CN112940676B - UV adhesive - Google Patents

UV adhesive Download PDF

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Publication number
CN112940676B
CN112940676B CN202110182513.9A CN202110182513A CN112940676B CN 112940676 B CN112940676 B CN 112940676B CN 202110182513 A CN202110182513 A CN 202110182513A CN 112940676 B CN112940676 B CN 112940676B
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parts
adhesive
glue
following components
chemical industry
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CN112940676A (en
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艾瑞克.C.王
张杨飞
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Shenzhen Unitak Electronic Materials Co ltd
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Shenzhen Unitak Electronic Materials Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J201/00Adhesives based on unspecified macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

In order to solve the problems of insufficient reliability and volatilization of organic matters in the existing UV adhesive, the application provides the UV adhesive which comprises the following components: modified photosensitive resin, reactive diluent, photoinitiator, thixotropic filler, coupling agent, adhesion promoter and wetting agent; wherein the modified photosensitive resin comprises the following components in parts by weight: the Japanese Kagaku Kogyo Co Ltd., no. UN-9200A, the Japanese chemical industry Co., ltd., KEA-24, and the Taiwan Changxing chemical industry Co., ltd., DR-U299 in Taiwan area. The UV adhesive provided by the application has extremely low volatility, stronger adhesive force, better flexibility and shock resistance; in particular, the UV glue has greatly improved water resistance and air tightness, and is particularly suitable for the assembly of optical devices.

Description

UV adhesive
Technical Field
The application belongs to an ultraviolet curing adhesive, and particularly relates to a UV adhesive.
Background
The UV glue has the advantages of high curing speed, low energy consumption in the curing process, no Organic Solvent (VOCs) in the glue, energy conservation, environmental protection, high efficiency and the like. Therefore, the application range and the use amount of the composition are increased year by year.
In China, the production and consumption of electronic products are large, a large amount of electronic products are produced each year, and a large amount of UV glue is needed in the process so as to meet various requirements of bonding, fixing, reinforcing, filling and sealing and the like.
In many electronic products, there are a series of optical devices, and there are high requirements for weather resistance such as water resistance, thermal shock resistance and air tightness. If the materials used are not as required, the performance and reliability of the device will be directly affected. Therefore, the materials used need to be specifically designed for such applications to meet their specific requirements.
UV gels are generally limited by the limitations of material purity and formulation composition, and can produce some small molecular weight organic volatiles during curing. The organic matters are not crosslinked and fixed through chemical reaction, and the organic matters can be volatilized slowly after the glue is solidified, and especially when the ambient temperature is increased, the organic matters are more obvious. Organic volatiles generated by the glue can contaminate surrounding devices. If the glue is used for bonding and fixing optical devices, residual organic matters after the glue is solidified slowly volatilize to cause device pollution, so that the imaging performance of the optical devices is reduced, the actual use effect of equipment is affected, and the quality and the service life of the equipment are reduced.
Disclosure of Invention
Aiming at the problems of insufficient reliability and volatilization of organic matters in the existing UV adhesive, the application provides the UV adhesive.
The technical scheme adopted by the application for solving the technical problems is as follows:
the application provides a UV adhesive, which comprises the following components: modified photosensitive resin, reactive diluent, photoinitiator, thixotropic filler, coupling agent, adhesion promoter and wetting agent;
wherein the modified photosensitive resin comprises the following components in parts by weight:
the Japanese Kagaku Kogyo Co Ltd., no. UN-9200A, the Japanese chemical industry Co., ltd., KEA-24, and the Taiwan Changxing chemical industry Co., ltd., DR-U299 in Taiwan area.
Optionally, the UV glue comprises the following components in parts by weight:
40-60 parts of modified photosensitive resin, 30-60 parts of reactive diluent, 2-8 parts of photoinitiator, 3-10 parts of thixotropic filler, 0.5-5 parts of coupling agent, 0.5-5 parts of adhesion promoter and 0.1-0.4 part of wetting agent.
Optionally, the modified photosensitive resin comprises the following components in parts by weight:
10-20 parts of Japanese chemical industry Co Ltd, 5-15 parts of Japanese chemical industry Co Ltd, and DR-U29920-40 parts of Taiwan Changxing chemical industry Co Ltd in Taiwan area.
