CN110387163A - A kind of low viscosity aqueous UV ink and preparation method thereof - Google Patents
A kind of low viscosity aqueous UV ink and preparation method thereof Download PDFInfo
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- CN110387163A CN110387163A CN201910666707.9A CN201910666707A CN110387163A CN 110387163 A CN110387163 A CN 110387163A CN 201910666707 A CN201910666707 A CN 201910666707A CN 110387163 A CN110387163 A CN 110387163A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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Abstract
The invention discloses a kind of low viscosity aqueous UV ink, according to mass percent, it is composed of the following components: water soluble acrylic acid prepolymer 30%~50%, aqueous active diluent 20%~50%, solvent 10%~30%, photoinitiator 1%~4%, pigment 5%~10%, auxiliary agent 2%~5%, styrene used in the aqueous UV ink-making process of the present invention can effectively improve ink film mechanical strength, acrylic acid and HEMA are conducive to improve ink water solubility, simultaneously because hydroxyethyl methacrylate is provided simultaneously with double bond and aldehyde radical, so that the ink photo-curing rate is greatly improved.
Description
Technical field
The invention belongs to ink preparation technical fields, are related to a kind of low viscosity aqueous UV ink, further relate to a kind of low viscosity
The preparation method of aqueous UV ink.
Background technique
UV ink refers under ultraviolet light irradiation, and the list in ink vehicle is made using the ultraviolet light of different wave length and energy
Body aggregates into polymer, makes ink film forming and dry ink.Its main component is prepolymer, reactive diluent, photoinitiator,
Auxiliary element is pigment, filler, additive etc..UV printing ink color matching ability is strong, has good printability, while having solidification
The features such as speed is fast, wear resistance is high, glossiness is good, while having good adhesive force and resistance to medium.In addition, not wrapped in UV ink
Containing volatile organic solvent, meet the themes of the times of Green Development.
Patent " a kind of the aqueous UV ink of flexographic printing and preparation method thereof ", (application publication number: CN103275551 A, it is public
Cloth day: 2013.9.4) in prepare UV ink composition in only prepolymer, do not include monomer, it is low so as to cause crosslinking degree, because
Prepolymer content is up to 60% or more in this patent, the prepolymer being prepared in the patent does not purify, and impurity is more,
Solidification rate will be reduced.
Patent " a kind of coloured UV ink of glass " (application publication number: CN105315769A, date of publication: 2016.2.10)
It is middle to use hexafunctional aliphatic urethane acrylates, trifunctional aliphatic urethane acrylate and organosilicon modified polyester tree
Rouge causes prepolymer content in the ink system to be up to 59% or more as prepolymer, illustrates that reactive diluent and prepolymer are handed over
Connection degree is low, and prepolymer preparation process is also more many and diverse in the patent.
Meanwhile UV ink also have the shortcomings that it is some obvious.Reactive diluent used in UV ink is usually multifunctional
Group's esters of acrylic acid, leading to UV ink price is twice of common ink.Additionally due to the penetration power of ultraviolet light is poor, layer of ink bottom
Portion's irradiation dynamics is inadequate, and so as to cause curing degree deficiency, adhesive force is poor.UV ink does not have resistance to medium and difficulty simultaneously
With cleaning, these all greatly limit UV ink in the popularization and use in market.
Summary of the invention
The object of the present invention is to provide a kind of low viscosity aqueous UV ink, solve ink solidification existing in the prior art
The problem of time length.
It is a further object of the present invention to provide a kind of preparation methods of low viscosity aqueous UV ink.
The technical scheme adopted by the invention is that a kind of low viscosity aqueous UV ink, according to mass percent, by with the following group
It is grouped as: water soluble acrylic acid prepolymer 30%~50%, aqueous active diluent 20%~50%, solvent 10%~30%, light
Initiator 1%~4%, pigment 5%~10%, auxiliary agent 2%~5%, the sum of said components mass percent are 100%.
