CN117487485A - Solvent-free strippable glue and preparation method and application thereof - Google Patents
Solvent-free strippable glue and preparation method and application thereof Download PDFInfo
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- CN117487485A CN117487485A CN202311618935.1A CN202311618935A CN117487485A CN 117487485 A CN117487485 A CN 117487485A CN 202311618935 A CN202311618935 A CN 202311618935A CN 117487485 A CN117487485 A CN 117487485A
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- glue
- photoinitiator
- acrylate
- strippable
- solvent
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- 239000003292 glue Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 52
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 40
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 35
- 239000011737 fluorine Substances 0.000 claims abstract description 35
- 239000004814 polyurethane Substances 0.000 claims abstract description 33
- 229920002635 polyurethane Polymers 0.000 claims abstract description 33
- -1 acrylic ester Chemical class 0.000 claims abstract description 31
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims abstract description 23
- LVGFPWDANALGOY-UHFFFAOYSA-N 8-methylnonyl prop-2-enoate Chemical compound CC(C)CCCCCCCOC(=O)C=C LVGFPWDANALGOY-UHFFFAOYSA-N 0.000 claims abstract description 20
- IQYMRQZTDOLQHC-ZQTLJVIJSA-N [(1R,4S)-2-bicyclo[2.2.1]heptanyl] prop-2-enoate Chemical compound C1C[C@H]2C(OC(=O)C=C)C[C@@H]1C2 IQYMRQZTDOLQHC-ZQTLJVIJSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 35
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000000049 pigment Substances 0.000 claims description 12
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 4
- LKFPLZRHLNYVKX-UHFFFAOYSA-N 2-(dimethylamino)-2-[(4-methylphenyl)methyl]-1-(2-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=CC=C(N2CCOCC2)C=1C(=O)C(CC)(N(C)C)CC1=CC=C(C)C=C1 LKFPLZRHLNYVKX-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical class C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 25
- 239000002904 solvent Substances 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 34
- 238000003756 stirring Methods 0.000 description 27
- 238000004321 preservation Methods 0.000 description 19
- 230000002209 hydrophobic effect Effects 0.000 description 18
- 230000001070 adhesive effect Effects 0.000 description 10
- 239000000853 adhesive Substances 0.000 description 9
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 7
- PUBNJSZGANKUGX-UHFFFAOYSA-N 2-(dimethylamino)-2-[(4-methylphenyl)methyl]-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=C(C)C=C1 PUBNJSZGANKUGX-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000012790 adhesive layer Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 2
- PSGCQDPCAWOCSH-BOURZNODSA-N exo-1,7,7-Trimethylbicyclo(2.2.1)hept-2-yl acrylate Chemical compound C1C[C@]2(C)C(OC(=O)C=C)C[C@H]1C2(C)C PSGCQDPCAWOCSH-BOURZNODSA-N 0.000 description 2
- ZYMKZMDQUPCXRP-UHFFFAOYSA-N fluoro prop-2-enoate Chemical compound FOC(=O)C=C ZYMKZMDQUPCXRP-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of peelable glue, and particularly relates to solvent-free peelable glue, and a preparation method and application thereof. The solvent-free strippable glue comprises aliphatic fluorine-containing polyurethane acrylic ester, functional monomers and a photoinitiator; the functional monomers are norbornyl acrylate, lauryl methacrylate and isodecyl acrylate; the mass ratio of the norbornyl acrylate, the lauryl methacrylate and the isodecyl acrylate is 27-50:4.5-22:5, a step of; the mass fraction of the aliphatic fluorine-containing polyurethane acrylic ester is 27-55%. The invention adopts aliphatic fluorine-containing polyurethane acrylic ester with specific content as main component, and three types of norbornyl acrylate, lauryl methacrylate and isosunflower-based acrylic ester with specific proportion are used as functional monomers, and the photoinitiator, on the basis of ensuring that solvent-free strippable glue has good resistivity and water resistance, the solvent is shielded, and the strippable glue is endowed with good mechanical property and stability.