Optionally, the reactive diluent comprises a monofunctional acrylate and a multifunctional acrylate.
Optionally, the reactive diluent comprises the following components in parts by weight:
15-25 parts of isobornyl acrylate, 15-25 parts of N, N-dimethylacrylamide and 1-5 parts of tri (2-hydroxyethyl) isocyanurate triacrylate.
Optionally, the photoinitiator includes one or more of α, α -dimethylbenzoyl ketal, α -diethoxyacetophenone, 2-hydroxy-2-methyl-phenylpropanone-1, 1-hydroxy-cyclohexylbenzophenone, 2-hydroxy-2-methyl-p-hydroxyethyl etherphenylpropanone-1, 2-methyl-1- (4-methylthiophenyl) -2-morpholinophenone-1, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1, 2,4,6- (trimethylbenzoyl) diphenylphosphine oxide, and bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide.
Optionally, the thixotropic filler comprises one or more of the Evonik Degussa brand AEROSIL series, the WACKER brand HDK series, and the CABOT brand CAB-O-SIL series.
Optionally, the coupling agent includes one or more of the Dow Corning brand Z series, momentive (Michaelis-co. America) brand A-151, A-171, A-186, A-187, A-189, A-174, A-1524, A-1160, and A-1230, japanese Kokai brand KBM503, KBM903, KBM603, and KBM 1003.
Optionally, the adhesion promoter comprises one or more of EM39 of changxing chemistry, SR9050, SR9051 of sartomer, and PM-2 of japan chemical.
Optionally, the wetting agent includes one or more of Digao brand TEGO Wet270 and TEGO Wet280, and German Pick brand BYK-301 and BYK-333.
According to the UV adhesive provided by the application, the specific brands of Japanese chemical industry Co Ltd No. UN-9200A, japanese chemical industry brand KEA-24 and Taiwan Changxing chemical industry Co Ltd in Taiwan area DR-U299 are adopted as modified photosensitive resins, and polymerization reaction can be carried out with reactive diluents, photoinitiators, thixotropic fillers, coupling agents, adhesion promoters and wetting agents under illumination conditions, so that the modified photosensitive resins of different brands are mutually bonded to form a reticular space crosslinking structure on a microscopic scale, thereby having extremely low volatility, stronger adhesive force, better flexibility and shock resistance; in particular, the UV adhesive is greatly improved in water resistance and air tightness, so that the UV adhesive is particularly suitable for the assembly of optical devices, such as the adhesion and fixation of glass lenses, PC lenses and metal frames, further the service life of the optical devices is prolonged, the equipment performance and reliability are improved, and the pollution to lenses and the like is avoided.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the application more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides a UV adhesive, which comprises the following components: modified photosensitive resin, reactive diluent, photoinitiator, thixotropic filler, coupling agent, adhesion promoter and wetting agent;
wherein the modified photosensitive resin comprises the following components in parts by weight:
the Japanese Kagaku Kogyo Co Ltd., no. UN-9200A, the Japanese chemical industry Co., ltd., KEA-24, and the Taiwan Changxing chemical industry Co., ltd., DR-U299 in Taiwan area.
The inventor has carried out experiments on raw material modified photosensitive resin adopted by UV glue in the field for a long time, and found that because of different preparation environments (such as solvent, temperature, reaction time and the like) of the resin and different component contents of the raw material, different brands of modified photosensitive resin produced by different companies have larger differences in properties (such as molecular weight range, glass transition temperature, ratio of reactive functional groups, types of auxiliary functional groups and the like), and meanwhile, different brands of modified photosensitive resin have reactions, so that larger performance differences are caused on final products when the modified photosensitive resin is applied, in order to meet the performance requirements of the UV glue on preventing volatilization of organic matters, adhesive force, water resistance, air tightness and the like when the UV glue is applied to optical devices, the inventor tries to carry out substitution experiments on various brands of modified photosensitive resin produced by import or home-made, and accidentally found that the UV glue produced by one combination mode shows excellent effects different from other combinations when the UV glue is subjected to thermal shock resistance, air tightness tests, and other performances such as preventing volatilization of organic matters are kept at a better level, and the UV glue is further adjusted to the corresponding experiment formula files after the application is further found by the application, the application is further adjusted by the method is carried out after the application is carried out a plurality of experimental files: the UV adhesive with extremely low volatility, stronger adhesive force, better flexibility, impact resistance, water resistance and air tightness is obtained by respectively adopting the Japanese chemical industry Co Ltd No. UN-9200A, the Japanese chemical industry Co Ltd No. KEA-24 and the Taiwan Changxing chemical industry Co Ltd No. DR-U299 in Taiwan area to be mixed as modified photosensitive resin.
