CN116904127B - Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof - Google Patents
Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof Download PDFInfo
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- 210000004400 mucous membrane Anatomy 0.000 title claims description 27
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000010410 layer Substances 0.000 claims description 70
- 239000012790 adhesive layer Substances 0.000 claims description 63
- 239000000853 adhesive Substances 0.000 claims description 45
- 230000001070 adhesive effect Effects 0.000 claims description 45
- -1 acrylic ester modified graphene Chemical class 0.000 claims description 39
- 238000001723 curing Methods 0.000 claims description 36
- 239000000758 substrate Substances 0.000 claims description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 25
- 229910021389 graphene Inorganic materials 0.000 claims description 25
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- 239000011347 resin Substances 0.000 claims description 20
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 18
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 claims description 12
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 11
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 11
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- 229920000053 polysorbate 80 Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 2
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 210000004877 mucosa Anatomy 0.000 claims description 2
- 239000005056 polyisocyanate Substances 0.000 claims description 2
- 229920001228 polyisocyanate Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- FXIVKZGDYRLHKF-UHFFFAOYSA-N C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 Chemical compound C(C)OP(OC(C1=C(C=C(C=C1C)C)C)=O)(=O)C1=CC=CC=C1 FXIVKZGDYRLHKF-UHFFFAOYSA-N 0.000 claims 1
- 230000001681 protective effect Effects 0.000 abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 229920000139 polyethylene terephthalate Polymers 0.000 description 12
- 239000005020 polyethylene terephthalate Substances 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
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- 238000012360 testing method Methods 0.000 description 12
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 10
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- 239000002390 adhesive tape Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 125000000524 functional group Chemical group 0.000 description 3
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- 238000003848 UV Light-Curing Methods 0.000 description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
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- 230000003287 optical effect Effects 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VNTHLSTXUSEHJY-UHFFFAOYSA-N C(C(=C)C)(=O)OC1=CC=CC=C1.C(C(=C)C)(=O)OCCO Chemical compound C(C(=C)C)(=O)OC1=CC=CC=C1.C(C(=C)C)(=O)OCCO VNTHLSTXUSEHJY-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000003522 acrylic cement Substances 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention relates to the technical field of protective films, and particularly discloses a double-sided high-temperature-resistant UV (ultraviolet) adhesive-reducing film and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of protective films, in particular to a double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing film and a preparation method thereof.
Background
In the processing and manufacturing process, the material is protected, fixed and supported by the protective film, so that the material can be well bonded and fixed, after the processing is finished, the material is required to be peeled off, the performance of the adhered material is not affected, and the protective film is required to be used for facilitating peeling and picking up. The UV anti-adhesion protective film has good viscosity in the early stage, and can be easily stripped by reducing the adhesive strength through curing the adhesive layer by ultraviolet irradiation during the later stripping. The UV viscosity reducing adhesive is used as a novel adhesive material, can greatly ensure the production yield and efficiency, and has wide application in the manufacturing and processing processes of large-scale integrated circuits, optical instruments, semiconductor devices and the like.
However, most of the UV mucous membrane is not high-temperature resistant, and is used in special processing processes, such as laser engraving of a metal rear cover of a mobile phone, high-performance toughened glass manufacturing process and the like, the manufacturing process needs to be subjected to high temperature of 120 ℃ or more, the mucous membrane can be softened, the later stage is not easy to peel, and small molecules with an adhesive layer can be remained on the surface of a protected object, so that the use of the protected object is affected. Chinese patent CN105086730B discloses a double-component curing UV (ultraviolet) adhesive-reducing agent, wherein a component A is composed of a curing resin, a photosensitive monomer, a photopolymerization initiator, a diluent and an auxiliary agent, one or a mixture of the NCO curing agent and the mercapto curing agent is used as a component B, and the two components are mixed to obtain the double-component UV adhesive-reducing agent. Chinese patent application CN110628355A discloses a double-sided mucosa-reducing film and a preparation method thereof, comprising in order: the adhesive comprises a first release film layer, an ultraviolet viscosity-reducing acrylic adhesive layer, a flexible substrate layer, a thermal viscosity-reducing adhesive layer and a second release film layer. Can be easily peeled off by heating and ultraviolet irradiation, has no residual glue and can not damage the adherends. However, the UV curing adhesive is not resistant to high temperature, so that substances remain, and the UV curing adhesive has a certain influence on the protected object. Based on the above, the invention provides the UV anti-adhesion protective film with high temperature resistance.
