CN111500181B - Preparation method of ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating - Google Patents
Preparation method of ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating Download PDFInfo
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- CN111500181B CN111500181B CN202010431524.1A CN202010431524A CN111500181B CN 111500181 B CN111500181 B CN 111500181B CN 202010431524 A CN202010431524 A CN 202010431524A CN 111500181 B CN111500181 B CN 111500181B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention provides a preparation method of ultraviolet-moisture dual-curing acid-and-alkali-resistant three-proofing paint, which relates to the field of paint and comprises the following steps of S1, adding hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding a blocking agent, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding a catalyst, and continuing to react for 3 hours to obtain an intermediate product. The ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating prepared by the invention not only avoids the problem that the shadow area can not be completely cured by adopting a single UV-curing conformal coating, but also improves the acid-and-alkali-resistant performance of the conformal coating, so that the protective performance is more reliable, and the ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating is especially suitable for the fields of new energy automobiles, chemical printing and dyeing, sewage treatment and the like.
Description
Technical Field
The invention relates to the field of coatings, in particular to a preparation method of ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating.
Background
The three-proofing paint is a coating with a special formula, is used for protecting a circuit board and related equipment from being corroded by the environment, and has good high and low temperature resistance; the UV three-proofing paint is an ultraviolet dual-curing electronic coating paint, and places which cannot be cured by light can be cured by moisture.
The production efficiency of coating and curing can be greatly improved by UV curing, but the problem that shadow areas cannot be cured easily on PCBs with plug-in components due to pure UV-curing three-proofing materials affects the product performance.
Disclosure of Invention
The invention aims to provide a preparation method of ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating, which aims to solve the technical problem that a shadow area can not be cured easily on a PCB (printed circuit board) with an insert made of a UV-curing conformal material.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating comprises the following steps,
s1, adding hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding an end-capping reagent, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding a catalyst, and continuously reacting for 3 hours to obtain an intermediate product;
s2, adding the intermediate product into a photoinitiator, an active diluent, a leveling agent and an accelerator, and uniformly stirring to obtain a finished product.
Preferably, in S1, the blocking agent is one or more of hexamethylene diisocyanate, 2, 4-toluene diisocyanate, 2, 6-toluene diisocyanate, and 4, 4' -diphenylmethane diisocyanate.
Preferably, in S1, the catalyst is one or more of tin acetate, dibutyltin dilaurate, stannous octoate, dibutyltin bis (dodecyl sulfur), and dibutyltin diacetate.
Preferably, in S2, the photoinitiator is one or more of diphenyl-2, 4, 6-trimethylbenzoyloxyphosphorus, trimethylbenzoyldiphenylphosphine oxide, 1-hydroxycyclohexylphenylketone, 2-hydroxy-methylphenylpropane-1-one, benzophenone, 2-methyl-1-4-methylthiophenyl-2-morpholinyl-1-propanone, and 2, 4-diethylthioxanthone.
Preferably, in S2, the active diluent is one or more of 1-octene, 1-nonene, 1, 7-octadiene, 1, 8-nonadiene and 1, 9-decadiene.
Preferably, in S2, the accelerator is one of N, N-dimethylcyclohexylamine, bis (2-dimethylaminoethyl) ether, N-dimethylbenzylamine, N-ethylmorpholine, N '-diethylpiperazine, triethanolamine, and N, N' -dimethylpyridine.
The invention has the beneficial effects that:
1. according to the ultraviolet-moisture dual-curing acid-and-alkali-resistant conformal coating, during reaction, ultraviolet light is used for realizing rapid curing, subsequent operation of a production line is not influenced, isocyanate groups in molecules are further crosslinked through moisture absorption condensation reaction to realize curing of a shadow area, so that complete curing is realized, the problem that complete curing of the shadow area cannot be realized by adopting a single UV curing conformal coating is avoided, and the protection reliability is improved;
2. by using the active diluent with a pure carbon chain structure, the stability of the whole structure is improved, the acid and alkali resistance of the product is greatly improved, the viscosity of the system can be effectively reduced, and the environmental protection and potential safety hazard caused by using a solvent are avoided while the convenience and easiness of operation are not influenced;
3. through isocyanate groups in molecules, the isocyanate groups react with residual hydroxyl on the surface of the circuit board while moisture is cured, so that better adhesion to a base material can be provided;
4. the period of complete curing of the whole system is accelerated by adding an auxiliary agent for promoting the moisture absorption condensation reaction.