In some embodiments, the UV gel comprises the following weight components:
40-60 parts of modified photosensitive resin, 30-60 parts of reactive diluent, 2-8 parts of photoinitiator, 3-10 parts of thixotropic filler, 0.5-5 parts of coupling agent, 0.5-5 parts of adhesion promoter and 0.1-0.4 part of wetting agent.
In a preferred embodiment, the UV glue comprises the following components by weight:
40-45 parts of modified photosensitive resin, 40-50 parts of reactive diluent, 2.5-5.0 parts of photoinitiator, 5-8 parts of thixotropic filler, 1-3 parts of coupling agent, 1-3 parts of adhesion promoter and 0.1-0.3 part of wetting agent.
Specifically, the modified photosensitive resin comprises the following components in parts by weight: 40 parts, 42 parts, 45 parts, 49 parts, 50 parts, 52 parts, 55 parts, 59 parts, or 60 parts. The reactive diluent comprises the following components in parts by weight: 30, 32, 35, 39, 40, 42, 45, 49, 50, 52, 55, 59 or 60 parts. The photoinitiator comprises the following components in parts by weight: 2 parts, 3 parts, 5 parts, 6 parts or 8 parts. The thixotropic filler comprises the following components in parts by weight: 3 parts, 5 parts, 6 parts, 8 parts or 10 parts. The coupling agent comprises the following components in parts by weight: 0.5 part, 1 part, 2 parts, 3 parts, 4 parts or 5 parts. The adhesion promoter comprises the following components in parts by weight: 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts. The wetting agent may be used in an amount of 0.1 parts, 0.2 parts, 0.3 parts or 0.4 parts by weight.
In some embodiments, the modified photosensitive resin comprises the following components by weight:
10-20 parts of Japanese chemical industry Co Ltd, 5-15 parts of Japanese chemical industry Co Ltd, and DR-U29920-40 parts of Taiwan Changxing chemical industry Co Ltd in Taiwan area.
In a preferred embodiment, the modified photosensitive resin is composed of the following components by weight:
10-15 parts of Japanese chemical industry Co Ltd, 8-12 parts of Japanese chemical industry Co Ltd, and DR-U29925-35 parts of Taiwan Changxing chemical industry Co Ltd in Taiwan area.
It should be noted that, the chemical industry Co., ltd. No. UN-9200A on Japanese, the chemical industry Co., ltd. KEA-24 on Japanese and the Taiwan Changxing chemical industry Co., ltd. DR-U299 on Taiwan area need to be mixed and added in a certain range to play a synergistic effect, meanwhile, as the modified photosensitive resin composition has a certain additive amount in the UV glue, the content of the modified photosensitive resin of a single grade is too large, the content of the modified photosensitive resin of other grades is correspondingly reduced, and the performance improvement is not obvious; the inventor finds that the performance of the UV adhesive is improved when the number of Japanese chemical industry Co Ltd No. 9200A, japanese chemical medicine chemical industry Co Ltd KEA-24 and Taiwan Changxing chemical industry Co Ltd DR-U299 in Taiwan area are in the above range through a large number of experiments.
In some embodiments, the reactive diluent molecular structure contains one or several "-c=c-", which can participate in polymerization reactions, including one or more of mono-functional acrylates and multi-functional acrylates.
In some embodiments, the reactive diluents include mono-functional acrylates and multi-functional acrylates.
