CN107629639A - A kind of ultraviolet-curing paint - Google Patents
A kind of ultraviolet-curing paint Download PDFInfo
- Publication number
- CN107629639A CN107629639A CN201710995490.7A CN201710995490A CN107629639A CN 107629639 A CN107629639 A CN 107629639A CN 201710995490 A CN201710995490 A CN 201710995490A CN 107629639 A CN107629639 A CN 107629639A
- Authority
- CN
- China
- Prior art keywords
- parts
- ultraviolet
- epoxy
- curing paint
- diacrylate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Paints Or Removers (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of ultraviolet-curing paint, it is characterized in that, count in parts by weight composed of the following components：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）58 parts of diphenyl phosphine oxide, 13 parts of 1 hydroxy-cyclohexyl, one phenyl ketone, 0.5 1.5 parts of triaryl matte hexafluoro antimonate.The present invention has the advantages that：（1）The fast completion of cure of resin solidification speed；（2））Resin system viscosity is relatively low；（3））Hardness of film height, high and low temperature resistance and good toughness after solidification.
Description
Technical field
The present invention relates to a kind of coating, more particularly, to a kind of ultraviolet-curing paint.
Background technology
In the past few years, ultraviolet-curing paint fibre coating, CD coatings/DVD adhesives, credit card, timber,
Suffer from very rapidly developing in beverage can, packaging for foodstuff, journal surface, medicine equipment and automobile industry.Ultraviolet light solidifies
Coating possesses huge market potential, and its ratio in whole coating products increases year by year.Ultraviolet-curing paint master
To be made up of oligomer, monomer, light trigger and auxiliary agent.The key reaction course of ultraviolet light solidification solidification is to cause light by radiation
Decomposition of initiator, generation living radical trigger monomer/oligomer polymerization crosslinking.
The resin used in ultraviolet light solidification at present is just two kinds of substantially acrylic resin and epoxy resin, wherein third
Olefin(e) acid resin, it is the resin made of esters of acrylic acid and methyl acrylic ester and other olefinic type monomers are copolymerized, passes through selection
Different resin structure, different formulas, production technology and solvent compositions, can synthesize different type, different performance and difference should
With the acrylic resin of occasion, acrylic resin can be divided into thermoplastic acrylic resin again according to structure and the difference of membrane formation mechanism
And thermosetting acrylic resin.With main suction of the acrylic resin of acrylate and methacrylate monomers copolymerization to light
Receive peak to be in outside solar spectrum scope, so obtained acrylic resin paint has excellent light resistance and anti-outdoor aging
Energy.Thermosetting acrylic resin refers to carry certain functional group in the structure, in painting by the amino resins with addition,
Functional group reactionses in epoxy resin, polyurethane etc. form network structure, and the general relative molecular weight of thermosetting resin is relatively low.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 coordinate amino-acrylonitrile acid baking vanish is made, at present automobile, motorcycle, bicycle,
Using quite varied on the products such as coil.
But the energy at present used in acrylate ultraviolet light curable coating photocuring on the market is higher, is obtained after solidification
Although film hardness it is higher, it is more crisp, can not impact resistance, its high and low temperature resistance, and it is not water-fast intolerant to dirt.It is such as a kind of
A kind of light-cured resin reported in Chinese patent literature and application thereof, its application publication number are the A of CN 106866889, should
Light-cured resin is made up of based on weight/mass percentage composition following component：EMA is 4.6-10.8%, ethyl acetate
It is 0.1-0.6% for 4.6-9.2%, polyurethane acrylic resin 80-90%, benzophenone -1.The light-cured resin of the present invention
Cost of material is cheap, and it is convenient to obtain, and is easy to store, nontoxic to human body, drops in good penetrability on fiber, film forming rapidly may be used
Control, solid flexible, easily operation of cutting into slices, 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 border and lumen are clear, and feature is obvious, are easy to differentiate.But it is there is also more deficiency, such as it makes
It is mostly small molecule acrylate, after photocuring, its crosslink density is larger for it, although having preferable hardness, toughness
It is not high, and its high and low temperature resistance is poor can not meet daily use.