Another technical solution of the present invention is a kind of preparation method of low viscosity aqueous UV ink, according to following
Step carries out:
Step 1, water soluble acrylic acid prepolymer is prepared:
Styrene and acrylic acid are weighed, sodium hydrogensulfite is added as catalyst and obtains styrene after reacting a period of time
Acrylic copolymer adds hydroxyethyl methacrylate, and addition uses triethylamine as catalyst, after reacting a period of time,
Obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Ethylenediamine and glycidyl methacrylate are weighed, is stirred evenly, after reacting a period of time at room temperature, obtains water
Property reactive diluent；
Step 3, mixed solution is prepared:
Water soluble acrylic acid prepolymer and aqueous active diluent are proportionally added into solvent and are uniformly mixed, magnetic force is placed in and stirs
It mixes in device and stirs, after stirring a period of time, obtain mixed solution；
Step 4, aqueous UV ink is prepared:
It is proportionally added into pigment, auxiliary agent and photoinitiator into mixed solution obtained in step 3, continues to stir, obtain
Aqueous UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
0.5~2s is irradiated under the controller of source, so that aqueous UV ink solidification.
In step 1, the molar ratio of styrene and acrylic acid is 1:1~2~3, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:1~2, and sodium hydrogensulfite accounts for the 3%~10% of styrene and acrylic acid gross mass, and triethylamine accounts for styrene-acrylonitrile copolymer
The 3%~10% of acid copolymer and hydroxyethyl methacrylate gross mass.
In step 1, the reaction time of styrene and acrylic acid is 2~3h, and reaction temperature is 55~65 DEG C, styrene-acrylonitrile copolymer
The reaction time of acid copolymer and hydroxyethyl methacrylate be 20~for 24 hours, reaction temperature be 50~60 DEG C.
In step 2, the molar ratio of ethylenediamine and glycidyl methacrylate is 1:4~6.
In step 2, the reaction time of ethylenediamine and glycidyl methacrylate is 5.5~6.5h.
In step 3, solvent is the mixed solution of water, ethyl alcohol and THF, and the molar ratio of the water, ethyl alcohol and THF is 6:3:1.
In step 3, reaction temperature is 60~80 DEG C, and the reaction time is 0.5~1h, and revolving speed is 500~800r/min.
In step 4, photoinitiator is 2- isopropyl thioxanthone, trimethylbenzoyl diphenyl phosphate oxidation, 2- hydroxyl -2-
Any one or a few mixing in methyl phenyl ketone, pigment are methyl orange, and auxiliary agent is defoaming agent.
In step 4, reaction temperature is 40~60 DEG C, and the reaction time is 1~2h, and revolving speed is 300~500r/min.
The invention has the advantages that the present invention using styrene and acrylic acid under water bath condition with hydroxyethyl methacrylate
Ethyl ester obtains the polyfunctional group of styrene acrylic copolymer grafted methacrylic acid hydroxyl ethyl ester under the catalytic action of triethylamine
Oligomer can substantially reduce the cost for preparing aqueous UV ink；And due to ethylenediamine tetraacetic glycidyl methacrylate
Functional group is more, it is prone to polymerize；In addition, styrene can effectively improve ink film mechanical strength, acrylic acid and HEMA are conducive to
It is water-soluble to improve ink, simultaneously because hydroxyethyl methacrylate is provided simultaneously with double bond and aldehyde radical, so that the ink photocuring speed
Rate is greatly improved.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of water soluble acrylic acid prepolymer in a kind of low viscosity aqueous UV ink of the present invention；
Fig. 2 is the infrared spectrogram of aqueous active diluent in a kind of low viscosity aqueous UV ink of the present invention；
Fig. 3 be in a kind of low viscosity aqueous UV ink of the present invention photoinitiator levels to aqueous UV ink solidification time effects
Effect picture；
Fig. 4 be in a kind of low viscosity aqueous UV ink of the present invention water soluble acrylic acid prepolymer to the aqueous UV ink solidification time
The effect picture of influence；
Fig. 5 be in a kind of low viscosity aqueous UV ink of the present invention water soluble acrylic acid prepolymer to aqueous UV ink wear resistance shadow
Loud effect picture；
Fig. 6 be in a kind of low viscosity aqueous UV ink of the present invention aqueous active diluent to aqueous UV ink solidification time shadow
Loud effect picture；
Fig. 7 is that aqueous active diluent influences aqueous UV ink wear resistance in a kind of low viscosity aqueous UV ink of the present invention
Effect picture.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of low viscosity aqueous UV ink of the present invention, composed of the following components according to mass percent: water soluble acrylic acid is pre-
Polymers 30%~50%, aqueous active diluent 20%~50%, solvent 10%~30%, photoinitiator 1%~4%, pigment
5%~10%, auxiliary agent 2%~5%, the sum of said components mass percent is 100%.
