CN109111771A - A kind of moisture cured high reliability UV conformal coating and preparation method thereof - Google Patents
A kind of moisture cured high reliability UV conformal coating and preparation method thereof Download PDFInfo
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- CN109111771A CN109111771A CN201810543541.7A CN201810543541A CN109111771A CN 109111771 A CN109111771 A CN 109111771A CN 201810543541 A CN201810543541 A CN 201810543541A CN 109111771 A CN109111771 A CN 109111771A
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- conformal coating
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- acid ester
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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Abstract
The present invention relates to a kind of moisture cured high reliability UV conformal coatings, it comprises the following raw materials by weight percent: organic-silicon-modified 20~40 parts of polybutadiene acrylic acid ester resin, 30~50 parts of dicyclopentadiene acrylate monomer, 15-25 parts of acrylate monomer containing rigid radical, 1~7 part of photoinitiator.Moisture cured high reliability UV conformal coating prepared by the present invention can solve the defect of conventional conformal coating not salt spray resistance；Synthesis organic-silicon-modified polybutadiene acrylic acid ester resin because have on strand moisture cured first ethoxysilane groups, obtained conformal coating has the function of UV and moisture dual cure, can solve the problems, such as on wiring board because caused by chip dash area solidification it is difficult；It is amenable to the reliability test of high/low-temperature impact, can protect wiring board has under harsh environment temperature with excellent performance.
Description
Technical field
The invention belongs to photo-curing material fields, are related to a kind of moisture cured high reliability UV conformal coating and its system
Preparation Method, the application demand suitable for the protection of high-end line plate.
Background technique
Conformal coating (conformal coating) is exactly coated in the printed wiring board (PCB) for having welded plug connector elements
Very thin protection materials.It can enhance the anti-moisture and soil-repellent ability of electronic circuit and component and prevent solder joint and conductor from being invaded
Erosion can also play the role of shielding and eliminate electromagnetic interference and prevent line short, improve the insulation performance of wiring board.This
Outside, coating protective film is also beneficial to the rub resistance and solvent resistance of route and component, and can release temperature cyclically-varying
Caused pressure improves the stability of electronic product, prolongs the service life.In addition to being used for electronics industry, conformal coating is in vapour
It is also widely used in terms of turner industry, aerospace industries, national defense industry and bioengineering.
It is coating material solidified that photocureable coating is also known as ultraviolet light (UV), is one kind of radiation curable coating, refers mainly to irradiate in light
Down can crosslinking curing film forming rapidly a kind of new coating, because of its efficient coating and the features such as environmental-friendly, in coating row
Industry is used widely.Compared with solvent based coating, photocureable coating has fast curing rate, object volatile solvent, saves energy
Source, expense be low, can automated production the features such as.
But conventional UV solidification conformal coating also has its shortcoming, such as solidification energy is high, dash area solidifies not
Sufficiently, water absorption rate high and low temperature poor in flexibility and the disadvantages of insufficient salt spray resistance, it is of the invention moisture cured highly reliable
Property UV conformal coating can solve these defects.
Summary of the invention
It is showed in salt spray resistance, the insufficient aspect of dash area solidification to solve UV solidification conformal coating in the prior art
Bad problem, the present invention provides a kind of moisture cured high reliability UV conformal coatings and preparation method thereof, to reach
Conformal coating is able to satisfy the demand of high reliability.
The technical scheme to solve the above technical problems is that
A kind of moisture cured high reliability UV conformal coating, comprises the following raw materials by weight percent: organic-silicon-modified
20~40 parts of polybutadiene acrylic acid ester resin, 30~50 parts of dicyclopentadiene acrylate monomer, the propylene containing rigid radical
15-25 parts of acid ester monomer, 1~7 part of photoinitiator.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the organic-silicon-modified polybutadiene acrylic acid ester resin, refers to epoxidized polybutadiene, acrylic acid
Change with the organosilicon with polybutadiene rubber structure and organosilicon structures of the silane coupling agent synthesis containing isocyanate groups
Property polybutadiene acrylic acid ester resin, the epoxidized polybutadiene includes: the Epolead of Japanese Daicel company
PB3600, Epolead PB4700, No. CAS: 71342-74-0.Silane coupling agent containing isocyanate groups has: 3- isocyanic acid
Ester group propyl trimethoxy silicane (CAS:15396-00-6), 3- isocyanate group propyl-triethoxysilicane (CAS:24801-
88-5), the synthetic method of organic-silicon-modified polybutadiene acrylic acid ester resin is: 1 mole of epoxidized polybutadiene, 2 are rubbed
Your acrylic acid, catalyst triphenylphosphine (50ppm) is added in the three-necked flask with thermometer, and temperature is controlled in 100-
Stop heating after 120 degree, reaction 3 hours, 2 moles of the silane coupling agent containing isocyanate groups is added, temperature control is existed
70-80 degree stops heating after reaction 2 hours, obtains organic-silicon-modified polybutadiene acrylic acid ester resin, this resin have UV and
The function of moisture dual cure.