Disclosure of Invention
In order to solve the technical problems, the invention provides a double-sided high-temperature-resistant UV (ultraviolet) adhesive-reducing film and a preparation method thereof, and solves the problem that the UV adhesive-reducing protective film is poor in high-temperature resistance.
In order to achieve the above purpose, the invention discloses a double-sided high temperature resistant UV (ultraviolet) mucosa-reducing film which comprises a first release film layer, a first high temperature resistant adhesive layer, a substrate layer, a second high temperature resistant adhesive layer and a second release film layer, wherein the first release film layer and the second release film layer are respectively attached to the first high temperature resistant adhesive layer and the second high temperature resistant adhesive layer, and the first high temperature resistant adhesive layer and the second high temperature resistant adhesive layer are respectively positioned on two sides of the substrate layer;
The first high-temperature-resistant adhesive layer and the second high-temperature-resistant adhesive layer have the same components and are composed of high-temperature-resistant adhesives, and the high-temperature-resistant adhesives comprise the following raw materials in parts by weight: 35-65 parts of curing resin, 12-25 parts of acrylic ester modified graphene, 30-45 parts of organic solvent, 3-8 parts of photoinitiator, 0.2-0.5 part of curing agent and 1-3 parts of auxiliary agent;
The thickness of the first release film layer is 50-60 mu m, the thickness of the first high-temperature-resistant adhesive layer is 35-45 mu m, the thickness of the second high-temperature-resistant adhesive layer is 12-15 mu m, and the thickness of the second release film layer is 30-40 mu m.
Preferably, the first release film layer and the second release film layer have the same composition and comprise one of a polyethylene terephthalate (PET) release film layer and an organosilicon release film.
Preferably, the substrate layer comprises a corona polyethylene terephthalate substrate layer.
Preferably, the high temperature resistant adhesive is prepared by the following steps:
Ultrasonically dispersing carboxylated graphene into N, N-dimethylformamide, adding pentaerythritol triacrylate, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
And (2) uniformly mixing an organic solvent, a curing resin and acrylate modified graphene, adding a photoinitiator, reacting, adding an auxiliary agent and a curing agent after the reaction is finished, and uniformly stirring and mixing at 60-65 ℃ to obtain the high-temperature-resistant adhesive.
Further, the raw materials in the step (1) are as follows in parts by weight: 3200-4500 parts of N, N-dimethylformamide, 100 parts of carboxylated graphene, 180-250 parts of pentaerythritol triacrylate, 2-4 parts of 4-Dimethylaminopyridine (DMAP) and 48-65 parts of N, N' -Dicyclohexylcarbodiimide (DCC).
Preferably, the carboxylated graphene in the step (1) is prepared by the following steps:
And (3) ultrasonically dispersing 100 parts by weight of graphene oxide into 38000 parts by weight of deionized water, adding 450 parts by weight of chloroacetic acid and 520 parts by weight of sodium hydroxide, reacting for 24 hours at 35 ℃, filtering after the reaction, washing with deionized water, and vacuum drying for 8 hours at 60 ℃ to obtain carboxylated graphene.
Further, the temperature of the reaction in the step (1) is 25-35 ℃, and the reaction time is 24-36h.
Further, the cured resin in the step (2) consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate, wherein the mass ratio of the acrylic acid to the phenyl methacrylate to the 2-hydroxyethyl methacrylate is 25:45:30.
Further, the organic solvent in the step (2) comprises one of acetone, ethanol, n-butanol, toluene and xylene.
Further, the curing agent in the step (2) is polyisocyanate, and the curing agent comprises one of toluene diisocyanate, hexamethylene diisocyanate and isophorone diisocyanate.
Further, the photoinitiator in the step (2) comprises one of 1-hydroxycyclohexyl phenyl ketone, 4-hydroxybenzophenone and ethyl 2,4, 6-trimethylbenzoyl phenyl phosphonate.
Further, in the step (2), the auxiliary agent comprises an antifoaming agent, and the antifoaming agent comprises one of tween 80, polyoxypropylene glycerol ether and alkylphenol polyoxyethylene.