The content 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, there is provided one kind can high-low temperature resistant, a kind of tough and tensile ultraviolet-curing paint of the coating property that is obtained after solidification.
To achieve these goals, the present invention uses following technical scheme：
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：Epoxy acrylic 60-80 parts, propylene oxide
Acid esters diluent 50-65 parts, Tricyclodecane Dimethanol diacrylate 20-45 parts, borosilicate modified epoxy 20-30 parts, two
Contracting tripropylene glycol diacrylate 20-35 parts, trimethylolpropane trimethacrylate 60-80 parts, ethoxylation trihydroxy methyl third
Alkane triacrylate 5-15 parts, 2,4,6（Trimethylbenzoyl）Diphenyl phosphine oxide 5-8 parts, the phenyl of 1- hydroxy-cyciohexyls one
Ketone 1-3 parts, triaryl matte hexafluoro antimonate 0.5-1.5 parts.
Preferably, count in parts by weight composed of the following components：Epoxy acrylic 65-75 parts, epoxy acrylate are dilute
Release agent 55-60 parts, Tricyclodecane Dimethanol diacrylate 25-40 parts, borosilicate modified epoxy 22-28 parts, two contractings 3 third
Omega-diol diacrylate 25-30 parts, trimethylolpropane trimethacrylate 65-75 parts, ethoxylated trimethylolpropane 3 third
Olefin(e) acid ester 5-15 parts, 2,4,6（Trimethylbenzoyl）Diphenyl phosphine oxide 5-8 parts, the phenyl ketone 1- of 1- hydroxy-cyciohexyls one
3 parts, triaryl matte hexafluoro antimonate 0.5-1.5 parts.
Preferably, count in parts by weight composed of the following components：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 three
Base benzoyl）7 parts of diphenyl phosphine oxide, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro antimonate 1
Part.
From the longer acrylic monomers and epoxy monomer of segment in the present invention, be used in conjunction with each other both ensure that it is original
Intensity and hardness, improve the final toughness for being formed by curing thing again.Trimethylolpropane trimethacrylate, propylene oxide simultaneously
The addition of the low viscosity resins such as acid esters diluent, ethoxylated trimethylolpropane triacrylate can effectively reduce system
Overall viscosity, contribute to the filming performance of resin.Further, since borosilicate modified epoxy in its main chain due to containing Si-O-B
Structure, its high and low temperature resistance is superior, is capable of the high and low temperature resistance of reinforced resin material.2,4,6（Trimethylbenzoyl）
Phase between three kinds of diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one, triaryl matte hexafluoro antimonate different initiators
Mutually coordinate, the efficiency of initiation of photocuring can be greatly improved, ensure that acrylic resin can completely solidify with epoxy resin,
The solidification energy of photocuring can also be reduced.
Preferably, the preparation method of described borosilicate modified epoxy is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -20-0 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid,
48-52 parts triethylamine, 50 parts of organic solvents are added in reactor and are sufficiently stirred, and then add 45- in the low liquid funnel of constant pressure
50 parts of dimethylchlorosilanes and 50 parts of organic solvents, are slowly added dropwise into there-necked flask, and it is small to continue reaction 3-5 after being added dropwise
When, reaction is filtered to remove the triethylamine hydrochloride of generation after terminating, filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three
（Dimethyl silicon substrate）Borate；
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 80-100 DEG C and atmosphere, by step（a）In obtain three（Dimethyl-silicon
Base）50 parts of borate, 50 parts of toluene, the platinum catalyst of 0.05-0.2 parts platiniferous 2%, then add 75- in constant pressure funnel
30 parts of 80 parts of allyl glycidyl ethers, toluene, constant pressure funnel is then slowly dropped to, continues to react 4- after completion of dropwise addition
6 hours, reaction added 1-3 parts activated carbon stirring 0.5-2 hours after terminating, filtering, solvent and low-boiling-point substance is evaporated off, obtains borosilicate
Modified epoxy.
Preferably, described step（a）In organic solvent for tetrahydrofuran, absolute ether, dichloromethane, n-hexane
In one kind.
