CN110041876B - Ultraviolet curing adhesive, preparation method and application - Google Patents
Ultraviolet curing adhesive, preparation method and application Download PDFInfo
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- CN110041876B CN110041876B CN201910264777.1A CN201910264777A CN110041876B CN 110041876 B CN110041876 B CN 110041876B CN 201910264777 A CN201910264777 A CN 201910264777A CN 110041876 B CN110041876 B CN 110041876B
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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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Abstract
The invention discloses an ultraviolet curing adhesive and a preparation method thereof, wherein the adhesive comprises the following components in parts by weight: 40-55 parts of light-cured resin, 40-50 parts of acrylate active monomer, 3-10 parts of photoinitiator and 0.5-8 parts of carbon black; in the preparation process of the adhesive, a mercury lamp or UV LED lamp is used for irradiation curing with a light source with a wave band of 250-760 nm. The low-light-transmittance ultraviolet curing adhesive prepared by the invention has the light transmittance of less than 0.1% at the wavelength of 270-800 nm, is suitable for rapid packaging of light leakage prevention elements such as comprehensive display screen frames, photographic lenses, mobile phones and the like, has the advantages of rapid curing, high light-shielding property, low water absorption, good bonding force and the like, and is an environment-friendly high-efficiency light-shielding material.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an ultraviolet curing adhesive and a preparation method and application thereof.
Background
The application of the adhesive in the electronic industry requires heat conduction, electric conduction and insulation besides mechanical fixation, and meets the requirements of impact-resistant assembly, packaging, substrate protection and the like. With the progress of science and technology, mobile phones, flat panels and televisions enter a full-screen era, the frame of an electronic appliance is narrower, the body of the electronic appliance is thinner and the weight of the electronic appliance is lighter under the full-screen trend, so that higher requirements are provided for adhesives, in order to meet the requirement of attractiveness, the frame is designed to be narrower and narrower, conventional rubber gaskets and RTVs cannot meet the requirements of various detection indexes, and adhesive products with higher requirements need to be researched and developed.
Disclosure of Invention
In order to overcome the defects that a rubber gasket in the prior art has no bonding force, is easy to slip off in the assembling process, can cover the display of a screen due to the size of the gasket, has long RTV curing time, releases low molecules to influence the display screen, and solves the problem that the backlight source is likely to leak light due to the narrow frame, the invention provides the adhesive which is high in light shielding property of colloid and good in bonding force due to the fact that ultraviolet light is cured quickly, and has low light transmittance (the light transmittance is equal to or less than 0.1% under the wavelength of 270-800 nm) by processing carbon black, and the preparation method of the adhesive.
In order to achieve the purpose, the technical scheme adopted by the invention is that the ultraviolet curing adhesive comprises the following components in parts by weight: 40-55 parts of light-cured resin, 40-50 parts of acrylate active monomer, 3-10 parts of photoinitiator and 0.5-8 parts of carbon black.
According to the invention, carbon black is used as a coloring agent, the particle size of the carbon black is optimized, and the carbon black can be modified to realize low light transmittance and high adhesiveness at a relatively thin thickness, so that the carbon black can not agglomerate after being placed for a long time; by optimizing the photoinitiator, the low-energy curing realizes thicker (0.4mm) colloid curing thickness and high adhesiveness under different proportions.
As a preferred embodiment of the uv curable adhesive of the present invention, the photocurable resin is at least one of urethane acrylate, epoxy acrylate, and polyester acrylate.
In a preferred embodiment of the uv curable adhesive of the present invention, the acrylate reactive monomer is at least one of isooctyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, 2-phenoxyethyl acrylate, cyclotrimethylolpropane formal acrylate, tetrahydrofurfuryl acrylate, lauryl acrylate, 1, 6-hexanediol diacrylate, ethoxylated bisphenol a diacrylate, pentaerythritol triacrylate, and trimethylolpropane trimethacrylate.
As a preferred embodiment of the uv curable adhesive of the present invention, the photoinitiator is at least one of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-propanone, 2,4, 6-trimethylbenzoyl-diphenylphosphorus oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxy-cyclohexyl-phenyl ketone, 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinebenzylphenyl) butanone, and phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide.