The monofunctional acrylate includes one or more of isobornyl methacrylate, 2 (2-ethoxyethoxy) ethyl acrylate, isobornyl acrylate, lauric acid acrylate, N-dimethylacrylamide, acryloylmorpholine, hydroxyethyl (meth) acrylate, hydroxypropyl (meth) acrylate, ethoxylated hydroxyethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, N-hexyl (meth) acrylate, isooctyl (meth) acrylate, cyclohexyl (meth) acrylate, stearyl (meth) acrylate, tetrahydrofurfuryl (meth) acrylate, glycidyl (meth) acrylate, 2-phenoxyethyl (meth) acrylate, and nonylphenol (meth) acrylate.
The above mono-functional acrylates are all commercially available, for example, isobornyl methacrylate available from SARTOMER brand SR423, U.S.A.; 2 (2-ethoxyethoxy) ethyl acrylate is commercially available from SARTOMER brand SR256, U.S.A.; isobornyl acrylate is commercially available from IBXA, organic chemical trade designation, osaka, japan; lauric acid acrylic ester is commercially available from taiwan long chemical industry limited company, trade name EM215 in taiwan area of china; n, N-dimethylacrylamide is available from Nippon and Kabushiki Kaisha under the name DMAA; acrylonitrile is commercially available from Nippon Chemie (KJ CHEMICAL) under the trademark ACMO.
The multifunctional acrylate includes tri (2-hydroxyethyl) isocyanurate triacrylate, pentaerythritol tetraacrylate, ethylene glycol di (meth) acrylic acid, diethylene glycol di (meth) acrylic acid, triethylene glycol di (meth) acrylic acid, cyclohexanedimethanol diacrylate, alkoxylated hexanediol di (meth) acrylate, alkoxylated cyclohexanedimethanol di (meth) acrylate, alkoxylated neopentyl glycol di (meth) acrylate, 1, 3-butanediol di (meth) acrylate, 1, 4-butanediol di (meth) acrylate, 1, 6-hexanediol di (meth) acrylate, neopentyl glycol diacrylate, polyethylene glycol (200) di (meth) acrylate, polyethylene glycol (400) di (meth) acrylate, ethoxylated bisphenol A di (meth) acrylate, tricyclodecane dimethanol di (meth) acrylate, propoxylated neopentyl glycol di (meth) acrylate, trimethylol propane tri (meth) acrylate, tri (2-hydroxyethyl) isocyanurate tri (meth) acrylate, ethoxylated trimethylol propane tri (meth) acrylate, propoxylated trimethylolpropane tri (meth) acrylate, pentaerythritol di (400) di (meth) acrylate, one or more of di (trimethylolpropane) tetra (meth) acrylate.
The above-mentioned multifunctional acrylates are all commercially available, for example, tris (2-hydroxyethyl) isocyanurate triacrylate commercially available from SARTOMER brand SR368NS, U.S.A.; pentaerythritol tetraacrylate is available from Taiwan Changxing chemical industry Co., ltd. Under the trademark EM241 in Taiwan area of China.
In a preferred embodiment, the reactive diluent comprises the following components by weight:
isobornyl acrylate (available from osaka organic chemical company IBXA, japan), N-dimethylacrylamide (available from japan Xingjiu corporation, DMAA), 20-25 parts, and tris (2-hydroxyethyl) isocyanurate triacrylate (available from SARTOMER, usa, SR368 NS), 3-5 parts.
The reactive diluents are used as one of main polymerization monomers of the UV adhesive, and the combination of different reactive diluents has great influence on the volatility and reliability of the UV adhesive, and the three different reactive diluents of isobornyl acrylate, N-dimethyl acrylamide and tri (2-hydroxyethyl) isocyanurate triacrylate are mixed, so that the reactive diluents have certain overlapping in function, but the action mechanism and the crosslinking site are different, and the different reactive diluents can promote each other, so that the crosslinking density of a reaction product is improved to the greatest extent, the UV adhesive has better flexibility and impact resistance, and the water resistance and the air tightness are ensured.