Preferably, described step（b）Platinum catalyst for isopropyl alcohol solution of chloroplatinic acid, Karst catalyst, allyl
One kind in base silicon (oxygen) alkane platinum complex.Preferably,
The preparation method of described ultraviolet-curing paint coating is as follows：By epoxy acrylic, epoxy acrylate diluent, three
Cyclodecane Dimethanol Diacrylate, borosilicate modified epoxy, tri (propylene glycol) diacrylate, trimethylolpropane tris
Acrylate and ethoxylated trimethylolpropane triacrylate are added in container according to parts by weight, then by container
It is put into baking oven and raises temperature to 45 DEG C, heats 30-90 minutes, then take out, add 2,4,6（Trimethylbenzoyl）Two
Phenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred disperse 0.5-3
Hour, then ultrasonic disperse 0.5-2 hours, finally with vacuum drying chamber deaeration, it is kept in dark place to obtain ultraviolet-curing paint.
Therefore, the present invention has the advantages that：（1）The fast completion of cure of resin solidification speed；（2））Resin system glues
Spend relatively low；（3））Hardness of film height, high and low temperature resistance and good toughness after solidification.
Technical scheme is made to further describe explanation below by specific embodiment.
If without specified otherwise, the raw material that use is said in embodiments of the invention is raw material commonly used in the art, is implemented
Method employed in example, it is the conventional method of this area.
Embodiment 1
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：60 parts of epoxy acrylic, epoxy acrylate
50 parts of diluent, 20 parts of Tricyclodecane Dimethanol diacrylate, 20 parts of borosilicate modified epoxy, tripropylene glycol dipropyl
20 parts of olefin(e) acid ester, 60 parts of trimethylolpropane trimethacrylate, 5 parts of ethoxylated trimethylolpropane triacrylate, 2,4,6
（Trimethylbenzoyl）5 parts of diphenyl phosphine oxide, 1 part of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro-antimonic acid
0.5 part of salt.
The preparation method of described borosilicate modified epoxy is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -20 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid, 48 parts
Triethylamine, 50 parts of tetrahydrofurans are added in reactor and are sufficiently stirred, and 45 parts of dimethyl are then added in the low liquid funnel of constant pressure
Chlorosilane and 50 parts of tetrahydrofurans, are slowly added dropwise into there-necked flask, continue reaction 3 hours after being added dropwise, after reaction terminates
The triethylamine hydrochloride of generation is filtered to remove, filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three（Dimethyl silicon substrate）Boron
Acid esters.
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 80 DEG C and atmosphere, by step（a）In obtain three（Dimethyl-silicon
Base）The isopropyl alcohol solution of chloroplatinic acid of 50 parts, 0.05 part 50 parts of borate, toluene platiniferous 2%, then add in constant pressure funnel
Enter 30 parts of 75 parts of allyl glycidyl ethers, toluene, be then slowly dropped to constant pressure funnel, continue to react after completion of dropwise addition
4 hours, reaction added 1 part of activated carbon after terminating and stirred 0.5 hour, filtering, solvent and low-boiling-point substance is evaporated off, and obtained borosilicate modification
Epoxy resin.
The preparation method of described ultraviolet-curing paint coating is as follows：Epoxy acrylic, epoxy acrylate are diluted
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 raises temperature to 45 DEG C, is heated 30 minutes, is then taken out, add 2,4,6（Trimethylbenzoyl
Base）Diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred are disperseed
0.5 hour, then ultrasonic disperse 0.5 hour, finally with vacuum drying chamber deaeration, was kept in dark place to obtain ultraviolet-curing paint.
Embodiment 2
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：80 parts of epoxy acrylic, epoxy acrylate
65 parts of diluent, 45 parts of Tricyclodecane Dimethanol diacrylate, 30 parts of borosilicate modified epoxy, tripropylene glycol dipropyl
35 parts of olefin(e) acid ester, 80 parts of trimethylolpropane trimethacrylate, 15 parts of ethoxylated trimethylolpropane triacrylate, 2,4,
6（Trimethylbenzoyl）8 parts of diphenyl phosphine oxide, 3 parts of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro antimony
1.5 parts of hydrochlorate.
