CN115433537B - High-cohesiveness ultraviolet light curing adhesive and preparation method and application thereof - Google Patents
High-cohesiveness ultraviolet light curing adhesive and preparation method and application thereof Download PDFInfo
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- CN115433537B CN115433537B CN202211120235.5A CN202211120235A CN115433537B CN 115433537 B CN115433537 B CN 115433537B CN 202211120235 A CN202211120235 A CN 202211120235A CN 115433537 B CN115433537 B CN 115433537B
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- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- 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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention provides a high-cohesiveness ultraviolet light curing adhesive, and a preparation method and application thereof. The ultraviolet light curing adhesive comprises 55-65 parts of light curing resin, 3-8 parts of tackifying resin, 5-15 parts of polymethyl methacrylate (PMMA) powder, 0.5-3 parts of gas-phase white carbon black, 5-10 parts of acrylic ester active monomer, 0.5-3 parts of coupling agent, 0.5-3 parts of defoaming agent, 0.3-1 part of flatting agent and 3-8 parts of photoinitiator. The invention also provides a preparation method of the adhesive. The adhesive disclosed by the invention is mainly improved in the aspects of adhesive force, high and low temperature change resistance, shrinkage rate and the like.
Description
Technical Field
The invention relates to an adhesive, in particular to an ultraviolet light curing adhesive with high cohesiveness and a preparation method thereof, and belongs to the technical field of adhesives.
Background
With the development of lightweight electronic products such as mobile phones, computers, cameras, etc., camera modules are becoming more precise and smaller. In the camera module, a plurality of components are bonded by using an adhesive, wherein the application of UV (ultraviolet) glue is particularly wide, and the UV glue is used for a plurality of glue points in the current camera module manufacturing.
The application of the UV adhesive on plastic substrates is very wide, and relates to the fields of electronic products, vehicle-mounted cameras of automobiles, cosmetic packaging materials and the like. The common plastic base material ABS, PC, ABS +PC alloy, PET, PMMA and the like. The adhesion is a focus of attention, especially the smaller and smaller components, the smaller and smaller amounts of glue, and the higher the requirements on aging resistance, the higher performance adhesives are urgently required.
Disclosure of Invention
In order to solve the technical difficulties commonly existing in the prior art. The invention aims to provide a high-performance UV adhesive with good adhesion, high temperature resistance, low shrinkage, low attenuation and the like after curing and a preparation method thereof.
In order to achieve the above purpose, the invention provides a high-cohesiveness ultraviolet light curing adhesive, which comprises the following raw materials in parts by weight:
55-65 parts of photo-curing resin, 3-8 parts of tackifying resin, 5-15 parts of polymethyl methacrylate PMMA slurry, 0.5-3 parts of gas phase white carbon black, 5-10 parts of acrylic ester active monomer, 3-8 parts of photoinitiator, 0.5-3 parts of coupling agent, 0.5-3 parts of defoaming agent and 0.3-1 part of leveling agent.
In the adhesive of the invention, the adopted photo-curing resin is prepared according to the following steps:
vacuum distilling phthalic anhydride polyester diol 2000 at 120-180 deg.c for 4-8 hr, and cooling to 50 deg.c to obtain purified phthalic anhydride polyester diol 2000;
mixing isophorone diisocyanate IPDI, dicyclohexylmethane diisocyanate HMDI and a catalyst, dropwise adding the purified phthalic anhydride polyester diol 2000 at room temperature, wherein-NCO is-OH=1-3:1, stirring, heating to 55-70 ℃ for reaction for 3-5h, measuring the-NCO content by a di-n-butylamine method, adding a mixed solution of hydroxyethyl methacrylate HEMA and hydroquinone polymerization inhibitor when the reaction reaches a metering point, reacting for 2h at 60-80 ℃, measuring the-NCO content by the di-n-butylamine method, cooling and discharging to obtain the photo-curing resin.
Wherein the mixing mass ratio of isophorone diisocyanate IPDI and dicyclohexylmethane diisocyanate HMDI is 4-8:1.