Description
Technical Field
The invention belongs to the technical field of peelable glue, and particularly relates to solvent-free peelable glue, and a preparation method and application thereof.
Background
The strippable glue is a silk-like ink printed by silk screen, and is mainly characterized in that the strippable glue can be easily stripped by hands or tools after the product is processed, and the strippable glue cannot remain on the product. At present, the strippable glue is widely applied to a circuit board PCB, and a strippable film is formed through solidification treatment (such as heating or ultraviolet irradiation), so that temporary and effective protection is provided for the position of the circuit board PCB, which does not need soldering tin in a tin passing furnace, wave soldering and reflow soldering process.
Although solvent-based strippable adhesives have been widely used in the field of electronic products, including flat cable positioning, pin sealing, liquid crystal panels, cell phone keys, and the like. However, in the application process, the solvent needs to be evaporated and then solidified, so that the production risk is high, the solvent waste is caused, the cost is increased, and the transportation and the storage are not facilitated. At present, various types of acrylic esters are used as base materials of common peelable adhesives, but the main chain structure and side groups of the acrylic esters can seriously influence the performance of the peelable adhesives, so that the peelable adhesives are poor in water resistance, high in absorptivity, brittle at low temperature, sticky at high temperature (low in brittleness and high viscosity), and lose due strength, and further the peelable adhesives applied to electronic products still have the problems of poor water resistance and low resistivity.
Therefore, it is desirable to provide a solvent-free peelable glue that has good resistivity and water resistance.
Disclosure of Invention
The present invention is directed to solving one or more of the problems of the prior art and providing at least one of a beneficial choice or creation of conditions. The invention provides a solvent-free strippable glue stock which has good resistivity and water resistance.
The invention is characterized in that: the strippable glue comprises aliphatic fluorine-containing polyurethane acrylic ester, functional monomers and photoinitiators; the functional monomers are norbornyl acrylate, lauryl methacrylate and isodecyl acrylate; the mass ratio of the norbornyl acrylate, the lauryl methacrylate and the isodecyl acrylate is 27-50:4.5-22:5, a step of; the aliphatic fluorine-containing polyurethane acrylic ester accounts for 27-55% of the mass of the strippable glue. The invention adopts aliphatic fluorine-containing polyurethane acrylic ester with specific content as base material, and three types of norbornyl acrylate, lauryl methacrylate and isosunflower-based acrylic ester with specific proportion are used as functional monomers, and the photoinitiator, so that the strippable glue has good resistivity and water resistance.
Accordingly, in a first aspect the present invention provides a solvent-free peelable glue.
Specifically, the solvent-free strippable glue comprises aliphatic fluorine-containing polyurethane acrylic ester, a functional monomer and a photoinitiator;
the functional monomers comprise norbornyl acrylate, lauryl methacrylate and isodecyl acrylate;
the mass ratio of the norbornyl acrylate, the lauryl methacrylate and the isodecyl acrylate is 27-50:4.5-22:5, a step of;
the aliphatic fluorine-containing polyurethane acrylic ester accounts for 27-55% of the mass of the strippable glue.
Preferably, the mass ratio of the norbornyl acrylate (IBOA), the Lauryl Methacrylate (LMA) and the isodecyl acrylate (ISODA) is 30-45:5-20:5.