As a preferable embodiment of the ultraviolet curing adhesive, the carbon black is one or more mixed modified carbon blacks with different particle sizes, wherein the particle size of the mixed modified carbon black is 5 nm-100 mu m. According to the invention, the particle size of the carbon black is optimized, and after modification, low light transmittance and high adhesion can be realized under a thinner thickness, and the carbon black can not agglomerate after being placed for a long time.
As a preferred embodiment of the uv curable adhesive of the present invention, the particle size of the carbon black is 5nm to 50 μm, preferably, 15nm to 50 μm; the carbon black is 1 to 6 parts by weight, more preferably 2 to 4 parts by weight. The inventor of the application finds that when the carbon black is between 15nm and 50 mu m, the light transmittance is lower, the adhesiveness is high, and the carbon black can not agglomerate after being placed for a long time.
As a preferred embodiment of the uv curable adhesive of the present invention, the treatment of the modified carbon black comprises the following steps:
1) cleaning the surface of carbon black, namely taking one or more types of untreated carbon black mixed with different particle sizes and with the particle size of 5 nm-100 mu m, wherein the ratio of the carbon black to absolute ethyl alcohol is 5:200, adding 300g of zirconia balls (with the particle size of 1mm/3mm/10mm and the ratio of 5:3:2) into the mixture, grinding the mixture for 2-6 h at the rotating speed of 7000-20000 r/s, adding 1000g of deionized water at 80 ℃ into the mixture, stirring the mixture for 30min, sucking out the mixed liquid of upper alcohol and water after the carbon black is settled for 3h, and repeating the washing step for more than three times;
2) coating a monomer on the surface of the carbon black, namely obtaining the carbon black in the step 1), adding 500g of absolute ethyl alcohol, putting the carbon black into an ultrasonic cleaning machine, ultrasonically dispersing and stirring for 20-40 min, then dropwise adding a DPGDA monomer at a speed controlled at 10g/min, and continuously ultrasonically dispersing for 1.5-3 h after dropwise adding;
3) and (3) drying the modified carbon black, namely heating the dispersion liquid to 75-85 ℃, pumping off absolute ethyl alcohol and water at negative 0.9MPa, and drying the obtained powder in an oven at 100 ℃ for 1h to obtain the treated carbon black.
The carbon black is modified in order to fully color and disperse the carbon black and achieve higher light shading degree and OD value, and meanwhile, the acrylic monomer is used as a carrier, and a dispersing agent is not needed.
The invention improves the defects of small particle size, large specific surface area, high surface energy, easy agglomeration and the like of carbon black particles, utilizes ultrasonic dispersion and coats the surface with acrylate monomers for surface modification, reduces the use of a surfactant, and simultaneously improves the light shielding property, the adhesion property and the curing depth due to the selection of the particle size.
The invention also provides a preparation method of the ultraviolet curing adhesive, which comprises the following steps:
s1, putting the light-cured resin and the acrylate active monomer into a planetary stirrer, and mixing and stirring for 0.5-2 h;
s2, adding the treated carbon black, and stirring for 2-5 hours;
s3, putting the uniformly mixed glue into a ball mill for ball milling for 3-6 h;
s4, pouring the ball-milled glue back to a planetary machine, adding a photoinitiator, stirring for 1-2 hours, and then defoaming in vacuum and discharging;
and S5, the glue is dispensed on the electronic element through a glue dispenser, and then the electronic element is placed in a light curing machine for illumination reaction for 10-150 seconds, so that the adhesive is obtained.
As a preferred embodiment of the preparation method of the ultraviolet curing adhesive of the present invention, in the step S5, an illumination wavelength band is 200 to 760nm, preferably 250 to 500nm, and more preferably, one or a mixture of several wavelengths of 250 to 405nm of a mercury lamp or a UV LED lamp.
The ultraviolet curing adhesive provided by the invention can be used for comprehensively packaging frames of display screens, photographic lenses, mobile phones and other light leakage prevention elements.
