CN114574091A - UV-moisture dual-curing three-proofing paint for optical module and preparation method and application thereof - Google Patents
UV-moisture dual-curing three-proofing paint for optical module and preparation method and application thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
- C08G18/3863—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur containing groups having sulfur atoms between two carbon atoms, the sulfur atoms being directly linked to carbon atoms or other sulfur atoms
- C08G18/3865—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur containing groups having sulfur atoms between two carbon atoms, the sulfur atoms being directly linked to carbon atoms or other sulfur atoms containing groups having one sulfur atom between two carbon atoms
- C08G18/3868—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur containing groups having sulfur atoms between two carbon atoms, the sulfur atoms being directly linked to carbon atoms or other sulfur atoms containing groups having one sulfur atom between two carbon atoms the sulfur atom belonging to a sulfide group
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Abstract
The invention relates to the technical field of optical module packaging, in particular to a UV-moisture dual-curing three-proofing paint for an optical module and a preparation method and application thereof.A self-repairing agent, tackifying resin and NCO end-capped polymer dihydric alcohol are taken as base materials, a low-odor low-irritation active diluent is adopted, and a photoinitiator, a sensitizer and an auxiliary agent are matched to prepare the self-repairing UV-moisture dual-curing three-proofing paint; the invention adopts a UV and moisture dual curing mechanism, has high curing speed and high curing efficiency, and can cure the non-illuminated place by moisture. The UV-moisture dual-curing three-proofing paint can be coated on the surface of the optical module component by adopting a spraying or brushing process, the coating thickness is 1-300 mu m, the coating process is simple, the coating efficiency is high, the production cost is low, and the formed UV-moisture dual-curing three-proofing paint film has excellent adhesive force, wear resistance, humidity and heat resistance, salt mist resistance, acid and alkali resistance, impact resistance and electrical insulation performance, and is suitable for optical modules and communication equipment.
Description
Technical Field
The invention relates to the technical field of optical module packaging, in particular to UV-moisture dual-curing three-proofing paint for an optical module and a preparation method and application thereof.
Background
With the increasing use frequency of the optical module and the increasing transmission requirement of the optical module on heat, the expected thickness of the isolation layer is thinner and thinner, the chemical resistance is better and better, and the optical module has excellent high and low temperature resistance, ultraviolet resistance, ozone aging resistance and electrical insulation performance. The polymer coating is usually used for protecting the surface of the material due to the characteristics of economy, easy coating, wide application range and the like, and can endow the material with good physical and chemical durability. Patent publication No. CN211928247U discloses a method for plating a polymer hydrophobic nano-film layer on the surface of an optical module PCBA and an optical device by using a PECVD method, which plays the role of water resistance, moisture resistance and salt fog resistance and can completely replace the existing ceramic or metal tube shell.
The three-proofing paint is a coating material with a special formula, and is coated on the surface of a circuit board to form a layer of transparent protective film, and the protective film can protect the circuit board from being damaged in the environments of humidity, mould, salt mist, chemical corrosion, high dust, vibration and the like, so that the reliability of the circuit board is improved, and the safety coefficient of the whole electronic element is increased. The patent with publication number CN111286251A discloses an environment-friendly three-proofing paint based on a synthetic rubber system, and a preparation method and application thereof, wherein the three-proofing paint comprises the following components: 10-30 parts of resin, 5-25 parts of tackifier, 0.1-3.0 parts of antioxidant, 45-85 parts of organic solvent and 0.001-0.01 part of fluorescent indicator, wherein the curing mode is solvent volatilization type curing at room temperature. The three-proofing paint based on the synthetic rubber system prepared by the method has the characteristics of stable property, short surface drying time, good glossiness, adhesion performance, corrosion resistance and the like. Although the three-proofing paint has good adhesion to various substrates, the solvent-containing three-proofing paint is not suitable for application in optical module assemblies.