In some embodiments, the photoinitiator includes one or more of α, α -dimethylbenzoyl ketal, α -diethoxyacetophenone, 2-hydroxy-2-methyl-phenylpropanone-1, 1-hydroxy-cyclohexylbenzophenone, 2-hydroxy-2-methyl-p-hydroxyethyl etherphenylpropanone-1, 2-methyl-1- (4-methylthiophenyl) -2-morpholinophenone-1, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1, 2,4,6- (trimethylbenzoyl) diphenylphosphine oxide, and bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide.
In some embodiments, the thixotropic filler is selected from the group consisting of gas phase carbon dioxide.
In a preferred embodiment, the thixotropic filler comprises one or more of the Evonik Degussa brand AEROSIL series, the WACKER brand HDK series, and the CABOT brand CAB-O-SIL series.
The Evonik Degussa company brand AEROSIL series include one or more of AEROSIL380, AEROSIL 300, AEROSIL 200, AEROSIL R8200, AEROSIL R812, AEROSIL R202, AEROSIL R972, and AEROSIL R974.
The WACKER brand HDK series includes one or more of H13, H15, H20, N20, V15, C10, T30, and T4.
The CABOT company brand CAB-O-SIL series includes one or more of TS-530, TS-610, TS-720, LM-150, M-5, and EH-5.
In some embodiments, the coupling agent is selected from silane coupling agents.
In a preferred embodiment, the coupling agent comprises Dow Corning brand Z series, momentive (Michaelis-Mei. U.S.) brand A-151, A-171, A-186, A-187, A-189, A-174, A-1524, A-1160, and A-1230, one or more of the japanese letter brands KBM503, KBM903, KBM603 and KBM 1003.
The Dow Corning brand Z series includes one or more of Z-6011, Z-6043, Z-6030, Z-6040, and Z-6518.
In some embodiments, the adhesion promoter is selected from phosphate ester promoters.
In a preferred embodiment, the adhesion promoter comprises one or more of EM39 of changxing chemistry, SR9050, SR9051 of hadamard, and PM-2 of japan chemical.
In some embodiments, the wetting agent is selected from polyether siloxane based wetting agents.
In a preferred embodiment, the wetting agent comprises one or more of Digao brand TEGO Wet270 and TEGO Wet280, and German Pick brand BYK-301 and BYK-333.
Another embodiment of the present application provides a method for preparing the UV gel as described above, comprising the following steps:
drying the active diluent for later use; controlling the ambient temperature to be 25 ℃ and the relative humidity to be less than or equal to 50%; selecting a reaction kettle with a high-speed dispersing device and a constant-temperature interlayer, adding the modified photosensitive resin and the reactive diluent, and stirring at a constant temperature of 40 ℃ until the modified photosensitive resin is completely dissolved; then adding a wetting agent, a coupling agent and an adhesion promoter, and uniformly stirring; keeping the temperature to 30 ℃, adding thixotropic agent, dispersing at high speed for 2 hours, and ensuring that the edge linear speed of the high-speed disperser reaches 10m/S; adding a photoinitiator, and stirring until the photoinitiator is completely dissolved; vacuumizing (the vacuum degree is more than 0.095 MPa) until bubbles in the glue completely disappear; detecting, filtering and packaging.
The application is further illustrated by the following examples.
Example 1
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
the ultraviolet curing adhesive is prepared by the following steps: selecting a reaction kettle with a high-speed dispersing device and a constant-temperature interlayer, adding the component A and the component B, and stirring at a constant temperature of 40 ℃ until the component A is completely dissolved; then adding the component D, the component E and the component G, and uniformly stirring; keeping the temperature to 30 ℃, adding the component F, dispersing at high speed for 2 hours, and ensuring that the edge linear speed of the high-speed disperser reaches 10m/S; adding the component C, and stirring for 30 minutes until the component C is completely dissolved; vacuumizing for 15 minutes, and ensuring that the vacuum degree is less than 0.01MPa until bubbles disappear; detecting, filtering with 200 mesh filter screen, and packaging according to required specification.
Example 2
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 3
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 4
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 5
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 6
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 7
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Example 8
The embodiment is used for explaining the UV adhesive and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Comparative example 1
The comparative example is used for comparing and explaining the UV adhesive disclosed by the application and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
wherein the modified photosensitive resin having the designation CNUVE151NS is available from SARTOMER, U.S.A.
