CN118048090A - UV/EB dual-cured black three-proofing paint and preparation method thereof - Google Patents
UV/EB dual-cured black three-proofing paint and preparation method thereof Download PDFInfo
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- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims description 4
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 claims description 4
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 4
- VEBCLRKUSAGCDF-UHFFFAOYSA-N ac1mi23b Chemical compound C1C2C3C(COC(=O)C=C)CCC3C1C(COC(=O)C=C)C2 VEBCLRKUSAGCDF-UHFFFAOYSA-N 0.000 claims description 4
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- 238000002156 mixing Methods 0.000 claims description 4
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 claims description 3
- BTJPUDCSZVCXFQ-UHFFFAOYSA-N 2,4-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC(CC)=C3SC2=C1 BTJPUDCSZVCXFQ-UHFFFAOYSA-N 0.000 claims description 3
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- YLGYACDQVQQZSW-UHFFFAOYSA-N n,n-dimethylprop-2-enamide Chemical compound CN(C)C(=O)C=C YLGYACDQVQQZSW-UHFFFAOYSA-N 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
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- Paints Or Removers (AREA)
Abstract
The invention discloses a UV/EB dual-cured black three-proofing paint and a preparation method thereof, wherein the paint comprises the following raw material components in parts by weight: 100 parts of aliphatic polyurethane acrylate; 70-80 parts of acrylate monomer; 10-25 parts of propylene modifier; 30-50 parts of UV light curing acrylic monomers; 5-15 parts of black filler; the black filler is a mixture of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 1: 0.5-2. Under the condition that the apparent color of the three-proofing paint is black, the three-proofing paint can carry out polymerization reaction under the dual actions of UV and EB, and the glue has good curing degree, shearing strength and high temperature and high humidity resistance after curing.
Description
Technical Field
The invention belongs to the technical field of paint surface coatings, relates to black three-proofing paint, and in particular relates to UV/EB dual-cured black three-proofing paint and a preparation method thereof.
Background
Printed Circuit Boards (PCBs) are fabricated with integrated circuits, transistors, diodes, passive components (e.g., resistors, capacitors, connectors, etc.) and other various electronic components, and are connected by wires to form electrical signal connections and their intended functions. The printed circuit board may be composed of one, two or more layers of circuitry made of a dielectric core material having poor electrical conductivity to ensure pure electrical transmission, with additional metal and dielectric layers spaced as needed. The standard dielectric material for circuit boards is a flame retardant composite consisting of woven fiberglass cloth and epoxy, known as FR-4, while the metal traces and planes of the circuit are typically composed of copper.
Three-proofing paint (also called circuit board coating glue and insulating paint) is used for protecting the circuit board and related equipment from corrosion of the environment. The coating glue is coated on the surface of the circuit board to form a layer of light and flexible three-proofing protective film with the thickness of about 25-250 mu m, and sensitive electrical components and parts can be isolated from severe environments, so that the reliability of the circuit board is improved, the safety coefficient of the circuit board is increased, and the service life of the circuit board is ensured. The Chinese patent publication No. CN109749698A discloses a preparation method of a double-component transparent LED organosilicon coating adhesive, which comprises an A component and a B component, wherein the A component comprises alpha-omega-dihydroxy polydimethylsiloxane and a diluent in a weight ratio: (50.0-75.0): (25.0-50.0), wherein the component B comprises a cross-linking agent, a diluent, a tackifier, a catalyst and an anti-yellowing agent in weight ratio: (35.0-50.0): (20.0-40.0): (15.0-30.0): (0.0-0.3): (0.5-1.5), and the component A and the component B are mixed according to the weight ratio of 10:1. The preparation of the double-component transparent LED organosilicon coating adhesive has the advantages of low viscosity, good transparency, good elasticity, good adhesion, good yellowing resistance, good weather resistance, no corrosiveness and environmental friendliness, can adapt to the alternating change of temperature and height of an LED display screen in use, can not crack, can not cause the light transmittance of an LED lamp to be reduced due to yellowing of an adhesive layer, and can play a long-term effective protection role on the display screen module. The silicone coating is transparent.