Drawings
FIG. 1 is a flow diagram of a synthesis of the present invention;
FIG. 2 is a schematic diagram of the preparation reaction of the present invention.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood, the invention is further described below with reference to the specific embodiments and the attached drawings, but the following embodiments are only the preferred embodiments of the invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
Specific embodiments of the present invention are described below with reference to the accompanying drawings.
Example 1
Adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring, heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 160kg of hexamethylene diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuing to react for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by 1-nonene and 1, 7-octadiene according to the mass ratio of 3: 7), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product, wherein the reaction process and the reaction principle are shown in a figure 1-2.
Example 2
Adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 170kg of 2, 4-toluene diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuing to react for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by 1-nonene and 1, 7-octadiene according to the mass ratio of 3: 7), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product, wherein the reaction process and the reaction principle are shown in a figure 1-2.
Example 3
Adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring, heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 240kg of diphenylmethane diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuously reacting for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by 1-nonene and 1, 7-octadiene according to the mass ratio of 3: 7), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product, wherein the reaction process and the reaction principle are shown in a figure 1-2.
The finished product obtained as described in examples 1 to 3 was tested by the following method:
the test method comprises the following steps:
respectively spraying the finished products prepared in the embodiments 1-3 on FR-4 grade PCB boards, wherein the wet film thickness is 200um, the light of a 1000W mercury lamp is used for 30 seconds, and the finished products are placed in a light-proof oven at 50 ℃ and 50% RH for 3 days;
and (3) performing high-low temperature cyclic impact on the cured PCB, wherein the impact condition is in a range from-65 ℃ to 125 ℃, the 15min high temperature and the 15min low temperature are one cycle, the total impact is 100 cycles, after the impact is finished, the appearance of the product is compared with whether the product is intact, and a hundred-grid wiping paint film is scratched to observe whether the product falls off.
The results of the experiment are shown in table 1:
TABLE 1
Through comparison tests, the difference of the blocking agent in the step one can be found out, the mechanical property and the high and low temperature impact resistance of the final product are greatly influenced, and the blocking agent can influence the hardness degree of the final cured product. The final product using hexamethylene diisocyanate (example 1) was soft to film and poor in mechanical properties, and the product was peeled off by wiping; the use of diphenylmethane diisocyanate (example 3) results in a harder film-forming final product and cracks in the event of high and low temperature impact. The best results were tested using 2, 4-toluene diisocyanate in example 2.
Example 4
This example was carried out using 2, 4-toluene diisocyanate as the blocking agent in example 2, as follows: adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 170kg of 2, 4-toluene diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuing to react for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by isooctyl acrylate and trimethylolpropane triacrylate according to the mass ratio of 10: 0.5), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product.
Example 5
This example was carried out using 2, 4-toluene diisocyanate as the blocking agent in example 2, as follows: adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 170kg of 2, 4-toluene diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuing to react for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by isobornyl acrylate and 1, 6-hexanediol diacrylate according to the mass ratio of 10: 0.5), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product.
Example 6
This example was carried out using 2, 4-toluene diisocyanate as the blocking agent in example 2, as follows: adding 900kg of hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding 170kg of 2, 4-toluene diisocyanate, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding 1kg of dibutyltin dilaurate, and continuing to react for 3 hours to obtain an intermediate product;
adding 40kg of photoinitiator (prepared by the photoinitiator 184 and the photoinitiator TPO according to the mass ratio of 1: 1), 120kg of reactive diluent (prepared by 1-nonene and 1, 7-octadiene according to the mass ratio of 3: 7), 1kg of flatting agent BYK333 and 1kg of catalyst N, N-dimethylcyclohexylamine into the intermediate product, and uniformly stirring to obtain a finished product.
Comparative example 1
Adopts 1-2577 dukangning three-proofing paint.
Comparative example 2
HumisealUV40-250 three-proofing paint is adopted.
Examples 4 to 6 and comparative examples 1 to 2 were each tested as follows:
description of the test methods: the surface resistance adopts the standard of ASTMD 150; the breakdown voltage adopts the standard of ASTMD 149; the dielectric constant adopts an ASTMD257 standard; the acid and alkali resistance test is to test whether the circuit board can be electrified to work normally after the circuit board is placed in 5 percent hydrofluoric acid and 5 percent sodium hydroxide solution for 48 hours; moisture curing time test the product was placed in a dark oven at 50 ℃ and 50% RH open until the three-proofing paint performance no longer changed.