specifically, IBOA, LMA, ISODA with a specific proportion is adopted as a functional monomer, and the solvent can be shielded under the combined action of the IBOA, LMA, ISODA, so that the peelable adhesive film is endowed with good toughness, adhesive force and low shrinkage. The IBOA can effectively reduce the viscosity of the strippable glue, improve the construction performance and improve the leveling property of the strippable glue; in addition, the IBOA is used as a reactive diluent of the epoxy acrylic acid oligomer, so that the internal stress of the peelable adhesive layer can be obviously reduced, and the volume shrinkage rate of the peelable adhesive layer can be reduced, thereby obviously improving the adhesive force, the shrinkage rate, the impact resistance, the scratch resistance, the weather resistance and other characteristic indexes of the radiation-cured adhesive layer, and simultaneously, the hardness and the flexibility of the radiation-cured adhesive layer are not reduced. IBOA, if used in a protective coating for optical discs, has excellent adhesion to fine grain surfaces and scratch resistance, and has excellent finishing properties and gives a coating film having significantly improved gloss. The particular linear structure of the LMA increases leveling. ISODA is an excellent reactive monomer for photocuring, which can endow the system with good adhesiveness, flexibility, pigment wettability, hydrophobicity and low surface tension. The three functional monomers interact and match with the prepolymer aliphatic fluorine-containing polyurethane acrylate with specific content, so that the prepolymer aliphatic fluorine-containing polyurethane acrylate has good resistivity, water resistance, viscosity and mechanical properties.
Preferably, the aliphatic fluorine-containing polyurethane acrylate accounts for 30-50% of the mass of the strippable glue.
Preferably, the aliphatic fluorinated urethane acrylate is a hydrophobic aliphatic fluorinated urethane acrylate.
Specifically, the invention takes the hydrophobic aliphatic fluorine-containing polyurethane acrylate with specific content as the base material, and the benzene ring and fluorine element in the molecular chain endow the system with excellent hardness, water resistance, pigment wettability, chemical resistance and acid-base resistance while realizing rapid solidification. In addition, the hydrophobic aliphatic fluorine-containing polyurethane acrylic ester is matched with a specific type and content of functional monomer and photoinitiator, so that the strippable glue has good resistivity, water resistance and mechanical property.
Preferably, the strippable glue comprises 27-55% of aliphatic fluorine-containing polyurethane acrylate, 32-80% of functional monomer and 0.9-5.5% of photoinitiator in percentage by mass.
Further preferably, the strippable glue comprises, by mass, 30-50% of aliphatic fluorine-containing polyurethane acrylate, 35-75% of functional monomer and 1-5% of photoinitiator.
Preferably, the strippable glue further comprises at least one of a leveling agent and a pigment.
Preferably, the peelable glue further comprises a leveling agent and a pigment; the preparation raw materials of the strippable glue comprise, by mass, 27-55% of aliphatic fluorine-containing polyurethane acrylic ester, 32-80% of functional monomers, 0.9-5.5% of photoinitiators, 0.1-1.1% of flatting agents and 0.03-0.11% of pigments.
Further preferably, the strippable glue comprises, by mass, 30-50% of aliphatic fluorine-containing polyurethane acrylate, 35-75% of functional monomer, 1-5% of photoinitiator, 0.1-1% of leveling agent and 0.03-0.1% of pigment.
Preferably, the photoinitiator comprises at least one of 1-hydroxycyclohexylphenyl ketone (photoinitiator 184), 2- (4-methylbenzyl) -2- (dimethylamino) -1- (morpholinophenyl) -1-butanone (photoinitiator 379).
Preferably, the mass ratio of the photoinitiator 184 to the photoinitiator 379 is 1:0.27-8.
Further preferably, the mass ratio of the photoinitiator 184 to the photoinitiator 379 is 1:0.3-7.
Preferably, the leveling agent comprises at least one of polyether modified dimethyl siloxane and acrylic resin leveling agent.
Preferably, the pigment is a dye blue.
The second aspect of the invention provides a preparation method of the solvent-free strippable glue in the first aspect of the invention.
Specifically, the preparation method of the solvent-free peelable glue comprises the following steps:
and mixing the raw material components to obtain the strippable glue.
Preferably, the preparation method of the solvent-free strippable glue comprises the following steps:
(1) Heating the aliphatic fluorine-containing polyurethane acrylate, and then adding part of functional monomers to obtain a first mixture;
(2) Mixing the remaining raw material components with the first mixture obtained in the step (1) to obtain the solvent-free peelable glue.