Wherein the catalyst is an organic bismuth catalyst, and the bismuth content is 20+/-0.5%.
In the adhesive, the polymethyl methacrylate PMMA slurry adopted is prepared according to the following steps:
stirring and mixing isobornyl acrylate and polymethyl methacrylate particles at 60-80 ℃ under stirring until the particles are completely dissolved, and changing the appearance into colorless/semitransparent resin liquid;
the resin liquid was subjected to three-roll grinding by a three-roll grinder and was ground with a minimum roll gap to obtain polymethyl methacrylate PMMA syrup of less than 3. Mu.m.
Wherein, the mixing mass ratio of the isobornyl acrylate to the polymethyl methacrylate particles is 50-100:50-100.
In the adhesive of the invention, the tackifying resin is at least one of rosin resin, hydrogenated rosin resin and terpene resin.
In the adhesive, the gas-phase white carbon black is at least one of hydrophobic gas-phase white carbon black with the particle size of 10-20 nm.
In the adhesive, the adopted acrylic ester active monomer is at least one of isooctyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, acryloylmorpholine, N-dimethylacrylamide, glycidyl methacrylate, 1, 6-hexanediol diacrylate and trimethylolpropane trimethacrylate.
In the adhesive of the invention, the coupling agent is at least one of the marks KH550, KH560, KH570 and KH 792.
In the adhesive, the defoaming agent is at least one of organic polymer and organic silicon resin. Wherein the organic polymer is polyether and polyacrylate; the organic silicon resin is polydimethylsiloxane and polysiloxane.
In the adhesive, the leveling agent is at least one of an organosilicon leveling agent, an acrylic ester leveling agent and a modified acrylic ester leveling agent.
In the adhesive, the photoinitiator is at least one of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholino-1-propanone, 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxy-cyclohexyl-phenyl ketone, 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinophenyl) butanone, benzoin dimethyl ketal and methyl benzoate.
In order to achieve the technical purpose, the invention also provides a preparation method of the high-cohesiveness ultraviolet light curing adhesive, which comprises the following steps:
mixing and stirring the photo-curing resin, polymethyl methacrylate PMMA slurry, acrylic ester active monomer and gas phase white carbon black for 0.5-2h;
adding a coupling agent, a defoaming agent and a leveling agent, and stirring for 0.5-2h;
adding a photoinitiator, vacuumizing to-0.1 MPa, and maintaining the pressure and stirring for 2-4 hours;
and (5) vacuum defoaming and discharging to obtain the ultraviolet-cured adhesive with high cohesiveness.
The high-cohesiveness ultraviolet light curing adhesive can be used for bonding electronic elements with camera grooves; in particular, the method comprises the steps of,
the high-cohesiveness ultraviolet light curing adhesive is coated/extruded and dispensed on the element, and the light reaction is carried out for 5-30 seconds to initiate the curing of the adhesive, so that the bonding of the electronic element is completed.
Wherein, the wave band of illumination is one or a mixture of wave bands of 200nm-760nm of a mercury lamp or a UV LED lamp. Specifically, the wave band of illumination is one or a mixture of wave bands of 250nm-500nm of a mercury lamp or a UV LED lamp; more specifically, the wave band of illumination is one or a mixture of wave bands of 300nm-405nm of mercury lamps or UV LED lamps.
The ultraviolet light curable adhesive is prepared by uniformly mixing a specific light curable resin (polyurethane acrylic ester) serving as a main resin, a tackifying resin, polymethyl methacrylate PMMA slurry filler, gas phase white carbon black, an acrylic ester active monomer, a photoinitiator, a coupling agent, a defoaming agent and a leveling agent, and can replace the existing imported UV adhesive of the type of Lobata and Delu. Meanwhile, under the condition of the same bonding effect, the adhesive provides ultraviolet light curing high bonding property through self-synthesis of polyurethane acrylic ester, and meanwhile, the synthetic resin is confirmed to have lower attenuation property on bonding force at high and low temperatures; thereby realizing the replacement of the existing partial UV glue.
