CN107629639B - A kind of ultraviolet-curing paint - Google Patents
A kind of ultraviolet-curing paint Download PDFInfo
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- CN107629639B CN107629639B CN201710995490.7A CN201710995490A CN107629639B CN 107629639 B CN107629639 B CN 107629639B CN 201710995490 A CN201710995490 A CN 201710995490A CN 107629639 B CN107629639 B CN 107629639B
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Abstract
The invention discloses a kind of ultraviolet-curing paints, it is characterized in that, it is composed of the following components according to parts by weight: 60-80 parts of epoxy acrylic, 50-65 parts of epoxy acrylate diluent, 20-45 parts of Tricyclodecane Dimethanol diacrylate, 20-30 parts of borosilicate modified epoxy, 20-35 parts of tri (propylene glycol) diacrylate, 60-80 parts of trimethylolpropane trimethacrylate, 5-15 parts of ethoxylated trimethylolpropane triacrylate, 2, 4, 6(trimethylbenzoyl) 5-8 parts of diphenyl phosphine oxide, 1-3 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, 0.5-1.5 parts of triaryl matte hexafluoro antimonate.The invention has the following beneficial effects: the fast completion of cures of (1) resin solidification speed；(2)) resin system viscosity is lower；(3)) hardness of film height, high and low temperature resistance and good toughness after solidifying.
Description
Technical field
The present invention relates to a kind of coating, more particularly, to a kind of ultraviolet-curing paint.
Background technique
In the past few years, ultraviolet-curing paint fibre coating, CD coating/DVD adhesive, credit card, timber,
Very rapid development is suffered from beverage can, food packaging, journal surface, medical instrument and automobile industry.Ultraviolet light solidification
Coating possesses huge market potential, and the ratio in entire coating products increases year by year.Ultraviolet-curing paint master
It to be made of oligomer, monomer, photoinitiator and auxiliary agent.It is to cause light by radiation that ultraviolet light, which solidifies cured key reaction course,
Decomposition of initiator generates living radical and causes monomer/oligomer polymerization crosslinking.
Resin used in ultraviolet light solidification at present is just substantially acrylic resin and two kinds of epoxy resin, wherein third
Olefin(e) acid resin is the resin made of esters of acrylic acid and methyl acrylic ester and the copolymerization of other olefinic type monomers, passes through selection
Different resin structure, different formulas, production technology and solvent compositions, can synthesize different type, different performance and difference and answer
With the acrylic resin of occasion, acrylic resin can be divided into thermoplastic acrylic resin according to structure and the difference of membrane formation mechanism again
And thermosetting acrylic resin.Main suction with the acrylic resin of acrylate and methacrylate monomers copolymerization to light
It receives peak to be in except solar spectrum range, so acrylic resin paint obtained has excellent light resistance and anti-outdoor aging
Energy.Thermosetting acrylic resin refers to has certain functional group in the structure, the amino resins for passing through and being added in painting,
Functional group reactions in epoxy resin, polyurethane etc. form reticular structure, and the general relative molecular weight of thermosetting resin is lower.Thermosetting
Property acrylic coating have excellent richness, gloss, hardness, solvent resistance, weatherability, in high-temperature baking it is non-discolouring, do not return
It is yellow.Most important application be with amino resins cooperation amino-acrylonitrile acid baking vanish is made, at present automobile, motorcycle, bicycle,
Using very extensive on the products such as coil.