Further, the dicyclopentadiene acrylate monomer refers to the 512AS (No. CAS: 65983- of Hitachi, Japan chemical conversion
31-5) with 512M (No. CAS: 68586-19-6), strand contains the molecular structure of cyclopentadiene.
Further, the acrylate monomer containing rigid radical, refer to 4- tert-butylcyclohexyl acrylate (CAS:
84100-23-2) and methacrylic acid is to t-butyl cyclohexyl methacrylate (CAS:46729-07-1), such as: SARTOMER company
SR217 and SR218, molecular structural formula are as follows:
Methacrylic acid is to t-butyl cyclohexyl methacrylate
4- tert-butylcyclohexyl acrylate
Further, the photoinitiator be trade mark 1173(2- hydroxy-2-methyl -1- phenylacetone), 184(1- hydroxy-cyclohexyl
Benzophenone), 907(2- methyl-1-(4- first mercaptophenyl)-2- morpholine-1- acetone), 369(2- benzyl-2- dimethylamino-1-
(4- morpholinyl phenyl) -1- butanone), bis- (2,4, the 6- trimethylbenzoyl) phenylphosphine oxides of 819(), 651 (α, α '-dimethyl
Benzil ketals), ITX (isopropyl thioxanthone), BP (benzophenone), OMBB (o-benzoyl yl benzoic acid methyl esters), TPO
One of (2,4,6- trimethyl benzoyl diphenyl base phosphorous oxide) or any several mixture.
The preparation method of the moisture cured high reliability UV conformal coating of one kind of the present invention include: weigh it is organic
20~40 parts of Si modification polybutadiene acrylic acid ester resin, contains rigid radical at 30~50 parts of dicyclopentadiene acrylate monomer
15-25 parts of acrylate monomer, 1~7 part of photoinitiator, sequentially add in blender, be evacuated to vacuum degree be -0.08
~-0.05MPa is stirred 0.5~2 hour in 500~1000 revs/min, is stirred evenly, hung naturally to room temperature, sealed package is
It can.
The beneficial effects of the present invention are: moisture cured high reliability UV conformal coating prepared by the present invention, is polymerizeing
Three kinds of organosilicon, polybutadiene and dicyclopentadiene rubber-type molecular structures, such molecule knot are introduced in the macromolecular chain of object
Structure has better water resistance and salt fog resistance, can solve the defect of conventional conformal coating not salt spray resistance.The organosilicon of synthesis
Modified polybutadiene acrylate because have on strand moisture cured first ethoxysilane groups, what is obtained is conformal
Coating has the function of UV and moisture dual cure, can solve on wiring board because caused by chip dash area solidify difficult ask
Topic.The polybutadiene rubber structure of introducing, has excellent low temperature flexibility, and obtained conformal coating has wider using temperature
Degree, is amenable to the reliability test of high/low-temperature impact, can protect wiring board has under harsh environment temperature with excellent
Performance.
Specific embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Synthetic example
The synthetic method of organic-silicon-modified polybutadiene acrylic acid ester resin is: by 1 mole of epoxidized polybutadiene, 2 moles
Acrylic acid, 0.15g catalyst triphenylphosphine be added in the three-necked flask with thermometer, by temperature control at 110 degree, instead
Stop heating after answering 3 hours, 2 moles of the silane coupling agent containing isocyanate groups is added, temperature is controlled into the reaction at 80 degree
Stop heating after 2 hours, obtains organic-silicon-modified polybutadiene acrylic acid ester resin.
Embodiment 1
Accurately weigh the following raw material, organic-silicon-modified polybutadiene acrylic acid ester resin, 30g；The 512AS, 40g of Hitachi's chemical conversion；
The SR217 of SARTOMER company, 20g；Photoinitiator 184,3g；Photoinitiator TPO, 1g；Above-mentioned each component is sequentially added double
In planetary power mixing and blending machine, being evacuated to vacuum degree is -0.08MPa, stirs 2 hours, stirs evenly in 500 revs/min, from
It so hangs to room temperature, obtains moisture cured high reliability UV conformal coating, sealed package.
Embodiment 2
Accurately weigh the following raw material, organic-silicon-modified polybutadiene acrylic acid ester resin, 40g；The 512M, 30g of Hitachi's chemical conversion；
The SR217 of SARTOMER company, 18g；Photoinitiator 184,1g；Photoinitiator 1173,1g；Above-mentioned each component is sequentially added double
In planetary power mixing and blending machine, being evacuated to vacuum degree is -0.05MPa, stirs 1 hour, stirs evenly in 750 revs/min, from
It so hangs to room temperature, obtains moisture cured high reliability UV conformal coating, sealed package.