With the continuous development of science and technology, more and more enterprises tend to use black coating glue in order to keep secret the circuit design on the PCB and the used electronic components and parts, avoid the copy and copy of competitors with low cost. Conventional curing methods of the coating adhesive are classified into thermal curing and photo curing, the thermal curing may have thermal damage to electronic components (some thermally sensitive electronic components are not suitable), and the heating and cooling require time, and a dam process is required on the PCB substrate while the thermal curing is performed to prevent the outflow of the adhesive during the thermal curing. Thus, the unit Hour capacity UPH (English is called Units Per Hour) of the whole heating process is small. Radiation polymerization can significantly increase UPH, which is of particular advantage for this particular application.
Electron Beam (EB) and Ultraviolet (UV) are the two most common initiation methods for commercial radiation polymerization. While both UV and EB initiation are radiation polymerized, the particles that initiate the reaction and their interactions with the species result in distinct energy deposition profiles that can affect the proper application of each of the initiation methods. During ultraviolet polymerization, energy deposition is governed by the beer-lambert law, and energy deposition is always greatest at the surface and then exponentially decreases deep into the film or coating, making the polymer surface stronger than its internal strength (even in the case of insufficient internal polymer strength). Unlike photopolymerization, the force of electron energy accelerated deposition results in EB polymerization being more susceptible to oxygen inhibition, but rather superior in curing thick or opaque films; since oxygen inhibition is a problem during EB polymerization, most industrial processes use nitrogen inertization to ensure acceptable surface cure; however, continuous nitrogen flows are costly and there is a need to find a cheaper way to overcome oxygen inhibition.
Disclosure of Invention
Based on the defects, the invention provides the UV/EB dual-cured black three-proofing paint.
In order to achieve the purpose, the invention provides a UV/EB dual-cured black three-proofing paint which comprises the following raw material components in parts by weight:
the black filler is a mixture of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 1: 0.5-2, and the absorption wavelength of the photoinitiator is 320-350nm.
Optimally, the functionality of the aliphatic polyurethane acrylate is 2-6, and the molecular weight is 1×10 4～5×104.
Further, the refractive index of the aliphatic polyurethane acrylate is 1.40-1.50, and the glass transition temperature is 83.0-85.0 ℃.
Further, the aliphatic urethane acrylate is a mixture of one or more selected from the group consisting of Changxing DR-U282, changxing DR-U384, changxing DR-U386, changxing DR-U388, changxing DR-U331 and Sadama CN8881 NS.
Still further, the acrylic monomer is a mixture of one or more selected from the group consisting of isobornyl methacrylate, isodecyl acrylate, tetrahydrofurfuryl acrylate, and isobornyl acrylate.
Specifically, the propylene modifier is a mixture composed of one or more selected from hydroxyethyl methacrylate, acryloylmorpholine and N, N-dimethylacrylamide.
Specifically, the UV light-cured acrylic ester monomer is a mixture composed of one or more selected from tricyclodecane dimethanol diacrylate, dodecyl acrylate and triethylene glycol dimethacrylate.
Optimally, the photoinitiator is one selected from the group consisting of photoinitiator 369, photoinitiator 907, photoinitiator TPO, photoinitiator BMS, photoinitiator ITX, photoinitiator 184, photoinitiator DETX, photoinitiator 1173, and photoinitiator BDK.
Specifically, the material comprises the following raw material components in parts by weight:
The invention also aims to provide a preparation method of the UV/EB dual-cured black three-proofing paint, which comprises the following steps: dispersing a formula amount of the black filler in a formula amount of the acrylic monomer to form a black slurry; and uniformly mixing the black slurry with the aliphatic polyurethane acrylic ester, the propylene modifier, the photoinitiator and the UV light curing acrylic ester monomer according to the formula amount.
