CN110028839A - A kind of electronic beam curing ink-jet ink and its preparation method and application - Google Patents
A kind of electronic beam curing ink-jet ink and its preparation method and application Download PDFInfo
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- CN110028839A CN110028839A CN201910254686.XA CN201910254686A CN110028839A CN 110028839 A CN110028839 A CN 110028839A CN 201910254686 A CN201910254686 A CN 201910254686A CN 110028839 A CN110028839 A CN 110028839A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0041—Digital printing on surfaces other than ordinary paper
- B41M5/0047—Digital printing on surfaces other than ordinary paper by ink-jet printing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0041—Digital printing on surfaces other than ordinary paper
- B41M5/007—Digital printing on surfaces other than ordinary paper on glass, ceramic, tiles, concrete, stones, etc.
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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
- C09D11/30—Inkjet printing inks
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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
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- Inks, Pencil-Leads, Or Crayons (AREA)
- Ink Jet Recording Methods And Recording Media Thereof (AREA)
Abstract
The invention discloses a kind of electronic beam curing ink-jet inks and its preparation method and application.The electronic beam curing ink-jet ink, according to parts by weight, including the following raw material: 15-35 parts of urethane acrylate, 20-35 parts of isobornyl acrylate, 5-10 parts of organic pigment toner, 0.5-1 parts of fumed silica, 5-10 parts of lauryl methacrylate, three 5-20 parts of (2- ethoxy) isocyanuric acid triacrylates, 5-10 parts of tristyrylphenol polyoxyethylene ether methacrylate, 1-5 parts of dispersing agent, 3-5 parts of auxiliary agent.It is required in this invention to be filled in the reaction vessel using 99.99% high-purity nitrogen, ink-jet ink is solidified using electronics beam scanning again, it and then is that ink-jet ink forms the comprehensive good ink and color layers such as strong hardness, the corrosion of, water boiling resistance good at film toughness, solvent resistant and scratch-resistant on liquid-crystalline glasses, and the combination for passing through color, colorful pattern is formed in glass surface, it is beautiful to increase product.
Description
Technical field
The present invention relates to solidification new material technology field, in particular to a kind of electronic beam curing ink-jet ink and its preparation side
Method and application.
Background technique
Electronic beam curing (abbreviation EB solidifies) technology is not the new technology just having in recent years, it and traditional UV light are solid
Change equally, belongs to radiation curing field.EB curing technology is applied to vapour for the first time by the beginning of the seventies in last century, Ford, the U.S.
Vehicle components and instrument coating.Both at home and abroad, plastic industry irradiates " reinforcing " film fastness at film take-up end using EB technology, promotes
The curing reaction of unsaturated olefin.
But in ink and print field, EB solidification is rarely known by the people.Theoretically, EB electron beam curing ink and UV ultraviolet light
Solidify branch of two classes as radiation curing field ink, due to not using photoinitiator, raw materials are more compared with UV ink
Energy conservation and environmental protection, in terms of the migration trend of ink printed product, EB ink is free of photoinitiator, solves light contained by UV ink and draws
Agent problem easy to migrate is sent out, also free from extraneous odour generates, and is particularly suitable for the field high to environmental protection and healthy requirement.Estimable
Place is, difference and traditional highly exothermic mercury lamp photocuring, and the heat that when EB ink solidification generates is less, fully belongs to freeze off
Change, not will lead to printing element temperature distortion.The ev energy that high-power electron beam generates is much higher than a UV photon energy, institute
It is shorter with the EB ink solidification time, it is solidified into film property also more thoroughly.So various, EB ink is that press realizes environmentally protectiveization
Provide the support in terms of more structurally sound curing apparatus.
Printing is divided into several big modes such as hectograph, relief printing plate, soft version, intaglio plate, silk screen and ink-jet from equipment type.Wherein spray
Aqueous jet is arrived from traditional solvent-based inkjet in the field that ink rapidly increases in recent years as press, arrives UV ink-jet, and
The UV-LED ink-jet etc. more optimized to environmental protection, green are strengthened with the harsh degree of environmental protection.But in this kind of spy of glass
Above different material, especially LCD above LED liquid crystal glass substrate, how to realize the definition printing of four colors, and successfully solve print
The adhesive force of brush finished product color ink, water boiling resistance, scratch-resistant and other indices such as ageing-resistant require performance, become a disaster
Topic.
