CN104559465A - Environment-friendly aqueous printing ink and preparation method thereof - Google Patents
Environment-friendly aqueous printing ink and preparation method thereof Download PDFInfo
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- CN104559465A CN104559465A CN201310507628.6A CN201310507628A CN104559465A CN 104559465 A CN104559465 A CN 104559465A CN 201310507628 A CN201310507628 A CN 201310507628A CN 104559465 A CN104559465 A CN 104559465A
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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
Abstract
The invention relates to aqueous printing ink and particularly relates to environment-friendly aqueous printing ink applicable to printing substrates such as paper and plastic films and a preparation method of the environment-friendly aqueous printing ink. The environment-friendly aqueous printing ink is prepared from an acrylic resin water solution, a polyacrylic ester emulsion A, a polyacrylic ester emulsion B, pigments, a wetting dispersant, a defoaming agent, wax slurry and deionized water. The environment-friendly aqueous printing ink is high in drying speed and good in wear resistance and is applicable to the printing of packaging materials such as paper and plastic films.
Description
Technical field
The present invention relates to water color ink, particularly a kind of environment-friendly type aqueous ink being applicable to the printing element such as paper, plastics film and preparation method thereof.
Background technology
In China's present stage, what in food printing packaging, usage quantity was maximum is Chlorinated Polypropylene III ink, polyurethane ink, polyacrylic ester ink, containing a large amount of organic solvents such as benzene, toluene, butanone, ethyl acetate in this kind of solvent type ink, in the use procedure of solvent type ink, the solvent contamination air of volatilization, harm operator's is healthy, and the food in the residual solvent meeting severe contamination packaging in packing articles, the research and development therefore carrying out environment-friendlyink ink are imperative.
In numerous environment-friendlyink ink, water color ink is a more promising class.The bulk solvent of water color ink is water, cleanliness without any pollution after water volatilization, operator's in use safety and Health toxicological harmless, and glassware for drinking water is conductive can not gather electrostatic, and production scene is very safe.Water color ink has unrivaled advantage relative to solvent type ink in environmental protection, health, safety, is green product worthy of the name.
Disclose in patent CN1542066A a kind of with anion polyurethane dispersion liquid for grind resin, with acrylic ester emulsion and sub-acid amides linking agent for film-forming resin, be applicable to the water color ink of BOPP and PET film printing; The cross-linked network solidified due to urethane used and acrylate resin is two resin systems be separated, and the second-order transition temperature of acrylic ester emulsion used is too high, therefore the attachment fastness existing defects of made ink.
Disclose a kind of aqueous thermal-resistant anti-boiling ink in patent CN1702123A, this ink take water soluble acrylic resin as dispersion resin, with polyaminoester emulsion, ACRYLIC EMULSION and solidifying agent for film-forming resin, has prepared the water color ink of resistance to 120 DEG C of boilings; Due to the existence of acrylic resin in this ink, it is made to be difficult to meet the requirement of resistance to boiling.
Disclose in patent CN101003703A a kind of adopt water soluble polyurethane resin and water-borne acrylic resin to prepare water-based adagio and the compound white ink of intaglio plate, this compound white ink for solvent, has the good feature of environmental protection with the ethanol of a large amount of water and minute quantity; But due to Choice of Resin, this compound white ink sticking power existing defects on a plastic film.
A kind of water-based plastic composite inner-printing ink is disclosed in patent CN101429359A, this water-based plastic composite inner-printing ink adopts water-borne acrylic resin to be dispersion resin, take waterborne polyurethane resin as matrix resin, prepared water-based plastic composite inner-printing ink with pigment, auxiliary agent etc.; Due to the selection of this water-based plastic composite inner-printing ink resin used, make its sticking power on low polar plas film substrate not good.
Disclose a kind of composite special water-based ink for plastic inner printing in patent CN102153910A, this composite special water-based ink for plastic inner printing adopts T
gfor the aqueous acrylic emulsions of-40 DEG C ~ 25 DEG C are film-forming resin, adopt solid propenoic acid resin as grind resin; Due to single resin structure, there is larger restriction to the suitability of base material in this composite special water-based ink for plastic inner printing.