Embodiment 3
Accurately weigh the following raw material, organic-silicon-modified polybutadiene acrylic acid ester resin, 20g；The 512AS, 50g of Hitachi's chemical conversion；
The SR218,25g of SARTOMER company；Photoinitiator 1173: 3g；Photoinitiator 819:2g sequentially adds above-mentioned each component
In double-planet power mixing and blending machine, being evacuated to vacuum degree is -0.06MPa, is stirred 1.5 hours in 700 revs/min, and stirring is equal
It is even, it hangs naturally and obtains moisture cured high reliability UV conformal coating, sealed package to room temperature.
Embodiment 4
Accurately weigh the following raw material, organic-silicon-modified polybutadiene acrylic acid ester resin, 35g；The 512M, 40g of Hitachi's chemical conversion；
The SR218 of SARTOMER company, 25g；Photoinitiator 184,3g；Photoinitiator TPO, 1g；Above-mentioned each component is sequentially added double
In planetary power mixing and blending machine, being evacuated to vacuum degree is -0.07MPa, stirs 1 hour, stirs evenly in 800 revs/min, from
It so hangs to room temperature, obtains moisture cured high reliability UV conformal coating, sealed package.
Embodiment 5
Accurately weigh the following raw material, organic-silicon-modified polybutadiene acrylic acid ester resin, 25g；The 512AS, 45g of Hitachi's chemical conversion；
The SR217 of SARTOMER company, 25g;Photoinitiator 1173,3g；Photoinitiator TPO, 4g；Above-mentioned each component is sequentially added double
In planetary power mixing and blending machine, being evacuated to vacuum degree is -0.08MPa, is stirred 0.5 hour in 1000 revs/min, and stirring is equal
It is even, it hangs naturally and obtains moisture cured high reliability UV conformal coating, sealed package to room temperature.
Comparative example 1
Accurately weigh the following raw material, the CN8881 (two degrees of functionality, polyester-type) of Sartomer, 30g；IBOA, 60g；HEA,
10g；Photoinitiator 184,3g；Photoinitiator TPO, 1g；Above-mentioned each component is sequentially added in double-planet power mixing and blending machine,
Being evacuated to vacuum degree is -0.08MPa, stirs 2 hours in 500 revs/min, stirs evenly, hung naturally to room temperature, and it is solid to obtain UV
Change conformal coating, sealed package.
Comparative example 2
Accurately weigh the following raw material, bis- degree of functionality of 5220(of Taiwan Changxing company, polyether-type), 35g；THFA, 41g；IBOA,
15g；Photoinitiator 1173,3g；Photoinitiator TPO, 1g；Above-mentioned each component is sequentially added into double-planet power mixing and blending machine
Interior, being evacuated to vacuum degree is -0.05MPa, stirs 1 hour in 750 revs/min, stirs evenly, hung naturally to room temperature, obtained
UV solidifies conformal coating, sealed package.
Pass through the performance of the moisture cured high reliability UV conformal coating of following experimental test one kind of the invention.
Test example
Salt spray resistance test: GB/T 10125-1997 standard testing is pressed.
Water absorption rate test: GB/T 1034-1998 standard testing, 100 degree of boiling water, 2h are pressed.
Test result is as shown in table 1:
Sample made from 1 embodiment 1-5 of table and common UV solidify conformal coating contrast test result
| Sample | Shade solidification effect | Water absorption rate | Salt spray resistance | Low temperature flexibility |
| The sample of embodiment 1 | OK | 0.3% | It is outstanding, no rust spot | It is outstanding |
| The sample of embodiment 2 | OK | 0.4% | It is outstanding, no rust spot | It is outstanding |
| The sample of embodiment 3 | OK | 0.5% | It is outstanding, no rust spot | It is outstanding |
| The sample of embodiment 4 | OK | 0.4% | It is outstanding, no rust spot | It is outstanding |
| The sample of embodiment 5 | OK | 0.5% | It is outstanding, no rust spot | It is outstanding |
| The sample of comparative example 1 | NG | 1.2% | Generally, there is rust spot | - 40 degree embrittlements |
| The sample of comparative example 2 | NG | 1.0% | Generally, there is rust spot | - 40 degree embrittlements |
It can be seen from the results above that the moisture cured high reliability UV conformal coating of one kind of the invention and existing common
UV solidification conformal coating is compared, and has good salt spray resistance, has better shade solidification effect, low temperature flexibility is more preferably.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of moisture cured high reliability UV conformal coating, which is characterized in that by the raw material group of following weight percent
At: organic-silicon-modified 20~40 parts of polybutadiene acrylic acid ester resin, contains just 30~50 parts of dicyclopentadiene acrylate monomer
15-25 parts of acrylate monomer, 1~7 part of photoinitiator of property group；
The organic-silicon-modified polybutadiene acrylic acid ester resin, synthetic method is: 1 mole of epoxidized polybutadiene, 2 are rubbed
Your acrylic acid, catalyst triphenylphosphine 0.15g is added in the three-necked flask with thermometer, and temperature is controlled in 100-
Stop heating after 120 degree, reaction 3 hours, 2 moles of the silane coupling agent containing isocyanate groups is added, temperature control is existed
70-80 degree stops heating after reaction 2 hours, obtains organic-silicon-modified polybutadiene acrylic acid ester resin.
