CN110041876A - A kind of ultraviolet cured adhesive sticks agent and preparation method and application - Google Patents
A kind of ultraviolet cured adhesive sticks agent and preparation method and application Download PDFInfo
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- CN110041876A CN110041876A CN201910264777.1A CN201910264777A CN110041876A CN 110041876 A CN110041876 A CN 110041876A CN 201910264777 A CN201910264777 A CN 201910264777A CN 110041876 A CN110041876 A CN 110041876A
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- carbon black
- acrylate
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- ultraviolet cured
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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
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
- C09J167/06—Unsaturated polyesters having carbon-to-carbon unsaturation
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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
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of ultraviolet cured adhesives to stick agent and preparation method thereof, and adhesive comprises the following components in parts by weight: 40~55 parts of light-cured resin, 40~50 parts of acrylate reactive monomer, 3~10 parts of photoinitiator, 0.5~8 part of carbon black；Solidification is irradiated using mercury lamp or UV LED light 250~760nm wave band light source in adhesive preparation process of the present invention.Low-transmittance ultra-violet curing gluing agent prepared by the present invention, at 270~800nm of wavelength, light transmittance < 0.1%, suitable for the leakproofs optical element fast packing such as comprehensive display screen frame, phtographic lens, mobile phone, with rapid curing, high light-proofness, low water absorption, the advantages that good bonding force is the high shading efficiency material of environment-friendly type.
Description
Technical field
The present invention relates to adhesive technology field, it is specifically related to a kind of ultraviolet cured adhesive and sticks agent and preparation method and answer
With.
Background technique
Application of the adhesive in electronics industry also requires thermally conductive, conductive, insulation, and fit other than being mechanically fixed
Shock resistance assembly, encapsulation and protection substrate etc. is answered to require.With the development of science and technology mobile phone and plate, television set enter screen comprehensively
In the epoch, electronic apparatus frame is narrower, fuselage is thinner, weight is lighter under comprehensive screen trend, therefore proposes higher want to adhesive
It asks, in order to reach beautiful requirement, frame design is more and more narrow, and every Testing index has been not achieved in conventional rubber sheet gasket, RTV
It is required that needing to research and develop the adhesive product of requirements at the higher level.
Summary of the invention
In order to overcome in the prior art rubber sheet gasket do not have bonding force, in an assembling process be easy slide, gasket size meeting
Cover the display of screen, RTV curing time is long, releases low molecule influences display screen, while solving that frame is narrow to be may cause
The defects of light leakage occurs for backlight, the present invention provides a kind of ultraviolet rapid curing, made by treated carbon black the light-proofness of colloid it is high,
With good bonding power low-transmittance (under 270~800nm wavelength, light transmittance be equal to or less than 0.1%) adhesive and its
Preparation method.
To achieve the above object, the technical solution adopted by the present invention is that a kind of ultraviolet cured adhesive sticks agent, including it is following heavy
Measure the component of part: 40~55 parts of light-cured resin, 40~50 parts of acrylate reactive monomer, 3~10 parts of photoinitiator, carbon black
0.5~8 part.