The present invention provides a kind of preparation methods of low viscosity aqueous UV ink, specifically follow the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
Styrene and acrylic acid are weighed, sodium hydrogensulfite is added as catalyst and obtains styrene after reacting a period of time
Acrylic copolymer adds hydroxyethyl methacrylate, and addition uses triethylamine as catalyst, after reacting a period of time,
Obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Ethylenediamine and glycidyl methacrylate are weighed, is stirred evenly, after reacting a period of time at room temperature, obtains water
Property reactive diluent；
Step 3, mixed solution is prepared:
Water soluble acrylic acid prepolymer and aqueous active diluent are proportionally added into solvent and are uniformly mixed, magnetic force is placed in and stirs
It mixes in device and stirs, after stirring a period of time, obtain mixed solution；
Step 4, aqueous UV ink is prepared:
It is proportionally added into pigment, auxiliary agent and photoinitiator into mixed solution obtained in step 3, continues to stir, obtain
Aqueous UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
0.5~2s is irradiated under the controller of source, so that aqueous UV ink solidification.
In step 1, the molar ratio of styrene and acrylic acid is 1:1~2~3, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:1~2, and bisulfite sodium content accounts for the 3%~10% of styrene and acrylic acid gross mass, and triethylamine content accounts for benzene
The 3%~10% of ethylene acrylic acid co polymer and hydroxyethyl methacrylate gross mass.
In step 1, the reaction time of styrene and acrylic acid is 2~3h, and reaction temperature is 55~65 DEG C, styrene-acrylonitrile copolymer
The reaction time of acid copolymer and hydroxyethyl methacrylate be 20~for 24 hours, reaction temperature be 50~60 DEG C.
In step 2, the molar ratio of ethylenediamine and glycidyl methacrylate is 1:4~6.
In step 2, the reaction time of ethylenediamine and glycidyl methacrylate is 5.5~6.5h.
In step 3, solvent is the mixed solution of water, ethyl alcohol and THF, and the molar ratio of the water, ethyl alcohol and THF is 6:3:1.
In step 3, reaction temperature is 60~80 DEG C, and the reaction time is 0.5~1h, and revolving speed is 500~800r/min.
In step 4, photoinitiator is 2- isopropyl thioxanthone, trimethylbenzoyl diphenyl phosphate oxidation, 2- hydroxyl -2-
Any one or a few mixing in methyl phenyl ketone, pigment are methyl orange, and auxiliary agent is defoaming agent.
In step 4, reaction temperature is 40~60 DEG C, and the reaction time is 1~2h, and revolving speed is 300~500r/min.
In step 1, under the catalysis of sodium hydrogensulfite, reaction obtains styrene acrylic copolymerization for styrene and acrylic acid
Object, then by the styrene acrylic copolymer being prepared into and hydroxyethyl methacrylate under the catalysis of triethylamine, reaction is obtained
Water soluble acrylic acid prepolymer, chemical equation are as follows:
In step 2, ethylenediamine and glycidyl methacrylate, reaction obtain aqueous active diluent, chemical equation
Formula is as follows:
Fig. 1 is the infrared spectrogram of water soluble acrylic acid prepolymer, it can be seen from the figure that 3434cm-1Place is methylol-OH
Stretching vibration absworption peak；2993cm-1Place is C-H stretching vibration absworption peak；1747cm-1Place is C=O stretching vibration absworption peak；
1573cm-1Place is C=C stretching vibration absworption peak；1471cm-1Place is phenyl ring skeletal vibration absorption peak, realizes expected product benzene
The synthesis of ethylene acrylic acid co polymer grafted methacrylic acid hydroxyl ethyl ester.
Fig. 2 is the infrared spectrogram of aqueous active diluent, it can be seen from the figure that 3378cm-1Place is that methylol-OH stretches
Contracting vibration absorption peak；2935cm-1Place is C-H stretching vibration absworption peak；1714cm-1Place is C=O stretching vibration absworption peak；
1604cm-1Place is C=C stretching vibration absworption peak, realizes the synthesis of expected product ethylenediamine tetraacetic methacrylic acid glycerol amide.
Fig. 3 is effect picture of the photoinitiator levels to aqueous UV ink solidification time effects, it can be seen from the figure that aqueous
When photoinitiator dosage is 4% in UV ink, ink has more excellent curing rate, and photoinitiator accounting is higher, solidification
Speed is faster, welcomes turnover in accounting for 4%, photoinitiator accounting is higher later, and curing rate is slower.