According to the ultraviolet light curing adhesive, the influence of the resin on the attenuation of the adhesive force at high and low temperatures is reduced through the specific light curing resin, meanwhile, the shrinkage rate of the adhesive is reduced through polymethyl methacrylate (PMMA) slurry, and the prepared adhesive has good adhesive force, high temperature resistance, low shrinkage rate and low attenuation after curing.
The ultraviolet light curing adhesive can replace the existing imported UV adhesive with the model of the Letai and Delu part, and the service cycle of the UV adhesive is prolonged.
Detailed Description
The invention provides a high-cohesiveness ultraviolet light curing adhesive, which comprises the following components in parts by weight:
55-65 parts of photo-curing resin, 3-8 parts of tackifying resin, 5-15 parts of polymethyl methacrylate PMMA slurry, 0.5-3 parts of gas phase white carbon black, 5-10 parts of acrylic ester active monomer, 3-8 parts of photoinitiator, 0.5-3 parts of coupling agent, 0.5-3 parts of defoaming agent and 0.3-1 part of leveling agent.
In one embodiment of the present invention, the weight part of the photocurable resin is 55-65 parts. The specific parts by weight may be 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65 parts.
Specifically, the adopted photo-curing resin is prepared according to the following steps:
vacuum distilling phthalic anhydride polyester diol 2000 at 120-180 deg.c for 4-8 hr, and cooling to 50 deg.c to obtain purified phthalic anhydride polyester diol 2000;
mixing isophorone diisocyanate IPDI, dicyclohexylmethane diisocyanate HMDI and a catalyst (the total mass ratio is 0.1% -3%), dropwise adding the purified phthalic anhydride polyester diol 2000 at room temperature, wherein-NCO is-OH=1-3:1 (such as 1:1,1:2, 1:3), stirring, heating to 55-70 ℃ for reaction for 3-5h, measuring-NCO content by a di-n-butylamine method, adding a mixed solution of hydroxyethyl methacrylate HEMA (the total mass ratio is 3% -8%) and hydroquinone polymerization inhibitor (the total mass ratio is 0.05% -2%) when the mixed solution is reacted to a metering point, reacting for 2h at 60-80 ℃, measuring-NCO content by a di-n-butylamine method, measuring-NCO content to be less than 0.5%, cooling and discharging to obtain the photo-cured resin.
Wherein the mixing mass ratio of isophorone diisocyanate IPDI and dicyclohexylmethane diisocyanate HMDI is 4-8:1. Specifically, the mixing mass ratio of isophorone diisocyanate IPDI to dicyclohexylmethane diisocyanate HMDI may be 4:1,5:1,6:1,7:1,8:1.
Wherein the catalyst is an organic bismuth catalyst, and the bismuth content is 20+/-0.5%.
In one embodiment of the present invention, the weight part of the tackifying resin is 3 parts to 8 parts. In particular, it may be 4 parts, 5 parts, 6 parts, 7 parts or 8 parts.
Specifically, the tackifying resin is at least one of rosin resin, hydrogenated rosin resin and terpene resin.
In a specific embodiment of the invention, the polymethyl methacrylate PMMA syrup is 5-15 parts by weight. Specific polymethyl methacrylate PMMA syrup may contain 6, 7, 8, 9, 10, 11, 12, 13, 14, 15 parts by weight.
Specifically, polymethyl methacrylate PMMA syrup is prepared according to the following steps:
heating at 60deg.C-80deg.C (such as 65deg.C, 70deg.C, 75deg.C), mixing isobornyl acrylate with polymethyl methacrylate particles until the particles are completely dissolved, and changing into colorless/semitransparent resin liquid;
the resin liquid was subjected to three-roll grinding by a three-roll grinder and was ground with a minimum roll gap to obtain polymethyl methacrylate PMMA syrup of less than 3. Mu.m.