Preferably, in step (1), the heating is water bath heating; the temperature of the water bath heating is 55-90 ℃, and the time of the water bath heating is 22-40min.
Further preferably, the temperature of the water bath heating is 60-80 ℃, and the time of the water bath heating is 25-35min.
Preferably, in the step (1), after adding part of the functional monomers, heating is performed, and the heating adopts a mode of heat preservation and stirring.
Preferably, the temperature of the heat preservation stirring is 35-90 ℃, and the time of the heat preservation stirring is 50-70min.
Further preferably, the temperature of the heat preservation stirring is 40-80 ℃, and the time of the heat preservation stirring is 55-65min.
Preferably, the step (2) specifically includes the following steps:
s1: mixing the photoinitiator and part of the functional monomers, and heating the first mixture obtained in the step (1) to obtain a second mixture;
s2: and (3) mixing the pigment, the leveling agent and the second mixture obtained in the step (2), heating, and then adding the residual functional monomer to prepare the solvent-free peelable glue.
Preferably, step S1 is to mix the photoinitiator and part of the functional monomers first, and then add the mixture to the first mixture obtained in step (1).
Preferably, in step S1, the heating is performed by using a heat-preserving stirring manner.
Preferably, the temperature of the heat preservation stirring is 35-90 ℃, and the time of the heat preservation stirring is 50-70min.
Further preferably, the temperature of the heat preservation stirring is 40-80 ℃, and the time of the heat preservation stirring is 55-65min.
Preferably, step S2 is to add the pigment and the leveling agent to the second mixture obtained in step (2), heat the mixture, and then add the remaining functional monomer to obtain the solvent-free peelable glue.
Preferably, in step S2, the heating is performed by using a heat-preserving stirring manner.
Preferably, the temperature of the heat preservation stirring is 35-90 ℃, and the time of the heat preservation stirring is 50-70min.
Further preferably, the temperature of the heat preservation stirring is 40-80 ℃, and the time of the heat preservation stirring is 55-65min.
Preferably, in the step S2, after the residual functional monomers are added, the heat preservation is continued, wherein the heat preservation time is 50min-3.5h; further preferably, the incubation time is 1-3 hours.
A third aspect of the present invention provides an application of the solvent-free peelable glue according to the first aspect of the present invention in the field of electronic products.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
the invention adopts aliphatic fluorine-containing polyurethane acrylic ester with specific content as base material, and three types of norbornyl acrylate, lauryl methacrylate and isosunflower-based acrylic ester with specific proportion are used as functional monomers, and a photoinitiator is combined, so that the solvent-free strippable glue is shielded on the basis of ensuring good resistivity and water resistance, and good mechanical property and stability are provided for the strippable glue.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
The solvent-free strippable glue comprises 40% of hydrophobic aliphatic fluorine-containing polyurethane acrylic ester, 55% of functional monomer, 4% of photoinitiator, 0.97% of flatting agent polyether modified dimethyl siloxane and 0.03% of dye blue;
among functional monomers, IBOA: LMA: the mass ratio of ISODA is 40:10:5, a step of;
the mass ratio of photoinitiator 184 to photoinitiator 379 was 3:1.
A preparation method of solvent-free strippable glue comprises the following steps:
(1) Placing hydrophobic aliphatic fluorine-containing polyurethane acrylate in a 100mL beaker in a shading thousand-level clean room, heating the hydrophobic aliphatic fluorine-containing polyurethane acrylate to 70 ℃ in a sealed water bath, preserving heat for 30min, transferring the heated hydrophobic aliphatic fluorine-containing polyurethane acrylate into a three-neck flask, preserving heat at 50 ℃ and stirring for 1h; one third of the functional monomers are taken to rinse the beaker and transferred into a three-neck flask, and the mixture is stirred for 1h at 50 ℃ to obtain a first mixture;
(2) In the beaker of the step (1), a third of functional monomer is adopted to dissolve the photoinitiator, and the photoinitiator is added into the first mixture obtained in the step (1), and the mixture is stirred for 1h at 50 ℃ in a heat-preserving way, so as to obtain a second mixture;
(3) And (3) adding dye blue and a leveling agent into the second mixture obtained in the step (2), keeping the temperature at 50 ℃ and stirring for 1h, adding the rest one third of functional monomers, keeping the temperature and stirring for 1h, cooling to 40 ℃ and discharging to obtain the blue transparent solvent-free strippable glue, and carrying out shading preservation.