In recent decades, it about LCD glass printing, is toasted from solvent type silk screen, arrives the one-pass molding of UV silk screen, then arrive
UV and UV-LED are ink-jet printed, more or less solve some pain spots of industry.At the same time, research both at home and abroad and solution
The patent of UV ink-jet and document are more above glass, but the very big limitation due to being limited by rate of drying, using big in formula
Photoinitiator is measured, and in order to increase hardness and toughness after laser curing velocity and film forming, is needed using polyfunctional acrylic ester
Monomer, after causing UV and UV-LED ink-jet photocuring to form a film, the layer of ink of color ink is crisp and does not have toughness.Water boiling resistance and corrosion energy
Power is very poor.
It in recent years, is to solve liquid-crystalline glasses adhesion problem, some clients have selected to have returned to again traditional passes through early period
Coupling agent is sprayed, and heats the method for solving adhesive force, this aspect can generate VOCs organic volatile pollution problem, on the other hand
Need a large amount of cumbersome technique, product high rejection rate.
So industry suddenly develops a kind of electronic beam curing ink-jet ink and preparation method thereof.
Summary of the invention
The present invention is intended to provide a kind of electronic beam curing ink-jet ink and its preparation method and application, to solve above-mentioned technology
Problem.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
In a first aspect, a kind of electronic beam curing ink-jet ink provided by the invention, according to parts by weight, including it is following former
Material: 15-35 parts of urethane acrylate, 20-35 parts of isobornyl acrylate, 5-10 parts of organic pigment toner, gas phase titanium dioxide
0.5-1 parts of silicon, 5-10 parts of lauryl methacrylate, three 5-20 parts of (2- ethoxy) isocyanuric acid triacrylates, three
5-10 parts of styrylphenol polyoxyethylene ether methacrylate, 1-5 parts of dispersing agent, 3-5 parts of auxiliary agent.
Preferably, the urethane acrylate, according to parts by weight, including the following raw material: the first isocyanate-monomer
1-6 parts, 5-10 parts of pentaerythritol triacrylate, 0.01-0.1 parts of polymerization inhibitor, 0.01-0.1 parts of catalyst, polyester polyol
10-20 parts, 3-15 parts of acrylic ester copolymer oligomer, 20-35 parts of isobornyl acrylate, the second isocyanate-monomer 2-8
Part, 1-5 parts of end hydroxy butadiene.
Preferably, the urethane acrylate is to be made using following methods:
After first isocyanate-monomer and pentaerythritol triacrylate are mixed, it is warming up to 50-70 DEG C, reacts 1.5-
2h adjusts the temperature to 70-90 DEG C, and polymerization inhibitor and catalyst is added, and after mixing evenly, polyester polyol, insulation reaction is added
1.5-2.5h is added acrylic ester copolymer oligomer, isobornyl acrylate, stirs evenly, add the second isocyanates list
Body, insulation reaction 1-2h are added end hydroxy butadiene, are gathered after the content of isocyano in system is not higher than 0.2%
Urethane acrylate.
It is further preferred that the polymerization inhibitor is 2,6- di-tert-butyl-4-methy phenol.
It is further preferred that the polyester polyol be polycaprolactone glycol, polycaprolactonetriol, polycarbonate glycol,
One or more of polycarbonate triol.
It is further preferred that first isocyanate-monomer and the second isocyanate-monomer are identical or different isocyanide
Acid ester monomer, the isocyanate-monomer be selected from one of isocyanates ethyl acrylate, isophorone diisocyanate or
It is a variety of.
Preferably, the organic pigment toner in paratonere, pigment yellow, pigment blue, high pigment nanometer carbon black one
Kind is a variety of.
Preferably, the auxiliary agent is silane coupling agent.
Second aspect, a kind of preparation side of electronic beam curing ink-jet ink as described in relation to the first aspect provided by the invention
Method includes the following steps:
(1) by urethane acrylate, dispersing agent, organic pigment toner, fumed silica, lauryl
Base ester, three (2- ethoxy) isocyanuric acid triacrylates, the mixing of tristyrylphenol polyoxyethylene ether methacrylate,
High-speed stirred is uniform, is sanded using sand mill, and mixed material is obtained；
(2) after mixing the resulting mixed material of step (1) and auxiliary agent, and viscosity is adjusted using isobornyl acrylate,
Electronic beam curing ink-jet ink is made.