A photo-curable adhesive was prepared in the same manner as in example 1.
Comparative example 2
The comparative example is used for comparing and explaining the UV adhesive disclosed by the application and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Comparative example 3
The comparative example is used for comparing and explaining the UV adhesive disclosed by the application and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Comparative example 4
The comparative example is used for comparing and explaining the UV adhesive disclosed by the application and the preparation method thereof, and the ultraviolet curing adhesive is prepared according to the following components by weight:
a photo-curable adhesive was prepared in the same manner as in example 1.
Performance testing
The following performance tests were performed on the UV adhesives prepared in examples 1 to 8 and comparative examples 1 to 4 described above:
and (3) measuring the viscosity of the ultraviolet curing adhesive:
reference standard: ASTM D3795-2000a (2012)
Detection instrument: BROOKFIELD laminometer, CAP2000+
Test conditions: the temperature is 25 ℃, the needle number is 6#, and the rotating speed is 5RPM
Hardness measurement after curing of the adhesive:
using a die with a groove with a diameter of 50mm and a depth of 3mm, pouring the adhesive into the die, scraping off excessive glue, placing the die into a UV curing machine for 900mJ energy curing, standing the manufactured sample in a room temperature environment with a relative humidity of 50% at 23 ℃ for 4 hours, superposing the two pieces (with a thickness of not less than 6 mm), and measuring the hardness of the sample by using a Shore D durometer.
Determination of adhesive bond strength of cured adhesive:
cutting a transparent PC board with the thickness of 0.5mm into square slices with the thickness of 5X 5mm; glue is coated on a glass slide, and the coating thickness is 0.1mm; placing PC sheet, bonding area is 5×5mm, and adhesive layerThickness 0.1mm; using an illuminance of 100mW/cm 2 The ultraviolet light wave band 200 nm-450 nm mercury lamp irradiates for 9 seconds, and the accumulated curing energy is 900mJ/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the And standing the cured sample at room temperature of 25 ℃ for 2 hours, and measuring.
The bonding strength (in MPa) of the glue was measured by pushing the PC sheet at a speed of 2mm/min parallel to the bonding surface until it breaks and falls off using a multifunctional push-pull tester (Nordson Dage, model DAGE 4000, manufacturer, UK) at 25℃at room temperature.
Determination of adhesive volatility:
solidifying the glue into a spline with the thickness of 10 multiplied by 2 multiplied by 1mm, weighing about 2g of sample pieces, placing the sample pieces into a 100ml conical flask, and covering a clean glass slide on a bottleneck; placing the conical flask on a heating plate, setting the heating temperature to 90 ℃ and heating for 48 hours; after heating, observing whether the bottleneck glass slide has obvious pollutants, and if so, obtaining a result NG.
Adhesive reliability test:
cutting a transparent PC board with the thickness of 1.5mm into rectangular slices with the thickness of 100mm multiplied by 25 mm; coating glue on one end of the PC sheet, overlapping the PC sheet by the other sheet, wherein the bonding area is 25mm multiplied by 12.5mm, and the thickness of the glue layer is 0.1mm; using an illuminance of 100mW/cm 2 The ultraviolet light wave band 200 nm-450 nm mercury lamp irradiates for 9 seconds, and the accumulated curing energy is 900mJ/cm 2 . And (3) placing the solidified sample into a cold and hot impact test box, setting-40 ℃/1-80 ℃/1 hour as one cycle, and testing for 50 cycles. The change in shear strength is detected and the result is NG with the change.
Immersing the cured sample into deionized water, immersing at room temperature of 25 ℃ for 240 hours, observing whether the adhesive layer is cracked or not, detecting the change of the shearing strength by using an electronic universal tensile machine (manufactured by LABSANS, model LD 23-104), wherein the attenuation of the shearing strength is more than 40%, and obtaining a result NG.
The test results obtained are filled in Table 1.