The invention has the beneficial effects that:
(1) the invention does not need long-time room temperature curing, saves time and improves productivity;
(2) the defect that small molecules are separated out in the moisture curing process of the RTV is eliminated, and adverse reactions to the display screen are reduced;
(3) the problems that the rubber gasket is small in bonding force and easy to fall off are solved;
(4) because of high light-shielding property, the problem of light leakage can be solved at a thinner thickness, the weight is reduced compared with thermosol, the electronic device is suitable for the trend of lightness and thinness, and the electronic workpiece cannot be damaged due to high temperature;
(5) the carbon black is dispersed by using an acrylic monomer as a carrier, and a dispersing agent is not needed.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The raw materials in the following examples are all commercially available general-purpose materials unless otherwise specified.
In order to fully color and disperse the carbon black and achieve higher light shading degree and OD value, the carbon black is treated as follows:
1) cleaning the surface of carbon black, namely taking one or more types of untreated carbon black mixed with different particle sizes and with the particle size of 5 nm-100 mu m, wherein the ratio of the carbon black to absolute ethyl alcohol is 5:200, adding 300g of zirconia balls (with the particle size of 1mm/3mm/10mm and the ratio of 5:3:2) into the mixture, grinding the mixture for 2-6 h at the rotating speed of 7000-20000 r/s, adding 1000g of deionized water at 80 ℃ into the mixture, stirring the mixture for 30min, sucking out the mixed liquid of upper alcohol and water after the carbon black is settled for 3h, and repeating the washing step for more than three times;
2) coating a monomer on the surface of the carbon black, namely obtaining the carbon black in the step 1), adding 500g of absolute ethyl alcohol, putting the carbon black into an ultrasonic cleaning machine, ultrasonically dispersing and stirring for 20-40 min, then dropwise adding a DPGDA monomer at a speed controlled at 10g/min, and continuously ultrasonically dispersing for 1.5-3 h after dropwise adding;
3) and (3) drying the modified carbon black, namely heating the dispersion liquid to 80 ℃, pumping off absolute ethyl alcohol and water at negative 0.9MPa, and drying the obtained powder in an oven at 100 ℃ for 1h to obtain the treated carbon black.
Example 1
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 50 parts of urethane acrylate, 20 parts of isobornyl acrylate, 15 parts of isooctyl acrylate, 8 parts of 1, 6-hexanediol diacrylate, 0.3 part of modified carbon black with the particle size of 15nm, 0.7 part of modified carbon black with the particle size of 3 mu m, 2 parts of 2-benzyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone and 4 parts of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate; the acrylate active monomer is isobornyl acrylate, isooctyl acrylate and 1, 6-hexanediol diacrylate; the photoinitiator is 2-benzyl phenyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone and 1-hydroxy-cyclohexyl phenyl ketone.
The preparation method of the ultraviolet curing adhesive comprises the following steps of:
s1, adding a light curing agent and an acrylic acid active monomer into a reaction container, controlling the temperature to be 20-40 ℃, and mixing for 0.5-2 hours by using a planetary mixer;
s2, adding the treated carbon black, and stirring for 2-5 hours;
s3, putting the uniformly mixed glue into a ball mill containing zirconia balls with different particle sizes for ball milling for 3-6 h, wherein the particle sizes of the zirconia balls are 1mm, 3mm and 10mm respectively, the proportion of the three particle sizes is 6:3:1 respectively, and the adding amount of the zirconia balls is 10% of that of the glue;
s4, pouring the ball-milled glue back to a planetary machine, adding a photoinitiator, stirring for 1-2 hours, and then defoaming in vacuum and discharging;
s5, the glue is dispensed by a glue dispenser at the glue dispensing position of the electronic workpiece by 0.1-0.2 mm, and then the electronic workpiece is placed in a light curing machine for illumination reaction for 10-150 seconds, so that the electronic workpiece is obtained.
The ultraviolet curing light source can adopt a 1000W medium-pressure mercury lamp with the light intensity of 80mw/cm2The effective light radiation center wavelength is 365 nm.
Example 2
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, 22 parts of 2-phenoxyethyl acrylate, 16 parts of cyclotrimethylolpropane methylal acrylate, 8 parts of isooctyl acrylate, 0.5 part of modified carbon black with the particle size of 7nm, 3.5 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 2 parts of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate or epoxy acrylate; the acrylate active monomer is 2-phenoxyethyl acrylate, cyclotrimethylolpropane methylal acrylate and isooctyl acrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1-hydroxy-cyclohexyl-phenyl ketone.