The third aspect, the electron beam ink-jet ink of one kind provided by the invention as described in relation to the first aspect are printed in liquid-crystalline glasses
The application of aspect.
Compared with prior art, the beneficial effects of the present invention are:
Compared with the UV ink-jet or UV-LED ink-jet technology newly released in recent years, the present invention does not use photoinitiator, former
Material cost greatly reduces, and is irradiated cured ink jet coatings by electron beam, very participates in film forming, nonmigratory risk does not have yet
Odorous and overload heat generates, and solidification process has good protectiveness to liquid-crystalline glasses.
The present invention has used the polyurethane acroleic acid that adhesive force is good on glass due to being added at one time coupling agent
Ester, it is possible to solve the problems, such as fastness and other resistance requirements indexs on liquid-crystalline glasses, such as water boiling resistance (moisture-proof
Gas), solvent resistant burn into scratch-resistant, resistance to greasy dirt and the trace of resistance to finger etc..
Feature of environmental protection green raw material of the present invention due to could be used without any organic volatile, and the preparation of ink-jet ink
Journey Integral sealing is good, and production process also disposal of pollutants problem integrally reduces the destructive power to environment.
It is required in this invention to be filled in the reaction vessel using 99.99% high-purity nitrogen then solid using electronics beam scanning
Change ink-jet ink, and then is that ink-jet ink forms that hardness is strong, water boiling resistance good at film toughness, solvent resistant corrode on liquid-crystalline glasses
And the comprehensive good ink and color layer such as scratch-resistant, and by the combination of color, colorful pattern is formed in glass surface, increases and produces
Product are beautiful.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
In a first aspect, a kind of electronic beam curing ink-jet ink provided by the invention, according to parts by weight, including it is following former
Material: 15-35 parts of urethane acrylate, 20-35 parts of isobornyl acrylate, 5-10 parts of organic pigment toner, gas phase titanium dioxide
0.5-1 parts of silicon, 5-10 parts of lauryl methacrylate, three 5-20 parts of (2- ethoxy) isocyanuric acid triacrylates, three
5-10 parts of styrylphenol polyoxyethylene ether methacrylate, 1-5 parts of dispersing agent, 3-5 parts of auxiliary agent.
In embodiments of the present invention, the electronic beam curing ink-jet ink, according to parts by weight, including the following raw material:
30-35 parts of urethane acrylate, 20-35 parts of isobornyl acrylate, 5-6 parts of organic pigment toner, fumed silica
0.5-1 parts, 5-6 parts of lauryl methacrylate, three 7-8 parts of (2- ethoxy) isocyanuric acid triacrylates, triphen second
8-10 parts of alkenyl benzene phenol polyethenoxy ether metacrylic acid ester, 2.5-3 parts of dispersing agent, 3-5 parts of auxiliary agent.
In embodiments of the present invention, the urethane acrylate, according to parts by weight, including the following raw material: first
1-6 parts of isocyanate-monomer, 5-10 parts of pentaerythritol triacrylate, 0.01-0.1 parts of polymerization inhibitor, 0.01-0.1 parts of catalyst,
10-20 parts of polyester polyol, 3-15 parts of acrylic ester copolymer oligomer, 20-35 parts of isobornyl acrylate, the second isocyanates
2-8 parts of monomer, 1-5 parts of end hydroxy butadiene.
Further, the urethane acrylate, according to parts by weight, including the following raw material: the first isocyanates list
3-6 parts of body, 7-10 parts of pentaerythritol triacrylate, 0.01-0.1 parts of polymerization inhibitor, 0.01-0.1 parts of catalyst, polyester polyols
13-18 parts of alcohol, 8-12 parts of acrylic ester copolymer oligomer, 25-30 parts of isobornyl acrylate, the second isocyanate-monomer 3-8
Part, 1.5-2 parts of end hydroxy butadiene.