TABLE 1
As can be seen from comparison of the test results of examples 1 to 5 and comparative examples 1 to 4 in Table 1, the UV adhesive prepared by using specific grades of Japanese Industrial chemical Co., ltd., no. UN-9200A, japanese chemical industry Co., ltd., KEA-24 and Taiwan Changxing Industrial chemical Co., ltd., taiwan area, DR-U299, as modified photosensitive resins, has higher viscosity, hardness and adhesive strength, and better reliability, and simultaneously effectively inhibits volatilization of organic matters of the UV adhesive, and as can be seen from the test results of comparative documents 1 to 4, the absence of any one of the preferred modified photosensitive resins of the present application causes insufficient performance of the UV adhesive in various aspects, thereby failing to produce better application effects.
As can be seen from comparing the test results of examples 5 to 8 in Table 1, on the basis of the modified photosensitive resin provided by the present application, the co-addition of isobornyl acrylate (IBXA, organic chemical Co., ltd., japan), N-dimethylacrylamide (DMAA, japan) and tri (2-hydroxyethyl) isocyanurate triacrylate (SR 368NS, SARTOMER Co., ltd.) has a good auxiliary effect for improving the volatility resistance and reliability of UV adhesives.
The UV glue prepared in the above embodiments 1-8 and comparative examples 1-4 is applied to a monitoring camera assembly, and the specific implementation method is as follows:
the corresponding position of the metal outer frame of the monitoring camera is coated with UV glue, the outer diameter of the glue groove is 37mm, the inner diameter of the glue groove is 30mm, the glue dispensing width is 3.5mm, the glue consumption of a single point is controlled to be 0.08-0.10 g, and the glue dispensing height is about 0.5mm;
placing the glass lens or the PC lens at the corresponding dispensing position to ensure that the lens and the PC lens are in complete contact with the adhesive without gaps or bubbles;
the device is initially fixed by using a UV-LED light source with the dominant wavelength of 365nm, and the irradiation power of UV lamp light is 200mW/cm 2 Irradiation time is 3S, irradiation energy is 600mJ/cm 2
Using a UV mercury lamp having a dominant wavelength of 365nmPerforming secondary curing on the device, wherein the irradiation power of UV light is 100mW/cm 2 Irradiation time is 5S, irradiation energy is 500mJ/cm 2
The appearance of the cured sample was visually checked for foaming, cracking and peeling. If the appearance is normal, the test of volatility, adhesive strength, water resistance, thermal shock resistance and air tightness is carried out, the test method is as follows, and the test results are shown in table 2.
Determination of volatility:
and placing the manufactured sample in a 90 ℃ oven, continuously baking for 48H, and detecting the change of the light transmittance of the glass lens. And if the light transmittance is reduced by more than 5%, judging that the test result is NG.
Measurement of adhesion:
placing the manufactured sample on a pushing machine, and applying pushing force on the glass lens, wherein the pushing force is more than 20
Kg-f, judging result OK, smaller than 20Kg-f, result NG.
Determination of Water resistance:
the prepared sample is placed in deionized water at 25 ℃ and soaked continuously for 10 days (240H), then the adhesive force of the glass lens is detected, and if the adhesive force is smaller than 10Kg-f, the result is NG.
Measurement of thermal shock resistance:
placing the manufactured sample in a cold and hot impact test box, setting-40 ℃/1-80 ℃/1 hour as one cycle, and testing 50 cycles; if the glue layer is whitish, cracked, air bubble or the adhesion force is less than 10Kg-f, then NG is the result.
Measurement of air tightness:
and (3) carrying out underwater airtight inflation on the sample which passes the water resistance and cold and hot impact tests, observing whether the glue bonding part has air leakage phenomenon or not, and judging the air tightness test result NG if the glue bonding part has air leakage.
TABLE 2
As can be seen from comparing the test results of examples 1-5 and comparative examples 1-4 in Table 2, when the UV adhesive prepared from the specific-brand modified photosensitive resin provided by the application is applied to camera assembly, the UV adhesive has higher adhesive force, better water resistance and thermal shock resistance, and simultaneously effectively inhibits the volatilization of organic matters of the UV adhesive, and avoids the pollution to the camera lens.