However energy used in acrylate ultraviolet light curable coating photocuring on the market is higher at present, obtains after solidification
Although film hardness it is higher, it is more crisp, can not impact resistance, high and low temperature resistance, and its not resistant not resistant to water.Such as it is a kind of
A kind of light-cured resin reported in Chinese patent literature and application thereof, application publication number are 106866889 A of CN, should
Light-cured resin is grouped as based on mass percentage by following group: ethyl methacrylate 4.6-10.8%, ethyl acetate
It is 0.1-0.6% for 4.6-9.2%, polyurethane acrylic resin 80-90%, benzophenone -1.Light-cured resin of the invention
Cost of material is cheap, and it is convenient to obtain, and is easy to store, non-toxic to humans, and drop good penetrability on fiber, film forming rapidly may be used
Control, solid flexible, slice is easy to operate, and success rate is high, and the fiber cross section cut out clearly easily distinguishes that the extruding of fiber is smaller,
Fiber degree of scatter is high, and boundary and lumen are clear, and feature is obvious, are easy to differentiate.But its there is also more deficiencies, such as it makes
It is mostly small molecule acrylate, after photocuring, crosslink density is larger, although having preferable hardness, toughness
It is not high, and its high and low temperature resistance is poor is unable to satisfy daily use.
Summary of the invention
The present invention be in order to overcome photocureable coating not high-low temperature resistant in the prior art, the coating property obtained after solidification compared with
It is crisp, provide one kind can high-low temperature resistant, a kind of tough and tensile ultraviolet-curing paint of the coating property obtained after solidification.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 60-80 parts of epoxy acrylic, epoxy
50-65 parts of acrylate diluent, 20-45 parts of Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy 20-30
Part, 20-35 parts of tri (propylene glycol) diacrylate, 60-80 parts of trimethylolpropane trimethacrylate, three hydroxyl first of ethoxylation
5-15 parts of base propane triacrylate, 5-8 parts of 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxide, 1- hydroxy-cyciohexyl one
1-3 parts of phenyl ketone, 0.5-1.5 parts of triaryl matte hexafluoro antimonate.
Preferably, composed of the following components according to parts by weight: 65-75 parts of epoxy acrylic, epoxy acrylate are dilute
Release 55-60 parts of agent, 25-40 parts of Tricyclodecane Dimethanol diacrylate, 22-28 parts of borosilicate modified epoxy, two contractings 3 third
25-30 parts of omega-diol diacrylate, 65-75 parts of trimethylolpropane trimethacrylate, ethoxylated trimethylolpropane 3 third
5-15 parts of olefin(e) acid ester, 5-8 parts of 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxide, one phenyl ketone 1- of 1- hydroxy-cyciohexyl
3 parts, 0.5-1.5 parts of triaryl matte hexafluoro antimonate.
Preferably, composed of the following components according to parts by weight: 70 parts of epoxy acrylic, epoxy acrylate diluent
58 parts, 30 parts of Tricyclodecane Dimethanol diacrylate, 25 parts of borosilicate modified epoxy, tri (propylene glycol) diacrylate
28 parts, 70 parts of trimethylolpropane trimethacrylate, 7 parts of ethoxylated trimethylolpropane triacrylate, 2,4,6 (front threes
Base benzoyl) 7 parts of diphenyl phosphine oxide, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte hexafluoro antimonate 1
Part.
The longer acrylic monomers of segment and epoxy monomer are selected in the present invention, be used in conjunction with each other both ensure that it is original
Intensity and hardness, and improve and be finally formed by curing the toughness of object.Trimethylolpropane trimethacrylate, propylene oxide simultaneously
The addition of the low viscosity resins such as acid esters diluent, ethoxylated trimethylolpropane triacrylate can be effectively reduced system
Overall viscosity facilitates the filming performance of resin.Further, since borosilicate modified epoxy is due to containing Si-O-B in its main chain
Structure, high and low temperature resistance is superior, is capable of the high and low temperature resistance of reinforced resin material.2,4,6 (trimethylbenzoyls)
Phase between the different initiators of diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl, three kinds of triaryl matte hexafluoro antimonate
Mutually cooperation, can greatly improve the efficiency of initiation of photocuring, ensure that acrylic resin can completely solidify with epoxy resin,
The solidification energy of photocuring can also be reduced.