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
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 40 parts of polyester acrylate, 40 parts of hydroxyethyl acrylate, 8 parts of modified carbon black with the particle size of 5nm, 2 parts of 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, 2 parts of 2-hydroxy-2-methyl-1-phenyl-1-acetone and 2 parts of phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
The light-cured resin in the embodiment is polyester acrylate; the acrylate active monomer is hydroxyethyl acrylate; the photoinitiator is 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide.
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
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 20 parts of urethane acrylate, 15 parts of epoxy acrylate, 20 parts of polyester acrylate, 22 parts of tetrahydrofuran acrylate, 20 parts of lauryl acrylate, 8 parts of ethoxylated bisphenol A diacrylate, 0.3 part of modified carbon black with the particle size of 15nm, 0.7 part of carbon black with the particle size of 100 mu m and 10 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone.
The light-cured resin in the embodiment is urethane acrylate, epoxy acrylate, or polyester acrylate; the acrylate active monomer is tetrahydrofuran acrylate, lauryl acrylate and ethoxylated bisphenol A diacrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone.
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 5
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, 22 parts of 2-phenoxyethyl acrylate, 16 parts of cyclotrimethylolpropane methylal acrylate, 8 parts of isooctyl acrylate, 0.5 part of modified carbon black with the particle size of 7nm, 3.5 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 2 parts of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate or epoxy acrylate; the acrylate active monomer is 2-phenoxyethyl acrylate, cyclotrimethylolpropane methylal acrylate and isooctyl acrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1-hydroxy-cyclohexyl-phenyl ketone.
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 6
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 30 parts of urethane acrylate, 18 parts of epoxy acrylate, 22 parts of pentaerythritol triacrylate, 25 parts of trimethylolpropane trimethacrylate, 0.5 part of modified carbon black with the particle size of 7nm, 3.5 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 2 parts of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate or epoxy acrylate; the acrylate active monomer is pentaerythritol triacrylate or trimethylolpropane trimethacrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1-hydroxy-cyclohexyl-phenyl ketone.
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.
Comparative example 1
In the embodiment of the ultraviolet curing adhesive of the present comparative example, the ultraviolet curing adhesive comprises the following components in parts by weight: 20 parts of urethane acrylate, 10 parts of epoxy acrylate, 30 parts of pentaerythritol triacrylate, 30 parts of trimethylolpropane trimethacrylate, 0.5 part of carbon black with the particle size of 7nm, 3.5 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 2 parts of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate or epoxy acrylate; the acrylate active monomer is pentaerythritol triacrylate or trimethylolpropane trimethacrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1-hydroxy-cyclohexyl-phenyl ketone.
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.
Comparative example 2
As an embodiment of the ultraviolet curing adhesive with low light transmittance, the ultraviolet curing adhesive comprises the following components in parts by weight: 40 parts of urethane acrylate, 20 parts of epoxy acrylate, 20 parts of 2-phenoxyethyl acrylate, 15 parts of cyclotrimethylolpropane methylal acrylate, 8 parts of isooctyl acrylate, 0.5 part of modified carbon black with the particle size of 7nm, 1.5 parts of 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1 part of 1-hydroxy-cyclohexyl-phenyl ketone.
The light-cured resin in the embodiment is urethane acrylate or epoxy acrylate; the acrylate active monomer is 2-phenoxyethyl acrylate, cyclotrimethylolpropane methylal acrylate and isooctyl acrylate; the photoinitiator is 2-methyl-1- [4- (methylthio) phenyl ] -2-morpholinyl-1-acetone and 1-hydroxy-cyclohexyl-phenyl ketone.
The preparation method of the UV curable adhesive of this embodiment is the same as that of embodiment 1 except that a UV LED lamp is used for illumination, and will not be described in detail herein.
Comparative example 3
This comparative example differs from example 1 only in that the carbon black used is an unmodified carbon black.
