CN101659809A - Water-based UV black ink with super-high solid content and preparation method thereof - Google Patents
Water-based UV black ink with super-high solid content and preparation method thereof Download PDFInfo
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Abstract
The invention discloses water-based UV black ink with super-high solid content and a preparation method thereof. The black ink comprises the following components in percentage by weight: 20%-60% of high-functionality water-based polyurethane acrylate, 5%-8% of compound photoinitiator, 15%-35% of hydrophilic acrylate diluted body or prepolymer, 10%-25% of solvent and 5%-15% of nano-carbon black pigment. The light curing time of the water-based UV black colored paint of the invention is shorter than 5 seconds, the bottom layer can be completely cured, the comprehensive properties of adhesive force, hardness, toughness and the like are excellent, and the water-based UV black colored paint can be widely applied to the fields of ink, wood paint and the like; the solid content is as high as 80%;and the water-based UV black ink has short drying and curing time, simple construction technology and high production efficiency, can be diluted by water or ethanol or other nontoxic solvents for regulating the viscosity, is suitable for various production modes and production requirements, and is environment-friendly and nontoxic.
Description
Technical field
The present invention relates to a kind of water-based UV black ink with super-high solid content, and the preparation method of this black ink.
Background technology
Along with science and technology development, traditional solvent type ink exposes many problems, as a large amount of VOC (volatile organic compounds) of discharging in atmosphere, operating environment, packing content thing and HUMAN HEALTH has all been caused grave danger etc.Therefore, development is that " green ink " of representative is an important development trend of following printing ink with water color ink, radiation curable ink.
Water-based UV printing ink is emerging in recent years a kind of novel " green ink ", and it can obtain increasing concern in conjunction with the advantage of water color ink and UV printing ink.But present water-based UV printing ink still has following weak point: contain a large amount of water usually in (1) water-based UV printing ink, solid content is lower, because the surface tension of water is big, vaporization heat is high, so dry time consumption and energy consumption, complex process, production efficiency is lower; (2) low-melting ink vehicle in the water-based UV printing ink, as polymkeric substance such as urethane acrylate, polyester acrylate and epoxy acrylates, the normal single functionality hydroxy acrylate end-blocking that adopts, the unsaturated functionality of system is low, solidification rate is slow, cross-linking density, sticking power and mechanical property etc. are all not ideal enough, so its over-all properties is compared big in addition gap with solvent type ink; (3) charcoal blacks dispersed not ideal enough in water-based system, and because the extinction shielding effect of charcoal blacks is very strong, can produces China ink layer bottom and be difficult to the solidified phenomenon.
Summary of the invention
The objective of the invention is to overcome the deficiency that existing water-based UV printing ink exists, a kind of water-based UV black ink with super-high solid content is provided.The water-based UV black ink solid content is up to more than 80% among the present invention, and photocuring time＜5 second are dry, set time is short, the production efficiency height; But the bottom completely solidified, high comprehensive performances such as sticking power, hardness, snappiness can be widely used in fields such as printing ink, wood lacquer; Viscosity is regulated in the dilution of innoxious solvent such as used water or ethanol during use, is fit to the multiple mode of production and production requirement, environment-protecting asepsis.
Another object of the present invention provides the preparation method of described black ink.
For realizing purpose of the present invention, adopt following technical scheme:
A kind of water-based UV black ink with super-high solid content, its component and content are:
(1) high official can aqueous polyurethane acrylate 20%～60%
(2) the Compositional type light trigger 5%～8%
(3) hydrophilic acrylate dilutes body or prepolymer 15%～35%
(4) solvent 10～25%
(5) nano carbon black pigment 5%～15%
All percentage ratios are weight percentage.