Preferably, the borosilicate modified epoxy the preparation method is as follows:
(a) there-necked flask takes 10 parts of boron under -20-0 DEG C and nitrogen atmosphere with constant pressure funnel according to parts by weight
Acid, 48-52 parts of triethylamines, 50 parts of organic solvents are added in reaction kettle and are sufficiently stirred, and are then added in the low liquid funnel of constant pressure
45-50 parts of dimethylchlorosilanes and 50 parts of organic solvents, are slowly added dropwise into there-necked flask, the reaction was continued 3-5 after being added dropwise
Hour, it is filtered to remove the triethylamine hydrochloride of generation after reaction, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three
(dimethyl silicon substrate) borate；
(b) there-necked flask matches constant pressure funnel, under 80-100 DEG C and atmosphere, by three (diformazan obtained in step (a)
Base silicon substrate) 50 parts of borate, 50 parts, 0.05-0.2 parts platiniferous 2% of toluene platinum catalyst, then in constant pressure funnel plus
Enter 30 parts of 75-80 parts of allyl glycidyl ethers, toluene, is then slowly dropped to constant pressure funnel, continues after completion of dropwise addition
1-3 parts of active carbons are added after reaction and stir 0.5-2 hours for reaction 4-6 hours, and filtering is evaporated off solvent and low-boiling-point substance, obtains
To borosilicate modified epoxy.
Preferably, the organic solvent in the step (a) is tetrahydrofuran, anhydrous ether, methylene chloride, n-hexane
One of.
Preferably, the platinum catalyst of the step (b) is isopropyl alcohol solution of chloroplatinic acid, Karst catalyst, allyl
One of base silicon (oxygen) alkane platinum complex.Preferably,
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 30-90 minutes, is then taken out, add 2,4,6 (trimethylbenzene first
Acyl group) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred point
It dissipates 0.5-3 hours, then ultrasonic disperse 0.5-2 hours, finally uses vacuum oven deaeration, be kept in dark place to obtain ultraviolet light solidification
Coating.
Therefore, the invention has the following beneficial effects: the fast completion of cures of (1) resin solidification speed；(2)) resin system is viscous
It spends lower；(3)) hardness of film height, high and low temperature resistance and good toughness after solidifying.
Technical solution of the present invention is made to further describe explanation below by specific embodiment.
If saying that the raw material of use is raw material commonly used in the art without specified otherwise, in the embodiment of the present invention, implement
Method employed in example, is the conventional method of this field.
Embodiment 1
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 60 parts of epoxy acrylic, propylene oxide
50 parts of acid esters diluent, 20 parts of Tricyclodecane Dimethanol diacrylate, 20 parts of borosilicate modified epoxy, tripropylene glycol
20 parts of diacrylate, 60 parts of trimethylolpropane trimethacrylate, 5 parts of ethoxylated trimethylolpropane triacrylate,
2,4,6 5 parts of (trimethylbenzoyl) diphenyl phosphine oxides, 1 part of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte six
0.5 part of fluorine antimonate.
The borosilicate modified epoxy the preparation method is as follows:
(a) there-necked flask match constant pressure funnel, under -20 DEG C and nitrogen atmosphere, take according to parts by weight 10 parts of boric acid,
48 parts of triethylamines, 50 parts of tetrahydrofurans are added in reaction kettle and are sufficiently stirred, and 45 part two is then added in the low liquid funnel of constant pressure
Methylchlorosilane and 50 parts of tetrahydrofurans, are slowly added dropwise into there-necked flask, and the reaction was continued 3 hours after being added dropwise, reaction knot
The triethylamine hydrochloride of generation is filtered to remove after beam, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three (dimethyl-silicons
Base) borate.
(b) there-necked flask matches constant pressure funnel, under 80 DEG C and atmosphere, by three (dimethyl-silicon obtained in step (a)
Base) 50 parts of borate, 50 parts, 0.05 part platiniferous 2% of toluene isopropyl alcohol solution of chloroplatinic acid, then in constant pressure funnel plus
Enter 30 parts of 75 parts of allyl glycidyl ethers, toluene, is then slowly dropped to constant pressure funnel, the reaction was continued after completion of dropwise addition
4 hours, 1 part of active carbon is added after reaction and stirs 0.5 hour, solvent and low-boiling-point substance is evaporated off in filtering, and it is modified to obtain borosilicate
Epoxy resin.