In embodiments of the present invention, the urethane acrylate is to be made using following methods:
After first isocyanate-monomer and pentaerythritol triacrylate are mixed, it is warming up to 50-70 DEG C, reacts 1.5-
2h adjusts the temperature to 70-90 DEG C, and polymerization inhibitor and catalyst is added, and after mixing evenly, polyester polyol, insulation reaction is added
1.5-2.5h is added acrylic ester copolymer oligomer, isobornyl acrylate, stirs evenly, add the second isocyanates list
Body, insulation reaction 1-2h are added end hydroxy butadiene, are gathered after the content of isocyano in system is not higher than 0.2%
Urethane acrylate.
Further, the polymerization inhibitor is 2,6- di-tert-butyl-4-methy phenol.
Further, the catalyst is dibutyl tin dilaurate.
Further, the molecular weight of the polyester polyol is 2000-3000.
Further, the polyester polyol is polycaprolactone glycol, polycaprolactonetriol, polycarbonate glycol, poly- carbon
One or more of acid esters triol.
Further, first isocyanate-monomer and the second isocyanate-monomer are identical or different isocyanates
Monomer, the isocyanate-monomer are selected from one of isocyanates ethyl acrylate, isophorone diisocyanate or a variety of.
Further, the mass ratio of the first isocyanic acid acid ester monomer and the pentaerythritol triacrylate is 1:2-
4；The second isocyanic acid acid ester monomer and the mass ratio of polyester polyol are 1:2~6, further, second isocyanide
Sour acid ester monomer and the mass ratio of polyester polyol are 1:2.6~3.6.
In embodiments of the present invention, the acrylic ester copolymer oligomer is super to be provided by TaiWan, China Changxing chemistry
Branched polyester resin product is selected from model DR-E522, DR-E528,6361-100- provided by the chemistry of TaiWan, China Changxing
C, one of 6363 Hyperbranched Polyester Resin or a variety of.
In embodiments of the present invention, the dispersing agent is Lu Borun Solsperse 24000SC hyper-dispersant.
In embodiments of the present invention, the organic pigment toner is selected from paratonere, pigment yellow, pigment blue, high pigment and receives
One of rice carbon black is a variety of.
In embodiments of the present invention, the auxiliary agent is silane coupling agent.
Further, the silane coupling agent is selected from γ-glycidyl ether oxypropyltrimethoxysilane, silane coupled
One of agent KH-172, γ-methacryloxypropyl trimethoxy silane is a variety of.
Second aspect, a kind of preparation side of electronic beam curing ink-jet ink as described in relation to the first aspect provided by the invention
Method includes the following steps:
(1) by urethane acrylate, dispersing agent, organic pigment toner, fumed silica, lauryl
Base ester, three (2- ethoxy) isocyanuric acid triacrylates, the mixing of tristyrylphenol polyoxyethylene ether methacrylate,
High-speed stirred is uniform, is sanded using sand mill, and mixed material is obtained；
(2) after mixing the resulting mixed material of step (1) and auxiliary agent, and viscosity is adjusted using isobornyl acrylate,
Electronic beam curing ink-jet ink is made.
The third aspect, the electron beam ink-jet ink of one kind provided by the invention as described in relation to the first aspect are printed in liquid-crystalline glasses
The application of aspect.
The embodiment of the present invention is described in detail below.
Isobornyl acrylate employed in following embodiment, lauryl methacrylate, three (2- ethoxys)
The compositions such as isocyanuric acid triacrylate, tristyrylphenol polyoxyethylene ether methacrylate, be it is commercially available industry at
Product, it is desirable that purity reaches 90% or more.
Fumed silica employed in following embodiment is the new oil product of nanoscale, and such as Degussa R-972 is produced
Product.