From the above, research and development are applicable to the water color ink of multiple base material, have become the emphasis that this field is studied at present.
Summary of the invention
An object of the present invention is to provide one can meet the Environmental Safety requirements such as food, medicine, beverage and sanitary product, and it is fast to have rate of drying, the environment-friendly type aqueous ink that the attachment fastness on paper, plastics film is good, stripping strength is high; Hazardous and noxious substances can not be produced after wrapped product with the material that this environment-friendly type aqueous ink is printed.
Another object of the present invention is to provide a kind of preparation method of environment-friendly type aqueous ink.
Composition and the content of environment-friendly type aqueous ink of the present invention are:
The preparation method of environment-friendly type aqueous ink of the present invention comprises the following steps:
(1) in Scattered Kettle, add acrylic resin aqueous solution, wetting dispersing agent and defoamer, after stirring, add pigment and deionized water, fully after dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) add mill base prepared by polyacrylate dispersion A, polyacrylate dispersion B, wax slurry and step (1) in a reservoir, after mixing, discharging, obtains described environment-friendly type aqueous ink; Wherein the content of acrylic resin aqueous solution is 15 ~ 20wt%, the content of polyacrylate dispersion A is 25 ~ 30wt%, the content of polyacrylate dispersion B is 25 ~ 30wt%, the content of pigment is 10 ~ 15wt%, the content of wetting dispersing agent is 0.5 ~ 1.5wt%, the content of defoamer is 0.3 ~ 0.7wt%, and the content of wax slurry is 1 ~ 3wt%, and the content of deionized water is 10 ~ 20wt%.
Described acrylic resin aqueous solution can be prepared by following methods:
By etc. the deionized water of mass parts and solid propenoic acid resin join in reactor, by room temperature to 60 ~ 70 DEG C, continue to drip aminating agent under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is the acrylic resin aqueous solution of 45 ~ 50wt%.
The number-average molecular weight of described solid propenoic acid resin is 5000 ~ 10000, and acid number is 190 ~ 250mgKOH/g.
Described aminating agent is selected from the mixture of one or more in Monoethanolamine MEA BASF, diethanolamine, trolamine, ammoniacal liquor, triethylamine.
The T of described polyacrylate dispersion A
gbe 30 ~ 40 DEG C, it is prepared from by the material reaction of following component and content:
The preparation method of described polyacrylate dispersion A comprises the following steps:
(1) (methyl) acrylate that the content in polyacrylate dispersion A is 15 ~ 25wt% will prepared, content is the vinyl monomer of 15 ~ 25wt%, content is the active function monomer of 2 ~ 7wt%, content is the diacetone-acryloamide(DAA) of 2 ~ 4wt%, and content is the nonionic emulsifying agent of 60 ~ 70wt% in the nonionic emulsifying agent of 0.5 ~ 2wt%, content is that the anionic emulsifier of 60 ~ 70wt% in the anionic emulsifier of 0.2 ~ 1wt% and deionized water join in emulsifying kettle, (the general rotating speed stirred is 500 ~ 1500 revs/min to stirring and emulsifying, the time of stirring and emulsifying is 30 ~ 60 minutes), obtained pre-emulsion,
(2) will be that the initiator of 0.1 ~ 0.7wt% is dissolved in deionized water preparing the content in polyacrylate dispersion A, obtained initiator solution;
(3) by deionized water and remaining nonionic emulsifying agent, anionic emulsifier be that the buffer reagent of 0.1 ~ 0.5wt% joins in reactor preparing the content in polyacrylate dispersion A, by room temperature to 60 ~ 85 DEG C under whipped state, start to drip pre-emulsion (preferred pre-emulsion dropwised in 2 ~ 3 hours) prepared by step (1) and initiator solution (preferred initiator solution dropwised in 3 ~ 4 hours) prepared by step (2) simultaneously; After pre-emulsion and initiator solution dropwise, to continue at 60 ~ 85 DEG C insulation reaction 2 ~ 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion A of 50%.