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 30 minutes, is then taken out, add 2,4,6 (trimethylbenzoyls
Base) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred dispersion
0.5 hour, then ultrasonic disperse 0.5 hour, finally used vacuum oven deaeration, is kept in dark place to obtain ultraviolet-curing paint.
Embodiment 2
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 80 parts of epoxy acrylic, propylene oxide
65 parts of acid esters diluent, 45 parts of Tricyclodecane Dimethanol diacrylate, 30 parts of borosilicate modified epoxy, tripropylene glycol
35 parts of diacrylate, 80 parts of trimethylolpropane trimethacrylate, 15 parts of ethoxylated trimethylolpropane triacrylate,
2,4,6 8 parts of (trimethylbenzoyl) diphenyl phosphine oxides, 3 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte six
1.5 parts of fluorine antimonate.
(a) there-necked flask takes 10 parts of boric acid, 52 under 0 DEG C and nitrogen atmosphere with constant pressure funnel according to parts by weight
Part triethylamine, 50 parts of anhydrous ethers are added in reaction kettle and are sufficiently stirred, and 50 parts of diformazans are then added in the low liquid funnel of constant pressure
Base chlorosilane and 50 parts of anhydrous ethers, are slowly added dropwise into there-necked flask, and the reaction was continued 5 hours after being added dropwise, and reaction terminates
It is filtered to remove the triethylamine hydrochloride of generation afterwards, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three (dimethyl silicon substrates)
Borate.
(b) there-necked flask matches constant pressure funnel, under 100 DEG C and atmosphere, by three (dimethyl obtained in step (a)
Silicon substrate) 50 parts of borate, 50 parts, 0.2 part platiniferous 2% of toluene Karst catalyst, be then added in constant pressure funnel
30 parts of 80 parts of allyl glycidyl ethers, toluene, are then slowly dropped to constant pressure funnel, and the reaction was continued after completion of dropwise addition 6
Hour, 3 parts of active carbons are added after reaction and stir 2 hours, solvent and low-boiling-point substance is evaporated off in filtering, obtains the modified ring of borosilicate
Oxygen resin.
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 90 minutes, is then taken out, add 2,4,6 (trimethylbenzoyls
Base) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred dispersion 3
Hour, then ultrasonic disperse 2 hours, finally use vacuum oven deaeration, are kept in dark place to obtain ultraviolet-curing paint.
Embodiment 3
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 65 parts of epoxy acrylic, propylene oxide
55 parts of acid esters diluent, 25 parts of Tricyclodecane Dimethanol diacrylate, 22 parts of borosilicate modified epoxy, tripropylene glycol
25 parts of diacrylate, 65 parts of trimethylolpropane trimethacrylate, 5 parts of ethoxylated trimethylolpropane triacrylate,
2,4,6 6 parts of (trimethylbenzoyl) diphenyl phosphine oxides, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte six
1 part of fluorine antimonate.
The borosilicate modified epoxy the preparation method is as follows:
(a) there-necked flask match constant pressure funnel, under -10 DEG C and nitrogen atmosphere, take according to parts by weight 10 parts of boric acid,
50 parts of triethylamines, 50 parts of methylene chloride are added in reaction kettle and are sufficiently stirred, and 47 part two is then added in the low liquid funnel of constant pressure
Methylchlorosilane and 50 parts of methylene chloride, are slowly added dropwise into there-necked flask, and the reaction was continued 4 hours after being added dropwise, reaction knot
The triethylamine hydrochloride of generation is filtered to remove after beam, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three (dimethyl-silicons
Base) borate.