Embodiment 1
A kind of preparation method of electronic beam curing ink-jet ink provided in this embodiment, includes the following steps:
(1) following raw materials according to parts by weight: 5 parts of isocyanates IPDI monomer, pentaerythritol triacrylate 10 are taken
(molecular weight is for part, 0.05 part of 2,6 di tert butyl 4 methyl phenol, 0.1 part of dibutyl tin dilaurate, polycarbonate glycol
2000) 15 parts, 10 parts of DR-E522 dissaving polymer, 30 parts of isobornyl acrylate, isocyanates ethyl acrylate (AOI)
5 parts, 1.5 parts of end hydroxy butadiene (HTPB)；
Isocyanates IPDI monomer and pentaerythritol triacrylate are added into reactor, is warming up to 70 DEG C, reaction
1.5h；80 DEG C are warming up to, 2,6- di-tert-butyl-4-methy phenol and dibutyl tin dilaurate is added, after mixing evenly, once
Property be added polycarbonate glycol, react 1.5h, obtain urethane acrylate semi-finished product；Into semi-finished product urethane acrylate
TaiWan, China work Xinghua is added, the DR-E522 dissaving polymer provided, isobornyl acrylate are provided, stirs evenly, be diluted to
Viscosity is lower than the mixture of 300 centipoises under room temperature；Add isocyanates ethyl acrylate (AOI), the insulation reaction at 80 DEG C
1-2h, when detect confirmation system in NCO percentage composition be lower than 0.2% after, be added 1.5g end hydroxy butadiene (HTPB) into
Row reinforcement, obtains urethane acrylate；
(2) following raw material according to parts by weight: 35 parts of the resulting urethane acrylate of step (1), Lu Borun is weighed
3 parts of Solsperse 24000SC hyper-dispersant, 6 parts of organic pigment 57:1 red powder, 1 part of fumed silica, methacrylic acid
5 parts of dodecyl ester, three 8 parts of (2- ethoxy) isocyanuric acid triacrylates, tristyrylphenol polyoxyethylene ether methyl
10 parts of acrylate, 2 parts of γ-glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy
1.5 parts of base silane, 30 parts of isobornyl acrylate；
It is ultra-dispersed that Lu Borun Solsperse 24000SC is sequentially added into step (1) resulting urethane acrylate
Agent, organic pigment 57:1 red powder, fumed silica, lauryl methacrylate, three (2- ethoxy) isocyanuric acids
Triacrylate, tristyrylphenol polyoxyethylene ether methacrylate, high-speed stirred is uniform, carries out sand using sand mill
Mill detects the particle diameter of confirmation organic pigment 57:1 red powder using laser particle analyzer, when detecting that organic pigment 57:1 is red
When the partial size of toner is less than 200 nanometers, γ-glycidyl ether oxypropyltrimethoxysilane and γ-methacryl is added
Oxygroup propyl trimethoxy silicane, and using isobornyl acrylate adjust viscosity, until under the conditions of 35 DEG C viscosity less than 70
Centipoise is to get ink-jet ink.
Embodiment 2
A kind of preparation method of electronic beam curing ink-jet ink provided in this embodiment, includes the following steps:
(1) following raw materials according to parts by weight: 4 parts of isocyanates IPDI monomer, pentaerythritol triacrylate 10 are taken
(molecular weight is for part, 0.05 part of 2,6 di tert butyl 4 methyl phenol, 0.1 part of dibutyl tin dilaurate, polycarbonate glycol
2500) 13 parts, 10 parts of DR-E522 dissaving polymer, 25 parts of isobornyl acrylate, isocyanates ethyl acrylate (AOI)
5 parts, 1.5 parts of end hydroxy butadiene (HTPB)；
Isocyanates IPDI monomer and pentaerythritol triacrylate are added into reactor, is warming up to 70 DEG C, reaction
1.5h；80 DEG C are warming up to, 2,6- di-tert-butyl-4-methy phenol and dibutyl tin dilaurate is added, after mixing evenly, once
Property be added polycarbonate glycol, react 1.5h, obtain urethane acrylate semi-finished product；Into semi-finished product urethane acrylate
TaiWan, China work Xinghua is added, the DR-E522 dissaving polymer provided, isobornyl acrylate are provided, stirs evenly, be diluted to
Viscosity is lower than the mixture of 300 centipoises under room temperature；Add isocyanates ethyl acrylate (AOI), the insulation reaction at 80 DEG C
1-2h, when detect confirmation system in NCO percentage composition be lower than 0.2% after, be added 1.5g end hydroxy butadiene (HTPB) into
Row reinforcement, obtains urethane acrylate；
(2) following raw material according to parts by weight: 33 parts of the resulting urethane acrylate of step (1), Lu Borun is weighed
2.5 parts of Solsperse 24000SC hyper-dispersant, 5.5 parts of organic pigment 15:4 blue powder, 1 part of fumed silica, methyl-prop
5 parts of olefin(e) acid dodecyl ester, three 8 parts of (2- ethoxy) isocyanuric acid triacrylates, tristyrylphenol polyoxyethylene ether
10 parts of methacrylate, 2 parts of γ-glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxypropyl three
1.5 parts of methoxy silane, 25 parts of isobornyl acrylate；
It is ultra-dispersed that Lu Borun Solsperse 24000SC is sequentially added into step (1) resulting urethane acrylate
Agent, organic pigment 14# yellow powder, fumed silica, lauryl methacrylate, three (2- ethoxy) isocyanuric acids three
Acrylate, tristyrylphenol polyoxyethylene ether methacrylate, high-speed stirred is uniform, carries out sand using sand mill
Mill detects the particle diameter of confirmation organic pigment 15:4 blue powder using laser particle analyzer, when having detected organic pigment 15:4
When the partial size of blue powder is less than 200 nanometers, γ-glycidyl ether oxypropyltrimethoxysilane and γ-metering system is added
Acryloxypropylethoxysilane trimethoxy silane, and viscosity is adjusted using isobornyl acrylate, until viscosity is less than under the conditions of 35 DEG C
60 centipoises are to get ink-jet ink.