The test structure is shown in table 2:
TABLE 2
The comparison of test data shows that the conventional acrylic acid reactive diluent has great influence on the finished product in the aspect of acid and alkali resistance; all the diluents used in the embodiments 4, 5 and 6 are acrylic diluents, and ester bonds containing the diluents are hydrolyzed and broken in an acid-base environment to damage the whole structure, so that the effects of protecting the circuit board are lost; comparative example 2 and comparative example 3 are relatively high-end three-proofing paints with good corrosion resistance on the market, the problem also exists, and the main resin of the paint is easy to hydrolyze or break in acid-base environment; the finished product produced by the invention breaks through in resin and active diluent, so that the product can better cope with severe acid-base working environment.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. The preparation method of the ultraviolet-moisture dual-curing acid and alkali resistant conformal coating is characterized by comprising the following steps of:
s1, adding hydroxyl polybutadiene resin into a reaction kettle, stirring and heating to 90-100 ℃, vacuumizing for 1 hour, introducing nitrogen to break vacuum, cooling to 30-40 ℃, adding an end-capping reagent, stirring uniformly, heating to 80 ℃, reacting for 2 hours, adding a catalyst, and continuously reacting for 3 hours to obtain an intermediate product;
s2, adding the intermediate product into a photoinitiator, an active diluent, a leveling agent and an accelerator, and uniformly stirring to obtain a finished product;
in S2, the active diluent is one or more of 1-octene, 1-nonene, 1, 7-octadiene, 1, 8-nonadiene and 1, 9-decadiene.
2. The preparation method of the ultraviolet-moisture dual-curing acid-and-alkali-resistant three-proofing paint according to claim 1, characterized in that: in S1, the blocking agent is one or more of hexamethylene diisocyanate, 2, 4-toluene diisocyanate, 2, 6-toluene diisocyanate and 4, 4' -diphenylmethane diisocyanate.
3. The preparation method of the ultraviolet-moisture dual-curing acid-and-alkali-resistant three-proofing paint according to claim 1, characterized in that: in the S1, the catalyst is one or more of tin acetate, dibutyltin dilaurate, stannous octoate, dibutyltin bis (dodecyl sulfur) and dibutyltin diacetate.
4. The preparation method of the ultraviolet-moisture dual-curing acid-and-alkali-resistant three-proofing paint according to claim 1, characterized in that: in the S2, the photoinitiator is one or more of diphenyl-2, 4, 6-trimethylbenzoyloxyphosphorus, trimethylbenzoyldiphenylphosphine oxide, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-methyl phenyl propane-1-one, benzophenone, 2-methyl-1-4-methylthiophenyl-2-morpholinyl-1-propanone, and 2, 4-diethylthioxanthone.
5. The preparation method of the ultraviolet-moisture dual-curing acid-and-alkali-resistant three-proofing paint according to claim 1, characterized in that: in the S2, the accelerator is one of N, N-dimethylcyclohexylamine, bis (2-dimethylaminoethyl) ether, N, N-dimethylbenzylamine, N-ethylmorpholine, N, N '-diethylpiperazine, triethanolamine and N, N' -dimethylpyridine.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101959912A (en) * | 2008-02-29 | 2011-01-26 | 株式会社钟化 | Curable composition |
| CN103926795A (en) * | 2013-01-16 | 2014-07-16 | 施敏打硬株式会社 | Photocurable Composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US6844376B1 (en) * | 2002-10-23 | 2005-01-18 | Henkel Corporation | Polyurethane compositions containing both radiation and moisture curable groups |
| JP2008159437A (en) * | 2006-12-25 | 2008-07-10 | Hitachi Kasei Polymer Co Ltd | Single liquid type coating agent for both light curing and moisture curing, electric-electronic component subjected to insulating treatment by the same, and its manufacturing method |
| CN109321125A (en) * | 2018-09-14 | 2019-02-12 | 依工特种材料（苏州）有限公司 | A kind of UV moisture dual cure three-proofing coating |
| CN109575871A (en) * | 2018-12-04 | 2019-04-05 | 万华化学集团股份有限公司 | A kind of ultraviolet radioactive and the adhesive composition of moisture dual cure and application thereof |
| CN110885625B (en) * | 2019-12-12 | 2021-08-31 | 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 |
| CN110885664A (en) * | 2019-12-15 | 2020-03-17 | 今商科技(上海)有限公司 | Light-moisture curing adhesive with high-efficiency water-vapor barrier property and ultralow water absorption rate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101959912A (en) * | 2008-02-29 | 2011-01-26 | 株式会社钟化 | Curable composition |
| CN103926795A (en) * | 2013-01-16 | 2014-07-16 | 施敏打硬株式会社 | Photocurable Composition |
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