(b) there-necked flask matches constant pressure funnel, under 95 DEG C and atmosphere, by three (dimethyl-silicon obtained in step (a)
Base) 50 parts of borate, 50 parts, 0.1 part platiniferous 2% of toluene Karst catalyst, 75 are then added in constant pressure funnel
Part allyl glycidyl ether, 30 parts of toluene, are then slowly dropped to constant pressure funnel, and it is 5 small that the reaction was continued after completion of dropwise addition
When, 2 parts of active carbons are added after reaction and stir 1 hour, filtering is evaporated off solvent and low-boiling-point substance, obtains borosilicate modified epoxy
Resin.
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 50 minutes, is then taken out, add 2,4,6 (trimethylbenzoyls
Base) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred dispersion 2
Hour, then ultrasonic disperse 1 hour, finally uses vacuum oven deaeration, is kept in dark place to obtain ultraviolet-curing paint.
Embodiment 4
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 75 parts of epoxy acrylic, propylene oxide
60 parts of acid esters diluent, 40 parts of Tricyclodecane Dimethanol diacrylate, 28 parts of borosilicate modified epoxy, tripropylene glycol
30 parts of diacrylate, 75 parts of trimethylolpropane trimethacrylate, 15 parts of ethoxylated trimethylolpropane triacrylate,
2,4,6 5 parts of (trimethylbenzoyl) diphenyl phosphine oxides, 3 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte six
1.5 parts of fluorine antimonate.
The borosilicate modified epoxy the preparation method is as follows:
(a) there-necked flask match constant pressure funnel, under -5 DEG C and nitrogen atmosphere, take according to parts by weight 10 parts of boric acid,
48 parts of triethylamines, 50 parts there is n-hexane to be added in reaction kettle to be sufficiently stirred, 48 part two is then added in the low liquid funnel of constant pressure
Methylchlorosilane and 50 parts of n-hexanes, are slowly added dropwise into there-necked flask, and the reaction was continued 3 hours after being added dropwise, and reaction terminates
It is filtered to remove the triethylamine hydrochloride of generation afterwards, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three (dimethyl silicon substrates)
Borate.
(b) there-necked flask matches constant pressure funnel, under 85 DEG C and atmosphere, by three (dimethyl-silicon obtained in step (a)
Base) 50 parts of borate, 50 parts, 0.15 part platiniferous 2% of toluene allyl silicon (oxygen) alkane platinum complex, then constant pressure addition leak
80 parts of allyl glycidyl ethers, 30 parts of toluene are added in bucket, are then slowly dropped to constant pressure funnel, completion of dropwise addition is subsequent
1.5 parts of active carbons are added after reaction and stir 0.5 hour for continuous reaction 4 hours, and filtering is evaporated off solvent and low-boiling-point substance, obtains
Borosilicate modified epoxy.
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 60 minutes, is then taken out, add 2,4,6 (trimethylbenzoyls
Base) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred dispersion 1
Hour, then ultrasonic disperse 2 hours, finally use vacuum oven deaeration, are kept in dark place to obtain ultraviolet-curing paint.
Embodiment 5
A kind of ultraviolet-curing paint, it is composed of the following components according to parts by weight: 70 parts of epoxy acrylic, propylene oxide
58 parts of acid esters diluent, 30 parts of Tricyclodecane Dimethanol diacrylate, 25 parts of borosilicate modified epoxy, tripropylene glycol
28 parts of diacrylate, 70 parts of trimethylolpropane trimethacrylate, 7 parts of ethoxylated trimethylolpropane triacrylate,
2,4,6 7 parts of (trimethylbenzoyl) diphenyl phosphine oxides, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyl, triaryl matte six
1 part of fluorine antimonate.
The borosilicate modified epoxy the preparation method is as follows:
(a) there-necked flask match constant pressure funnel, under -20 DEG C and nitrogen atmosphere, take according to parts by weight 10 parts of boric acid,
48 parts of triethylamines, 50 parts of anhydrous ethers are added in reaction kettle and are sufficiently stirred, and 50 part two is then added in the low liquid funnel of constant pressure
Methylchlorosilane and 50 parts of anhydrous ethers, are slowly added dropwise into there-necked flask, and the reaction was continued 3-5 hours after being added dropwise, reaction
After be filtered to remove the triethylamine hydrochloride of generation, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three (dimethyl-silicons
Base) borate.