The T of described polyacrylate dispersion B
gfor-30 ~ 0 DEG C, it is prepared from by the material reaction of following component and content:
The preparation method of described polyacrylate dispersion B comprises the following steps:
(1) (methyl) acrylate that the content in polyacrylate dispersion B is 15 ~ 25wt% will prepared, content is the vinyl monomer of 15 ~ 25wt%, content is the active function monomer of 2 ~ 7wt%, content is the two hydrazides monomers of 2 ~ 4wt%, and content is the nonionic emulsifying agent of 60 ~ 70wt% in the nonionic emulsifying agent of 0.5 ~ 2wt%, content is that the anionic emulsifier of 60 ~ 70wt% in the anionic emulsifier of 0.2 ~ 1wt% and deionized water join in emulsifying kettle, (the general rotating speed stirred is 500 ~ 1500 revs/min to stirring and emulsifying, the time of stirring and emulsifying is 30 ~ 60 minutes), obtained pre-emulsion,
(2) will be that the initiator of 0.1 ~ 0.7wt% is dissolved in deionized water preparing the content in polyacrylate dispersion B, obtained initiator solution;
(3) by deionized water and remaining nonionic emulsifying agent, anionic emulsifier with join in reactor at the buffer reagent preparing the content 0.1 ~ 0.5wt% in polyacrylate dispersion B, by room temperature to 60 ~ 85 DEG C under whipped state, start to drip pre-emulsion (preferred pre-emulsion dropwised in 2 ~ 3 hours) prepared by step (1) and initiator solution (preferred initiator solution dropwised in 3 ~ 4 hours) prepared by step (2) simultaneously; After pre-emulsion and initiator solution dropwise, to continue at 60 ~ 85 DEG C insulation reaction 2 ~ 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion B of 50%.
In the component of polyacrylate dispersion A and polyacrylate dispersion B, described (methyl) acrylate is selected from the mixture of one or more in methyl methacrylate, methyl acrylate, ethyl propenoate, butyl methacrylate, butyl acrylate, Isooctyl acrylate monomer.Described vinyl monomer is selected from the mixture of one or more in vinylbenzene, vinyl toluene, vinyl-acetic ester, propionate, vinyl butyrate, 2 ethyl hexanoic acid vinyl acetate, vinyl laurate, acetic acid-1-ethylene methacrylic ester, vinyl pivalate.Described active function monomer is selected from the mixture of one or more in hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, Propylene glycol monoacrylate, hy-droxybutyl, acrylamide, N hydroxymethyl acrylamide, vinylformic acid, glycidyl acrylate, vinyl cyanide.
In the component of polyacrylate dispersion A and polyacrylate dispersion B, described nonionic emulsifying agent is selected from the mixture of one or more in Voranol EP 2001, polyoxyethylene alkyl phenyl ether, polyoxyethylene alkylallyl ether, polyoxyethylene sorbitan alcohol fatty acid ester, polyoxyethylene sorbitol fatty acid ester, glycerol fatty acid ester.Described anionic emulsifier is selected from the mixture of one or more in ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate, cetyl benzenesulfonic acid sodium, B-53.Described initiator is selected from the mixture of one or more in ammonium persulphate, Potassium Persulphate, Sodium Persulfate.Described buffer reagent is selected from the mixture of one or more in sodium carbonate, sodium bicarbonate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, bicarbonate of ammonia.
In the component of polyacrylate dispersion B, two described hydrazides monomers are selected from the mixture of one or more in Malaysia acid dihydrazide, fumaric acid two hydrazides, methylene-succinic acid two hydrazides, citraconic acid two hydrazides.
In the component of environment-friendly type aqueous ink of the present invention, described pigment is selected from the mixture of one or more in phthalocyanine blue, phthalein viridescent, permanent bordeaux, diarylide yellow, carbon black, titanium dioxide.Described wetting dispersing agent is selected from the mixture of one or more in DISPERBYK-182, DISPERBYK-190, DISPERBYK-193, Silok-7111, Silok-7116W, Silok-7117.Described defoamer is selected from the mixture of one or more in BYK-012, BYK-016, BYK-017, BYK-024, BYK-034, BYK-044, BYK-094.Described wax slurry is AQUAACER539, AQUAACER552 or their mixture of German BIC Corp.