Fig. 4 is effect picture of the water soluble acrylic acid prepolymer to aqueous UV ink solidification time effects, it can be seen from the figure that
When accounting is that the laser curing velocity of 30% aqueous UV ink is most fast to prepolymer in entire aqueous UV ink system, with prepolymer
Accounting in whole system gradually increases, and the laser curing velocity of aqueous UV ink is but greatly reduced therewith, when prepolymer contains
When measuring higher, the reactive diluent, photoinitiator levels in system are relatively fewer, if photoinitiator accounting mistake in whole system
The low energy that will be unable to that ultraviolet light is made full use of to be given off, and photoinitiator itself decomposes generated living radical number
Amount is unable to satisfy required quantity in system, and so as to cause aqueous UV ink, in solidification, speed is slower.
Fig. 5 is the effect picture that water soluble acrylic acid prepolymer influences aqueous UV ink wear resistance, it can be seen from the figure that with
The increase of prepolymer content in entire ink system, ink film wear resistance constantly decline, prepolymer accounting is higher, aqueous UV ink
Middle other compositions accounting is opposite to be reduced, however the double bond negligible amounts contained by performed polymer itself, so as to cause entire body
Double bond content is insufficient in system, and ink is caused to be formed by cross-linked structure intensity deficiency when solidifying on carrier therewith, thus
Ink film wear resistance is caused to decline therewith.
Fig. 6 is effect picture of the aqueous active diluent to aqueous UV ink solidification time effects, it can be seen from the figure that with
Reactive diluent proportion in aqueous UV ink gradually increase, the cure times of aqueous UV ink can contract therewith
It is short, because the reactive diluent that the present invention uses is the ethylenediamine tetraacetic glycidyl methacrylate of laboratory synthesis, itself
With diluted effect, to make aqueous UV ink system oneself viscosity decline, so that molecular motion ability mentions significantly in ink
It rises.
Fig. 7 is the effect picture that aqueous active diluent influences aqueous UV ink wear resistance, it can be seen from the figure that with
Reactive diluent content increases in aqueous UV ink, and the cured coating film wear resistance of ink experienced first to gradually increase gradually becomes again
Small process is because reactive diluent used in the present invention is ethylenediamine tetraacetic glycidyl methacrylate, theoretically
Double bond there are four just having in one reactive diluent small molecule, thus double bond content in entire aqueous UV ink system is caused to increase
It is more, so that being conducive to ink film forms fine and close cross-linked network structure, improve the wear resistance of ink film；However, working as aqueous UV ink
When middle reactive diluent accounting is increasing, the main reason for wear resistance of ink film is begun to decline instead, and this occurs, is
Double bond content excessively causes the double bond for being not involved in reaction to be deposited in ink film surface, leads to the decline of ink film wear resistance.
Embodiment 1
A kind of preparation method of low viscosity aqueous UV ink, follows the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
The molar ratio of weighing styrene and acrylic acid, styrene and acrylic acid is 1:1, and sodium hydrogensulfite is added as catalysis
Agent, bisulfite sodium content account for the 3% of styrene and acrylic acid gross mass, and reaction temperature is 60 DEG C, after reacting 3h, obtain benzene second
Alkene acrylic copolymer；
It is added hydroxyethyl methacrylate into styrene acrylic copolymer, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:1, and addition uses triethylamine as catalyst, and triethylamine content accounts for styrene acrylic copolymer and metering system
The 3% of sour hydroxyl ethyl ester gross mass, reaction temperature are 55 DEG C, after reaction for 24 hours, obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Weigh ethylenediamine and glycidyl methacrylate, the molar ratio of ethylenediamine and glycidyl methacrylate
It for 1:4, stirs evenly, after reacting 6h at room temperature, obtains aqueous active diluent；
Step 3, mixed solution is prepared:
30% water soluble acrylic acid prepolymer and 50% aqueous active diluent are added in 10% solvent and are uniformly mixed,
It is placed in magnetic stirring apparatus and stirs, reaction temperature is 60 DEG C, reaction time 0.5h, revolving speed 500r/min and obtains mixing molten
Liquid；
Step 4, aqueous UV ink is prepared:
Into mixed solution obtained in step 3 be added 5% methyl orange, 3% defoaming agent and 2% trimethylbenzene first
Acyl diphenyl phosphate oxidation continues to stir, and reaction temperature is 40 DEG C, reaction time 2h, revolving speed 300r/min and obtains aqueous UV
Ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
0.5s is irradiated under the controller of source, so that aqueous UV ink solidification.