（a）There-necked flask matches somebody with somebody constant pressure funnel, and under 0 DEG C and nitrogen atmosphere, 10 parts of boric acid, 52 are taken according to parts by weight
Part triethylamine, 50 parts of absolute ethers are added in reactor 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 absolute ethers, are slowly added dropwise into there-necked flask, continue reaction 5 hours after being added dropwise, reaction terminates
The triethylamine hydrochloride of generation is filtered to remove afterwards, and filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three（Dimethyl silicon substrate）
Borate.
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 100 DEG C and atmosphere, by step（a）In obtain three（Dimethyl
Silicon substrate）The Karst catalyst of 50 parts, 0.2 part 50 parts of borate, toluene platiniferous 2%, then adds 80 in constant pressure funnel
Part allyl glycidyl ether, 30 parts of toluene, are then slowly dropped to constant pressure funnel, and it is small to continue reaction 6 after completion of dropwise addition
When, reaction adds 3 parts of activated carbons after terminating and stirred 2 hours, filtering, solvent and low-boiling-point substance is evaporated off, obtains borosilicate modified epoxy
Resin.
The preparation method of described ultraviolet-curing paint coating is as follows：Epoxy acrylic, epoxy acrylate are diluted
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 raises temperature to 45 DEG C, is heated 90 minutes, is then taken out, add 2,4,6（Trimethylbenzoyl
Base）Diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred scattered 3
Hour, then ultrasonic disperse 2 hours, finally with vacuum drying chamber deaeration, are kept in dark place to obtain ultraviolet-curing paint.
Embodiment 3
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：65 parts of epoxy acrylic, epoxy acrylate
55 parts of diluent, 25 parts of Tricyclodecane Dimethanol diacrylate, 22 parts of borosilicate modified epoxy, tripropylene glycol dipropyl
25 parts of olefin(e) acid ester, 65 parts of trimethylolpropane trimethacrylate, 5 parts of ethoxylated trimethylolpropane triacrylate, 2,4,6
（Trimethylbenzoyl）6 parts of diphenyl phosphine oxide, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro-antimonic acid
1 part of salt.
The preparation method of described borosilicate modified epoxy is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -10 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid, 50 parts
Triethylamine, 50 parts of dichloromethane are added in reactor and are sufficiently stirred, and 47 parts of dimethyl are then added in the low liquid funnel of constant pressure
Chlorosilane and 50 parts of dichloromethane, are slowly added dropwise into there-necked flask, continue reaction 4 hours after being added dropwise, after reaction terminates
The triethylamine hydrochloride of generation is filtered to remove, filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three（Dimethyl silicon substrate）Boron
Acid esters.
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 95 DEG C and atmosphere, by step（a）In obtain three（Dimethyl-silicon
Base）The Karst catalyst of 50 parts, 0.1 part 50 parts of borate, toluene platiniferous 2%, 75 parts are then added in constant pressure funnel
30 parts of allyl glycidyl ether, toluene, constant pressure funnel is then slowly dropped to, continues reaction 5 hours after completion of dropwise addition,
Reaction adds 2 parts of activated carbons after terminating and stirred 1 hour, filtering, solvent and low-boiling-point substance is evaporated off, obtains borosilicate modified epoxy tree
Fat.
The preparation method of described ultraviolet-curing paint coating is as follows：Epoxy acrylic, epoxy acrylate are diluted
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 raises temperature to 45 DEG C, is heated 50 minutes, is then taken out, add 2,4,6（Trimethylbenzoyl
Base）Diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred scattered 2
Hour, then ultrasonic disperse 1 hour, finally with vacuum drying chamber deaeration, is kept in dark place to obtain ultraviolet-curing paint.
Embodiment 4
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：75 parts of epoxy acrylic, epoxy acrylate
60 parts of diluent, 40 parts of Tricyclodecane Dimethanol diacrylate, 28 parts of borosilicate modified epoxy, tripropylene glycol dipropyl
30 parts of olefin(e) acid ester, 75 parts of trimethylolpropane trimethacrylate, 15 parts of ethoxylated trimethylolpropane triacrylate, 2,4,
6（Trimethylbenzoyl）5 parts of diphenyl phosphine oxide, 3 parts of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro antimony
1.5 parts of hydrochlorate.