Another object of the present invention is achieved in that
A kind of preparation method of water-based UV black ink with super-high solid content may further comprise the steps:
Step 1, by mass parts, under nitrogen atmosphere protection, place reactor to mix 35～60 parts hydroxy-terminated polymer intermediates, 3～10 parts hydrophilic chain extender, 10～25 parts acetone and 0.01～0.1 part catalyzer, and drip 15～30 parts vulcabond, and temperature is controlled between 40～70 ℃ insulation reaction 1～3h, utilize the n-Butyl Amine 99 method to measure NCO content until reaching theoretical value, synthetic water based polyurethane performed polymer;
Step 2, according to experimental design, add mass parts in the above-mentioned synthetic water based polyurethane performed polymer and be 20～40 parts high functionality terminal hydroxy group monomer, temperature is controlled between 60～90 ℃, hold with complete closed polymkeric substance NCO, add 15～35 parts of hydrophilic acrylates, 10～25 parts of small amount of acetone solvent adjustment viscosity in the reaction process, thereby obtain the aqueous polyurethane acrylate oligopolymer of high functionality;
Step 3, at last, above-mentioned aqueous polyurethane acrylate oligopolymer is 90～95 parts by mass parts adds the weak base neutralization, temperature of reaction is controlled between 40～50 ℃, then with the nanometer black pigment that adds 5～15 parts in the system, high speed dispersion 1～2h adds 5～8 parts Compositional type efficiency light initiator at last, stir, obtain the water-based UV black ink of high solids content.
Further concrete enforcement of preparation method as UV black ink of the present invention is:
Described hydroxy-terminated polymer intermediate comprises one or more the mixture in polyoxyethylene glycol, polypropylene glycol, polytetramethylene glycol, PTMG, hydroxy-terminated polybutadienes, polycaprolactone dibasic alcohol or the PCDL.
Described vulcabond is tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate and 4, the one or more kinds of mixtures in the 4-diphenyl-methyl methane diisocyanate.
The mol ratio of described vulcabond and dibasic alcohol is 2～4: 1.
Described high functionality terminal hydroxy group monomer comprises the prepolymer of pentaerythritol triacrylate, pentaerythritol diacrylate monomer or hydroxyl polyfunctional acrylic ester.
Described hydrophilic acrylate comprises wherein one or more mixtures of 2-Hydroxy ethyl acrylate, methacrylic acid-2-hydroxy methacrylate, vinylformic acid-3-hydroxy propyl ester, methacrylic acid-2-hydroxy propyl ester, vinylformic acid-own ester of 6-carboxyl.
Described black pigment is the nano level carbon black powder, and particle diameter is about 20～50nm.
Described light trigger comprises benzophenone, 2-phenyl methyl phenyl ketone, 2,2-diethoxy acetophenone, 2,2-dimethyl-2-hydroxy acetophenone, 2-hydroxy-2-methyl-1-phenyl-acetone, two (2,4,6-Three methyl Benzene formyl) phenyl phosphine oxide, 2,4,6-Three methyl Benzene formyl hexichol phosphine oxide, 2-methylol-2-methoxyl group-2-phenyl methyl phenyl ketone, Alpha-hydroxy phenylcyclohexane ketone, anthraquinone, 2-ethyl-anthraquinone, isopropyl thioxanthone etc. are one or more mixtures wherein.
The principle of UV black ink of the present invention is: the present invention is to be main raw material with vulcabond, end hydroxy polyether/intermediate polyester, wetting ability multi-hydroxy carboxy acid, hydroxy acrylate end-blocking with polyfunctionality, synthesize the water-based UV resin of high functionality, and will have the multiple light trigger mixing formation Compositional type light trigger of different absorption spectrums.Because the cross-linking density of molecule segment and the light-initiated efficient of light trigger are all improved largely, therefore can make ink film from the top layer to the equal crosslinking curing fully of bottom, form anchorage effect closely with substrate surface, thereby have the solidification rate close, cross-linking density, hardness, sticking power, mechanical property and solvent resistance with varnish.Simultaneously, added less acrylate monomer or the performed polymer of molecular weight in this black ink, can regulate, obtained high solids content, and can further be dispersed in water, ethanol or the acetone equal solvent, satisfied the different modes of production and production requirement viscosity.