The photocuring three-proofing paint solves the problem of VOC (volatile organic compounds) from the system, the active diluent also participates in the reaction while acting as a solvent, the state of the optimal conversion rate can be achieved by optimizing the formula, and the volatilization of small molecules is limited to the maximum extent. The patent with publication number CN110885625A discloses a preparation method of flame-retardant UV-moisture dual-curing polyurethane acrylate tri-proof paint, which adopts UV-moisture dual-curing polyurethane acrylate resin containing phosphate ester compounds as a base material, adopts a low-odor low-irritation reactive diluent and is matched with a photoinitiator. The UV three-proofing paint prepared by the method does not contain volatile organic solvents, but has insufficient adhesive force and poor chemical resistance, and cannot meet the requirement of chemical resistance of optical module components.
Therefore, there is a strong need for a solvent-free UV-moisture conformal coating for optical module assemblies, which has excellent air tightness, high chemical resistance, high humidity resistance, high cold and hot impact resistance, and the like, to meet the high-speed development requirements in the field of communications.
Disclosure of Invention
In order to solve the problems, the invention provides the UV-moisture dual-curing conformal coating for optical module packaging, and the preparation method and the application thereof.
In order to achieve the purpose, the technical scheme of the invention is that the UV-moisture dual-curing three-proofing paint for the optical module comprises the following components in parts by weight: 20-50 parts of reactive diluent, 10-30 parts of self-repairing agent, 5-15 parts of tackifying resin, 5-15 parts of NCO-terminated polymer dihydric alcohol, 1-5 parts of photoinitiator, 1-5 parts of photo sensitizer and 1-10 parts of auxiliary agent.
Further, the self-repairing agent is prepared from polyether glycol, hydroxyethyl acrylate, isophorone diisocyanate and 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol.
Further, in the preparation of the self-repairing agent, the amount of the isophorone diisocyanate substance is 1-8 times of the sum of the amounts of the other components in the self-repairing agent, the ratio of the amount of the 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol substance to the amount of the polyether diol substance is 1:3-3:1, and the ratio of the hydroxyethyl acrylate to the polyether diol substance is 1:2-2: 1.
Further, the molecular weight of the polyether glycol is 300-1000.
Preferably, the reactive diluent is at least one of hydroxyethyl acrylate, N-butyl acrylate, hydroxypropyl methacrylate, 2-dithiodiethanol diacrylate, isooctyl acrylate, pentaerythritol tetraacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, ethyl 3- (N, N-dimethylamino) acrylate, isobornyl acrylate, tetrahydrofuran acrylate, pentaerythritol tetra-3-mercaptopropionate, and pentaerythritol tetra (3-mercaptobutanoate).
Preferably, the tackifying resin is at least one of aliphatic urethane acrylate, aromatic urethane acrylate and polyether urethane acrylate, and specifically, the product model can be sartomer CN972, sartomer CN999, Changxing 615-100, Ruo FSP60359, Ruo FSP 8788, Ruo FSP 8531, Ruo FSP2159, Ruo Unicryl R9488, LuCure8730, LuCure8352, LuCure2651, Basff UA9030A and Basff LR 8987; the NCO-terminated polymer dihydric alcohol is one or a mixture of more than two of polycaprolactone dihydric alcohol, polytetrahydrofuran ether dihydric alcohol or polycarbonate dihydric alcohol with the 2-end capped by IPDI and the molecular weight of 1000-5000. The polymer diol with the NCO end capping does not participate in the reaction in the UV curing stage, so that the initial adhesion is stronger, and the later stage participates in moisture curing crosslinking, thereby enhancing the bonding performance.
Preferably, the photoinitiator is at least one of benzoin bis methyl ether, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1-hydroxycyclohexyl phenyl ketone and benzophenone; the light sensitizer is at least one of isopropyl thioxanthone, 9, 10-diethoxyanthracene, 9, 10-dibutoxyanthracene and N-vinyl carbazole.