As a rule, low T
gpolyacrylate resin to PET, nylon, BOPP, PE, all there is good sticking power, but when only adopting such resin-made for ink, the ink layer of printing can instead glue usually.High T
gpolyacrylate resin all poor to multiple plastics film sticking power.Therefore two classes are had different T by the present invention
gpolyacrylic ester with the use of, overcome the anti-sticky problem of ink layer.
Polyacrylate dispersion A prepared by the present invention and polyacrylate dispersion B is with different reactive functional groups, when the film printing environment-friendly type aqueous ink of the present invention is dry in the drying tunnel of printing press, two resinoids with functional group can there is crosslinking reaction, this significantly improves the sticking power of ink layer on printing element further, makes the environment-friendly type aqueous ink prepared by the present invention all have good printing effect on multiple printing element.
Environment-friendly type aqueous ink setting speed of the present invention is fast, and crocking resistance is good, is suitable for the printing of the wrapping material such as paper, plastics film.
Below by specific embodiment, the present invention is described in further detail, but should not be understood as limiting the scope of the invention.All based on above-mentioned technological thought, the amendment utilizing ordinary skill knowledge and usual technique means to make, replacement, change, all belong to scope of the present invention.
Embodiment
Embodiment 1
1. the preparation of polyacrylate dispersion A
(1) 25kg methyl methacrylate, 15kg vinyl-acetic ester, 5kg Hydroxyethyl acrylate, 4kg diacetone-acryloamide(DAA), 0.3kg Voranol EP 2001,0.12kg ammonium lauryl sulfate and 11.6kg deionized water are joined in emulsifying kettle, with 500 revs/min of stirring and emulsifying 30 minutes, obtained pre-emulsion;
(2) 0.1kg ammonium persulphate is dissolved in 2.4kg deionized water, obtained initiator solution;
(3) 36kg deionized water, 0.2kg Voranol EP 2001,0.08kg ammonium lauryl sulfate and 0.2kg sodium carbonate are joined in reactor, by room temperature to 60 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2 hours, and initiator solution dropwised in 3 hours; After pre-emulsion and initiator solution dropwise, to continue at 60 DEG C insulation reaction 2 hours, cooling discharge, obtained solid content is the polyacrylate dispersion A of 50wt%.
2. the preparation of polyacrylate dispersion B
(1) 22kg butyl acrylate, 18kg vinyl pivalate, 4kg Propylene glycol monoacrylate, 3.2kg methylene-succinic acid two hydrazides, 0.816kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.476kg cetyl benzenesulfonic acid sodium and 10.72kg deionized water are joined in emulsifying kettle, with 700 revs/min of stirring and emulsifying 40 minutes, obtained pre-emulsion;
(2) 0.5kg Potassium Persulphate is dissolved in 3.18kg deionized water, obtained initiator solution;
(3) 36.1kg deionized water, 0.384kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.224kg cetyl benzenesulfonic acid sodium and 0.4kg sodium phosphate are joined in reactor, by room temperature to 70 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2 hours, and initiator solution dropwised in 3 hours; After pre-emulsion and initiator solution dropwise, to continue at 70 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is 50wt% polyacrylate dispersion B.
3. the preparation of acrylic resin aqueous solution
Be 5000 by 10kg deionized water and 10kg number-average molecular weight, acid number is that the solid propenoic acid resin of 190mgKOH/g joins in reactor, by room temperature to 60 DEG C, continue to drip Monoethanolamine MEA BASF under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is the acrylic resin aqueous solution of 45wt%.4. the preparation of environment-friendly type aqueous white ink
(1) in Scattered Kettle, add above-mentioned acrylic resin aqueous solution, 0.5kgDISPERBYK-182 and the 0.3kg BYK-012 prepared of 15kg, 10kg titanium dioxide and 15kg deionized water is added after stirring, after abundant dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) the 30kg above-mentioned polyacrylate dispersion A for preparing and 26.2kg polyacrylate dispersion B is added in a reservoir, with the mill base adding 3kgAQUAACER539 and step (1) and prepare, after mixing, discharging, obtained environment-friendly type aqueous white ink, technical indicator is in table 1.