The water-based UV black ink with super-high solid content of the present invention's preparation is the black non transparent body.
The invention has the beneficial effects as follows:
Black ink with existing other system is compared, and has following advantage:
(1) zero VOC or low VOC discharging, environment-protecting asepsis.In the water-based UV black ink of this patent exploitation, a spot of thinner can participate in photocured cross-linked reaction and be present in the ink film, a spot of water, ethanol or acetone equal solvent are very little to HUMAN HEALTH or environmental hazard, therefore have the environment-friendly advantage of zero VOC or low VOC discharging.
(2) the adaptation field is extensive, the production efficiency height.The present invention is by adding hydrophilic acrylate's thinner in the aqueous polyurethane acrylate, realized improving solid content and regulating the double effects of viscosity, this black ink is after being scattered in the innoxious solvents such as water or ethanol with certain proportion simultaneously, can form the emulsion or the dispersion of different viscosity and solid content, satisfy the different mode of production and production requirements such as roller coat, spraying, showering, the scope of application is more extensive.In addition, because black ink has higher solid content among the present invention, the time of heat oven dry or infrared drying is reduced greatly, can satisfy the big streamline operration requirement of producing of modernization, and set time is less than 5 seconds, the production efficiency height.
(3) excellent combination property.This patent adopts the end capped technology of polyfunctional acrylic ester, significantly improved the unsaturated link(age) content of polymer molecule, and adopted highly efficiency compositional type initiator to improve light-initiated efficient, the probability that makes polymer molecule react when solidifying significantly improves, and forming three-dimensional cross-linked reticulated structure, cross-linking density significantly increases.By proportioning, reaction conditions, ink film thickness and the UV curing process of strictness control reaction raw materials and other prescription, ink film shows excellent photocuring speed, sticking power, hardness, wear resistance, solvent resistance after curing.
Embodiment
The invention will be further described below in conjunction with example, but the present invention is not limited thereto.
Embodiment 1: prepare water-based UV black ink with super-high solid content according to the following steps.
Be equipped with raw material: the prescription according to table 1 is got the raw materials ready.
Table 1
In the there-necked flask that agitator, prolong, nitrogen path are housed, add dimethylol propionic acid, isophorone diisocyanate, polycaprolactone glycol, a small amount of dibutyl tin laurate and acetone, under nitrogen atmosphere protection, constantly stir and be warming up to 60 ℃, insulation 1～2h; To add pentaerythritol triacrylate in the system, and add an amount of acetone adjusting viscosity, under 70 ℃ of conditions, continue reaction 3～6h, thereby obtain the high-functionality water-based UV resin prepolymer.Be cooled to 30 ℃, obtain the acetone soln of performed polymer with adding the triethylamine neutralization in the prepolymer, and add hydroxyethyl methylacrylate, charcoal blacks high speed dispersion 1～2h.Add light triggers such as Darocur 1173, TPO, ITX, Irgacure819 at last and stir 1h, then obtain the water-based UV black ink of super-high solid content.
The water-based UV black ink ink film excellent performance of this patent invention sees Table 2.
Table 2
This test data shows, the water-based UV black ink of the present invention's preparation has solved the technical barrier of deep layer photocuring difficulty, has excellent photocuring speed, sticking power and other mechanical property, applicable to fields such as printing ink or wood lacquers; Aspect production and construction technology, because solid content is higher, shortened the predrying time of conventional water-based UV printing ink or varnish greatly, production efficiency obviously improves; Simultaneously, this water-based UV printing ink has zero VOC or low VOC discharging, to human body and environmentally friendly, has satisfied environmental protection, efficient, fine requirement.