The preparation method of described borosilicate modified epoxy is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -5 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid, 48 parts
Triethylamine, 50 parts there is n-hexane to be added in reactor to be sufficiently stirred, 48 parts of dimethyl are then added in the low liquid funnel of constant pressure
Chlorosilane and 50 parts of n-hexanes, are slowly added dropwise into there-necked flask, continue reaction 3 hours, mistake after reaction terminates after being added dropwise
The triethylamine hydrochloride of generation is filtered out, filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three（Dimethyl silicon substrate）Boric acid
Ester.
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 85 DEG C and atmosphere, by step（a）In obtain three（Dimethyl-silicon
Base）Pi-allyl silicon (oxygen) alkane platinum complex of 50 parts, 0.15 part 50 parts of borate, toluene platiniferous 2%, then leaked in constant pressure addition
80 parts of allyl glycidyl ethers, 30 parts of toluene are added in bucket, is then slowly dropped to constant pressure funnel, completion of dropwise addition is follow-up
Continuous reaction 4 hours, reaction add 1.5 parts of activated carbons after terminating and stirred 0.5 hour, filtering, solvent and low-boiling-point substance be evaporated off, obtains
Borosilicate modified epoxy.
The preparation method of described ultraviolet-curing paint coating is as follows：Epoxy acrylic, epoxy acrylate are diluted
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 raises temperature to 45 DEG C, is heated 60 minutes, is then taken out, add 2,4,6（Trimethylbenzoyl
Base）Diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred scattered 1
Hour, then ultrasonic disperse 2 hours, finally with vacuum drying chamber deaeration, are kept in dark place to obtain ultraviolet-curing paint.
Embodiment 5
A kind of ultraviolet-curing paint, count in parts by weight composed of the following components：70 parts of epoxy acrylic, epoxy acrylate
58 parts of diluent, 30 parts of Tricyclodecane Dimethanol diacrylate, 25 parts of borosilicate modified epoxy, tripropylene glycol dipropyl
28 parts of olefin(e) acid ester, 70 parts of trimethylolpropane trimethacrylate, 7 parts of ethoxylated trimethylolpropane triacrylate, 2,4,6
（Trimethylbenzoyl）7 parts of diphenyl phosphine oxide, 2 parts of one phenyl ketone of 1- hydroxy-cyciohexyls, triaryl matte hexafluoro-antimonic acid
1 part of salt.
The preparation method of described borosilicate modified epoxy is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -20 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid, 48 parts
Triethylamine, 50 parts of absolute ethers are added in reactor and are sufficiently stirred, and 50 parts of dimethyl are then added in the low liquid funnel of constant pressure
Chlorosilane and 50 parts of absolute ethers, are slowly added dropwise into there-necked flask, continue to react 3-5 hours after being added dropwise, reaction terminates
The triethylamine hydrochloride of generation is filtered to remove afterwards, and filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three（Dimethyl silicon substrate）
Borate.
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 100 DEG C and atmosphere, by step（a）In obtain three（Dimethyl
Silicon substrate）The Karst catalyst of 50 parts, 0.2 part 50 parts of borate, toluene platiniferous 2%, then adds 75 in constant pressure funnel
Part allyl glycidyl ether, 30 parts of toluene, are then slowly dropped to constant pressure funnel, and it is small to continue reaction 4 after completion of dropwise addition
When, reaction adds 3 parts of activated carbons after terminating and stirred 2 hours, filtering, solvent and low-boiling-point substance is evaporated off, obtains borosilicate modified epoxy
Resin.
The preparation method of described ultraviolet-curing paint coating is as follows：Epoxy acrylic, epoxy acrylate are diluted
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 raises temperature to 45 DEG C, is heated 60 minutes, is then taken out, add 2,4,6（Trimethylbenzoyl
Base）Diphenyl phosphine oxide, the phenyl ketone of 1- hydroxy-cyciohexyls one and triaryl matte hexafluoro antimonate, high-speed stirred scattered 3
Hour, then ultrasonic disperse 1 hour, finally with vacuum drying chamber deaeration, is kept in dark place to obtain ultraviolet-curing paint.