Preferably, the auxiliary agent is one or more of tris (hydroxymethyl) phosphine oxide, tris (3-hydroxypropyl) phosphine oxide, tris (3-hydroxybutyl) phosphine oxide, bis (3-hydroxypropyl) n-propylphosphine oxide, bis (3-hydroxypropyl) n-butylphosphine oxide, bis (3-hydroxypropyl) sec-butylphosphine oxide, bis (3-hydroxypropyl) phenylphosphine oxide, bis (3-hydroxybutyl) ethylphosphine oxide, bis (3-hydroxybutyl) n-pentylphosphine oxide, methyltriethoxysilane, vinyltrimethoxysilane, KH550, KH560, KH570 and hydroquinone.
The invention also provides a preparation method of the UV-moisture dual-curing three-proofing paint for the optical module, which comprises the following steps:
1) adding polyether glycol, hydroxyethyl acrylate, isophorone diisocyanate and 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol into a reaction kettle, stirring at 80 ℃ for reaction for 3-5h, cooling and discharging to obtain a self-repairing agent;
2) adding an active diluent, tackifying resin, the self-repairing agent prepared in the step 1), NCO-terminated polymer dihydric alcohol, an auxiliary agent, a photoinitiator and a photo sensitizer into a dispersion machine, stirring for 0.5h at the rotating speed of 1000-3000rmp, and discharging;
3) and (3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the vacuum degree of-0.1 Mpa to obtain the UV-moisture dual-curing three-proofing paint.
The invention also provides application of the UV-moisture dual-curing conformal coating for the optical module, and the UV-moisture dual-curing conformal coating is coated on the surface of the optical module by adopting a spraying or brushing process, wherein the coating thickness is 1-300 mu m.
Compared with the prior art, the invention has the following beneficial effects:
(1) the polyurethane acrylate prepared from polyether diol, hydroxyethyl acrylate, isophorone diisocyanate and 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol is used as a self-made self-repairing agent, a disulfide bond is introduced into the main chain of the acrylate polyurethane resin, the self-repairing capability of a base material of the polyurethane resin is regulated, and the protective performance of the UV-moisture dual-curing three-proofing paint is improved; the disulfide bond is a relatively weak reversible covalent bond, can respond to light, heat and stimulus of redox substances, can be broken through a reduction reaction to obtain a sulfydryl, can be used for connecting sulfur atoms in the same or different disulfide bonds through an oxidation reaction to form the disulfide bond again, and can be subjected to an exchange reaction under a relatively mild condition when a small amount of mercaptan exists in a system;
(2) the self-made self-repairing agent is added into the UV-moisture dual-curing three-proofing paint, so that the paint can be repeatedly self-repaired and stably used for a long time, and the chemical corrosion resistance and the damp-heat resistance of the coating are obviously improved; by introducing a polyurethane structure and selecting polyether diol with proper molecular weight, the toughness of the three-proofing paint can be effectively improved and the adhesive force of the three-proofing paint to a base material can be improved; by adding the photo sensitizer, the three-proofing paint bottom layer photoinitiator can be activated to generate active factors after being irradiated by ultraviolet light, so that the concentration of the active factors at the bottom layer can be increased, and the curing performance can be further improved; the cross-linking density of the paint film can be effectively improved by introducing the polyfunctional reactive diluent, and the density, adhesive force and mechanical property of the paint film can be effectively improved; therefore, the UV-moisture dual-curing three-proofing paint has the advantages of excellent chemical resistance and mechanical property, good high-temperature and high-humidity resistance and impact resistance, particularly good adhesion to PCBA, lens and other base materials, high chemical resistance and the like;
(3) the UV-moisture dual-curing three-proofing paint disclosed by the invention has the advantages that by introducing the moisture-curable isocyanate group, a paint film can continuously react with moisture in the air after photocuring is finished, so that a cross-linked network is formed, the bonding effect is greatly improved, the UV-moisture dual-curing three-proofing paint has the characteristic of UV rapid curing, can be subjected to post-curing through moisture, enhances the adhesive force and chemical resistance, is an efficient room-temperature/low-temperature curing three-proofing paint, is suitable for popularization and use, and can be cured through the reaction of the isocyanate group and the moisture in the air even if a light shielding part is formed; in addition, the sulfydryl or the disulfide bond in the system can also have click chemical reaction with the double bonds which are not completely reacted under certain conditions, so that not only is the oxygen inhibition reduced, but also the crosslinking density of the system can be improved, and the performance of the three-proofing paint is further improved;
(4) the high-chemical-resistance UV-moisture dual-curing three-proofing paint for the optical module and the communication equipment has the advantages of simple preparation process, energy conservation, environmental protection, low cost and the like, and has wide application prospect;
(5) according to the invention, the UV-moisture dual-curing three-proofing paint is coated on the surface of the optical module component by adopting a spraying or brushing process, the obtained paint film has good chemical resistance, high temperature and high humidity resistance and good cold and hot impact resistance, especially has good adhesive force to PCBA, lens, metal, ceramic and other base materials, has the advantages of high chemical resistance and the like, and can meet the reliability requirement of the optical module component; and the coating process is simple, the coating efficiency is high, and the production cost is low.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples. It should be noted that the following implementation of the method is a further explanation of the present invention, and should not be taken as a limitation of the present invention.