The present invention is using carbon black as colorant, and by the partial size of preferred carbon black, process is modified, can achieve compared with thin and thick
Degree is lower to realize low-transmittance, high adhesiveness, and placing carbon black for a long time will not reunite；By preferred photoinitiator, in different ratio
Under, low energy solidification realizes that colloid cured thickness is thicker (0.4mm), high adhesiveness.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, the light-cured resin is polyurethane acroleic acid
At least one of ester, epoxy acrylate, polyester acrylate.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, the acrylate reactive monomer is acrylic acid
Different monooctyl ester, isobornyl acrylate, hydroxy-ethyl acrylate, 2- phenoxyethyl acrylate, ring trimethylolpropane dimethoxym ethane
Acrylate, acrylic acid tetrahydrofuran ester, lauryl acrylate, 1,6 hexanediol diacrylate, bis- propylene of ethoxylated bisphenol A
At least one of acid esters, pentaerythritol triacrylate, trimethylol-propane trimethacrylate.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, the photoinitiator is 2- methyl-1-[4-
(methyl mercapto) phenyl] -2- morpholinyl -1- acetone, 2,4,6- trimethylbenzoy-dipheny phosphorous oxide, 2- hydroxyl -2- first
Base -1- phenyl -1- acetone, 1- hydroxy-cyclohexyl-phenyl ketone, 2- phenyl benzyl -2- dimethyl amine -1- (4- morpholine benzyl phenyl)
At least one of bis- (2,4,6- trimethylbenzoyl) phosphine oxides of butanone, phenyl.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, the carbon black is the one of partial size 5nm~100 μm
Kind or the mixed and modified carbon black of a variety of different-grain diameters.For the present invention by the partial size of preferred carbon black, process is modified, can achieve compared with
Low-transmittance, high adhesiveness are realized under thin thickness, placing carbon black for a long time will not reunite.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, particle size carbon black is 5nm~50 μm, it is preferable that
15nm~50 μm；The carbon black is 1 to 6 parts by weight, more preferably 2 to 4 parts by weight.Present inventor's discovery, when
The carbon black is at 15nm~50 μm, more low-transmittance, high adhesiveness, and placing carbon black for a long time will not reunite.
The preferred embodiment of agent is sticked as ultraviolet cured adhesive of the present invention, the processing of the modified carbon black includes following step
It is rapid:
1) surface clean of carbon black: the untreated charcoal for taking one or more different-grain diameters of partial size 5nm~100 μm to mix
Black, 300g zirconia ball (partial size 1mm/3mm/10mm, ratio 5:3:2) is added 7000 in carbon black and dehydrated alcohol ratio 5:200
2~6h of grinding point under~20000 turns/s revolving speed adds 1000g80 DEG C of deionized water stirring 30min, after carbon black settles 3h,
The mixed liquor of upper layer alcohol and water is sucked out, in triplicate the above washing step；
2) carbon black surface monomer cladding: obtaining step 1) carbon black, be added 500g dehydrated alcohol, be put into ultrasonic cleaning
In machine, ultrasonic disperse simultaneously stirs 20~40min, and DPGDA monomer is then added dropwise, and speed control is in 10g/min, after being added dropwise,
Continue 1.5~3h of ultrasonic disperse；
3) drying of modified carbon black: taking above-mentioned dispersion liquid, heats 75~85 DEG C, with negative 0.9MPa take out dehydrated alcohol and
Obtained powder is put into 100 DEG C of oven drying 1h by water, and the treated carbon black handled well is made.
The present invention reaches higher obscurity and OD value, carbon black is carried out to allow carbon black sufficiently to colour and disperse
It is modified, meanwhile, the present invention, as carrier, does not need dispersing agent using acrylic monomers.
The disadvantages of present invention improves carbon black particle partial size is small, large specific surface area, surface can be high, is easy to happen reunion, benefit
With ultrasonic wave dispersion, make surface with acrylate monomer cladding and be modified, reduces surfactant use, simultaneously as partial size
Selection, improve light-proofness, cementability and curing depth.
The present invention also provides the preparation methods that the ultraviolet cured adhesive described in one kind sticks agent, comprising the following steps:
S1. by light-cured resin, acrylate reactive monomer is put into planetary mixer, and 0.5~2h is mixed；
S2. processed carbon black is added, stirs 2~5h；
S3. by uniformly mixed glue, investment ball mill carries out 3~6h of ball milling；
S4. by the glue after ball milling, planet machine is refunded, photoinitiator is added, stirs 1~2h, then vacuum defoaming, discharging；
S5. it then by the glue by dispenser, puts on electronic component, is subsequently placed in photo solidification machine and carries out illumination reaction 10
~150 seconds to get.
The preferred embodiment that the preparation method of agent is sticked as ultraviolet cured adhesive of the present invention, in the step S5, illumination
Wave band is 200~760nm of mercury lamp or UV LED light, it is preferable that is 250~500nm, it is highly preferred that in 250~405nm one
Kind or the mixing of several wave bands.