Embodiment 2
A kind of preparation method of low viscosity aqueous UV ink, follows the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
The molar ratio of weighing styrene and acrylic acid, styrene and acrylic acid is 1:3, and sodium hydrogensulfite is added as catalysis
Agent, bisulfite sodium content account for the 5% of styrene and acrylic acid gross mass, and reaction temperature is 65 DEG C, after reacting 2h, obtain benzene second
Alkene acrylic copolymer；
It is added hydroxyethyl methacrylate into styrene acrylic copolymer, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:2, and addition uses triethylamine as catalyst, and triethylamine content accounts for styrene acrylic copolymer and metering system
The 5% of sour hydroxyl ethyl ester gross mass, reaction temperature are 60 DEG C, after reacting 20h, obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Weigh ethylenediamine and glycidyl methacrylate, the molar ratio of ethylenediamine and glycidyl methacrylate
It for 1:6, stirs evenly, after reacting 5.5h at room temperature, obtains aqueous active diluent；
Step 3, mixed solution is prepared:
40% water soluble acrylic acid prepolymer and 35% aqueous active diluent are added in 10% solvent and are uniformly mixed,
It is placed in magnetic stirring apparatus and stirs, reaction temperature is 70 DEG C, reaction time 1h, revolving speed 800r/min and obtains mixed solution；
Step 4, aqueous UV ink is prepared:
Into mixed solution obtained in step 3 be added 10% methyl orange, 4% defoaming agent and 1% 2- isopropyl
Thioxanthone continues to stir, and reaction temperature is 50 DEG C, reaction time 1.5h, revolving speed 500r/min, obtains aqueous UV oil
Ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
1.2s is irradiated under the controller of source, so that aqueous UV ink solidification.
Embodiment 3
A kind of preparation method of low viscosity aqueous UV ink, follows the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
The molar ratio of weighing styrene and acrylic acid, styrene and acrylic acid is 1:2, and sodium hydrogensulfite is added as catalysis
Agent, bisulfite sodium content account for the 10% of styrene and acrylic acid gross mass, and reaction temperature is 55 DEG C, after reacting 2.5h, obtain
Styrene acrylic copolymer；
It is added hydroxyethyl methacrylate into styrene acrylic copolymer, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:2, and addition uses triethylamine as catalyst, and triethylamine content accounts for styrene acrylic copolymer and metering system
The 10% of sour hydroxyl ethyl ester gross mass, reaction temperature are 50 DEG C, after reacting 22h, obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Weigh ethylenediamine and glycidyl methacrylate, the molar ratio of ethylenediamine and glycidyl methacrylate
It for 1:5, stirs evenly, after reacting 6.5h at room temperature, obtains aqueous active diluent；
Step 3, mixed solution is prepared:
50% water soluble acrylic acid prepolymer and 20% aqueous active diluent are added in 20% solvent and are uniformly mixed,
It is placed in magnetic stirring apparatus and stirs, reaction temperature is 80 DEG C, reaction time 0.6h, revolving speed 700r/min and obtains mixing molten
Liquid；
Step 4, aqueous UV ink is prepared:
Into mixed solution obtained in step 3 be added 6% methyl orange, 3% defoaming agent and 1% 2- isopropyl sulphur
Miscellaneous anthrone continues to stir, and reaction temperature is 60 DEG C, reaction time 1.5h, revolving speed 400r/min, obtains aqueous UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
1s is irradiated under the controller of source, so that aqueous UV ink solidification.