In the environment-friendly type aqueous ink of gained, the content of each component is: the content of acrylic resin aqueous solution is 15wt%, the content of polyacrylate dispersion A is 30wt%, the content of polyacrylate dispersion B is 26.2wt%, the content of titanium dioxide is 10wt%, the content of DISPERBYK-182 is 0.5wt%, the content of BYK-012 is the content of 0.3wt%, AQUAACER539 is 3wt%, and the content of deionized water is 15wt%.
The technical indicator of the environment-friendly type aqueous white ink of table 1
| Project | Technical indicator | Examination criteria |
| Color | Color standard white | GB/T13217.1-2009 |
| Viscosity | 29s(is coated with 4 glasss, 25 DEG C) | GB/T13217.4-2008 |
| Attachment fastness | 97% | GB/T13217.7-2009 |
| First dryness | 25mm/30s，25℃ | GB/T13217.5-2008 |
| Fineness | ≤9μm | GB/T13217.3-2008 |
Embodiment 2
1. the preparation of polyacrylate dispersion A
(1) 15kg methyl acrylate, 21.8kg vinyl toluene, 7kg Hydroxyethyl acrylate, 2kg diacetone-acryloamide(DAA), 1.4kg polyoxyethylene alkylallyl ether, 0.7kg cetyl benzenesulfonic acid sodium and 12.5kg deionized water are joined in emulsifying kettle, with 1500 revs/min of stirring and emulsifying 60 minutes, obtained pre-emulsion;
(2) 0.7kg Sodium Persulfate is dissolved in 5.5kg deionized water, obtained initiator solution;
(3) 32kg deionized water, 0.6kg polyoxyethylene alkylallyl ether, 0.3kg cetyl benzenesulfonic acid sodium and 0.5kg sodium phosphate are joined in reactor, by room temperature to 85 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously.Pre-emulsion dropwised in 3 hours, and initiator solution dropwised in 4 hours; After pre-emulsion and initiator solution dropwise, to continue at 85 DEG C insulation reaction 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion A of 50wt%.
2. the preparation of polyacrylate dispersion B
(1) 25kg butyl acrylate, 15kg vinylbenzene, 5kg hy-droxybutyl, 4kg Malaysia acid dihydrazide, 0.3kg polyoxyethylene alkyl phenyl ether, 0.12kg Sodium dodecylbenzene sulfonate and 11.6kg deionized water are joined in emulsifying kettle, with 500 revs/min of stirring and emulsifying 30 minutes, obtained pre-emulsion;
(2) 0.1kg ammonium persulphate is dissolved in 2.4kg deionized water, obtained initiator solution;
(3) 36kg deionized water, 0.2kg Voranol EP 2001,0.08kg ammonium lauryl sulfate and 0.2kg sodium carbonate are joined in reactor, by room temperature to 60 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2 hours, and initiator solution dropwised in 3 hours.After pre-emulsion and initiator solution dropwise, to continue at 60 DEG C insulation reaction 2 hours, cooling discharge, obtained solid content is 50wt% polyacrylate dispersion B.
3. the preparation of acrylic resin aqueous solution
Be 10000 by 10kg deionized water and 10kg number-average molecular weight, acid number is that the solid propenoic acid resin of 250mgKOH/g joins in reactor, by room temperature to 70 DEG C, continue to drip diethanolamine under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is 47.5wt% acrylic resin aqueous solution.