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
s1, coating a high-temperature-resistant adhesive on a first surface of a substrate layer, drying at 80-105 ℃ for 240-360 seconds to form a first high-temperature-resistant adhesive layer, coating a high-temperature-resistant adhesive on a second surface of the substrate layer, and drying at 75-100 ℃ for 180-240 seconds to form a second high-temperature-resistant adhesive layer;
S2, attaching a first release film to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, attaching a second release film to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer, and obtaining the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Preferably, the temperature gradient in the drying and forming process of the first high temperature resistant adhesive layer in S1 is as follows: the drying times at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ are the same at each temperature; the temperature gradient in the drying and forming process of the second high-temperature-resistant adhesive layer is as follows: the drying times at each temperature were the same at 75 ℃, 85 ℃, 95 ℃ and 100 ℃.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, acrylic acid, phenyl methacrylate, 2-hydroxyethyl methacrylate and acrylic ester modified graphene are used as a matrix, and under the action of an auxiliary agent and a curing agent, the prepared high-temperature-resistant adhesive has high viscosity, and after UV irradiation, the viscosity is greatly reduced, so that no residual adhesive stripping can be realized. The phenyl methacrylate contains a benzene ring rigid structure, so that the rigidity of a mucous membrane can be improved, the heat resistance is improved, 2-hydroxyethyl methacrylate has more functional groups than acrylic acid, the polarity of molecules can be enhanced, volatility is reduced, compatibility is improved, crosslinking mixing can be better, graphene oxide is contained in acrylate modified graphene, the graphene has excellent mechanical property, conductivity and heat resistance, the heat resistance of the mucous membrane can be further improved, the peeling strength of the mucous membrane before UV irradiation is reduced along with the increase of the addition amount of the acrylate modified graphene, the effective contact area of a glue layer on the surface of a substrate is reduced, the wettability of the UV mucous membrane is influenced, the peeling strength before UV irradiation is reduced, the influence on the peeling strength after UV irradiation is small, the graphene content is less, the graphene belongs to inorganic matters, in the irradiation process, the graphene has good optical property, the single-layer graphene has high transmittance and basically can penetrate to be used on UV adhesive reduction, and simultaneously the acrylate modified graphene contains a large amount of carbon functional groups, so that the volume of the adhesive is reduced, and the residual carbon functional group is reduced, and the volume of the adhesive is reduced, and the residual adhesive is not easily reduced, and the volume is reduced.
According to the invention, the carboxyl on the carboxylated graphene and the hydroxyl on the pentaerythritol triacrylate are subjected to esterification reaction to obtain the acrylic ester modified graphene, a large number of carbon-carbon double bond functional groups are introduced into the surface of the graphene, so that the dispersibility of the graphene is effectively improved, the graphene can be uniformly dispersed in a matrix, under the action of a photoinitiator, the curing resin and the acrylic ester modified graphene are subjected to polymerization reaction, the initial viscosity of the matrix can be greatly improved, the secondary pollution caused by insufficient initial viscosity in the processing shift and processing process is avoided, the processing yield is improved, the adhesive is dried by a multistage drying method, the formed high-temperature-resistant adhesive layer has the characteristics of flat surface, no bubbles and transparency, and meanwhile, the surface wettability and the adhesion performance of the substrate layer subjected to corona treatment are better, the adhesion between the substrate layer and the high-temperature-resistant adhesive layer is good, and the obtained UV (ultraviolet) mucous membrane reducing performance is excellent.
Drawings
FIG. 1 is a schematic illustration of a double-sided high temperature resistant UV-reduced film in accordance with the present invention;
In the figure: 1. a first release film layer; 2. a first high temperature resistant adhesive layer; 3. a substrate layer; 4. a second high temperature resistant adhesive layer; 5. and a second release film layer.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present invention are within the scope of protection of the present invention.