Embodiment 4
A kind of preparation method of low viscosity aqueous UV ink, follows the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
The molar ratio of weighing styrene and acrylic acid, styrene and acrylic acid is 1:1, and sodium hydrogensulfite is added as catalysis
Agent, bisulfite sodium content account for the 8% of styrene and acrylic acid gross mass, and reaction temperature is 57 DEG C, after reacting 2h, obtain benzene second
Alkene acrylic copolymer；
It is added hydroxyethyl methacrylate into styrene acrylic copolymer, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:2, and addition uses triethylamine as catalyst, and triethylamine content accounts for styrene acrylic copolymer and metering system
The 8% of sour hydroxyl ethyl ester gross mass, reaction temperature are 52 DEG C, after reacting 21h, obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Weigh ethylenediamine and glycidyl methacrylate, the molar ratio of ethylenediamine and glycidyl methacrylate
It for 1:5, stirs evenly, after reacting 6h at room temperature, obtains aqueous active diluent；
Step 3, mixed solution is prepared:
35% water soluble acrylic acid prepolymer and 22% aqueous active diluent are added in 30% solvent and are uniformly mixed,
It is placed in magnetic stirring apparatus and stirs, reaction temperature is 75 DEG C, reaction time 0.5h, revolving speed 600r/min and obtains mixing molten
Liquid；
Step 4, aqueous UV ink is prepared:
Into mixed solution obtained in step 3 be added 7% methyl orange, 2% defoaming agent and 4% photoinitiator,
Continue to stir including 2% 2- hydroxy-2-methyl propiophenone and 2% 2- isopropyl thioxanthone, reaction temperature is 50 DEG C, instead
It is 1h, revolving speed 450r/min between seasonable, obtains aqueous UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
1.5s is irradiated under the controller of source, so that aqueous UV ink solidification.
Embodiment 5
A kind of preparation method of low viscosity aqueous UV ink, follows the steps below:
Step 1, water soluble acrylic acid prepolymer is prepared:
The molar ratio of weighing styrene and acrylic acid, styrene and acrylic acid is 1:1, and sodium hydrogensulfite is added as catalysis
Agent, bisulfite sodium content account for the 4% of styrene and acrylic acid gross mass, and reaction temperature is 60 DEG C, after reacting 3h, obtain benzene second
Alkene acrylic copolymer；
It is added hydroxyethyl methacrylate into styrene acrylic copolymer, hydroxyethyl methacrylate and acrylic acid
Molar ratio is 1:2, and addition uses triethylamine as catalyst, and triethylamine content accounts for styrene acrylic copolymer and metering system
The 4% of sour hydroxyl ethyl ester gross mass, reaction temperature are 60 DEG C, after reaction for 24 hours, obtain water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Weigh ethylenediamine and glycidyl methacrylate, the molar ratio of ethylenediamine and glycidyl methacrylate
It for 1:5, stirs evenly, after reacting 6.5h at room temperature, obtains aqueous active diluent；
Step 3, mixed solution is prepared:
40% water soluble acrylic acid prepolymer and 25% aqueous active diluent are added in 17% solvent and are uniformly mixed,
It is placed in magnetic stirring apparatus and stirs, reaction temperature is 65 DEG C, reaction time 0.7h, revolving speed 800r/min and obtains mixing molten
Liquid；
Step 4, aqueous UV ink is prepared:
Into mixed solution obtained in step 3 be added 10% methyl orange, 5% defoaming agent and 3% photoinitiator,
Including 1% trimethylbenzoyl diphenyl phosphate oxidation, 1% 2- hydroxy-2-methyl propiophenone and 1% 2- isopropyl thioxanthone
Anthrone continues to stir, and reaction temperature is 60 DEG C, reaction time 2h, revolving speed 400r/min, obtains aqueous UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on the face LED formula UV light
2s is irradiated under the controller of source, so that aqueous UV ink solidification.
The present invention prepares water soluble acrylic acid prepolymer by styrene and acrylic acid, and styrene can effectively improve ink film machine
Tool intensity, acrylic acid and HEMA are conducive to improve ink water solubility, and resulting aqueous active diluent and water soluble acrylic acid is pre-
Polymers obtains full cross-linked, hence it is evident that the usage amount for reducing water soluble acrylic acid prepolymer, simultaneously due to hydroxyethyl methacrylate
Have double bond and aldehyde radical, effectively increases cure times and mechanical strength.
Claims (10)
1. a kind of low viscosity aqueous UV ink, which is characterized in that composed of the following components according to mass percent: aqueous acrylamide
Sour prepolymer 30%~50%, aqueous active diluent 20%~50%, solvent 10%~30%, photoinitiator 1%~4%,
Pigment 5%~10%, auxiliary agent 2%~5%, the sum of said components mass percent are 100%.