(b) there-necked flask matches constant pressure funnel, under 100 DEG C and atmosphere, by three (dimethyl obtained in step (a)
Silicon substrate) 50 parts of borate, 50 parts, 0.2 part platiniferous 2% of toluene Karst catalyst, be then added in constant pressure funnel
30 parts of 75 parts of allyl glycidyl ethers, toluene, are then slowly dropped to constant pressure funnel, and the reaction was continued after completion of dropwise addition 4
Hour, 3 parts of active carbons are added after reaction and stir 2 hours, solvent and low-boiling-point substance is evaporated off in filtering, obtains the modified ring of borosilicate
Oxygen resin.
The ultraviolet-curing paint coating the preparation method is as follows: by epoxy acrylic, epoxy acrylate dilute
Agent, Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trihydroxy methyl
Propane triacrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then
Container is put into baking oven and increases temperature to 45 DEG C, is heated 60 minutes, is then taken out, add 2,4,6 (trimethylbenzoyls
Base) diphenyl phosphine oxide, one phenyl ketone of 1- hydroxy-cyciohexyl and triaryl matte hexafluoro antimonate, high-speed stirred dispersion 3
Hour, then ultrasonic disperse 1 hour, finally uses vacuum oven deaeration, is kept in dark place to obtain ultraviolet-curing paint.
Performance test
The resin combination of embodiment 1-5 is passed through into photocuring, the film after photocuring passes through performance evaluation, specific item
Part is as follows, the result is as follows:
Pencil hardness: pencil hardness test is by standard GB/T/T6739-2006 test, and bear a heavy burden 500g
Glass transition temperature: setting DSC temperature range is 20-180 DEG C, 5 DEG C/min of heating rate.
Viscosity test: using the NDJ-7 type rotational viscometer of Shanghai balance equipment factory, control loop coolant-temperature gage at 30 DEG C,
The viscosity of resin sample to be measured at 30 DEG C of measurement.
Thermal decomposition temperature: setting TGA temperature range is 50-800 DEG C, 10 DEG C/min of heating rate.
Cubical contraction: the measurement work formula of cubical contraction is as follows
Wherein, η is that resin UV solidifies front and back cubical contraction, ρsFor the density for solidifying exemplar, ρlTo solidify preceding resin liquid
Density.
Water absorption rate: after the resin after the completion of solidification is placed in 100 DEG C of oven drying 5h, its weight m is surveyed0, then by batten
It is vertically arranged in the beaker for filling distilled water, distilled water liquid level is higher than batten, and removes the bubble on print.After 7 days, sample is taken out
Piece surveys its weight m after drying moisture1。
Claims (6)
1. a kind of ultraviolet-curing paint, characterized in that composed of the following components according to parts by weight: epoxy acrylate 60-
80 parts, 50-65 parts of epoxy acrylate diluent, 20-45 parts of Tricyclodecane Dimethanol diacrylate, borosilicate modified epoxy tree
20-30 parts of rouge, 20-35 parts of tri (propylene glycol) diacrylate, 60-80 parts of trimethylolpropane trimethacrylate, ethyoxyl
Change trimethylolpropane trimethacrylate 5-15 parts, 2,4,6(trimethylbenzoyl) 5-8 parts of diphenyl phosphine oxide, 1- hydroxyl-
1-3 parts, 0.5-1.5 parts of triaryl matte hexafluoro antimonate of one phenyl ketone of cyclohexyl；The borosilicate modified epoxy
The preparation method is as follows:
(a) there-necked flask match constant pressure funnel, under -20-0 DEG C and nitrogen atmosphere, take according to parts by weight 10 parts of boric acid,
48-52 parts of triethylamines, 50 parts of organic solvents are added in there-necked flask and are sufficiently stirred, and 45- is then added in constant pressure funnel
50 parts of dimethylchlorosilanes and 50 parts of organic solvents, are slowly added dropwise into there-necked flask, and the reaction was continued after being added dropwise, and 3-5 is small
When, it is filtered to remove the triethylamine hydrochloride of generation after reaction, filtrate washes 3 times, organic solvent is removed under reduced pressure, obtains three
(dimethyl silicon substrate) borate；
(b) there-necked flask matches constant pressure funnel, under 80-100 DEG C and nitrogen atmosphere, by three (diformazan obtained in step (a)
Base silicon substrate) 50 parts of borate, 50 parts, 0.05-0.2 parts platiniferous 2% of toluene platinum catalyst be added in there-necked flask, then in perseverance
It presses and 75-80 parts of allyl glycidyl ethers, 30 parts of toluene is added in dropping funel, be then slowly dropped in three-necked flask, drip
The reaction was continued after adding 4-6 hours, and 1-3 parts of active carbons are added after reaction and stir 0.5-2 hours, solvent is evaporated off in filtering
And low-boiling-point substance, obtain borosilicate modified epoxy.