Example 7
The cured products of examples 1-6 and comparative example 1 and a control group (prior art) are subjected to shear strength tests of glass, polycarbonate PC and polycarbonate PC, and prepared sample wafers with the length, width and length of 5cm x 5cm, and the test wavelength is 270nm-800nm, light transmittance, curing time, curing thickness, moisture permeability and adhesiveness are tested, and the test method is as follows:
glass & glass shear strength: curing the colloid between glass and glass (colloid thickness 0.15mm) using a UV mercury lamp/LED, and immediately performing a shear strength test; the test standard is GB/T7124;
shear strength of polycarbonate PC & polycarbonate PC: curing the colloid between PC-PC (colloid thickness 0.15mm) by using a UV mercury lamp/LED, and immediately carrying out a shear strength test; the test standard is GB/T7124;
light transmittance: curing the colloid into sample wafers with the size, length and width of 5cm x 5cm, and then testing the light transmittance with the wavelength of 270nm-800nm by an optical transmittance instrument (LH 1013);
moisture permeability: after the colloid is solidified, the colloid is placed at 38 ℃/90% humidity; and (4) testing standard: GB/T16928;
adhesion: solidifying the colloid on glass, putting the glass in 85% humidity at 85 ℃, and determining whether the colloid cracks or degummed after 1000 hours.
The test results are shown in table 1:
TABLE 1
As can be seen from table 1, the ultraviolet curing adhesive prepared in embodiments 1 to 6 of the present invention has a light transmittance of less than 0.1% at a wavelength of 270 to 800nm, is suitable for rapid encapsulation of light-tight components such as a comprehensive display screen frame, a photographic lens, a mobile phone, and the like, has advantages of short curing time, high shear strength, low moisture permeability, rapid curing, high light-shielding property, low water absorption, good adhesion, and the like, is an environment-friendly high-efficiency light-shielding material, and has a good application prospect. Compared with the example 1, the comparative examples 1-2 have the content of part of the components out of the range of the invention, and the results show that the performance is slightly reduced compared with the invention, which shows that the performances can be optimized only under the condition of simultaneously satisfying specific components and specific content; comparative example 3 adopts unmodified carbon black, and the curing time and transmittance of the modified carbon black are higher than those of the invention, and the shear strength and moisture permeability of the modified carbon black are low, so that the use of the modified carbon black is beneficial to improving the light shading property, the adhesion property, the curing depth and the low light transmittance; and the contrast group adopts a common curing adhesive sold on the market, and the test result shows that the performance of the adhesive is obviously improved compared with the contrast group.
Example 7
In the ultraviolet curing adhesive component of the invention, the particle size and the content of the modified carbon black affect the performance of the ultraviolet curing adhesive of the invention, and in order to examine the effect of the particle size and the content of the modified carbon black on the performance of the invention, in this example, except that the particle size and the content of the modified carbon black are different from those of example 2, the other steps are the same as those of example 2, and the applicant prepared an ultraviolet curing adhesive test group according to the method of example 2. The performance of the test group of the ultraviolet curing adhesive in the embodiment was tested according to the performance test method described in the embodiments 1 to 6. The compositions and performance test results of the ultraviolet curing adhesives in test groups 1-12 are shown in Table 2.
TABLE 2
As can be seen from Table 2, in the case where the modified carbon blacks are all 4 parts by weight, the properties are more excellent when the modified carbon blacks have particle diameters of 5nm to 50 μm, and the properties are most excellent when the particle diameters are 15nm to 50 μm, and the properties are more excellent when the modified carbon blacks are used in amounts of 1 to 6 parts, and more preferably 2 to 4 parts, when the particle diameters are all 15 nm. When the content exceeds 8 parts, the properties are deteriorated.
Example 8
In this example, the effect of the illumination band in the curing process on the present invention is examined, and in order to determine the effect of the illumination band on the performance of the uv curable adhesive prepared by the present invention, except that the illumination band is different from that in example 2, the other steps are the same as in example 2, and the applicant prepares a test group of uv curable adhesives according to the method in example 2. The performance of the test group of the ultraviolet curing adhesive in the embodiment was tested according to the performance test method described in the embodiments 1 to 6. The compositions and performance test results of the test groups 13-18 ultraviolet curing adhesives are shown in table 3.
