to 4 were used instead of the heat-sensitive adhesive main resin obtained in example 1, and other components, amounts and preparation methods were the same as those of application example 1.
Comparative application examples 1 to 4
The heat-sensitive adhesive for solar film was different from application example 1 only in that the heat-sensitive adhesive main resins obtained in comparative examples 1 to 4 were used in place of the heat-sensitive adhesive main resin obtained in example 1, and other components, amounts and preparation methods were the same as those of application example 1.
Performance test:
(1) Peel force: the thermosensitive adhesive for the solar film is coated by a micro-concave coating machine according to the coating weight of 3-5 g/m 3 Coating the PET base film on the surface, drying at 120 ℃, attaching another PET base film, rolling at 80 ℃, and curing at 55 ℃ for 50 hours to obtain a sample to be tested; the test was performed using a peel force tester and the tear test was performed at 4N/15 mm.
(2) Solvent resistance: soaking with butanone and other solvent for 4-24 hr to see if layering.
(3) Weather resistance test: the mixture was left for 72 hours at a temperature of 80℃and a humidity of 80%.
The solar film heat-sensitive adhesives obtained in examples 1 to 4 and comparative examples 1 to 4 were used in the above test methods, and the test results are shown in Table 1:
TABLE 1
From the data in table 1, it can be seen that: the thermosensitive adhesive for the solar film has excellent adhesive property, solvent resistance and weather resistance; specifically, the peel force test results of the thermosensitive adhesive for solar films obtained in application examples 1 to 4 showed that the substrate was broken, demonstrating that the adhesion of the pressure-sensitive adhesive to the substrate was excellent; the solvent resistance test solvent is soaked for 4 hours without layering, and the weather resistance test is without layering.
In contrast, the main resin of the thermosensitive adhesive provided in comparative application example 1 is poor in adhesion property due to the fact that isobornyl acrylate is not added, and the films cannot be adhered; the main resin of the thermosensitive adhesive obtained in comparative application example 2 has a viscosity of more than 10000cps, and the viscosity of the liquid is larger after being mixed with curing agent and the like, so that the thermosensitive adhesive cannot be coated; the viscosity of the thermosensitive adhesive provided in the comparative application example 3 is less than 1000cps, the pencil hardness after coating is insufficient and less than 1h, and the coating is easy to fall off; the heat-sensitive adhesive obtained in comparative application example 4 was satisfactory in viscosity and was able to be normally coated, but the adhesive force on the rear surface of the coating film was insufficient, and the film material was unable to bond a film/film after hot pressing.
The applicant states that the present invention is described by way of the above examples as a heat-sensitive adhesive main resin, a heat-sensitive adhesive for solar film and a method for producing the same, but the present invention is not limited to the above examples, i.e., it is not meant that the present invention must be practiced by relying on the above examples. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (36)
1. The thermosensitive adhesive main body resin is characterized by comprising the following components in parts by weight:
40 to 60 weight portions of acrylic monomer
Initiator 0.5-1 weight portions
0.05 to 0.15 weight portion of chain transfer agent;
the acrylic ester monomer comprises the following components in parts by weight:
2. the heat sensitive glue host resin of claim 1, wherein the initiator comprises azobisisobutyronitrile.
3. The heat sensitive glue host resin of claim 1, wherein the chain transfer agent comprises tertiary dodecyl mercaptan and/or chain transfer agent AMSD.
4. The heat sensitive glue matrix resin according to claim 1, wherein the heat sensitive glue matrix resin further comprises a solvent and/or an auxiliary agent.
5. The heat sensitive glue matrix resin according to claim 4, wherein the auxiliary agent comprises an ultraviolet light absorber and/or an epoxy resin.
6. The heat-sensitive adhesive body resin according to claim 5, wherein the content of the ultraviolet absorber in the heat-sensitive adhesive body resin is 0.2 to 0.3 parts by weight.
7. The heat-sensitive adhesive body resin according to claim 5, wherein the content of the epoxy resin in the heat-sensitive adhesive body resin is 1 to 3 parts by weight.
8. The heat sensitive glue host resin of claim 4, wherein the solvent comprises ethyl acetate and/or butanone.
9. The heat-sensitive glue body resin according to claim 4, wherein the content of the solvent in the heat-sensitive glue body resin is 40 to 60 parts by weight.
10. The heat-sensitive glue matrix resin according to claim 1, wherein the solid content of the heat-sensitive glue matrix resin is 49-51%.
11. The heat sensitive glue body resin according to claim 1, wherein the viscosity of the heat sensitive glue body resin is 3500-4500 cps.
12. A method for producing the heat-sensitive adhesive main body resin according to any one of claims 1 to 11, comprising: and adding an acrylic monomer, an initiator and a chain transfer agent into a solvent for reaction to obtain the heat-sensitive adhesive main resin.
13. The method of claim 12, further comprising the step of adding an auxiliary agent for mixing after the reaction is completed.