As can be seen from comparing the test results of examples 5 to 8 in Table 2, on the basis of the modified photosensitive resin provided by the present application, the co-addition of isobornyl acrylate (IBXA, organic chemical Co., ltd., japan), N-dimethylacrylamide (DMAA, japan) and tris (2-hydroxyethyl) isocyanurate triacrylate (SR 368NS, SARTOMER Co., ltd.) has a good auxiliary effect on the improvement of the performance of UV glue.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.

Claims (6)

1. The UV adhesive is characterized by comprising the following components in parts by weight:
40-60 parts of modified photosensitive resin, 30-60 parts of reactive diluent, 2-8 parts of photoinitiator, 3-10 parts of thixotropic filler, 0.5-5 parts of coupling agent, 0.5-5 parts of adhesion promoter and 0.1-0.4 part of wetting agent;
wherein the modified photosensitive resin comprises the following components in parts by weight:
10-20 parts of Japanese root chemical industry Co Ltd, 5-15 parts of Japanese chemical industry Co Ltd, and DR-U29920-40 parts of Taiwan Changxing chemical industry Co Ltd in Taiwan area;
the reactive diluent comprises the following components in parts by weight:
20-25 parts of IBXA (organic chemical trademark of Osaka, japan, xingzhou Co., ltd.) brand, 20-25 parts of DMAA (chemical trademark of Santa Classification of Japan) and 3-5 parts of SR368NS (chemical trademark of SARTOMER, america).
2. The UV glue of claim 1, wherein the photoinitiator comprises one or more of α, α -dimethylbenzoketal, α -diethoxyacetophenone, 2-hydroxy-2-methyl-phenylpropanone-1, 1-hydroxy-cyclohexylbenzophenone, 2-hydroxy-2-methyl-p-hydroxyethyl etherphenylpropanone-1, 2-methyl-1- (4-methylthiophenyl) -2-morpholinophenone-1, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1, 2,4,6- (trimethylbenzoyl) diphenyl phosphine oxide, and bis (2, 4, 6-trimethylbenzoyl) phenyl phosphine oxide.
3. The UV gel of claim 1, wherein the thixotropic filler comprises one or more of Evonik Degussa company trade mark AEROSIL series, WACKER trade mark HDK series, and CABOT company trade mark CAB-O-SIL series.
4. The UV glue of claim 1, wherein the coupling agent comprises one or more of dow corning brand Z series, momentive (U.S. michaux) brand a-151, a-171, a-186, a-187, a-189, a-174, a-1524, a-1160, and a-1230, japan signal brands KBM503, KBM903, KBM603, and KBM 1003.
5. The UV glue of claim 1, wherein the adhesion promoter comprises one or more of EM39 of changxing chemistry, SR9050 of hadamard, SR9051, and PM-2 of japan chemical.
6. The UV glue of claim 1, wherein the wetting agent comprises one or more of the diego marks TEGO Wet270 and TEGO Wet280, the german marks BYK-301 and BYK-333.
CN202110182513.9A 2021-02-08 2021-02-08 UV adhesive Active CN112940676B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006342222A (en) * 2005-06-08 2006-12-21 Mitsuyoshi Sato Light-curable resin composition
CN105820794A (en) * 2016-05-30 2016-08-03 三友(天津)高分子技术有限公司 Inorganic filler modified ultraviolet curing adhesive
CN106281052A (en) * 2015-05-20 2017-01-04 北京鼎材科技有限公司 A kind of photocuring Adhesive composition
CN111234712A (en) * 2019-12-23 2020-06-05 深圳日高胶带新材料有限公司 UV-cured optical pressure-sensitive adhesive and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006342222A (en) * 2005-06-08 2006-12-21 Mitsuyoshi Sato Light-curable resin composition
CN106281052A (en) * 2015-05-20 2017-01-04 北京鼎材科技有限公司 A kind of photocuring Adhesive composition
CN105820794A (en) * 2016-05-30 2016-08-03 三友(天津)高分子技术有限公司 Inorganic filler modified ultraviolet curing adhesive
CN111234712A (en) * 2019-12-23 2020-06-05 深圳日高胶带新材料有限公司 UV-cured optical pressure-sensitive adhesive and preparation method thereof

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