Example 1
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 500), 100g of hydroxyethyl acrylate, 100g of 2, 2' -dithiodiethanol and 1000g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for 3 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 300g of ethyl 3- (N, N-dimethylamino) acrylate, 100g of pentaerythritol tetra-3-mercaptopropionate, 100g of LuCure8352, 300g of self-made self-repairing agent, 100g of NCO-terminated polycaprolactone diol (molecular weight 1000), 20g of bis (3-hydroxybutyl) ethyl phosphine oxide, 30g of KH560, 30g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 20g of isopropyl thioxanthone into a dispersion machine, stirring for 0.5h at the rotating speed of 2000rmp, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 2
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 300), 120g of hydroxyethyl acrylate, 100g of 2, 2' -dithiodiethanol and 2000g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for 4 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 300g of isobornyl acrylate, 100g of LuCure8352, 50g of LuCure2651, 200g of self-made self-repairing agent, 50g of NCO-terminated polycaprolactone diol (molecular weight is 1000), 30g of bis (3-hydroxybutyl) n-pentylphosphine oxide, 70g of KH560, 20g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 50g of isopropyl thioxanthone into a dispersing machine, stirring for 0.5h at the rotating speed of 1000mp, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 3
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 500), 150g of hydroxyethyl acrylate, 100g of 3, 3' -dithiobis (propionohydrazide) and 3000g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for 5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 300g of ethyl 3- (N, N-dimethylamino) acrylate, 100g of tetrahydrofuran acrylate, 100g of pentaerythritol tetra-3-mercaptopropionate, 100g of LuCure8352, 250g of self-made self-repairing agent, 100g of polycarbonate diol (molecular weight 2000) terminated by NCO, 30g of bis (3-hydroxybutyl) N-pentylphosphine oxide, 30g of KH570, 10g of 2-hydroxy-2-methyl-1-phenyl-1-acetone and 20g of 9, 10-diethoxyanthracene into a dispersion machine, stirring at the rotating speed of 1000mp for 0.5h, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 4
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether diol (with the molecular weight of 1000), 100g of hydroxyethyl acrylate, 100g of 2, 2' -dithiodiethanol and 1200g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for reaction for 3-5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 200g of tetrahydrofuran acrylate, 50g of Pasteur UA9030A, 100g of self-made self-repairing agent, 100g of NCO-terminated polycarbonate diol (molecular weight 1000), 40g of tris (3-hydroxypropyl) phosphine oxide, 30g of methyltriethoxysilane, 40g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 40g N-vinylcarbazole into a dispersion machine, stirring at the rotating speed of 3000mp for 0.5h, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 5
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 1000), 100g of hydroxyethyl acrylate, 100g of 3, 3' -dithiobis (propionohydrazide) and 1800g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for reaction for 3-5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 300g of isobornyl acrylate, 50g of pentaerythritol tetra-3-mercaptopropionate, 75g of LuCure2651, 150g of self-made self-repairing agent, 150g of NCO-terminated polycaprolactone diol (molecular weight 500), 5g of bis (3-hydroxybutyl) ethylphosphine oxide, 5g of KH570, 40g of 1-hydroxycyclohexyl phenyl ketone and 10g of isopropyl thioxanthone into a dispersion machine, stirring for 0.5h at the rotation speed of 1000mp, and discharging;