Example 1
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Dispersing 100 parts by weight of carboxylated graphene into 3200 parts of N, N-dimethylformamide by ultrasonic, adding 180 parts of pentaerythritol triacrylate, 2 parts of 4-dimethylaminopyridine and 48 parts of N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting at 25 ℃ for 36 hours, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
(2) Uniformly mixing 30 parts by weight of acetone, 35 parts by weight of curing resin and 12 parts by weight of acrylic ester modified graphene, adding 3 parts by weight of photoinitiator 4-hydroxybenzophenone, reacting, and adding 1 part by weight of auxiliary agent Tween 80 and 0.2 part by weight of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 60 ℃ to obtain a high-temperature-resistant adhesive;
(3) Coating a high temperature resistant adhesive on a first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 60 seconds to form a first high temperature resistant adhesive layer with the thickness of 35 mu m, coating a high temperature resistant adhesive on a second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 45 seconds to form a second high temperature resistant adhesive layer with the thickness of 12 mu m;
(4) And attaching a first release film organic silicon release film with the thickness of 50 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 30 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Example 2
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Ultrasonically dispersing 100 parts by weight of carboxylated graphene into 4000 parts by weight of N, N-dimethylformamide, adding 220 parts by weight of pentaerythritol triacrylate, 3 parts by weight of 4-dimethylaminopyridine and 56 parts by weight of N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting at 30 ℃ for 32 hours, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
(2) Uniformly mixing 40 parts by weight of acetone, 52 parts by weight of curing resin and 20 parts by weight of acrylate modified graphene, adding 5 parts by weight of photoinitiator 4-hydroxybenzophenone, reacting, and adding 2 parts by weight of auxiliary agent Tween 80 and 0.4 part by weight of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 62 ℃ to obtain the high-temperature-resistant adhesive;
(3) Coating a high temperature resistant adhesive on a first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 75 seconds to form a first high temperature resistant adhesive layer with the thickness of 40 mu m, coating a high temperature resistant adhesive on a second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 55 seconds to form a second high temperature resistant adhesive layer with the thickness of 14 mu m;
(4) And attaching a first release film organic silicon release film with the thickness of 55 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 35 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Example 3
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Ultrasonically dispersing 100 parts by weight of carboxylated graphene into 4500 parts by weight of N, N-dimethylformamide, adding 250 parts by weight of pentaerythritol triacrylate, 4 parts by weight of 4-dimethylaminopyridine and 65 parts by weight of N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting at 35 ℃ for 24 hours, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
(2) Uniformly mixing 45 parts of acetone, 65 parts of curing resin and 25 parts of acrylic ester modified graphene, adding 8 parts of photoinitiator 4-hydroxybenzophenone, reacting, and adding 3 parts of auxiliary agent Tween 80 and 0.5 part of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 65 ℃ to obtain a high-temperature-resistant adhesive;
(3) Coating a high temperature resistant adhesive on the first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 90 seconds to form a first high temperature resistant adhesive layer with the thickness of 45 mu m, coating a high temperature resistant adhesive on the second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 60 seconds to form a second high temperature resistant adhesive layer with the thickness of 15 mu m;
(4) And attaching a first release film organic silicon release film with the thickness of 60 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 40 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Comparative example 1
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Uniformly mixing 40 parts by weight of acetone, 52 parts by weight of curing resin, 6.25 parts by weight of carboxylated graphene and 13.75 parts by weight of pentaerythritol triacrylate, adding 5 parts by weight of photoinitiator 4-hydroxybenzophenone, reacting, adding 2 parts by weight of auxiliary agent Tween 80 and 0.4 part by weight of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 62 ℃ to obtain a high-temperature-resistant adhesive;
(2) Coating a high temperature resistant adhesive on a first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 75 seconds to form a first high temperature resistant adhesive layer with the thickness of 40 mu m, coating a high temperature resistant adhesive on a second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 55 seconds to form a second high temperature resistant adhesive layer with the thickness of 14 mu m;
(3) And attaching a first release film organic silicon release film with the thickness of 55 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 35 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Comparative example 2
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Uniformly mixing 40 parts by weight of acetone, 52 parts by weight of curing resin and 20 parts by weight of pentaerythritol triacrylate, adding 5 parts by weight of photoinitiator 4-hydroxybenzophenone, reacting, and adding 2 parts by weight of auxiliary agent Tween 80 and 0.4 part by weight of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 62 ℃ to obtain the high-temperature-resistant adhesive;