Performance test
Embodiment 1- 5 resin combination is passed through into photocuring, the film after photocuring passes through performance evaluation, its actual conditions
It is as follows, its result such as following table：
Pencil hardness：Pencil hardness test is by standard GB/T/T6739-2006 tests, heavy burden 500g
Glass transition temperature：It is 20-180 DEG C to set DSC temperature ranges, 5 DEG C/min of heating rate.
Viscosity test：Using the NDJ-7 type rotation viscometers of Shanghai balance equipment factory, circulating water temperature is controlled at 30 DEG C,
The viscosity of resin sample to be measured at 30 DEG C of measure.
Heat decomposition temperature：It is 50-800 DEG C to set TGA temperature ranges, 10 DEG C/min of heating rate.
Cubical contraction：The measure work formula of cubical contraction is as follows
Wherein, cubical contraction before and after η solidifies for resin UV, ρsTo solidify the density of exemplar, ρlFor resin liquid before solidification
Density.
Water absorption rate：After resin after the completion of solidification is placed in into 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, its weight m is surveyed after drying moisture1。
| Project | Pencil hardness | Glass transition temperature（℃） | Viscosity（Pa·s） | Originate heat decomposition temperature（℃） | Cubical contraction（%） | Water absorption rate（%） |
| Embodiment 1 | 6H | 98.1 | 395 | 286 | 3.5 | 0.91 |
| Embodiment 2 | 6H | 103.5 | 425 | 325 | 4.7 | 0.88 |
| Embodiment 3 | 6H | 98.9 | 405 | 299 | 3.9 | 0.72 |
| Embodiment 4 | 6H | 101.3 | 420 | 315 | 4.3 | 0.82 |
| Embodiment 5 | 6H | 99.6 | 410 | 308 | 4.3 | 0.75 |
Claims (7)
1. a kind of ultraviolet-curing paint, it is characterized in that, count in parts by weight composed of the following components：Epoxy acrylic 60-80
Part, epoxy acrylate diluent 50-65 parts, Tricyclodecane Dimethanol diacrylate 20-45 parts, borosilicate modified epoxy
20-30 parts, tri (propylene glycol) diacrylate 20-35 parts, trimethylolpropane trimethacrylate 60-80 parts, ethoxylation
Trimethylolpropane trimethacrylate 5-15 parts, 2,4,6（Trimethylbenzoyl）Diphenyl phosphine oxide 5-8 parts, 1- hydroxyls-ring
The phenyl ketone 1-3 parts of hexyl one, triaryl matte hexafluoro antimonate 0.5-1.5 parts.
2. a kind of ultraviolet-curing paint according to claim 1, it is characterized in that, count in parts by weight by following components group
Into：Epoxy acrylic 65-75 parts, epoxy acrylate diluent 55-60 parts, Tricyclodecane Dimethanol diacrylate 25-40
Part, borosilicate modified epoxy 22-28 parts, tri (propylene glycol) diacrylate 25-30 parts, trimethylolpropane tris acrylic acid
Ester 65-75 parts, ethoxylated trimethylolpropane triacrylate 5-15 parts, 2,4,6（Trimethylbenzoyl）Dipheny oxide
Change phosphine 5-8 parts, the phenyl ketone 1-3 parts of 1- hydroxy-cyciohexyls one, triaryl matte hexafluoro antimonate 0.5-1.5 parts.
3. a kind of ultraviolet-curing paint according to claim 1, it is characterized in that, count in parts by weight by following components group
Into：70 parts of epoxy acrylic, 58 parts of epoxy acrylate diluent, 30 parts of Tricyclodecane Dimethanol diacrylate, borosilicate change
25 parts of epoxy resin of property, 28 parts of tri (propylene glycol) diacrylate, 70 parts of trimethylolpropane trimethacrylate, ethoxylation
7 parts of trimethylolpropane trimethacrylate, 2,4,6（Trimethylbenzoyl）7 parts of diphenyl phosphine oxide, 1- hydroxy-cyciohexyls
One 2 parts of phenyl ketone, 1 part of triaryl matte hexafluoro antimonate.