Embodiment 3
A kind of preparation method of electronic beam curing ink-jet ink provided in this embodiment, includes the following steps:
(1) following raw materials according to parts by weight: 3 parts of isocyanates IPDI monomer, pentaerythritol triacrylate 7 are taken
(molecular weight is for part, 0.05 part of 2,6 di tert butyl 4 methyl phenol, 0.1 part of dibutyl tin dilaurate, polycarbonate glycol
2000) 15 parts, 10 parts of DR-E522 dissaving polymer, 25 parts of isobornyl acrylate, isocyanates ethyl acrylate (AOI)
5 parts, 1.5 parts of end hydroxy butadiene (HTPB)；
Isocyanates IPDI monomer and pentaerythritol triacrylate are added into reactor, is warming up to 90 DEG C, reaction
1.5h；70 DEG C are warming up to, 2,6- di-tert-butyl-4-methy phenol and dibutyl tin dilaurate is added, after mixing evenly, once
Property be added polycarbonate glycol, react 1.5h, obtain urethane acrylate semi-finished product；Into semi-finished product urethane acrylate
TaiWan, China work Xinghua is added, the DR-E522 dissaving polymer provided, isobornyl acrylate are provided, stirs evenly, be diluted to
Viscosity is lower than the mixture of 300 centipoises under room temperature；Add isocyanates ethyl acrylate (AOI), the insulation reaction at 80 DEG C
1-2h is added end hydroxy butadiene (HTPB) and is mended after NCO percentage composition is lower than 0.2% in detection confirmation system
By force, urethane acrylate is obtained；
(2) following raw material according to parts by weight: 30 parts of the resulting urethane acrylate of step (1), Lu Borun is weighed
3 parts of Solsperse 24000SC hyper-dispersant, 6 parts of organic pigment 14# yellow powder, 1 part of fumed silica, methacrylic acid
5 parts of dodecyl ester, three 8 parts of (2- ethoxy) isocyanuric acid triacrylates, tristyrylphenol polyoxyethylene ether methyl
10 parts of acrylate, 2 parts of γ-glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy
1.5 parts of base silane, 30 parts of isobornyl acrylate；
It is ultra-dispersed that Lu Borun Solsperse 24000SC is sequentially added into step (1) resulting urethane acrylate
Agent, organic pigment 14# yellow powder, fumed silica, lauryl methacrylate, three (2- ethoxy) isocyanuric acids three
Acrylate, tristyrylphenol polyoxyethylene ether methacrylate, high-speed stirred is uniform, carries out sand using sand mill
Mill detects the particle diameter of confirmation organic pigment 14# yellow powder using laser particle analyzer, when detecting organic pigment 14# yellow
When the partial size of powder is less than 250 nanometers, γ-glycidyl ether oxypropyltrimethoxysilane and γ-methacryloxypropyl is added
Base propyl trimethoxy silicane, and using isobornyl acrylate adjust viscosity, until under the conditions of 35 DEG C viscosity less than 65 lis
Pool is to get ink-jet ink.