3) and (3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the vacuum degree of-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 6
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 300g of polyether glycol (molecular weight is 500), 100g of hydroxyethyl acrylate, 100g of 2,2 '-dithiodiethanol, 100g of 3, 3' -dithiobis (propionohydrazide) and 2400g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for reaction for 3-5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 150g of tetrahydrofuran acrylate, 100g of pentaerythritol tetra-3-mercaptopropionate, 120g of LuCure2651, 180g of self-made self-repairing agent, 100g of NCO-terminated polycaprolactone diol (molecular weight 500), 70g of bis (3-hydroxybutyl) ethylphosphine oxide, 20g of 1-hydroxycyclohexyl phenyl ketone and 20g of isopropyl thioxanthone into a dispersion machine, stirring for 0.5h at the rotating speed of 3000mp, and discharging;
3) and (3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the vacuum degree of-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 7
The embodiment provides a UV-moisture dual-curing three-proofing paint for a light module, and the preparation method comprises the following steps:
1) the self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 500), 216g of hydroxyethyl acrylate, 154g of 2, 2' -dithiodiethanol and 1600g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for reaction for 3-5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 300g of ethyl 3- (N, N-dimethylamino) acrylate, 150g of pentaerythritol tetra-3-mercaptopropionate, 100g of Changxing 615-one 100, 200g of self-made self-repairing agent, 120g of NCO-terminated polycaprolactone diol (molecular weight 2000), 20g of bis (3-hydroxypropyl) N-butylphosphine oxide, 20g of KH570, 20g of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 20g of 1-hydroxycyclohexyl phenyl ketone and 50g of isopropyl thioxanthone into a dispersion machine, stirring at the rotating speed of 2000mp for 0.5h, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Example 8
1) The self-made polyurethane acrylate is used as a self-repairing agent, and the preparation method comprises the steps of weighing 500g of polyether glycol (with the molecular weight of 500), 100g of hydroxyethyl acrylate, 100g of 2, 2' -dithiodiethanol and 2500g of isophorone diisocyanate (IPDI), adding into a reaction kettle, stirring at 80 ℃ for reaction for 3-5 hours, cooling and discharging to obtain the self-made self-repairing agent;
2) adding 250g of isobornyl acrylate, 50g of sardoma CN999, 40g of Runko FSP 8788, 300g of self-made self-repairing agent, 100g of NCO-terminated polycaprolactone diol (molecular weight is 1000), 5g of bis (3-hydroxypropyl) n-butyl phosphine oxide, 15g of KH570, 30g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, 10g of isopropyl thioxanthone and 10g of 9, 10-diethoxyanthracene into a dispersion machine, stirring for 0.5h at the rotating speed of 1500mp, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV-moisture dual-curing three-proofing paint.
Comparative example 1
Adding 300g of tetrahydrofuran acrylate, 50g of Pasteur UA9030A, 100g of NCO-terminated polycarbonate diol (molecular weight 1000), 40g of tris (3-hydroxypropyl) phosphine oxide, 30g of methyltriethoxysilane, 40g of 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide and 40g N-vinylcarbazole into a dispersion machine, stirring at the rotating speed of 3000mp for 0.5h, and discharging; and placing the obtained solution in a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV and moisture dual-curing three-proofing paint.