4. a kind of ultraviolet-curing paint according to claim 1 ~ 3, it is characterized in that, described borosilicate modified epoxy
Preparation method it is as follows：
（a）There-necked flask matches somebody with somebody constant pressure funnel, under -20-0 DEG C and nitrogen atmosphere, according to parts by weight take 10 parts of boric acid,
48-52 parts triethylamine, 50 parts of organic solvents are added in reactor and are sufficiently stirred, and then add 45- in the low liquid funnel of constant pressure
50 parts of dimethylchlorosilanes and 50 parts of organic solvents, are slowly added dropwise into there-necked flask, and it is small to continue reaction 3-5 after being added dropwise
When, reaction is filtered to remove the triethylamine hydrochloride of generation after terminating, filtrate is washed 3 times, organic solvent is removed under reduced pressure, obtains three
（Dimethyl silicon substrate）Borate；
（b）There-necked flask matches somebody with somebody constant pressure funnel, under 80-100 DEG C and atmosphere, by step（a）In obtain three（Dimethyl-silicon
Base）50 parts of borate, 50 parts of toluene, the platinum catalyst of 0.05-0.2 parts platiniferous 2%, then add 75- in constant pressure funnel
30 parts of 80 parts of allyl glycidyl ethers, toluene, constant pressure funnel is then slowly dropped to, continues to react 4- after completion of dropwise addition
6 hours, reaction added 1-3 parts activated carbon stirring 0.5-2 hours after terminating, filtering, solvent and low-boiling-point substance is evaporated off, obtains borosilicate
Modified epoxy.
5. a kind of ultraviolet-curing paint according to claim 4, it is characterized in that, described step（a）In it is organic molten
Agent is one kind in tetrahydrofuran, absolute ether, dichloromethane, n-hexane.
6. a kind of ultraviolet-curing paint according to claim 4, it is characterized in that, described step（b）Platinum catalyst
For one kind in isopropyl alcohol solution of chloroplatinic acid, Karst catalyst, pi-allyl silicon (oxygen) alkane platinum complex.
7. a kind of ultraviolet-curing paint according to claim 1 ~ 3, it is characterized in that, described ultraviolet-curing paint applies
The preparation method of material is as follows：By epoxy acrylic, epoxy acrylate diluent, Tricyclodecane Dimethanol diacrylate, boron
Silicon modified epoxy resin, tri (propylene glycol) diacrylate, trimethylolpropane trimethacrylate and the hydroxyl of ethoxylation three
Propane tri is added in container according to parts by weight, and then container is put into baking oven and raises temperature to 45
DEG C, 30-90 minutes are heated, then takes out, adds 2,4,6（Trimethylbenzoyl）Diphenyl phosphine oxide, 1- hydroxy-cyclohexans
The phenyl ketone of base one and triaryl matte hexafluoro antimonate, high-speed stirred disperse 0.5-3 hours, then ultrasonic disperse 0.5-2
Hour, finally with vacuum drying chamber deaeration, it is kept in dark place to obtain ultraviolet-curing paint.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710995490.7A CN107629639B (en) | 2017-10-23 | 2017-10-23 | A kind of ultraviolet-curing paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710995490.7A CN107629639B (en) | 2017-10-23 | 2017-10-23 | A kind of ultraviolet-curing paint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107629639A true CN107629639A (en) | 2018-01-26 |
| CN107629639B CN107629639B (en) | 2019-09-24 |
Family
ID=61104896
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710995490.7A Active CN107629639B (en) | 2017-10-23 | 2017-10-23 | A kind of ultraviolet-curing paint |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107629639B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439047A (en) * | 2018-09-30 | 2019-03-08 | 广州申威新材料科技有限公司 | A kind of preparation method of high abrasion UV low luster coating and its preparation method of UV dumb light coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761994A (en) * | 2015-04-10 | 2015-07-08 | 南昌航空大学 | Preparation method of photocuring organic silicon modified epoxy resin paint film |
-
2017
- 2017-10-23 CN CN201710995490.7A patent/CN107629639B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761994A (en) * | 2015-04-10 | 2015-07-08 | 南昌航空大学 | Preparation method of photocuring organic silicon modified epoxy resin paint film |