Claims (9)
1. a water-based UV black ink with super-high solid content is characterized in that, its component and content are:
(1) high official can aqueous polyurethane acrylate 20%～60%
(2) the Compositional type light trigger 5%～8%
(3) hydrophilic acrylate dilutes body or prepolymer 15%～35%
(4) solvent 10～25%
(5) nano carbon black pigment 5%～15%
All percentage ratios are weight percentage.
2. a method for preparing above-mentioned water-based UV black ink with super-high solid content is characterized in that, may further comprise the steps:
Step 1, by mass parts, under nitrogen atmosphere protection, place reactor to mix 35～60 parts hydroxy-terminated polymer intermediates, 3～10 parts hydrophilic chain extender, 10～25 parts acetone and 0.01～0.1 part catalyzer, and drip 15～30 parts vulcabond, and temperature is controlled between 40～70 ℃ insulation reaction 1～3h, utilize the n-Butyl Amine 99 method to measure NCO content until reaching theoretical value, synthetic water based polyurethane performed polymer;
Step 2, according to experimental design, add mass parts in the above-mentioned synthetic water based polyurethane performed polymer and be 20～40 parts high functionality terminal hydroxy group monomer, temperature is controlled between 60～90 ℃, hold with complete closed polymkeric substance NCO, add 15～35 parts of hydrophilic acrylates, 10～25 parts of small amount of acetone solvent adjustment viscosity in the reaction process, thereby obtain the aqueous polyurethane acrylate oligopolymer of high functionality;
Step 3, at last, above-mentioned aqueous polyurethane acrylate oligopolymer is 90～95 parts by mass parts adds the weak base neutralization, temperature of reaction is controlled between 40～50 ℃, then with the nanometer black pigment that adds 5～15 parts in the system, high speed dispersion 1～2h adds 5～8 parts Compositional type efficiency light initiator at last, stir, obtain the water-based UV black ink of high solids content.
3. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that described hydroxy-terminated polymer intermediate comprises one or more the mixture in polyoxyethylene glycol, polypropylene glycol, polytetramethylene glycol, PTMG, hydroxy-terminated polybutadienes, polycaprolactone dibasic alcohol or the PCDL.
4. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that, described vulcabond is tolylene diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate and 4, the one or more kinds of mixtures in the 4-diphenyl-methyl methane diisocyanate.
5. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that the mol ratio of described vulcabond and dibasic alcohol is 2～4: 1.
6. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that described high functionality terminal hydroxy group monomer comprises the prepolymer of pentaerythritol triacrylate, pentaerythritol diacrylate monomer or hydroxyl polyfunctional acrylic ester.
7. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that described hydrophilic acrylate comprises wherein one or more mixtures of 2-Hydroxy ethyl acrylate, methacrylic acid-2-hydroxy methacrylate, vinylformic acid-3-hydroxy propyl ester, methacrylic acid-2-hydroxy propyl ester, vinylformic acid-own ester of 6-carboxyl.
8. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that described black pigment is the nano level carbon black powder, its particle diameter is about 20～50nm.
9. according to the described method for preparing water-based UV black ink with super-high solid content of claim 2, it is characterized in that, described light trigger comprises benzophenone, 2-phenyl methyl phenyl ketone, 2, the 2-diethoxy acetophenone, 2,2-dimethyl-2-hydroxy acetophenone, 2-hydroxy-2-methyl-1-phenyl-acetone, two (2,4,6-Three methyl Benzene formyl) phenyl phosphine oxide, 2,4,6-Three methyl Benzene formyl hexichol phosphine oxide, 2-methylol-2-methoxyl group-2-phenyl methyl phenyl ketone, Alpha-hydroxy phenylcyclohexane ketone, anthraquinone, 2-ethyl-anthraquinone, isopropyl thioxanthones etc. are one or more mixtures wherein.
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| CN101955705A (en) * | 2010-10-27 | 2011-01-26 | 江苏科技大学 | UV spraying printing ink and preparation method thereof |
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