Wherein, the mixing mass ratio of the isobornyl acrylate to the polymethyl methacrylate particles is 50-100:50-100. For example, the mixing mass ratio may be 50:50, 50:60, 60:70, 70:80.
In one embodiment of the invention, the weight part of the fumed silica is 0.5-3 parts. Specific parts by weight may be 0.6, 0.7, 1, 1.1, 1.5, 1.8, 2.0, 2.1, 2.2, 2.5, 2.8, 3.0 parts.
Wherein the gas phase white carbon black is at least one of hydrophobic gas phase white carbon black with the particle size of 10-20 nm. For example, at least one of hydrophobic fumed silica with the particle size of 10-15nm is adopted; at least one of the hydrophobic fumed silica with the particle size of 15nm-20nm is adopted.
In one embodiment of the invention, the acrylate reactive monomer is 5 parts to 10 parts by weight. For example, the specific parts by weight are 6 parts, 7 parts, 8 parts, 9 parts and 10 parts.
Wherein the acrylic ester active monomer is at least one of isooctyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, acryloylmorpholine, N-dimethylacrylamide, glycidyl methacrylate, 1, 6-hexanediol diacrylate and trimethylolpropane trimethacrylate.
In one embodiment of the invention, the weight portion of the photoinitiator is 3-8. Wherein, the weight portions of the photoinitiator can be 4 portions, 5 portions, 6 portions, 7 portions and 8 portions.
Wherein the photoinitiator is at least one of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholino-1-propanone, 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxy-cyclohexyl-phenyl ketone, 2-phenylbenzyl-2-dimethyl amine-1- (4-morpholinophenyl) butanone, benzoin dimethyl ketal and methyl benzoate.
In one embodiment of the invention, the coupling agent is present in an amount of 0.5 parts to 3 parts by weight. The weight parts of the specific coupling agents can be 0.6, 0.7, 1, 1.1, 1.5, 1.8, 2.0, 2.1, 2.2, 2.5, 2.8, 3.0 parts.
Wherein the coupling agent is at least one of KH550, KH560, KH570 and KH 792.
In one embodiment of the invention, the defoamer is present in an amount of 0.5 parts to 3 parts by weight. The weight parts of the specific defoamer can be 0.6, 0.7, 1, 1.1, 1.5, 1.8, 2.0, 2.1, 2.2, 2.5, 2.8 and 3.0 parts.
The defoaming agent is at least one of organic polymer and organic silicon resin. Wherein the organic polymer is at least one of polyether and polyacrylate polymer; the organic silicon resin is at least one of polydimethylsiloxane and polysiloxane.
In one embodiment of the invention, the weight part of the leveling agent is 0.3-1 part. The weight parts of the specific leveling agent can be 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part and 0.9 part.
Wherein the leveling agent is at least one of an organosilicon leveling agent, an acrylic ester leveling agent and a modified acrylic ester leveling agent.
The invention also provides a preparation method of the high-cohesiveness ultraviolet light curing adhesive, which comprises the following steps:
mixing and stirring the photo-curing resin, polymethyl methacrylate PMMA slurry, acrylic ester active monomer and gas phase white carbon black for 0.5-2h;
adding a coupling agent, a defoaming agent and a leveling agent, and stirring for 0.5-2h;
adding a photoinitiator, vacuumizing to-0.1 MPa, and maintaining the pressure and stirring for 2-4 hours;
and (5) vacuum defoaming and discharging to obtain the ultraviolet-cured adhesive with high cohesiveness.
The high-cohesiveness ultraviolet light curing adhesive can be used for bonding electronic elements with camera grooves; in particular, the method comprises the steps of,
the high-cohesiveness ultraviolet light curing adhesive is coated/extruded and dispensed on the element, and the light reaction is carried out for 5-30 seconds to initiate the curing of the adhesive, so that the bonding of the electronic element is completed.
Wherein, the wave band of illumination is one or a mixture of wave bands of 200nm-760nm of a mercury lamp or a UV LED lamp. Specifically, the wave band of illumination is one or a mixture of wave bands of 250nm-500nm of a mercury lamp or a UV LED lamp; more specifically, the wave band of illumination is one or a mixture of wave bands of 300nm-405nm of mercury lamps or UV LED lamps.