It is anti-that ultra-violet curing gluing agent provided by the invention can be used for comprehensive display screen frame encapsulation, phtographic lens, mobile phone etc.
On light leakage element.
Beneficial effects of the present invention:
(1) present invention does not need to carry out long-time room temperature curing, saves the time and improves production capacity；
(2) defect that small molecule is precipitated in moisture-curable process by RTV is eliminated, is reduced bad to display screen generation anti-
It answers；
(3) it is small to solve rubber sheet gasket bonding force, the problem of being easy to fall off；
(4) because of its high light-proofness, the problem of relatively thin thickness just can solve light leakage, weight is reduced relative to thermosol
Amount adapts to trend frivolous at present, and electronic workpiece will not be caused to destroy because of temperature height；
(5) dispersion of carbon black does not need dispersing agent using acrylic monomers as carrier.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Each raw material involved by following embodiment is commercially available versatile material unless otherwise instructed.
The present invention reaches higher obscurity and OD value, carbon black is carried out to allow carbon black sufficiently to colour and disperse
Following processing:
1) surface clean of carbon black: the untreated charcoal for taking one or more different-grain diameters of partial size 5nm~100 μm to mix
Black, 300g zirconia ball (partial size 1mm/3mm/10mm, ratio 5:3:2) is added 7000 in carbon black and dehydrated alcohol ratio 5:200
2~6h of grinding point under~20000 turns/s revolving speed adds 1000g80 DEG C of deionized water stirring 30min, after carbon black settles 3h,
The mixed liquor of upper layer alcohol and water is sucked out, in triplicate the above washing step；
2) carbon black surface monomer cladding: obtaining step 1) carbon black, be added 500g dehydrated alcohol, be put into ultrasonic cleaning
In machine, ultrasonic disperse simultaneously stirs 20~40min, and DPGDA monomer is then added dropwise, and speed control is in 10g/min, after being added dropwise,
Continue 1.5~3h of ultrasonic disperse；
3) drying of modified carbon black: taking above-mentioned dispersion liquid, heats 80 DEG C, takes out dehydrated alcohol and water with negative 0.9MPa,
Obtained powder puts 100 DEG C of oven drying 1h into, and the treated carbon black handled well is made.
Embodiment 1
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 50 parts of urethane acrylate, 20 parts of isobornyl acrylate, Isooctyl acrylate monomer
15 parts, 8 parts of 1,6 hexanediol diacrylate, 0.3 part of partial size 15nm modified carbon black, 3 μm of partial size, 0.7 part of modified carbon black, 2- benzene
4 parts of 2 parts of base benzyl -2- dimethyl amine -1- (4- morpholine benzyl phenyl) butanone and 1- hydroxy-cyclohexyl-phenyl ketone.
Wherein, the light-cured resin of the present embodiment is urethane acrylate；Acrylate reactive monomer is that acrylic acid is different
Norbornene ester, Isooctyl acrylate monomer, 1,6 hexanediol diacrylate；Photoinitiator is 2- phenyl benzyl -2- dimethyl amine -1- (4-
Morpholine benzyl phenyl) butanone and 1- hydroxy-cyclohexyl-phenyl ketone.
At ambient temperature and pressure, in yellow light lamp room or under shading environment, the ultraviolet cured adhesive of the present embodiment sticks the system of agent
Preparation Method, comprising the following steps:
S1. light curing agent, acrylic acid activated monomer are added in reaction vessel, 20~40 DEG C of temperature control planetary mixer
Mix 0.5~2h；
S2. processed carbon black is added, stirs 2~5h；
S3. by uniformly mixed glue, investment is containing there are three types of the ball mills of the zirconia ball of different size partial size to carry out ball milling 3
~6h, wherein the partial size of zirconia ball is 1mm, 3mm, 10mm respectively, and the ratio of three kinds of partial sizes is 6:3:1 respectively, and zirconium ball adds
Enter 10% that amount is glue；
S4. by the glue after ball milling, planet machine is refunded, photoinitiator is added, stirs 1~2h, then vacuum defoaming, discharging；
S5. then by the glue by dispenser, 0.1~0.2mm of dispensing on electronic workpiece dispensing position is subsequently placed in light
Curing carry out illumination reaction 10-150s to get.