4. the preparation of environment-friendly type aqueous red ink
(1) in Scattered Kettle, add above-mentioned acrylic resin aqueous solution, 1.5kgDISPERBYK-190 and the 0.7kg BYK-016 prepared of 17.5kg, 10.8kg permanent bordeaux and 10kg deionized water is added after stirring, after abundant dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) add the 27.5kg above-mentioned polyacrylate dispersion A for preparing and 30kg polyacrylate dispersion B in a reservoir and add mill base prepared by 2kgAQUAACER552 and step (1), after mixing, discharging, obtained environment-friendly type aqueous red ink, technical indicator is in table 2.
In the environment-friendly type aqueous ink of gained, the content of each component is: the content of acrylic resin aqueous solution is 17.5wt%, the content of polyacrylate dispersion A is 27.5wt%, the content of polyacrylate dispersion B is 30wt%, the content of permanent bordeaux is 10.8wt%, the content of DISPERBYK-190 is 1.5wt%, the content of BYK-016 is the content of 0.7wt%, AQUAACER552 is 2wt%, and the content of deionized water is 10wt%.
The technical indicator of the environment-friendly type aqueous red ink of table 2
| Project | Technical indicator | Examination criteria |
| Color | Canonical red | GB/T13217.1-2009 |
| Viscosity | 32s(is coated with 4 glasss, 25 DEG C) | GB/T13217.4-2008 |
| Attachment fastness | 99% | GB/T13217.7-2009 |
| First dryness | 27mm/30s，25℃ | GB/T13217.5-2008 |
| Fineness | ≤9μm | GB/T13217.3-2008 |
Embodiment 3
1. the preparation of polyacrylate dispersion A
(1) 17.45kg ethyl propenoate, 25kg vinylbenzene, 2kg vinyl cyanide, 3kg diacetone-acryloamide(DAA), 0.8125kg glycerol fatty acid ester, 0.39kg ammonium lauryl sulfate and 11.5kg deionized water are joined in emulsifying kettle, with 1000 revs/min of stirring and emulsifying 45 minutes, obtained pre-emulsion;
(2) 0.4kg Potassium Persulphate is dissolved in 4.05kg deionized water, obtained initiator solution;
(3) 34.45kg deionized water, 0.4375kg glycerol fatty acid ester, 0.21kg ammonium lauryl sulfate and 0.3kg bicarbonate of ammonia are joined in reactor, by room temperature to 72.5 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously.Pre-emulsion dropwised in 2.5 hours, and initiator solution dropwised in 3.5 hours.After pre-emulsion and initiator solution dropwise, to continue at 72.5 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is 50wt% polyacrylate dispersion A.
2. the preparation of polyacrylate dispersion B
(1) 15kg Isooctyl acrylate monomer, 21.8kg vinyl butyrate, 7kg acrylamide, 2kg fumaric acid two hydrazides, 1.4kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.7kg B-53 and 12.5kg deionized water are joined in emulsifying kettle, with 1500 revs/min of stirring and emulsifying 60 minutes, obtained pre-emulsion;
(2) 0.7kg Potassium Persulphate is dissolved in 5.5kg deionized water, obtained initiator solution;
(3) 32kg deionized water, 0.6kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.3kg B-53 and 0.5kg SODIUM PHOSPHATE, MONOBASIC are joined in reactor, by room temperature to 85 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 3 hours, and initiator solution dropwised in 4 hours; After pre-emulsion and initiator solution dropwise, to continue at 85 DEG C insulation reaction 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion B of 50wt%.
3. the preparation of acrylic resin aqueous solution
Be 7500 by 10kg deionized water and 10kg number-average molecular weight, acid number is that the solid propenoic acid resin of 220mgKOH/g joins in reactor, by room temperature to 65 DEG C, continue to drip trolamine under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is 48wt% acrylic resin aqueous solution.4. the preparation of environment-friendly type aqueous Yellow ink
(1) in Scattered Kettle, add above-mentioned acrylic resin aqueous solution, 1kgDISPERBYK-193 and the 0.5kg BYK-017 prepared of 20kg, 15kg diarylide yellow and 12.5kg deionized water is added after stirring, after abundant dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) add the 25kg above-mentioned polyacrylate dispersion A for preparing and 25kg polyacrylate dispersion B in a reservoir and add mill base prepared by 1kgAQUAACER552 and step (1), after mixing, discharging, obtained environment-friendly type aqueous Yellow ink, technical indicator is in table 3.