The following detailed description of the preferred embodiments of the present invention will be provided in connection with.
The raw materials used in the following examples are all commercially available general-purpose materials unless otherwise specified.
Example 1
The embodiment provides a high-cohesiveness ultraviolet light curing adhesive, which comprises the following components in parts by weight: 65 parts of photo-curing resin, 10 parts of polymethyl methacrylate PMMA slurry, 5 parts of tackifying resin, 2 parts of gas phase white carbon black, 7 parts of acrylic ester active monomer, 0.5 part of coupling agent, 1.5 parts of defoamer, 1 part of flatting agent and 8 parts of photoinitiator.
The tackifying resin is as follows: 5 parts of hydrogenated rosin resin. The gas phase white carbon black is 2 parts of hydrophobic gas phase white carbon black with the particle size of 15 nm. The acrylic ester active monomer comprises the following components in parts by weight: 5 parts of isobornyl acrylate and 2 parts of acryloylmorpholine. The defoamer is polyacrylate defoamer 1.5 parts. The leveling agent is 1 part of acrylic leveling agent. The coupling agent is KH550 coupling agent 0.5 parts. The photoinitiator consists of the following components in parts by weight: 3 parts of 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinophenyl) butanone and 5 parts of 1-hydroxy-cyclohexyl-phenyl methanone.
The light-cured resin is self-synthesized polyurethane acrylic ester, and the synthesis process comprises the following steps:
adding phthalic anhydride polyester diol 2000 into a three-mouth bottle, distilling under reduced pressure for 8h under 120 ℃ to obtain purified phthalic anhydride polyester diol 2000, and uniformly mixing for later use; adding metered mixed solution of isophorone diisocyanate IPDI/dicyclohexylmethane diisocyanate HMDI (mixing ratio 4:1) and catalyst organobismuth (bismuth content: 20+/-0.5%) (total mass ratio 0.1% -3%) into a three-port bottle with a stirrer, a constant pressure dropping funnel and a thermometer, slowly dropping the mixed solution (wherein-NCO is-OH=2:1) at room temperature, mechanically stirring, heating to 65 ℃ for reaction for 3 hours, measuring-NCO content by a di-n-butylamine method, adding a certain amount of mixed solution of hydroxyethyl methacrylate HEMA (total mass ratio 3% -8%) and a polymerization inhibitor (total mass ratio 0.05% -2%) when the reaction is at the metering point, reacting for 2 hours at 80 ℃, measuring-NCO content again by a di-n-butylamine method, obtaining the required content (-NCO content is less than 0.5%), cooling and discharging, and writing the number and keeping in dark place.
Wherein, the process of self-prepared polymethacrylate slurry comprises the following steps:
isobornyl acrylate: the mixing mass ratio of the polymethyl methacrylate particles is 50:50;
heating, stirring and mixing at 60-80 ℃ under the stirring of a stirrer; until the particles are completely dissolved, the appearance becomes colorless/semitransparent resin liquid; pouring out the resin liquid, and performing roller passing three times by a three-roller grinder, and grinding by using a minimum roller gap; finally, the particle size is tested by a scraper, and no regrinding is needed when the particle size is smaller than 3 mu m, and the number is filled for standby.
The preparation method of the ultraviolet light curing adhesive in the embodiment comprises the following steps of:
s1, putting light-cured resin, polymethyl methacrylate PMMA slurry, tackifying resin and gas-phase white carbon black with preset weights and acrylate active monomers into a planetary stirrer, and mixing and stirring for 0.5-2h;
s2, adding a coupling agent, a defoaming agent and a leveling agent in a set proportion, and stirring for 0.5-2h;
s3, putting the photoinitiator into a planetary mixer, vacuumizing to-0.1 MPa, and maintaining the pressure for stirring for 2 hours; then defoaming and discharging are carried out through vacuum;
and S4, extruding the adhesive to be dispensed on the element, and then placing the element in a photo-curing machine to perform illumination reaction for 5 seconds to initiate curing of the adhesive, so as to obtain the ultraviolet curing adhesive with high cohesiveness.