According to the UV/EB dual-cured black three-proofing paint, by adopting components with specific types and contents, the glue can be subjected to polymerization reaction under the dual actions of UV and EB under the condition that the apparent color of the glue is black, and the glue has good curing degree, shearing strength and high temperature and high humidity resistance after being cured.
Detailed Description
The invention relates to a UV/EB dual-cured black three-proofing paint which comprises the following raw material components in parts by weight: 100 parts of aliphatic polyurethane acrylate; 70-80 parts of acrylate monomer; 10-25 parts of propylene modifier; 30-50 parts of UV light curing acrylic monomers; 3-10 parts of photoinitiator; 5-15 parts of black filler; the black filler is a mixture of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 1: 0.5-2, and the absorption wavelength of the photoinitiator is 320-350nm. By adopting the components with specific types and contents, the glue can be subjected to polymerization reaction under the dual actions of UV and EB under the condition that the apparent color of the glue is black, and has good curing degree, shearing strength and high temperature and high humidity resistance after being cured.
The functionality of the aliphatic polyurethane acrylate is preferably 2-6, and the molecular weight is preferably 1 multiplied by 10 4～5×104; the refractive index of the aliphatic polyurethane acrylate is preferably 1.40-1.50, and the glass transition temperature is preferably 83.0-85.0 ℃; in particular, the aliphatic urethane acrylate is preferably a mixture of one or more selected from the group consisting of Changxing DR-U282, changxing DR-U384, changxing DR-U386, changxing DR-U388, changxing DR-U331, and sand-gammaCN 8881 NS.
The acrylic monomer is preferably a mixture of one or more selected from isobornyl methacrylate, isodecyl acrylate, tetrahydrofurfuryl acrylate and isobornyl acrylate. The propylene modifier is preferably a mixture of one or more selected from the group consisting of hydroxyethyl methacrylate, acryloylmorpholine and N, N-dimethylacrylamide. The UV light curing acrylic monomer is preferably a mixture of one or more selected from tricyclodecane dimethanol diacrylate, dodecyl acrylate and triethylene glycol dimethacrylate. The photoinitiator is one selected from the group consisting of photoinitiator 369, photoinitiator 907, photoinitiator TPO, photoinitiator BMS, photoinitiator ITX, photoinitiator 184, photoinitiator DETX, photoinitiator 1173 and photoinitiator BDK, and is optimally photoinitiator 369.
The UV/EB dual-cured black three-proofing paint optimally comprises the following raw material components in parts by weight: 100 parts of aliphatic polyurethane acrylate; 76 parts of acrylate monomer; 24 parts of propylene modifier; 40 parts of UV light curing acrylic monomer; 5 parts of a photoinitiator; 6-12 parts of black filler, so that the physicochemical property of the black coating adhesive can be improved.
The preparation method of the UV/EB dual-cured black three-proofing paint comprises the following steps: dispersing a formula amount of the black filler in a formula amount of the acrylic monomer to form a black slurry; and uniformly mixing the black slurry with the aliphatic polyurethane acrylic ester, the propylene modifier, the photoinitiator and the UV light curing acrylic ester monomer according to the formula amount.
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described in the following, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments obtained under the premise of equivalent changes and modifications made by those skilled in the art based on the embodiments of the present invention shall fall within the scope of the present invention.
Examples 1 to 10, comparative examples 1 to 10
Examples 1-10 and comparative examples 1-10 each provide a UV/EB dual cure black tri-proof paint with the raw material components and contents as shown in Table 1.
TABLE 1 raw materials formulation table (unit g) for black three-proofing paint in examples 1-10 and comparative examples 1-10
Note that: isobornyl methacrylate is chang EM90, isodecyl acrylate (ISODA) is chang EM219, tetrahydrofurfuryl acrylate (THFA) is chang EM214, and isobornyl acrylate (IBOA) is chang EM70; hydroxyethyl methacrylate (HEMA) is purchased from guangda, acryloylmorpholine (ACMO) is purchased from kohl, N-Dimethylacrylamide (DMAA) is purchased from kohl; dodecyl acrylate is SR335, tricyclodecane dimethanol diacrylate is SR833NS, triethylene glycol dimethacrylate is SR205 NS (all from sartomer); both carbon black and white carbon black were purchased from cabot.