Embodiment 4
A kind of preparation method of electronic beam curing ink-jet ink provided in this embodiment, includes the following steps:
(1) following raw materials according to parts by weight: 6 parts of isocyanates IPDI monomer, pentaerythritol triacrylate 10 are taken
(molecular weight is for part, 0.1 part of 2,6 di tert butyl 4 methyl phenol, 0.15 part of dibutyl tin dilaurate, polycarbonate glycol
3000) 18 parts, 10 parts of DR-E522 dissaving polymer, 30 parts of isobornyl acrylate, isocyanates ethyl acrylate (AOI)
5 parts, 2 parts of end hydroxy butadiene (HTPB)；
Isocyanates IPDI monomer and pentaerythritol triacrylate are added into reactor, is warming up to 80 DEG C, reaction
1.5h；80 DEG C are warming up to, 2,6- di-tert-butyl-4-methy phenol and dibutyl tin dilaurate is added, after mixing evenly, once
Property be added polycarbonate glycol, react 1.5h, obtain urethane acrylate semi-finished product；Into semi-finished product urethane acrylate
TaiWan, China work Xinghua is added, the DR-E522 dissaving polymer provided, isobornyl acrylate are provided, stirs evenly, be diluted to
Viscosity is lower than the mixture of 300 centipoises under room temperature；Add isocyanates ethyl acrylate (AOI), the insulation reaction at 80 DEG C
1-2h is added end hydroxy butadiene (HTPB) and is mended after NCO percentage composition is lower than 0.2% in detection confirmation system
By force, urethane acrylate is obtained；
(2) following raw material according to parts by weight: 35 parts of the resulting urethane acrylate of step (1), Lu Borun is weighed
3 parts of Solsperse 24000SC hyper-dispersant, 6 parts of organic pigment 57:1 red powder, 1 part of fumed silica, methacrylic acid
5 parts of dodecyl ester, three 8 parts of (2- ethoxy) isocyanuric acid triacrylates, tristyrylphenol polyoxyethylene ether methyl
10 parts of acrylate, 2 parts of γ-glycidyl ether oxypropyltrimethoxysilane, γ-methacryloxypropyl trimethoxy
1.5 parts of base silane, 30 parts of isobornyl acrylate；
It is ultra-dispersed that Lu Borun Solsperse 24000SC is sequentially added into step (1) resulting urethane acrylate
Agent, organic pigment 14# yellow powder, fumed silica, lauryl methacrylate, three (2- ethoxy) isocyanuric acids three
Acrylate, tristyrylphenol polyoxyethylene ether methacrylate, high-speed stirred is uniform, carries out sand using sand mill
Mill detects the particle diameter of confirmation organic pigment 57:1 red powder using laser particle analyzer, when detecting that organic pigment 57:1 is red
When the partial size of toner is less than 250 nanometers, γ-glycidyl ether oxypropyltrimethoxysilane and γ-methacryl is added
Oxygroup propyl trimethoxy silicane, and using isobornyl acrylate adjust viscosity, until under the conditions of 35 DEG C viscosity less than 65
Centipoise is to get ink-jet ink.
Beneficial effect in order to further illustrate the present invention, the present invention are held using 99.99% high-purity nitrogen in reaction
It is filled in device, above-described embodiment products obtained therefrom is solidificated on liquid-crystalline glasses by electronics beam scanning forms ink and color layer respectively, and
Its hardness, water boiling resistance, solvent corrosion corrosion, scratch resistance are tested, test result is as shown in table 1.
1 test result of table
Above the embodiments of the present invention are described in detail, but the present invention is not limited to described embodiments.It is right
For those skilled in the art, in the case where not departing from the principle of the invention and spirit, these embodiments are carried out more
Kind change, modification, replacement and modification, still fall in protection scope of the present invention.
Claims (10)
1. a kind of electronic beam curing ink-jet ink, which is characterized in that according to parts by weight, including the following raw material: polyurethane propylene
15-35 parts of acid esters, 20-35 parts of isobomyl acrylate, 5-10 parts of organic pigment toner, 0.5-1 parts of fumed silica, methyl-prop
5-10 parts of olefin(e) acid dodecyl ester, three 5-20 parts of (2- ethoxy) isocyanuric acid triacrylates, triphenyl vinyl phenol polyoxy
5-10 parts of ethylene ether metacrylic acid ester, 1-5 parts of dispersing agent, 3-5 parts of auxiliary agent.