The medium pressure mercury lamp of 1000W, light intensity 80mw/cm can be used in ultra-violet curing light source2, photosynthetic active radiation central wavelength exists
365nm。
Embodiment 2
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, 2- Phenoxyethyl third
22 parts of olefin(e) acid ester, 16 parts of ring trimethylolpropane dimethoxym ethane acrylate, 8 parts of Isooctyl acrylate monomer, partial size are 7nm modified carbon black
0.5 part, 3.5 parts of 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone 2
Part.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate；Acrylate reactive list
Body is 2- phenoxyethyl acrylate, ring trimethylolpropane dimethoxym ethane acrylate, Isooctyl acrylate monomer；Photoinitiator is
2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Embodiment 3
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 40 parts of polyester acrylate, 40 parts of hydroxy-ethyl acrylate, partial size are 5nm Modified Activated Carbon
Black 8 parts, 2 parts of 2,4,6- trimethylbenzoy-dipheny phosphorous oxide, 2 parts of 2- hydroxy-2-methyl -1- phenyl -1- acetone, benzene
2 parts of phosphine oxide of base bis- (2,4,6- trimethylbenzoyls).
Wherein, the light-cured resin of the present embodiment is polyester acrylate；Acrylate reactive monomer is acrylic acid hydroxyl second
Ester；Photoinitiator is 2,4,6- trimethylbenzoy-dipheny phosphorous oxide, 2- hydroxy-2-methyl -1- phenyl -1- acetone, benzene
Bis- (2,4,6- trimethylbenzoyl) phosphine oxides of base.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Embodiment 4
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 20 parts of urethane acrylate, 15 parts of epoxy acrylate, polyester acrylate 20
Part, 22 parts of acrylic acid tetrahydrofuran ester, 20 parts of lauryl acrylate, 8 parts of ethoxylated bisphenol A diacrylate, partial size 15nm
0.3 part of modified carbon black, 100 μm of partial size, 0.7 part of carbon black, 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone 10
Part.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate, polyester acrylate；
Acrylate reactive monomer is acrylic acid tetrahydrofuran ester, lauryl acrylate, ethoxylated bisphenol A diacrylate；It is light-initiated
Agent is 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Embodiment 5
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, 2- Phenoxyethyl third
22 parts of olefin(e) acid ester, 16 parts of ring trimethylolpropane dimethoxym ethane acrylate, 8 parts of Isooctyl acrylate monomer, partial size are 7nm modified carbon black
0.5 part, 3.5 parts of 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone 2
Part.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate；Acrylate reactive list
Body is 2- phenoxyethyl acrylate, ring trimethylolpropane dimethoxym ethane acrylate, Isooctyl acrylate monomer；Photoinitiator is
2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Embodiment 6
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, three propylene of pentaerythrite
22 parts of acid esters, 25 parts of trimethylol-propane trimethacrylate, partial size are 0.5 part of 7nm modified carbon black, 2- methyl-1-[4-
(methyl mercapto) phenyl] 2 parts of 3.5 parts of -2- morpholinyl -1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate；Acrylate reactive list
Body is pentaerythritol triacrylate, trimethylol-propane trimethacrylate；Photoinitiator is 2- methyl-1-[4- (first sulphur
Base) phenyl] -2- morpholinyl -1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Comparative example 1
The ultraviolet cured adhesive of this comparative example sticks the embodiment of agent, and it includes following parts by weight that the ultraviolet cured adhesive, which sticks agent,
Component: 20 parts of urethane acrylate, 10 parts of epoxy acrylate, 30 parts of pentaerythritol triacrylate, trihydroxy methyl third
30 parts of alkane trimethyl acrylic ester, partial size are 0.5 part of 7nm carbon black, 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1-
2 parts of 3.5 parts of acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate；Acrylate reactive list
Body is pentaerythritol triacrylate, trimethylol-propane trimethacrylate；Photoinitiator is 2- methyl-1-[4- (first sulphur
Base) phenyl] -2- morpholinyl -1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
The preparation method that the ultraviolet cured adhesive of the present embodiment sticks agent is same as Example 1, is not described in detail herein.