Note that: the raw material formulations in example 1 and comparative example 8 were identical, except that the polymerization conditions at the subsequent application were different: in example 1, UV polymerization+EB polymerization, and in comparative example 8, EB polymerization alone,
The UV/EB dual-cured black three-proofing paint is prepared by the following method: dispersing a formula amount of the black filler in a formula amount of the acrylic monomer to form a black slurry; and uniformly mixing the black slurry with the aliphatic polyurethane acrylic ester, the propylene modifier and the UV light curing acrylic ester monomer according to the formula amount.
The UV/EB dual-cured black coating adhesive was then tested for performance as follows:
(1) Viscosity: this experiment uses a bovingfei (Brookfield) model rotary viscometer to measure the viscosity of the sunscreen composition (typically requiring a viscosity of less than 3000 CPs) using a CP51 type rotator head at an ambient temperature of 25 ℃.
(2) Optical density OD value: for the shading film material, the experiment adopts an ultraviolet-visible light spectrophotometer to test the average light transmittance T% of the sample in the wavelength range of 400 nm-700 nm. The optical density OD value was calculated according to the formula od=log10 (1/T%), with a higher OD value indicating a better light blocking performance of the sample (a light blocking film material OD value of greater than 2 is generally required) (the optical density OD value test was performed after a storage test, which is an aging at 40 ℃ for 14 days).
(3) Degree of cure: the present experiment uses an infrared spectrometer to test the depth distribution of double bond conversion after curing of a 200 μm thick sample of the opacifying composition. The test results require that the double bond conversion rate of each layer of sample is more than 90 percent (i.e. the curing degree reaches more than 90 percent).
(4) Hardness: the hardness of the shading film material under the thickness of a 4mm sample is tested by using a Shore hardness tester A or D type. Because of the thinness of the single layer film, the test is generally carried out by adjusting the thickness to 4mm in a multilayer superposition mode. And comparing the readings corresponding to the A type number and the D type number according to the test result. The larger the number, the higher the hardness of the sample. If the two numbers are in the same level, the hardness is higher with the larger number.
(5) Shear strength: the shearing strength of the light shielding film material is tested by a universal tensile testing machine. In the test process, the upper limit of the force sensor is 10000N, and the mechanical pulling speed is adjusted to be 100mm/min. Recording the separation condition of the substrate and the substrate under the tensile force of the sample, and dividing the maximum tensile force value of the substrate separation by the bonding area to obtain the shearing strength of the shading film.
(6) High temperature and high humidity resistance: the test is carried out at a high temperature of 85 ℃ and a relative humidity of 85%, and the accelerated aging of the shading film material is kept for longer than 500 hours. The following evaluations were performed on the samples after the test: 1. color change: no obvious chromatic aberration exists; 2. shear strength: the drop amplitude was controlled within 50% compared to before testing.
(7) Water absorption rate: the test selects a light shielding film sample with a size of 200 μm thick and a specification of 5cm×5 cm. The sample was immersed in pure water at normal temperature for 24 hours. The mass m1 and m2 were obtained by weighing the samples before and after the test, respectively. According to the formula: water absorption= (m 2-m 1)/m1×100%, and water absorption corresponding to the difference in mass of the sample before and after soaking was calculated. Wherein: m1 is the mass of the sample before soaking, m2 is the mass of the sample after soaking, and the water absorption rate of the sample is required to be not more than 1.5%.
(8) The curing mode is as follows: the test is carried out on samples for UV polymerization and EB polymerization tests. UV polymerization conditions: the light source is an LED cold light source with the wavelength of 365nm, the light intensity is 60mW/cm 2, and the irradiation time is 40s; EB polymerization conditions: the process was performed on an EB Lab200 electron beam processing system, and the acceleration voltage was set to 200keV and the movement speed was set to 3m/min without opening nitrogen aeration.