(2) Coating a high temperature resistant adhesive on a first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 75 seconds to form a first high temperature resistant adhesive layer with the thickness of 40 mu m, coating a high temperature resistant adhesive on a second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 55 seconds to form a second high temperature resistant adhesive layer with the thickness of 14 mu m;
(3) And attaching a first release film organic silicon release film with the thickness of 55 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 35 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
Comparative example 3
A preparation method of double-sided high temperature resistant UV (ultraviolet) mucous membrane reducing comprises the following steps:
(1) Ultrasonically dispersing 100 parts by weight of carboxylated graphene into 4000 parts by weight of N, N-dimethylformamide, adding 220 parts by weight of pentaerythritol triacrylate, 3 parts by weight of 4-dimethylaminopyridine and 56 parts by weight of N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting at 30 ℃ for 32 hours, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
(2) Uniformly mixing 40 parts by weight of acetone, 52 parts by weight of curing resin and 20 parts by weight of acrylate modified graphene, adding 5 parts by weight of photoinitiator 4-hydroxybenzophenone, reacting, and adding 2 parts by weight of auxiliary agent Tween 80 and 0.4 part by weight of curing agent toluene diisocyanate after the reaction is finished, wherein the curing resin consists of acrylic acid, methyl methacrylate and butyl methacrylate in a mass ratio of 25:45:30, and uniformly stirring and mixing at 62 ℃ to obtain a high-temperature-resistant adhesive;
(3) Coating a high temperature resistant adhesive on a first surface of a substrate layer corona polyethylene terephthalate substrate layer with the thickness of 50 mu m, respectively drying at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ for 75 seconds to form a first high temperature resistant adhesive layer with the thickness of 40 mu m, coating a high temperature resistant adhesive on a second surface of the substrate layer, respectively drying at 75 ℃, 85 ℃, 95 ℃ and 100 ℃ for 55 seconds to form a second high temperature resistant adhesive layer with the thickness of 14 mu m;
(4) And attaching a first release film organic silicon release film with the thickness of 55 mu m to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, and attaching a second release film organic silicon release film with the thickness of 35 mu m to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer to obtain the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
The graphene oxide used in the examples and comparative examples of the present invention is purchased from Hangzhou intelligent titanium purification technology Co., ltd, and is single-layer graphene oxide with an average thickness of 0.5-1.2nm and a diameter of 4-7 μm; the corona polyethylene terephthalate substrate layer is a corona PET (polyethylene terephthalate) available from Zhangjia Kong Kangde new photoelectric materials Co., ltd, and the model is KFDN-50G4; other reagents and starting materials were commercially available.
The high temperature resistant UV-cut film of examples 1-3 and comparative examples 1-3 was used as a sample for performance testing, corresponding to the following test:
(1) Initial tack: the initial tackiness test is carried out on a sample by referring to GB/T4852-2002 'pressure sensitive adhesive tape initial tackiness test method', a rolling ball slope stopping test method is adopted, an inclination angle of 30 degrees is adopted, and a stainless steel plate is adopted;
(2) Holding viscosity: the method comprises the steps of performing a holding viscosity test on a sample by referring to GB/T4851-2014 adhesive tape holding viscosity test method, using a holding force tester to perform the test, wherein the test temperature is 40 ℃ and the weight is 500g;
(3) Heat resistant holding power: the heat-resistant and viscosity-maintaining test is carried out on a sample by referring to GB/T4851-2014 adhesive tape viscosity-maintaining test method, a viscosity-maintaining tester is used for testing, the testing temperature is 120 ℃, and the weight is 500g;
(4) 180 ° peel strength: the test of the peeling strength of the sample is carried out by referring to GB/T2792-2014 test method of the peeling strength of adhesive tape, an electronic tensile tester is used, the adhesive tape is 25mm wide, the peeling speed is 300mm/min, the wavelength is 420nm after UV irradiation, peeling is carried out after irradiation, and whether residual adhesive exists or not is observed;
The test results are shown in table 1:
TABLE 1
As shown by the test results in Table 1, the high temperature resistant UV-reducing film corresponding to examples 1-3 of the invention has good high temperature resistance, the maximum holding power can reach 22min under the high temperature action of 120 ℃, the phenyl methacrylate contains a benzene ring rigid structure, and the phenyl methacrylate-2-hydroxyethyl methacrylate and the acrylic acid generate a synergistic effect to act together with graphene, so that the heat resistance of the UV-reducing film is effectively improved, and the heat resistance and the holding power are improved. The initial adhesion and the holding adhesion are good, the corresponding peel strength of the example 1 is the highest and is 21.5 before UV irradiation, the peel strength of the examples 1-3 is not greatly different after UV irradiation, and the peel strength of the mucosa before UV irradiation is reduced mainly due to the increase of the addition amount of the acrylic ester modified graphene, and the influence on the peel strength after UV irradiation is small. The acrylic ester modified graphene contains a large number of carbon-carbon double bond functional groups, so that the multifunctional oligomer and the multifunctional monomer generate a crosslinking reaction, and after UV irradiation, the acrylic ester modified graphene generates larger volume shrinkage to reduce the contact area, so that the viscosity reduction is realized, the acrylic ester modified graphene is easy to peel, and no residual glue is generated.