The ultraviolet curing light source can adopt 1000W medium pressure mercury lamp with light intensity of 80mw/cm 2 The effective optical radiation center wavelength is 365nm.
Example 2
The embodiment provides a high-cohesiveness ultraviolet light curing adhesive, which comprises the following components in parts by weight: 60 parts of photo-curing resin, 10 parts of polymethyl methacrylate PMMA slurry, 8 parts of tackifying resin, 2.5 parts of gas phase white carbon black, 10 parts of acrylic ester active monomer, 1 part of coupling agent, 2 parts of defoamer, 0.5 part of flatting agent and 6 parts of photoinitiator.
Wherein the photo-curing resin is 60 parts of self-synthesized polyurethane acrylic ester; 10 parts of polymethyl methacrylate PMMA slurry; the tackifying resin is as follows: 3 parts of rosin and 5 parts of terpene resin; 2.5 parts of hydrophobic gas-phase white carbon black with the particle size of 10 nm; the acrylic ester active monomer comprises the following components in parts by weight: 2 parts of isobornyl acrylate, 3 parts of glycidyl methacrylate and 5 parts of N, N-dimethylacrylamide; the leveling agent is 0.5 part of modified acrylic ester leveling agent; the coupling agent is 1 part of KH792 coupling agent; the defoaming agent is polysiloxane defoaming agent 2 parts; the photoinitiator consists of the following components in parts by weight: benzoin dimethyl ketal 1.5 parts and methyl benzoate 4.5 parts.
The preparation method of the uv curable adhesive of this embodiment is the same as that of embodiment 1, and will not be described in detail here.
Example 3
The embodiment provides a high-cohesiveness ultraviolet light curing adhesive, which comprises the following components in parts by weight: 55 parts of photo-curing resin, 15 parts of polymethyl methacrylate PMMA slurry, 8 parts of tackifying resin, 3 parts of gas phase white carbon black, 10 parts of acrylic ester active monomer, 2 parts of coupling agent, 1 part of defoamer, 1 part of flatting agent and 5 parts of photoinitiator.
Wherein the photo-curing resin is 55 parts of self-synthesized polyurethane acrylic ester; 15 parts of polymethyl methacrylate (PMMA) slurry; the tackifying resin is as follows: 3 parts of hydrogenated rosin resin and 5 parts of terpene resin; the gas-phase white carbon black is 3 parts of hydrophobic gas-phase white carbon black with the particle size of 10 nm; the acrylic ester active monomer comprises the following components in parts by weight: 3 parts of glycidyl methacrylate and 7 parts of N, N-dimethylacrylamide; the leveling agent is 1 part of modified acrylic ester leveling agent; the coupling agent comprises 1 part of KH570 coupling agent and 1 part of KH792 coupling agent; the defoaming agent is 1 part of polysiloxane defoaming agent; the photoinitiator consists of the following components in parts by weight: 2 parts of benzoin dimethyl ketal and 3 parts of methyl benzoyl formate.
The preparation method of the uv curable adhesive of this embodiment is the same as that of embodiment 1, and will not be described in detail here.
Example 4
The preparation method of the ultraviolet light curing adhesive of the embodiment is the same as that of embodiment 1 except that the ultraviolet light curing adhesive adopts a UV LED lamp for illumination, and detailed description thereof is omitted.
Comparative example 1
The formulation of the uv curable adhesive of this comparative example differs from that of example 1 only in the outsourced urethane acrylate (synthesized from phthalic anhydride polyester diol 1000).
Comparative example 2
The formulation of the uv curable adhesive of this comparative example differs from that of example 1 only in the outsourced urethane acrylate (synthesized from phthalic anhydride polyester diol 3000).