2. a kind of preparation method of low viscosity aqueous UV ink according to claim 1, which is characterized in that according to following step
It is rapid to carry out:
Step 1, water soluble acrylic acid prepolymer is prepared:
Styrene and acrylic acid are weighed, sodium hydrogensulfite is added as catalyst and obtains styrene-acrylonitrile copolymer after reacting a period of time
Acid copolymer, adds hydroxyethyl methacrylate, and addition uses triethylamine to obtain after reacting a period of time as catalyst
Water soluble acrylic acid prepolymer；
Step 2, aqueous active diluent is prepared:
Ethylenediamine and glycidyl methacrylate are weighed, is stirred evenly, after reacting a period of time at room temperature, obtains aqueous work
Property diluent；
Step 3, mixed solution is prepared:
Water soluble acrylic acid prepolymer and aqueous active diluent are proportionally added into solvent and are uniformly mixed, magnetic stirring apparatus is placed in
Middle stirring obtains mixed solution after stirring a period of time；
Step 4, aqueous UV ink is prepared:
It is proportionally added into pigment, auxiliary agent and photoinitiator into mixed solution obtained in step 3, continues to stir, obtains aqueous
UV ink；
Step 5, solidify:
The aqueous UV ink prepared in step 4 is uniformly applied to art paper surface, art paper is placed on LED formula UV area source control
0.5~2s is irradiated under device processed, so that aqueous UV ink solidification.
3. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 1
In, the molar ratio of styrene and acrylic acid is 1:1~2~3, the molar ratio of hydroxyethyl methacrylate and acrylic acid be 1:1~
2, bisulfite sodium content accounts for the 3%~10% of styrene and acrylic acid gross mass, and it is total that triethylamine content accounts for styrene acrylic
The 3%~10% of polymers and hydroxyethyl methacrylate gross mass.
4. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 1
In, the reaction time of styrene and acrylic acid is 2~3h, and reaction temperature is 55~65 DEG C, styrene acrylic copolymer and first
The reaction time of base hydroxy-ethyl acrylate be 20~for 24 hours, reaction temperature be 50~60 DEG C.
5. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 2
In, the molar ratio of ethylenediamine and glycidyl methacrylate is 1:4~6.
6. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 2
In, the reaction time of ethylenediamine and glycidyl methacrylate is 5.5~6.5h.
7. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 3
In, solvent is the mixed solution of water, ethyl alcohol and THF, and the molar ratio of the water, ethyl alcohol and THF is 6:3:1.
8. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 3
In, reaction temperature is 60~80 DEG C, and the reaction time is 0.5~1h, and revolving speed is 500~800r/min.
9. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 4
In, photoinitiator is 2- isopropyl thioxanthone, in trimethylbenzoyl diphenyl phosphate oxidation, 2- hydroxy-2-methyl propiophenone
Any one or a few mixing, pigment is methyl orange, and auxiliary agent is defoaming agent.
10. a kind of preparation method of low viscosity aqueous UV ink according to claim 2, which is characterized in that the step 4
In, reaction temperature is 40~60 DEG C, and the reaction time is 1~2h, and revolving speed is 300~500r/min.
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| CN110615865A (en) * | 2019-11-05 | 2019-12-27 | 江苏睿浦树脂科技有限公司 | Resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink and preparation method thereof |
| CN111234596A (en) * | 2020-03-04 | 2020-06-05 | 西安理工大学 | Self-cleaning ultraviolet light curing water-based ink and preparation method thereof |
| CN111793388A (en) * | 2020-06-08 | 2020-10-20 | 西安理工大学 | Fast-curing UV (ultraviolet) water-based conductive ink and preparation method thereof |
| CN111808472A (en) * | 2020-06-18 | 2020-10-23 | 西安理工大学 | Fast-curing UV (ultraviolet) water-based magnetic ink and preparation method thereof |
| CN113493627A (en) * | 2021-06-22 | 2021-10-12 | 西安理工大学 | Water-alcohol UV (ultraviolet) ink capable of realizing rapid photocuring and preparation method thereof |
| KR20220028289A (en) * | 2020-08-28 | 2022-03-08 | 한국화학연구원 | Novel compound, epoxy resin composition containing the same and cured product thereof |
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| CN110615865A (en) * | 2019-11-05 | 2019-12-27 | 江苏睿浦树脂科技有限公司 | Resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink and preparation method thereof |
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| CN113493627A (en) * | 2021-06-22 | 2021-10-12 | 西安理工大学 | Water-alcohol UV (ultraviolet) ink capable of realizing rapid photocuring and preparation method thereof |
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