TABLE 3
As can be seen from Table 3, the shear strength, moisture permeability and curing thickness are affected by different wavelengths of light, and it is seen that the shear strength and moisture permeability are higher when the wavelength of light is 250-405 nm.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The ultraviolet curing adhesive is characterized by comprising the following components in parts by weight: 40-55 parts of light-cured resin, 40-50 parts of acrylate active monomer, 3-10 parts of photoinitiator and 0.5-8 parts of carbon black;
the carbon black is one or more mixed modified carbon blacks with different particle sizes, wherein the particle size of the carbon black is 5 nm-100 mu m; the light-cured resin is at least one of polyurethane acrylate, epoxy acrylate and polyester acrylate; the acrylate active monomer is at least one of isooctyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, 2-phenoxyethyl acrylate, cyclotrimethylolpropane methylal acrylate, tetrahydrofuran acrylate, lauryl acrylate, 1, 6-hexanediol diacrylate, ethoxylated bisphenol A diacrylate, pentaerythritol triacrylate and trimethylolpropane trimethacrylate; 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-benzyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone and phenyl bis (2,4, 6-trimethylbenzoyl) phosphine oxide;
wherein the treatment of the modified carbon black comprises the steps of:
1) coating a surface monomer of the carbon black, namely performing ultrasonic dispersion on the carbon black, stirring for 20-40 min, then adding an acrylate monomer DPGDA for coating, and continuing performing ultrasonic dispersion for 1.5-3 h;
2) drying the modified carbon black, namely heating the dispersion liquid to 75-85 ℃, and drying to obtain the treated carbon black;
the preparation method of the ultraviolet curing adhesive comprises the following steps:
s1, putting the photo-curing resin and the acrylate active monomer into a planetary stirrer, and mixing and stirring for 0.5-2 h;
s2, adding the treated carbon black, and stirring for 2-5 h;
s3, putting the uniformly mixed glue into a ball mill for ball milling for 3-6 h;
s4, pouring the ball-milled glue back to a planetary machine, adding a photoinitiator, stirring for 1-2 hours, and then defoaming in vacuum and discharging;
and S5, dropping the adhesive on an electronic element through a dispenser, and then placing the electronic element in a photocuring machine for illumination reaction for 10-150 seconds to obtain the adhesive, wherein the illumination wave band is one or a mixture of more of 200-760 nm mercury lamps.
2. The ultraviolet-curable adhesive according to claim 1, wherein the carbon black has a particle size of 5nm to 50 μm, and the amount of the carbon black is 1 to 6 parts by weight.
3. The ultraviolet-curable adhesive according to claim 2, wherein the carbon black has a particle size of 15nm to 50 μm, and the amount of the carbon black is 2 to 4 parts by weight.
4. The ultraviolet curing adhesive according to claim 1, wherein in the step S5, the illumination wavelength band is one or a mixture of several wavelength bands of 250-500 nm of a mercury lamp.
5. The ultraviolet curing adhesive according to claim 1, wherein in the step S5, the illumination wavelength band is one or a mixture of several wavelength bands of 250-405 nm of a mercury lamp.
6. Use of the UV-curable adhesive according to any one of claims 1 to 5 for full-face display bezel packaging, photographic lens, and light leakage prevention element of mobile phone.
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| 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 |
| CN111320962B (en) * | 2020-03-25 | 2022-12-13 | 詹志豪 | Fast-curing UV adhesive and preparation method thereof |
| CN111724688B (en) * | 2020-07-17 | 2022-07-12 | Oppo广东移动通信有限公司 | Assembling method of display screen assembly, display screen assembly and electronic equipment |
| CN113667429B (en) * | 2021-08-19 | 2022-08-26 | 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 |
| CN113881389A (en) * | 2021-09-22 | 2022-01-04 | 矽时代材料科技股份有限公司 | Ultraviolet light curing foaming adhesive and preparation method and application thereof |
| CN114196369A (en) * | 2021-12-27 | 2022-03-18 | 东莞市阿普帮新材料科技有限公司 | Environment-friendly flame-retardant low-sensitization ultraviolet curing adhesive and preparation method thereof |
| CN114316879A (en) * | 2021-12-27 | 2022-04-12 | 深圳市库泰克电子材料技术有限公司 | UV (ultraviolet) shading adhesive with good hydrophobicity and low moisture permeability 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 |
| CN115322740B (en) * | 2022-08-26 | 2023-07-11 | 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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