Non-Patent Citations (1)
| Title |
|---|
| 杨凤等: "有机硅硼改性环氧树脂胶粘剂的研制", 《中国胶粘剂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109439047A (en) * | 2018-09-30 | 2019-03-08 | 广州申威新材料科技有限公司 | A kind of preparation method of high abrasion UV low luster coating and its preparation method of UV dumb light coating |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107629639B (en) | 2019-09-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11732141B2 (en) | Functionalized dimethoxyphenol monomers and methods for preparing such monomers | |
| Baştürk et al. | Flame retardant UV-curable acrylated epoxidized soybean oil based organic–inorganic hybrid coating | |
| CN110590987B (en) | Fluorine-silicon copolymerized acrylic resin and preparation method and application thereof | |
| US11028204B2 (en) | Curable compositions comprising mono-functional acrylates | |
| CN101932614A (en) | Method for preparing a hard film or coating from a cationically crosslinkable/polymerizable composition comprising an iodonium borate and giving off an acceptable odour | |
| CN103443149B (en) | Lipophile highly-branched polymers and the optical polymerism composition for including the lipophile highly-branched polymers | |
| CN101962430B (en) | Method for producing ultraviolet curable amino acrylate resin | |
| CN109735144B (en) | Photocuring POSS/fluorocarbon siloxane modified polyacrylate coating composition and application thereof | |
| CN107936746A (en) | A kind of organic-silicon-modified cation photocuring cycloaliphatic epoxy resin coating and its application | |
| CN104011130B (en) | Photocurable fluorine-containing copolymer composition | |
| CN105542098B (en) | A kind of modified aldehyde ketone resin and preparation method and application | |
| CN105198741B (en) | Hyperbranched monomer of a kind of tetrahydroxylic alcohol based on maleic anhydride and preparation method thereof | |
| CN107629639A (en) | A kind of ultraviolet-curing paint | |
| JP2003212975A (en) | Curable composition | |
| JP2015021045A (en) | Optical three-dimensional contouring resin composition consisting of cyclic ether group-containing (meth)acrylate | |
| CN108047893A (en) | A kind of environmental protection ultraviolet-curing paint | |
| US7655745B2 (en) | Polysilane compound and synthesis method, ultraviolet-ray curable ink composition, inkjet recording method and apparatus, and ink container | |
| CN106957590B (en) | Modified silicon-acrylic coatings of a kind of high-performance UV curing type PU and preparation method thereof | |
| US4289595A (en) | Ambient temperature curing photopolymerizable epoxide compositions utilizing epoxide ethers and methods | |
| CN109749085A (en) | A kind of crosslinking silicone type acrylate oligomer and its Photocurable composition of preparation | |
| Wazarkar et al. | Synthesis and Characterization of UV Oligomer based on Cardanol | |
| CN107652736B (en) | A kind of epoxy ultraviolet-curing paint | |
| US20130296485A1 (en) | Self-sensitive polymerizable liquid resin and use thereof | |
| CN106588860A (en) | Dimethyl dioxane pentyl alkanol methacrylate monomer and application thereof | |
| CN101875715B (en) | Epoxy modified polyurethane, UV-curing coat and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201202 Address after: 515636 No. 1, Lane 2, Dongtougongqian District, Stork Chao Sancun, Longhu Town, Chaoan District, Chaozhou City, Guangdong Province Patentee after: Li Yanling Address before: 313200 Zhejiang city of Huzhou province Deqing County Wukang Ring Road No. 190 Patentee before: ZHEJIANG TIMBER NEW MATERIAL Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201223 Address after: 510000 5th floor, No.2 workshop, No.9 Lanyu 4th Street, Guangzhou Economic and Technological Development Zone, Guangdong Province (North 502-503) Patentee after: Guangzhou Junjie Environmental Protection Technology Co.,Ltd. Address before: 515636 No.1, Lane 2, District 1, dongtougongqian, stork nest third village, Longhu Town, Chao'an District, Chaozhou City, Guangdong Province Patentee before: Li Yanling |
|
| TR01 | Transfer of patent right |