Comparative example 3
The formulation of the uv curable adhesive of this comparative example was different from that of example 1 only in that polymethyl methacrylate PMMA syrup was not added to this comparative example.
Comparative example 4
The formulation of the uv curable adhesive of this comparative example was different from that of example 1 only in that no tackifying resin was added to this comparative example.
Comparative example 5
The formulation of the uv curable adhesive of this comparative example was different from that of example 1 only in that the self-synthesized urethane acrylate was increased to 70 parts.
Comparative example 6
The formulation of the uv curable adhesive of this comparative example was different from that of example 1 only in that the ratio of the self-synthesized polymethyl methacrylate PMMA syrup was increased to 20 parts.
Comparative example 7
The formulation of the uv curable adhesive in this comparative example is different from that in example 1 in that:
70 parts of photo-curing resin, 10 parts of tackifying resin, 3 parts of polymethyl methacrylate PMMA slurry, 0.5 part of gas phase white carbon black, 15 parts of acrylic ester active monomer, 2 parts of photoinitiator, 4 parts of coupling agent, 4 parts of defoaming agent and 4 parts of leveling agent.
Example 5
The cured products of examples 1-4 and comparative examples 1-7, and of the prior art, specifically model le tai AA3311, were subjected to shear force, volume shrinkage, water absorption, solvent soak resistance, and high and low temperature cycle aging resistance tests as follows:
shear strength test: according to the measurement standard of GB/T7124-2008 adhesive tensile shear strength.
Volume shrinkage test: measured according to the GB/T15585 method.
Solvent resistance: and (3) curing the adhesive on the PC sheet, putting the PC sheet into an isopropanol solvent, soaking for 72 hours, and observing whether the PC sheet falls off. The test results are shown in Table 1.
TABLE 1
| Group of performance parameters | Shear Strength/MPa (glass)&PC） | Volume shrinkage/% | Water absorption/% | Solvent resistance h | High and low temperature cycle aging test/appearance | High and low temperature cyclic aging resistance 500h test/shear strength/MPa |
| Example 1 | 5.6 | 0.6 | 0.8 | 72 | No cracking | 5.3 |
| Example 2 | 5.8 | 0.6 | 0.9 | 72 | No cracking | 5.3 |
| Example 3 | 5.8 | 0.4 | 0.8 | 72 | No cracking | 5.2 |
| Example 4 | 6.2 | 0.5 | 0.9 | 72 | No cracking | 5.5 |
| Comparative example 1 | 3.2 | 1.5 | 1.2 | 72 | No cracking | 2.1 |
| Comparative example 2 | 4.8 | 1.8 | 1.3 | 72 | No cracking | 2.5 |
| Comparative example 3 | 4.5 | 3.3 | 0.9 | 72 | No cracking | 4 |
| Comparative example 4 | 3.6 | 1.1 | 0.6 | 72 | No cracking | 3.2 |
| Comparative example 5 | 7.3 | 3.1 | 1.2 | 168 | Cracking of | 6.5 |
| Comparative example 6 | 4.2 | 0.3 | 0.5 | 72 | No cracking | 2.2 |
| Comparative example 7 | 6.5 | 2 | 0.9 | 168 | No cracking | 5 |
| Letai AA3311 | 3 | 3.3 | 5.36 | 24 | No cracking | 1.5 |
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (10)
1. The raw material composition of the adhesive of the high-cohesiveness ultraviolet light curing agent comprises the following components in parts by weight:
55-65 parts of photo-curing resin, 3-8 parts of tackifying resin, 5-15 parts of polymethyl methacrylate (PMMA) slurry, 0.5-3 parts of gas-phase white carbon black, 5-10 parts of acrylic ester active monomer, 3-8 parts of photoinitiator, 0.5-3 parts of coupling agent, 0.5-3 parts of defoaming agent and 0.3-1 part of flatting agent;
the photo-curing resin is prepared according to the following steps:
vacuum distilling phthalic anhydride polyester diol 2000 at 120-180 deg.c for 4-8 hr, and cooling to 50 deg.c to obtain purified phthalic anhydride polyester diol 2000;