2. electronic beam curing ink-jet ink according to claim 1, which is characterized in that the urethane acrylate is pressed
Parts by weight meter, including the following raw material: the first 1-6 parts of isocyanate-monomer, 5-10 parts of pentaerythritol triacrylate, polymerization inhibitor
0.01-0.1 parts, 0.01-0.1 parts of catalyst, 10-20 parts of polyester polyol, 3-15 parts of acrylic ester copolymer oligomer, acrylic acid
20-35 parts of isobornyl thiocyanoacetate, 2-8 parts of the second isocyanate-monomer, 1-5 parts of end hydroxy butadiene.
3. electronic beam curing ink-jet ink according to claim 2, which is characterized in that the urethane acrylate is to adopt
It is made with following methods:
After first isocyanate-monomer and pentaerythritol triacrylate are mixed, it is warming up to 50-70 DEG C, reacts 1.5-2h, is adjusted
Temperature is saved to 70-90 DEG C, polymerization inhibitor and catalyst is added, after mixing evenly, polyester polyol, insulation reaction 1.5- is added
2.5h is added acrylic ester copolymer oligomer, isobornyl acrylate, stirs evenly, add the second isocyanate-monomer, protects
Temperature reaction 1-2h is added end hydroxy butadiene, obtains polyurethane after the content of isocyano in system is not higher than 0.2%
Acrylate.
4. electronic beam curing ink-jet ink according to claim 2, which is characterized in that the polymerization inhibitor is the tertiary fourth of 2,6- bis-
Base -4- methylphenol.
5. electronic beam curing ink-jet ink according to claim 2, which is characterized in that the polyester polyol is to gather in oneself
One or more of esterdiol, polycaprolactonetriol, polycarbonate glycol, polycarbonate triol.
6. electronic beam curing ink-jet ink according to claim 2, which is characterized in that first isocyanate-monomer and
Second isocyanate-monomer is identical or different isocyanate-monomer, and the isocyanate-monomer is selected from isocyanates acrylic acid
One of ethyl ester, isophorone diisocyanate are a variety of.
7. electronic beam curing ink-jet ink according to claim 1, which is characterized in that the organic pigment toner is selected from face
Expect one of red, pigment yellow, pigment blue, high pigment nanometer carbon black or a variety of.
8. electronic beam curing ink-jet ink according to claim 1, which is characterized in that the auxiliary agent is silane coupling agent.
9. a kind of preparation method of such as electronic beam curing ink-jet ink according to any one of claims 1 to 8, feature exist
In including the following steps:
(1) by urethane acrylate, dispersing agent, organic pigment toner, fumed silica, lauryl base
Ester, three (2- ethoxy) isocyanuric acid triacrylates, the mixing of tristyrylphenol polyoxyethylene ether methacrylate, it is high
Speed stirs evenly, and is sanded using sand mill, and mixed material is obtained；
(2) after mixing the resulting mixed material of step (1) and auxiliary agent, and viscosity is adjusted using isobornyl acrylate, be made
Electronic beam curing ink-jet ink.
10. a kind of if electronic beam curing ink-jet ink according to any one of claims 1 to 8 is in terms of liquid-crystalline glasses printing
Using.
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| GB2593284A (en) * | 2020-01-28 | 2021-09-22 | Fujifilm Speciality Ink Systems Ltd | A method of printing |
| GB2593284B (en) * | 2020-01-28 | 2023-04-19 | Fujifilm Speciality Ink Systems Ltd | A method of printing |
| CN111777883A (en) * | 2020-06-10 | 2020-10-16 | 惠州市奥亚皇冠涂料有限公司 | Antibacterial free radical UV nano composition |
| CN112662229A (en) * | 2020-12-15 | 2021-04-16 | 深圳市墨库图文技术有限公司 | Scratch-resistant neutral UV ink and preparation method and application thereof |
| GB2606449A (en) * | 2021-03-19 | 2022-11-09 | Fujifilm Speciality Ink Systems Ltd | Printing ink |
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