2. conformal coating according to claim 1, which is characterized in that the epoxidized polybutadiene is that Japanese Daicel is public
Epolead PB3600 or the Epolead PB4700 of department, the silane coupling agent containing isocyanate groups are 3- isocyanate group third
Base trimethoxy silane or 3- isocyanate group propyl-triethoxysilicane.
3. conformal coating according to claim 1, which is characterized in that the dicyclopentadiene acrylate monomer is Japan
The 512AS or 512M of Hitachi's chemical conversion.
4. conformal coating according to claim 1, which is characterized in that the acrylate monomer containing rigid radical refers to
4- tert-butylcyclohexyl acrylate or methacrylic acid are to t-butyl cyclohexyl methacrylate.
5. conformal coating according to claim 1, which is characterized in that the photoinitiator is 2- hydroxy-2-methyl -1- benzene
Benzylacetone, 1- hydroxy cyclohexyl phenylketone, 2- methyl-1-(4- first mercaptophenyl)-2- morpholine-1- acetone, 2- benzyl-2- diformazan
Amino -1-(4- morpholinyl phenyl) -1- butanone, bis- (2,4,6- trimethylbenzoyl) phenylphosphine oxides, α, α '-dimethyl benzene idol
Acyl ketal, isopropyl thioxanthone, benzophenone, o-benzoyl yl benzoic acid methyl esters, 2,4,6- trimethyl benzoyl diphenyl
One of base phosphorous oxide or any several mixture.
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| CN201810543541.7A CN109111771A (en) | 2018-05-31 | 2018-05-31 | A kind of moisture cured high reliability UV conformal coating and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112980337A (en) * | 2021-02-26 | 2021-06-18 | 烟台信友新材料有限公司 | High-temperature-resistant flame-retardant UV (ultraviolet) moisture dual-curing adhesive and preparation method thereof |
| CN113107102A (en) * | 2021-03-16 | 2021-07-13 | 苏州中材非金属矿工业设计研究院有限公司 | Building waterproof structure |
| CN113136128A (en) * | 2021-03-16 | 2021-07-20 | 苏州中材非金属矿工业设计研究院有限公司 | Solvent-free elastic asphalt waterproof coating and preparation method thereof |
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| WO2014152428A1 (en) * | 2013-03-15 | 2014-09-25 | Curatolo Benedict S | Dual curable composition |
| CN106163656A (en) * | 2014-02-06 | 2016-11-23 | 莫门蒂夫性能材料股份有限公司 | The silicon composition of moisture-curable |
| CN107384109A (en) * | 2017-07-25 | 2017-11-24 | 烟台德邦科技有限公司 | A kind of high reliability UV solidifications conformal coating and preparation method thereof |
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| CN102757728A (en) * | 2011-04-25 | 2012-10-31 | 陶氏环球技术有限公司 | Moisture-solidified antifouling paint composition |
| WO2014152428A1 (en) * | 2013-03-15 | 2014-09-25 | Curatolo Benedict S | Dual curable composition |
| CN106163656A (en) * | 2014-02-06 | 2016-11-23 | 莫门蒂夫性能材料股份有限公司 | The silicon composition of moisture-curable |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112980337A (en) * | 2021-02-26 | 2021-06-18 | 烟台信友新材料有限公司 | High-temperature-resistant flame-retardant UV (ultraviolet) moisture dual-curing adhesive and preparation method thereof |
| CN112980337B (en) * | 2021-02-26 | 2022-10-21 | 烟台信友新材料有限公司 | High-temperature-resistant flame-retardant UV (ultraviolet) moisture dual-curing adhesive and preparation method thereof |
| CN113107102A (en) * | 2021-03-16 | 2021-07-13 | 苏州中材非金属矿工业设计研究院有限公司 | Building waterproof structure |
| CN113136128A (en) * | 2021-03-16 | 2021-07-20 | 苏州中材非金属矿工业设计研究院有限公司 | Solvent-free elastic asphalt waterproof coating and preparation method thereof |
| CN113107102B (en) * | 2021-03-16 | 2023-01-24 | 苏州正硅防水科技有限公司 | Building waterproof structure |
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Application publication date: 20190101 |