Comparative example 2
The embodiment of agent, the ultraviolet light solidification are sticked as a kind of ultraviolet cured adhesive with low-transmittance of the invention
Adhesive comprises the following components in parts by weight: 40 parts of urethane acrylate, 20 parts of epoxy acrylate, 2- Phenoxyethyl third
20 parts of olefin(e) acid ester, 15 parts of ring trimethylolpropane dimethoxym ethane acrylate, 8 parts of Isooctyl acrylate monomer, partial size are 7nm modified carbon black
0.5 part, 1.5 parts of 2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone 1
Part.
Wherein, the light-cured resin of the present embodiment is urethane acrylate, epoxy acrylate；Acrylate reactive list
Body is 2- phenoxyethyl acrylate, ring trimethylolpropane dimethoxym ethane acrylate, Isooctyl acrylate monomer；Photoinitiator is
2- methyl-1-[4- (methyl mercapto) phenyl]-2- morpholinyl-1- acetone and 1- hydroxy-cyclohexyl-phenyl ketone.
The ultraviolet cured adhesive of the present embodiment sticks the preparation method of agent in addition to illumination is using UV LED light, other with implementation
Example 1 is identical, is not described in detail herein.
Comparative example 3
This comparative example is only that carbon black used is unmodified carbon black with the difference of embodiment 1.
Embodiment 7
The cured product of Examples 1 to 6 and comparative example 1, control group (prior art) is subjected to glass & glass, poly- carbon
The shear strength of acid esters PC& polycarbonate and obtained size length and width 5cm*5cm prototype test wavelength 270nm-800nm are saturating
Light rate, curing time, cured thickness, rate of perviousness, cementability performance test, test method are as follows:
Glass & glass shear strength: using UV mercury lamp/LED, by colloid solidification (colloid thickness between glass-glass
0.15mm), shear strength test is carried out immediately；Testing standard: GB/T7124；
The shear strength of polycarbonate & polycarbonate: using UV mercury lamp/LED, by colloid solidification between PC-PC
(colloid thickness 0.15mm), carries out shear strength test immediately；Testing standard: GB/T7124；
Light transmittance: being solidified into size length and width 5cm*5cm print for colloid, is then surveyed by optical lens refractoscope (LH1013)
Try wavelength 270nm-800nm light transmittance；
Rate of perviousness: after colloid solidification, 38 DEG C/90% humidity is placed；Testing standard: GB/T16928；
Cementability: colloid is solidificated on glass, is put into 85 DEG C of 85% humidity, confirms whether colloid has out after 1000h
It splits, degumming.
Test result is as shown in table 1:
Table 1
As can be seen from Table 1, the embodiment of the present invention 1~6 is prepared ultraviolet cured adhesive sticks agent, wavelength 270~
Under 800nm, light transmittance is respectively less than 0.1%, and it is quick to be suitable for the leakproofs optical elements such as comprehensive display screen frame, phtographic lens, mobile phone
Encapsulation, curing time is short, shear strength is high, rate of perviousness is low, has rapid curing, high light-proofness, low water absorption, good bonding
The advantages that power, is the high shading efficiency material of environment-friendly type, has a good application prospect.Wherein, comparative example 1~2 and embodiment 1
It compares, not within the scope of the present invention, as can be known from the results, performance slightly declines constituent part content compared with the present invention,
In the case of showing only while meeting specific ingredient and specific content, properties be can be only achieved most preferably；Comparative example 3
Using unmodified carbon black, curing time, transmitance is higher than the present invention, its shear strength is low, rate of perviousness is high, shows the present invention
The use of modified carbon black be conducive to improve light-proofness, cementability and curing depth, low light transmission performance；And control group is using commercially available
Upper common curing adhesive, from test result it is found that performance of the invention has and is obviously improved relative to control group.