Example 2
The solvent-free strippable glue comprises 40% of hydrophobic aliphatic fluorine-containing polyurethane acrylic ester, 55% of functional monomer, 4% of photoinitiator, 0.97% of flatting agent polyether modified dimethyl siloxane and 0.03% of dye blue;
among functional monomers, IBOA: LMA: the mass ratio of ISODA is 45:5:5, a step of;
the mass ratio of photoinitiator 184 to photoinitiator 379 was 3:1.
A preparation method of solvent-free strippable glue comprises the following steps:
(1) Placing the prepolymer in a 100mL beaker in a shading thousand-level clean room, heating the prepolymer to 70 ℃ in a sealed water bath, preserving heat for 30min, transferring the prepolymer into a three-neck flask, preserving heat at 50 ℃ and stirring for 1h; one third of the functional monomers are taken to rinse the beaker and transferred into a three-neck flask, and the mixture is stirred for 1h at 50 ℃ to obtain a first mixture;
(2) In the beaker of the step (1), a third of functional monomer is adopted to dissolve the photoinitiator, and the photoinitiator is added into the first mixture obtained in the step (1), and the mixture is stirred for 1h at 50 ℃ in a heat-preserving way, so as to obtain a second mixture;
(3) And (3) adding dye blue and a leveling agent into the second mixture obtained in the step (2), keeping the temperature at 50 ℃ and stirring for 1h, adding the rest one third of functional monomers, keeping the temperature and stirring for 2h, cooling to 40 ℃ and discharging to obtain the blue transparent solvent-free strippable glue, and carrying out shading preservation.
Example 3
The solvent-free strippable glue comprises 30% of hydrophobic aliphatic fluorine-containing polyurethane acrylic ester, 65% of functional monomer, 4% of photoinitiator, 0.9% of flatting agent polyether modified dimethyl siloxane and 0.1% of dye blue in percentage by mass;
among functional monomers, IBOA: LMA: the mass ratio of ISODA is 45:15:5, a step of;
the mass ratio of photoinitiator 184 to photoinitiator 379 was 3:1.
A preparation method of solvent-free strippable glue comprises the following steps:
(1) Placing the prepolymer in a 100mL beaker in a shading thousand-level clean room, heating the prepolymer to 70 ℃ in a sealed water bath, preserving heat for 30min, transferring the prepolymer into a three-neck flask, preserving heat at 50 ℃ and stirring for 1h; one third of the functional monomers are taken to rinse the beaker and transferred into a three-neck flask, and the mixture is stirred for 1h at 50 ℃ to obtain a first mixture;
(2) In the beaker of the step (1), a third of functional monomer is adopted to dissolve the photoinitiator, and the photoinitiator is added into the first mixture obtained in the step (1), and the mixture is stirred for 1h at 50 ℃ in a heat-preserving way, so as to obtain a second mixture;
(3) And (3) adding dye blue and a leveling agent into the second mixture obtained in the step (2), keeping the temperature at 50 ℃ and stirring for 1h, adding the rest one third of functional monomers, keeping the temperature and stirring for 2h, cooling to 40 ℃ and discharging to obtain the blue transparent solvent-free strippable glue, and carrying out shading preservation.