mixing isophorone diisocyanate IPDI, dicyclohexylmethane diisocyanate HMDI and a catalyst, dropwise adding the purified phthalic anhydride polyester diol 2000 at room temperature, wherein-NCO is-OH=1-3:1, stirring, heating to 55-70 ℃ for reaction for 3-5h, measuring the-NCO content by a di-n-butylamine method, adding a mixed solution of hydroxyethyl methacrylate HEMA and hydroquinone polymerization inhibitor when the reaction reaches a metering point, reacting for 2h at 60-80 ℃, measuring the-NCO content by the di-n-butylamine method, cooling and discharging to obtain the photo-curing resin;
the polymethyl methacrylate PMMA slurry is prepared by the following steps:
stirring and mixing isobornyl acrylate and polymethyl methacrylate particles at the temperature of 60-80 ℃ until the particles are completely dissolved and the appearance of the particles becomes colorless/semitransparent resin liquid;
carrying out three-roller grinding on the resin liquid for three times by a three-roller grinder to obtain polymethyl methacrylate PMMA slurry smaller than 3 mu m;
the isobornyl acrylate: the mixing mass ratio of the polymethyl methacrylate particles is 50-100:50-100.
2. The high-cohesiveness ultraviolet light curing adhesive according to claim 1, wherein the mixing mass ratio of isophorone diisocyanate IPDI and dicyclohexylmethane diisocyanate HMDI is 4-8:1; the catalyst is an organic bismuth catalyst, wherein the bismuth content is 20+/-0.5%.
3. The high-adhesion uv-curable adhesive according to claim 1, wherein the tackifying resin is at least one of a rosin resin, a hydrogenated rosin resin, a terpene resin;
the gas phase white carbon black is hydrophobic gas phase white carbon black with the particle size of 10-20 nm.
4. The high-adhesion uv-curable adhesive according to claim 1, wherein the acrylate-reactive monomer is at least one of isooctyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, acryloylmorpholine, N-dimethylacrylamide, glycidyl methacrylate, 1, 6-hexanediol diacrylate, trimethylolpropane trimethacrylate.
5. The high-adhesion uv-curable adhesive according to claim 1, wherein the coupling agent is at least one of the brands KH550, KH560, KH570 and KH 792;
the defoaming agent is at least one of polyether, polyacrylate and polysiloxane.
6. The high-cohesiveness ultraviolet light curing adhesive of claim 1, wherein the leveling agent is at least one of an organosilicon leveling agent, an acrylic leveling agent and a modified acrylic leveling agent;
the photoinitiator is at least one of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone, 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxy-cyclohexyl-phenyl ketone, 2-phenylbenzyl-2-dimethyl amine-1- (4-morpholinylphenyl) butanone, benzoin dimethyl ketal and methyl benzoyl formate.
7. The method for preparing the high-cohesiveness ultraviolet light curing adhesive of any one of claims 1 to 6, comprising the steps of:
mixing and stirring the photo-curing resin, polymethyl methacrylate (PMMA) slurry, tackifying resin, acrylic ester active monomer and gas phase white carbon black for 0.5-2h;
adding a coupling agent, a defoaming agent and a leveling agent, and stirring for 0.5-2h;
adding a photoinitiator, vacuumizing to-0.1 MPa, and maintaining the pressure and stirring for 2-4 hours;
and (3) vacuum defoaming and discharging to obtain the high-cohesiveness ultraviolet light curing adhesive.
8. The use of the high-adhesion uv-curable adhesive according to any one of claims 1 to 6 for bonding electronic components in camera cavities.
9. The use of the uv curable adhesive of claim 8, wherein the adhesive is cured by applying/extruding a spot-on-component, light-curing for 5-30 seconds, and completing the bonding of the electronic component.
10. The use of the high-adhesion UV-curable adhesive according to claim 9, wherein the light is applied in one or more of the wavelength bands of 200nm to 760nm of mercury lamp or UV LED lamp.
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