Embodiment 7
Ultraviolet cured adhesive of the present invention sticks in agent component, and the partial size and content of modified carbon black influence UV light of the invention
Change the performance of adhesive, for investigate modified carbon black partial size and content to inventive can influence, in the present embodiment, in addition to changing
Property carbon black partial size and content and 2 difference of embodiment except, other are same as Example 2, applicant according to embodiment 2 side
Method is prepared for ultraviolet cured adhesive and sticks agent test group.And the test method of the performance in accordance with the above-mentioned embodiment 1~6, it tests
The present embodiment ultraviolet cured adhesive sticks the performance of agent test group.1~12 ultraviolet cured adhesive of test group sticks agent composition and performance
Test result is as shown in table 2.
Table 2
As can be known from Table 2, when modified carbon black is all in the case of 4 parts by weight, when modified carbon black partial size is 5nm~50 μm,
Its performance more preferably, and when partial size be 15nm~50 μm, performance reaches most preferably, when the partial size of modified carbon black is 15nm, when with
Amount is 1 to 6 part, performance more preferably, and more preferably 2 to 4 parts.When content is more than 8 parts, performance is declined.
Embodiment 8
The present embodiment has investigated the illumination wave band in solidification process to influence of the invention, is that illumination wave band makes the present invention
Standby ultraviolet cured adhesive sticks the influence of agent performance, and in the present embodiment, other than illumination wave band and 2 difference of embodiment, other are
Same as Example 2, applicant is prepared for ultraviolet cured adhesive according to the method for embodiment 2 and sticks agent test group.And according to above-mentioned
The test method of performance described in Examples 1 to 6 tests the performance that the present embodiment ultraviolet cured adhesive sticks agent test group.Test
13~18 ultraviolet cured adhesives of group stick agent composition and the performance test results are as shown in table 3.
Table 3
As can be known from Table 3, the illumination of different wave length will affect shear strength, rate of perviousness, cured thickness, and from it is above-mentioned can
Know, when illumination wavelength is in 250~405nm, with higher shear strength, low rate of perviousness.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should be included within the scope of the present invention.
Claims (10)
1. a kind of ultraviolet cured adhesive sticks agent, which is characterized in that comprise the following components in parts by weight: light-cured resin 40~55
Part, 40~50 parts of acrylate reactive monomer, 3~10 parts of photoinitiator, 0.5~8 part of carbon black.
2. ultraviolet cured adhesive according to claim 1 sticks agent, which is characterized in that the light-cured resin is polyurethane third
At least one of olefin(e) acid ester, epoxy acrylate, polyester acrylate.
3. ultraviolet cured adhesive according to claim 1 sticks agent, which is characterized in that the acrylate reactive monomer is third
The different monooctyl ester of olefin(e) acid, isobornyl acrylate, hydroxy-ethyl acrylate, 2- phenoxyethyl acrylate, ring trimethylolpropane first
Acetal acrylate, acrylic acid tetrahydrofuran ester, lauryl acrylate, 1,6 hexanediol diacrylate, ethoxylated bisphenol A bis-
At least one of acrylate, pentaerythritol triacrylate, trimethylol-propane trimethacrylate.
4. ultraviolet cured adhesive according to claim 1 sticks agent, which is characterized in that the photoinitiator is 2- methyl-1-
[4- (methyl mercapto) phenyl] -2- morpholinyl -1- acetone, 2,4,6- trimethylbenzoy-dipheny phosphorous oxide, 2- hydroxyl -2-
Methyl-1-phenyl-1- acetone, 1- hydroxy-cyclohexyl-phenyl ketone, 2- phenyl benzyl-2- dimethyl amine-1- (4- morpholine benzyl benzene
Base) butanone, at least one of bis- (2,4,6- trimethylbenzoyl) phosphine oxides of phenyl.
5. ultraviolet cured adhesive according to claim 1 sticks agent, which is characterized in that the carbon black is partial size 5nm~100 μm
The mixed and modified carbon black of one or more different-grain diameters.