14. The preparation method according to claim 13, characterized in that it comprises the following steps:
(1) 8 to 12 weight parts of acrylic ester monomer, 0.2 to 0.4 weight part of initiator and 2 to 3 weight parts of solvent are mixed to obtain a first mixed solution; mixing 32-48 parts by weight of acrylic monomer, 24-36 parts by weight of solvent, 0.05-0.15 part by weight of chain transfer agent and 0.25-0.5 part by weight of initiator to obtain a second mixed solution; heating 8-12 parts by weight of solvent to obtain a heated solvent;
(2) Adding the first mixed solution obtained in the step (1) into the heating solvent obtained in the step (1), carrying out first heat preservation, adding the second mixed solution obtained in the step (1), carrying out second heat preservation, finally adding 6-9 parts by weight of solvent and 0.05-0.1 part by weight of initiator, carrying out third heat preservation, and adding an auxiliary agent, thereby obtaining the heat-sensitive adhesive main resin.
15. The method of claim 14, wherein the first incubation is at a temperature of 75-80 ℃.
16. The method of claim 14, wherein the first incubation time is 20 to 40 minutes.
17. The method of claim 14, wherein the second incubation is at a temperature of 75-80 ℃.
18. The method of claim 14, wherein the second incubation time is 1.5 to 2.5 hours.
19. The method of claim 14, wherein the third incubation is at a temperature of 75-80 ℃.
20. The method according to claim 14, wherein the third incubation time is 20 to 40 minutes.
21. A thermosensitive adhesive for solar film, characterized in that it comprises a combination of the thermosensitive adhesive main resin according to any one of claims 1 to 11 and a curing agent.
22. The thermosensitive adhesive for solar film according to claim 21, wherein the mass ratio of the main resin of thermosensitive adhesive and the curing agent is 5 (2-4).
23. The thermosensitive adhesive for solar film according to claim 22, wherein the preparation raw materials of the curing agent include a combination of isocyanate and polyether polyol.
24. The heat-sensitive adhesive for solar film according to claim 23, wherein the isocyanate comprises toluene diisocyanate and/or hexamethylene diisocyanate.
25. The heat-sensitive adhesive for solar film according to claim 23, wherein the molar ratio of isocyanate to polyether polyol is 1 (0.33-0.75).
26. The thermosensitive adhesive for solar film according to claim 21, wherein the solid content of the curing agent is 40 to 60%.
27. The thermosensitive adhesive for solar film according to claim 21, wherein the raw materials for preparing the thermosensitive adhesive for solar film further comprise any one or a combination of at least two of nano heat insulation paste, nano pigment or coupling agent.
28. The thermosensitive adhesive for solar film according to claim 27, wherein the mass of the coupling agent is 0.3 to 0.5g based on 1000g of the mass of the main resin of the thermosensitive adhesive.
29. A method for preparing the thermosensitive adhesive for solar film according to any one of claims 21 to 28, comprising: mixing the main resin of the thermosensitive adhesive with the curing agent, adding an optional solvent for dilution, adding an optional nano heat insulation slurry and an optional nano pigment for stirring, and finally adding an optional coupling agent for mixing to obtain the thermosensitive adhesive for the solar film.
30. A method of using the thermosensitive adhesive for solar films according to any one of claims 21 to 28, comprising: coating the solar film on the surface of the base film by using thermosensitive adhesive, drying, attaching another base film, rolling and curing.
31. Use according to claim 30, wherein the coating is performed by means of a micro-gravure coater.
32. Use according to claim 30, wherein the coating amount of the coating is 3-5 g/m 3 。
33. Use according to claim 30, wherein the drying temperature is 100-130 ℃.
34. Use according to claim 30, wherein the temperature of the rolling is 70-90 ℃.
35. Use according to claim 30, wherein the curing temperature is 50-60 ℃.
36. A method of use according to claim 30, wherein the curing time is from 48 to 72h.
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| CN103074011B (en) * | 2012-12-27 | 2015-03-18 | 广东达美新材料有限公司 | Single-component water-borne pressure sensitive adhesive for sun-proof and heat-insulating film |
| KR20170021912A (en) * | 2014-06-11 | 2017-02-28 | 닛토덴코 가부시키가이샤 | Pressure-sensitive adhesive sheet |
| CN106519106B (en) * | 2016-10-18 | 2019-05-10 | 无锡海特新材料研究院有限公司 | It is a kind of can high-speed coating super Acrylate pressure-sensitive adhesive emulsion and its preparation method and application |
| WO2018168284A1 (en) * | 2017-03-17 | 2018-09-20 | コニカミノルタ株式会社 | Optical film |
| CN107629738A (en) * | 2017-08-25 | 2018-01-26 | 无锡海特新材料研究院有限公司 | Solvent-type acrylic ester pressure-sensitive based on TPU base materials and preparation method thereof |
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