Example 4
The solvent-free strippable glue comprises, by mass, 50% of hydrophobic aliphatic fluorine-containing polyurethane acrylate, 45% of a functional monomer, 4% of a photoinitiator, 0.97% of leveling agent polyether modified dimethyl siloxane and 0.03% of dye blue;
in the functional monomer, the mass ratio of IBOA to LMA to ISODA is 35:5:5, a step of;
the mass ratio of photoinitiator 184 to photoinitiator 379 was 3:1.
A preparation method of solvent-free strippable glue comprises the following steps:
(1) Placing the prepolymer in a 100mL beaker in a shading thousand-level clean room, heating the prepolymer to 70 ℃ in a sealed water bath, preserving heat for 30min, transferring the prepolymer into a three-neck flask, preserving heat at 50 ℃ and stirring for 1h; one third of the functional monomers are taken to rinse the beaker and transferred into a three-neck flask, and the mixture is stirred for 1h at 50 ℃ to obtain a first mixture;
(2) In the beaker of the step (1), a third of functional monomer is adopted to dissolve the photoinitiator, and the photoinitiator is added into the first mixture obtained in the step (1), and the mixture is stirred for 1h at 50 ℃ in a heat-preserving way, so as to obtain a second mixture;
(3) And (3) adding dye blue and a leveling agent into the second mixture obtained in the step (2), keeping the temperature at 50 ℃ and stirring for 1h, adding the rest one third of functional monomers, keeping the temperature and stirring for 2h, cooling to 40 ℃ and discharging to obtain the blue transparent solvent-free strippable glue, and carrying out shading preservation.
Comparative example 1
Comparative example 1 differs from example 1 only in that the mass percentage of the hydrophobic aliphatic fluorinated urethane acrylate of comparative example 1 is 20%, otherwise identical to example 1.
Comparative example 2
Comparative example 2 differs from example 1 only in that the mass percentage of the hydrophobic aliphatic fluorinated urethane acrylate of comparative example 2 is 60%, otherwise identical to example 1.
Comparative example 3
Comparative example 3 differs from example 1 only in that comparative example 3 uses the same amount of fluorine-free aliphatic acrylate instead of the hydrophobic aliphatic fluorine-containing urethane acrylate, except that example 1 is used.
Comparative example 4
Comparative example 4 differs from example 1 only in that comparative example 4 uses the same amount of the fluoroacrylate instead of the hydrophobic aliphatic fluoroacrylate, and is otherwise identical to example 1.
Comparative example 5
Comparative example 5 differs from example 1 only in that comparative example 5 uses an equivalent amount of fluorine-free non-aliphatic acrylate instead of the hydrophobic aliphatic fluorine-containing urethane acrylate, except that example 1 is used.
Comparative example 6
Comparative example 6 differs from example 1 only in the functional monomer of comparative example 6, IBOA: LMA: the mass ratio of ISODA is 15:20:20, otherwise as in example 1.
Comparative example 7
Comparative example 7 differs from example 1 only in the functional monomer of comparative example 7, IBOA: LMA: the mass ratio of ISODA is 35:10:10, otherwise the same as in example 1.
Performance testing
The solvent-free peelable adhesives prepared in examples 1 to 4 and comparative examples 1 to 7 were subjected to the related tests, the test items and the test methods are shown in Table 1, and the test results are shown in tables 2 and 3:
table 1: test item and test method
Table 2: examples 1-4 solvent-free strippable test results
Table 3: comparative examples 1 to 7 solvent-free peelable adhesive property test results
As can be seen from tables 2-3, the peelable glue prepared by the invention has good resistivity, moisture permeability, water resistance and mechanical properties.
The mass percentage of the hydrophobic aliphatic fluorine-containing polyurethane acrylate of the comparative example 1 is 20%, which is not in the scope of the invention, so that the moisture permeability, the water absorption, the impedance and the tensile strength of the comparative example 1 are all worse than those of the example 1, and the 180-degree peeling force is obviously lower than that of the example 1. The mass percentage of the hydrophobic aliphatic fluorine-containing polyurethane acrylate of the comparative example 2 is 60 percent, which is out of the scope of the invention, so that the water absorption, the resistivity and the mechanical property of the comparative example 2 are all worse than those of the example 1, and the 180-degree stripping force is obviously lower than that of the example 1.