2. a kind of ultraviolet-curing paint according to claim 1, characterized in that according to parts by weight by following components group
At: 65-75 parts of epoxy acrylate, 55-60 parts of epoxy acrylate diluent, Tricyclodecane Dimethanol diacrylate 25-
40 parts, 22-28 parts of borosilicate modified epoxy, 25-30 parts of tri (propylene glycol) diacrylate, trimethylolpropane tris propylene
65-75 parts of acid esters, 5-15 parts of ethoxylated trimethylolpropane triacrylate, 2,4,6(trimethylbenzoyl) diphenyl
5-8 parts of phosphine oxide, 1-3 parts, 0.5-1.5 parts of triaryl matte hexafluoro antimonate of one phenyl ketone of 1- hydroxy-cyciohexyl.
3. a kind of ultraviolet-curing paint according to claim 1, characterized in that according to parts by weight by following components group
At: 70 parts of epoxy acrylate, 58 parts of epoxy acrylate diluent, 30 parts of Tricyclodecane Dimethanol diacrylate, borosilicate
25 parts of modified epoxy, 28 parts of tri (propylene glycol) diacrylate, 70 parts of trimethylolpropane trimethacrylate, ethyoxyl
Change 7 parts of trimethylolpropane trimethacrylate, 2,4,6(trimethylbenzoyl) 7 parts of diphenyl phosphine oxide, 1- hydroxy-cyclohexan
2 parts, 1 part of triaryl matte hexafluoro antimonate of one phenyl ketone of base.
4. a kind of ultraviolet-curing paint according to claim 1, characterized in that organic molten in the step (a)
Agent is one of tetrahydrofuran, anhydrous ether, methylene chloride, n-hexane.
5. a kind of ultraviolet-curing paint according to claim 1, characterized in that the platinum catalyst of the step (b)
For one of isopropyl alcohol solution of chloroplatinic acid, Karst catalyst, Allyl Siloxane platinum complex.
6. a kind of ultraviolet-curing paint described according to claim 1 ~ any one of 3, characterized in that the ultraviolet light
It is coating material solidified the preparation method is as follows: by epoxy acrylate, epoxy acrylate diluent, two propylene of Tricyclodecane Dimethanol
Acid esters, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trimethylolpropane trimethacrylate and ethyoxyl
Change trimethylolpropane trimethacrylate to be added in container according to parts by weight, then container is put into baking oven and increases temperature
To 45 DEG C, heat 30-90 minutes, then take out, add 2,4,6(trimethylbenzoyls) diphenyl phosphine oxide, 1- hydroxyl-
One phenyl ketone of cyclohexyl and triaryl matte hexafluoro antimonate, high-speed stirred are dispersed 0.5-3 hours, then ultrasonic disperse
0.5-2 hours, vacuum oven deaeration is finally used, is kept in dark place to obtain ultraviolet-curing paint.
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