The performance of each of the UV/EB dual-cured black coating adhesives in Table 1 was tested as described above, and the results are shown in Table 2.
TABLE 2 Performance test Table of Black coating gel in examples 1-10 and comparative examples 1-10
The foregoing is merely a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; while the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (10)
1. The UV/EB dual-cured black three-proofing paint is characterized by comprising the following raw material components in parts by weight:
100 parts of aliphatic polyurethane acrylate;
70-80 parts of acrylate monomer;
10-25 parts of propylene modifier;
30-50 parts of UV light curing acrylic monomers;
3-10 parts of a photoinitiator;
5-15 parts of black filler;
The black filler is a mixture of carbon black and white carbon black, and the mass ratio of the carbon black to the white carbon black is 1: 0.5-2, wherein the absorption wavelength of the photoinitiator is 320-350nm.
2. The UV/EB dual-cure black tri-proof paint as set forth in claim 1, wherein: the functionality of the aliphatic polyurethane acrylate is 2-6, and the molecular weight is 1 multiplied by 10 4~5×104.
3. The UV/EB dual-cure black tri-proof paint as set forth in claim 2, wherein: the refractive index of the aliphatic polyurethane acrylate is 1.40-1.50, and the glass transition temperature is 83.0-85.0 ℃.
4. The UV/EB dual-cure black tri-proof paint as set forth in claim 2, wherein: the aliphatic polyurethane acrylate is a mixture of one or more selected from the group consisting of Changxing DR-U282, changxing DR-U384, changxing DR-U386, changxing DR-U388, changxing DR-U331 and Shadama CN8881 NS.
5. The UV/EB dual-cure black tri-proof paint as claimed in claim 1 or 4, wherein: the acrylic acid monomer is one or a mixture of more selected from isobornyl methacrylate, isodecyl acrylate, tetrahydrofurfuryl acrylate and isobornyl acrylate.
6. The UV/EB dual-cured black tri-proof paint as set forth in claim 5, wherein: the propylene modifier is a mixture of one or more selected from hydroxyethyl methacrylate, acryloylmorpholine and N, N-dimethylacrylamide.
7. The UV/EB dual-cured black tri-proof paint as set forth in claim 6, wherein: the UV light curing acrylic ester monomer is a mixture composed of one or more selected from tricyclodecane dimethanol diacrylate, dodecyl acrylate and triethylene glycol dimethacrylate.
8. The UV/EB dual-cured black-coating paste of claim 1, wherein: the photoinitiator is one selected from the group consisting of photoinitiator 369, photoinitiator 907, photoinitiator TPO, photoinitiator BMS, photoinitiator ITX, photoinitiator 184, photoinitiator DETX, photoinitiator 1173, and photoinitiator BDK.
9. The UV/EB dual-cured black three-proofing paint according to claim 7, which is characterized by comprising the following raw material components in parts by weight:
100 parts of aliphatic polyurethane acrylate;
76 parts of acrylate monomer;
24 parts of propylene modifier;
40 parts of UV light curing acrylic monomer;
5 parts of a photoinitiator;
And 6-12 parts of black filler.
10. The method for preparing the UV/EB dual-cured black three-proofing paint according to any one of claims 1 to 9, which is characterized by comprising the following steps:
Dispersing a formula amount of the black filler in a formula amount of the acrylic monomer to form a black slurry;
And uniformly mixing the black slurry with the aliphatic polyurethane acrylic ester, the propylene modifier, the photoinitiator and the UV light curing acrylic ester monomer according to the formula amount.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410064765.5A CN118048090A (en) | 2024-01-17 | 2024-01-17 | UV/EB dual-cured black three-proofing paint and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410064765.5A CN118048090A (en) | 2024-01-17 | 2024-01-17 | UV/EB dual-cured black three-proofing paint and preparation method thereof |
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| Publication Number | Publication Date |
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| CN118048090A true CN118048090A (en) | 2024-05-17 |
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| Country | Link |
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| CN (1) | CN118048090A (en) |
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