Comparative examples 3-5 replaced the hydrophobic aliphatic fluorinated urethane acrylate of example 1 with equal amounts of non-fluorinated aliphatic acrylate, fluorinated acrylate, non-fluorinated non-aliphatic acrylate, respectively, such that the water absorption, 180 ° peel force of comparative examples 3-5 was much greater than example 1 and the tensile strength was less than example 1.
Of the functional monomers of comparative examples 6-7, IBOA: LMA: the mass ratio of ISODA is not in the range of the invention, so that the water absorption and the moisture permeability of comparative example 6 are higher than those of example 1, the impedance is lower than that of example 1, and the resistivity and the water resistance of the solvent-free strippable adhesive are better than those of comparative example 6. The impedance of comparative example 7 is lower than that of example 1, indicating that the solvent-free strippable glue of the present invention has a higher resistivity than comparative example 7.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The strippable glue is characterized by comprising aliphatic fluorine-containing polyurethane acrylic ester, functional monomers and a photoinitiator;
the functional monomers comprise norbornyl acrylate, lauryl methacrylate and isodecyl acrylate;
the mass ratio of the norbornyl acrylate, the lauryl methacrylate and the isodecyl acrylate is 27-50:4.5-22:5, a step of;
the aliphatic fluorine-containing polyurethane acrylic ester accounts for 27-55% of the mass of the strippable glue.
2. The peelable glue according to claim 1, wherein the peelable glue comprises, in mass%, 27-55% of aliphatic fluorinated polyurethane acrylate, 32-80% of functional monomer and 0.9-5.5% of photoinitiator.
3. The peelable glue of claim 1, further comprising at least one of a leveling agent, a pigment.
4. The peelable glue according to claim 3, wherein the peelable glue further comprises a leveling agent, a pigment; and the strippable glue comprises 27-55% of aliphatic fluorine-containing polyurethane acrylic ester, 32-80% of functional monomer, 0.9-5.5% of photoinitiator, 0.1-1.1% of flatting agent and 0.03-0.11% of pigment according to mass percentage.
5. The peelable glue according to claim 1, wherein the photoinitiator is selected from at least one of 1-hydroxycyclohexylphenyl ketone and 2- (4-methylbenzyl) -2- (dimethylamino) -1- (morpholinophenyl) -1-butanone.
6. The peelable glue according to claim 5, wherein the photoinitiator is 1-hydroxycyclohexyl phenyl ketone and 2- (4-methylbenzyl) -2- (dimethylamino) -1- (morpholinophenyl) -1-butanone; and the mass ratio of the 1-hydroxycyclohexyl phenyl ketone to the 2- (4-methylbenzyl) -2- (dimethylamino) -1- (morpholinophenyl) -1-butanone is 1:0.27-8.
7. The peelable glue according to claim 3, wherein the leveling agent comprises at least one of polyether modified dimethylsiloxane and acrylic leveling agent.
8. A method of preparing a peelable glue according to any one of claims 1 to 7, comprising the steps of:
and mixing the raw material components to obtain the strippable glue.
9. The method of preparing according to claim 8, comprising the steps of:
(1) Heating the aliphatic fluorine-containing polyurethane acrylate, and then adding part of functional monomers to obtain a first mixture;
(2) Mixing the rest raw material components and the first mixture obtained in the step (1) to obtain the strippable glue.
10. Use of the peelable glue according to any of claims 1-7 in the field of electronic products.
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| CN202311618935.1A CN117487485A (en) | 2023-11-30 | 2023-11-30 | Solvent-free strippable glue and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311618935.1A CN117487485A (en) | 2023-11-30 | 2023-11-30 | Solvent-free strippable glue and preparation method and application thereof |
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| CN (1) | CN117487485A (en) |
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