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The utility model provides a two-sided high temperature resistant UV subtracts mucosa which characterized in that: the high-temperature-resistant adhesive comprises a first release film layer, a first high-temperature-resistant adhesive layer, a substrate layer, a second high-temperature-resistant adhesive layer and a second release film layer, wherein the first release film layer and the second release film layer are respectively attached to the first high-temperature-resistant adhesive layer and the second high-temperature-resistant adhesive layer, and the first high-temperature-resistant adhesive layer and the second high-temperature-resistant adhesive layer are respectively positioned on two sides of the substrate layer;
The first high-temperature-resistant adhesive layer and the second high-temperature-resistant adhesive layer have the same components and are composed of high-temperature-resistant adhesives, and the high-temperature-resistant adhesives comprise the following raw materials in parts by weight: 35-65 parts of curing resin, 12-25 parts of acrylic ester modified graphene, 30-45 parts of organic solvent, 3-8 parts of photoinitiator, 0.2-0.5 part of curing agent and 1-3 parts of auxiliary agent;
The high-temperature-resistant adhesive is prepared by the following steps:
Ultrasonically dispersing carboxylated graphene into N, N-dimethylformamide, adding pentaerythritol triacrylate, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide, uniformly mixing, reacting, filtering after the reaction is finished, washing with dichloromethane, and vacuum drying at 60 ℃ for 8 hours to obtain acrylate modified graphene;
wherein 3200-4500 parts of N, N-dimethylformamide, 100 parts of carboxylated graphene, 180-250 parts of pentaerythritol triacrylate, 2-4 parts of 4-dimethylaminopyridine and 48-65 parts of N, N' -dicyclohexylcarbodiimide;
the reaction temperature is 25-35 ℃, and the reaction time is 24-36h;
Step (2) after uniformly mixing an organic solvent, a curing resin and acrylate modified graphene, adding a photoinitiator to react, adding an auxiliary agent and a curing agent after the reaction is finished, and uniformly stirring and mixing at 60-65 ℃ to obtain a high-temperature-resistant adhesive;
Wherein the cured resin consists of acrylic acid, phenyl methacrylate and 2-hydroxyethyl methacrylate, and the mass ratio of the acrylic acid to the phenyl methacrylate to the 2-hydroxyethyl methacrylate is 25:45:30;
The thickness of the first release film layer is 50-60 mu m, the thickness of the first high-temperature-resistant adhesive layer is 35-45 mu m, the thickness of the second high-temperature-resistant adhesive layer is 12-15 mu m, and the thickness of the second release film layer is 30-40 mu m.
2. The double-sided high temperature resistant UV-reduced film according to claim 1, wherein: the organic solvent in the step (2) comprises one of acetone, ethanol, n-butanol, toluene and xylene.
3. The double-sided high temperature resistant UV-reduced film according to claim 1, wherein: the curing agent in the step (2) is polyisocyanate, and comprises one of toluene diisocyanate, hexamethylene diisocyanate and isophorone diisocyanate.
4. The double-sided high temperature resistant UV-reduced film according to claim 1, wherein: the photoinitiator in the step (2) comprises one of 1-hydroxycyclohexyl phenyl ketone, 4-hydroxybenzophenone and ethyl 2,4, 6-trimethylbenzoyl phenylphosphonate.
5. The double-sided high temperature resistant UV-reduced film according to claim 1, wherein: the auxiliary agent in the step (2) comprises an antifoaming agent, wherein the antifoaming agent comprises one of Tween 80, polyoxypropylene glycerol ether and alkylphenol polyoxyethylene.
6. A method for preparing the double-sided high temperature resistant UV-cut mucous membrane according to any one of claims 1-5, characterized in that: the method comprises the following steps:
s1, coating a high-temperature-resistant adhesive on a first surface of a substrate layer, drying at 80-105 ℃ for 240-360 seconds to form a first high-temperature-resistant adhesive layer, coating a high-temperature-resistant adhesive on a second surface of the substrate layer, and drying at 75-100 ℃ for 180-240 seconds to form a second high-temperature-resistant adhesive layer;
S2, attaching a first release film to the surface of the first high-temperature-resistant adhesive layer to form a first release film layer, attaching a second release film to the surface of the second high-temperature-resistant adhesive layer to form a second release film layer, and obtaining the double-sided high-temperature-resistant UV (ultraviolet) mucous membrane.
7. The method for preparing the double-sided high temperature resistant UV (ultraviolet) mucous membrane according to claim 6, which is characterized in that: the temperature gradient in the drying and forming process of the first high-temperature-resistant adhesive layer in the step S1 is as follows: the drying times at 80 ℃, 90 ℃, 100 ℃ and 105 ℃ are the same at each temperature; the temperature gradient in the drying and forming process of the second high-temperature-resistant adhesive layer is as follows: the drying times at each temperature were the same at 75 ℃, 85 ℃, 95 ℃ and 100 ℃.
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