6. ultraviolet cured adhesive according to claim 5 sticks agent, which is characterized in that the particle size carbon black is 5nm~50 μm,
Preferably, the partial size is 15nm~50 μm；The carbon black is 1 to 6 parts by weight, it is highly preferred that carbon black is 2 to 4 parts by weight.
7. ultraviolet cured adhesive according to claim 5 or 6 sticks agent, which is characterized in that the processing packet of the modified carbon black
Include following steps:
1) the surface monomer cladding of carbon black: carbon black is subjected to ultrasonic disperse and stirs 20~40min, acrylate list is then added
Body is coated, and 1.5~3h of ultrasonic disperse is continued；
2) drying of modified carbon black: taking above-mentioned dispersion liquid, heats 75~85 DEG C, then be dried, and the processing carbon handled well is made
It is black.
8. the preparation method that a kind of ultraviolet cured adhesive as described in any one of claim 1 to 7 sticks agent, which is characterized in that packet
Include following steps:
S1. by light-cured resin, acrylate reactive monomer is put into planetary mixer, and 0.5~2h is mixed；
S2. processed carbon black is added, stirs 2~5h；
S3. by uniformly mixed glue, investment ball mill carries out 3~6h of ball milling；
S4. by the glue after ball milling, planet machine is refunded, photoinitiator is added, stirs 1~2h, then vacuum defoaming, discharging；
S5. then by the glue by dispenser, put on electronic component, be subsequently placed in photo solidification machine carry out illumination reaction 10~
150 seconds to get.
9. the preparation method that ultraviolet cured adhesive according to claim 8 sticks agent, which is characterized in that in the step S5,
Illumination wave band is one or more of 200~760nm of mercury lamp or UV LED light wave band mixing, it is preferable that it is 250~500nm,
It is highly preferred that being 250~405nm.
10. a kind of encapsulate in comprehensive display screen frame to any one of 9 ultra-violet curing gluing agent according to claim 1, photograph
It is applied on the leakproofs optical element such as camera lens, mobile phone.
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| CN201910264777.1A CN110041876B (en) | 2019-04-01 | 2019-04-01 | Ultraviolet curing adhesive, preparation method and application |
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| CN111320962A (en) * | 2020-03-25 | 2020-06-23 | 詹志豪 | Fast-curing UV adhesive and preparation method thereof |
| CN111349401A (en) * | 2020-03-10 | 2020-06-30 | 安徽富印新材料有限公司 | Insulating shading adhesive tape for fixing LED backlight module |
| CN111724688A (en) * | 2020-07-17 | 2020-09-29 | Oppo广东移动通信有限公司 | Assembling method of display screen assembly, display screen assembly and electronic equipment |
| CN113667429A (en) * | 2021-08-19 | 2021-11-19 | 矽时代材料科技股份有限公司 | Ultraviolet-curing heat-conducting adhesive tape and preparation method and application thereof |
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| CN115322740A (en) * | 2022-08-26 | 2022-11-11 | 昆山石梅新材料科技有限公司 | Ultraviolet light curing pressure-sensitive adhesive and preparation method thereof |
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| CN115074089A (en) * | 2022-07-13 | 2022-09-20 | 青岛索迷尔能源科技有限公司 | Preparation method of high-heat-conductivity modular phase-change heat storage unit |
| CN115404028A (en) * | 2022-07-13 | 2022-11-29 | 上海库弗新材料有限公司 | High-color-content ultraviolet-curing shading black adhesive and preparation method thereof |
| CN115404028B (en) * | 2022-07-13 | 2023-09-12 | 上海库弗新材料有限公司 | High-color-content ultraviolet light-cured shading black adhesive and preparation method thereof |
| CN115074089B (en) * | 2022-07-13 | 2023-11-17 | 青岛索迷尔能源科技有限公司 | Preparation method of high-heat-conductivity modularized phase-change heat storage unit |
| CN115322740A (en) * | 2022-08-26 | 2022-11-11 | 昆山石梅新材料科技有限公司 | Ultraviolet light curing pressure-sensitive adhesive and preparation method thereof |
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