Comparative example 2
Adding 300g of isobornyl acrylate, 200g of pentaerythritol tetra-3-mercaptopropionate, 75g of LuCure2651, 150g of NCO-terminated polycaprolactone diol (molecular weight 500), 5g of bis (3-hydroxybutyl) ethylphosphine oxide, 5g of KH570, 40g of 1-hydroxycyclohexyl phenyl ketone and 10g of isopropyl thioxanthone into a dispersion machine, stirring at the rotating speed of 1000mp for 0.5h, and discharging; and placing the obtained solution in a defoaming machine, and vacuumizing for 20min under the condition that the vacuum degree is-0.1 Mpa to finally obtain the UV and moisture dual-curing three-proofing paint.
Comparative example 3
A company UV-moisture dual cure tri-proof lacquer is commercially available under the designation 5001VYT 1.
The properties of the UV + moisture dual cure three-proofing paints in examples 1-8 and comparative examples 1-3 are compared in Table 1.
The comparative performance test methods in table 1 are described in detail below:
ultraviolet light curing: the ultraviolet light with the wavelength of about 200nm to 400nm is adopted for curing, and the radiation energy is 500 to 3000mJ/cm2；
Moisture curing: placing the mixture in a room with constant temperature and humidity (23 +/-2 ℃, 50 +/-10% RH) under the condition of absolute dark and standing; in order to ensure light shielding, the sample can be covered by aluminum foil paper; the curing results were then checked according to the designed target time.
All propertiesThe test conditions were: ultraviolet light curing 2000mJ/cm2And then moisture cured for 48 hours.
The chemical resistance test is to put the optical module assembly into fluorinated liquid FC-40, acetone and xylene respectively to be soaked for 100h, 360h and 500h and then to study the reliability of the optical module, and the poaching test is to boil the optical module in boiling hot water for 6h, 12h and 24h and then to study the reliability of the optical module.
As can be seen from table 1: the performances of the examples 1 to 8 are superior to those of the comparative examples 1 to 3 as a whole, and for example, the high and low temperature cycle times, the high temperature and high humidity time, the chemical resistance and the water boiling resistance are good. The UV-moisture dual-curing three-proofing paint has good compact performance and can effectively block water vapor and various chemicals.
Table 1 optical module assembly performance comparison
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it is not limited to the embodiments, and those skilled in the art should understand that the technical solutions of the present invention can be modified or substituted with equivalents without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The UV-moisture dual-curing three-proofing paint for the optical module is characterized by comprising the following components in parts by weight: 20-50 parts of reactive diluent, 10-30 parts of self-repairing agent, 5-15 parts of tackifying resin, 5-15 parts of NCO-terminated polymer dihydric alcohol, 1-5 parts of photoinitiator, 1-5 parts of photo sensitizer and 1-10 parts of auxiliary agent.
2. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 1, wherein: the self-repairing agent is prepared from polyether glycol, hydroxyethyl acrylate, isophorone diisocyanate and 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol.
3. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 2, characterized in that: in the preparation of the self-repairing agent, the amount of the isophorone diisocyanate is 1-8 times of the sum of the amounts of the other components, the ratio of the amount of the 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol to the amount of the polyether glycol is 1:3-3:1, and the ratio of the hydroxyethyl acrylate to the polyether glycol is 1:2-2: 1.
4. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 2, characterized in that: the molecular weight of the polyether diol is 300-1000.
5. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 1, wherein: the reactive diluent is at least one of hydroxyethyl acrylate, N-butyl acrylate, hydroxypropyl methacrylate, 2-dithiodiethanol diacrylate, isooctyl acrylate, pentaerythritol tetraacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, ethyl 3- (N, N-dimethylamino) acrylate, isobornyl acrylate, tetrahydrofuran acrylate, pentaerythritol tetra-3-mercaptopropionate and tetra (3-mercaptobutanoic acid) pentaerythritol ester.
6. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 1, wherein: the tackifying resin is at least one of aliphatic polyurethane acrylate, aromatic polyurethane acrylate and polyether polyurethane acrylate; the NCO-terminated polymer dihydric alcohol is one or a mixture of more than two of polycaprolactone dihydric alcohol, polytetrahydrofuran ether dihydric alcohol or polycarbonate dihydric alcohol with the 2-end capped by IPDI and the molecular weight of 1000-5000.
7. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 1, wherein: the photoinitiator is at least one of benzoin dimethyl ether, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1-hydroxycyclohexyl phenyl ketone and benzophenone; the light sensitizer is at least one of isopropyl thioxanthone, 9, 10-diethoxyanthracene, 9, 10-dibutoxyanthracene and N-vinyl carbazole.
8. A UV-moisture dual cure tri-proof paint for light modules as claimed in claim 1, wherein: the auxiliary agent is one or more of trihydroxymethyl phosphine oxide, tris (3-hydroxypropyl) phosphine oxide, tris (3-hydroxybutyl) phosphine oxide, bis (3-hydroxypropyl) n-propyl phosphine oxide, bis (3-hydroxypropyl) n-butyl phosphine oxide, bis (3-hydroxypropyl) sec-butyl phosphine oxide, bis (3-hydroxypropyl) phenyl phosphine oxide, bis (3-hydroxybutyl) ethyl phosphine oxide, bis (3-hydroxybutyl) n-pentyl phosphine oxide, methyl triethoxysilane, vinyl trimethoxysilane, KH550, KH560, KH570 and hydroquinone.
9. A method for preparing a UV-moisture dual-curing tri-proof paint for a light module according to any one of claims 1 to 8, comprising the steps of:
1) adding polyether glycol, hydroxyethyl acrylate, isophorone diisocyanate and 3,3 '-dithiobis (propionohydrazide) and/or 2, 2' -dithiodiethanol into a reaction kettle, stirring at 80 ℃ for reaction for 3-5h, cooling and discharging to obtain a self-repairing agent;
2) adding an active diluent, tackifying resin, the self-repairing agent prepared in the step 1), NCO-terminated polymer dihydric alcohol, an auxiliary agent, a photoinitiator and a photo sensitizer into a dispersion machine, stirring for 0.5h at the rotating speed of 1000-3000rmp, and discharging;
3) putting the solution obtained in the step 2) into a defoaming machine, and vacuumizing for 20min under the vacuum degree of-0.1 Mpa to obtain the UV-moisture dual-curing three-proofing paint.
10. Use of a UV-moisture dual-curing tri-proof paint for light modules according to any one of claims 1 to 8, characterized in that: and (3) coating the UV-moisture dual-curing three-proofing paint on the surface of the optical module component by adopting a spraying or brushing process, wherein the thickness of the coating is 1-300 mu m.
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| CN115466568A (en) * | 2022-10-27 | 2022-12-13 | 南京大学 | Ultraviolet light/moisture dual-curing protective coating and preparation method and application thereof |
| CN116426152A (en) * | 2023-04-24 | 2023-07-14 | 江苏顺丽成建筑新材料有限公司 | Novel waterproof building material and preparation method thereof |
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| CN110885625A (en) * | 2019-12-12 | 2020-03-17 | 深圳纽沃新材料有限公司 | Preparation method of flame-retardant UV-moisture dual-curing polyurethane acrylate three-proofing paint |
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| CN110684459A (en) * | 2019-11-01 | 2020-01-14 | 深圳纽沃新材料有限公司 | Flame-retardant UV-moisture dual-curing polyurethane acrylate three-proofing paint |
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| CN115368535A (en) * | 2022-08-24 | 2022-11-22 | 苏州合邦鑫材科技有限公司 | UV/moisture dual-curing composition and preparation method and application thereof |
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| CN115466568A (en) * | 2022-10-27 | 2022-12-13 | 南京大学 | Ultraviolet light/moisture dual-curing protective coating and preparation method and application thereof |
| CN116426152A (en) * | 2023-04-24 | 2023-07-14 | 江苏顺丽成建筑新材料有限公司 | Novel waterproof building material and preparation method thereof |
| CN116426152B (en) * | 2023-04-24 | 2023-11-28 | 江苏顺丽成建筑新材料有限公司 | Novel waterproof building material and preparation method thereof |
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