In the environment-friendly type aqueous ink of gained, the content of each component is: the content of acrylic resin aqueous solution is 20wt%, the content of polyacrylate dispersion A is 25wt%, the content of polyacrylate dispersion B is 25wt%, the content of diarylide yellow is 15wt%, the content of DISPERBYK-193 is 1wt%, the content of BYK-017 is the content of 0.5wt%, AQUAACER552 is 1wt%, and the content of deionized water is 12.5wt%.
The technical indicator of the environment-friendly type aqueous Yellow ink of table 3
| Project | Technical indicator | Examination criteria |
| Color | Standard yellow | GB/T13217.1-2009 |
| Viscosity | 35s(is coated with 4 glasss, 25 DEG C) | GB/T13217.4-2008 |
| Attachment fastness | 99% | GB/T13217.7-2009 |
| First dryness | 27mm/30s，25℃ | GB/T13217.5-2008 |
| Fineness | ≤9μm | GB/T13217.3-2008 |
Embodiment 4
1. the preparation of polyacrylate dispersion A
(1) 20kg methyl methacrylate, 20kg2-ethyl hexanoate, 4.5kg vinyl cyanide, 2.5kg diacetone-acryloamide(DAA), 0.96kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.576kg cetyl benzenesulfonic acid sodium and 13.04kg deionized water are joined in emulsifying kettle, with 1200 revs/min of stirring and emulsifying 50 minutes, obtained pre-emulsion;
(2) 0.5kg ammonium persulphate is dissolved in 3.16kg deionized water, obtained initiator solution;
(3) 33.8kg deionized water, 0.54kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.324kg cetyl benzenesulfonic acid sodium and 0.1kg SODIUM PHOSPHATE, MONOBASIC are joined in reactor, by room temperature to 80 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2.5 hours, and initiator solution dropwised in 4 hours.After pre-emulsion and initiator solution dropwise, to continue at 80 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is 50wt% polyacrylate dispersion A.
2. the preparation of polyacrylate dispersion B
(1) 17.45kg butyl acrylate, 25kg vinyl pivalate, 2kg Rocryl 410,3kg methylene-succinic acid two hydrazides, 0.8125kg polyoxyethylene sorbitol fatty acid ester, 0.39kg cetyl benzenesulfonic acid sodium and 11.5kg deionized water are joined in emulsifying kettle, with 1000 revs/min of stirring and emulsifying 45 minutes, obtained pre-emulsion;
(2) 0.4kg Sodium Persulfate is dissolved in 4.05kg deionized water, obtained initiator solution;
(3) 34.45kg deionized water, 0.4375kg polyoxyethylene sorbitol fatty acid ester, 0.21kg cetyl benzenesulfonic acid sodium and 0.3kg Sodium phosphate dibasic are joined in reactor, by room temperature to 72.5 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2.5 hours, and initiator solution dropwised in 3.5 hours; After pre-emulsion and initiator solution dropwise, to continue at 72.5 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is the polyacrylate dispersion B of 50wt%.
3. the preparation of acrylic resin aqueous solution
Be 8000 by 10kg deionized water and 10kg number-average molecular weight, acid number is that 210mgKOH/g solid propenoic acid resin joins in reactor, by room temperature to 70 DEG C, continue to drip ammoniacal liquor under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is the acrylic resin aqueous solution of 50wt%.
4. the preparation of environment-friendly type aqueous blue ink
(1) in Scattered Kettle, add above-mentioned acrylic resin aqueous solution, the 1.3kg prepared of 17kg
Silok-7111 and 0.6kg BYK-034, adds 12.5kg phthalocyanine blue and 14kg deionized water after stirring, fully after dispersion, be ground to fineness be less than 10 μm through sand mill, obtained mill base;
(2) add the 26kg above-mentioned polyacrylate dispersion A for preparing and 27.5kg polyacrylate dispersion B in a reservoir and add mill base prepared by 1.1kgAQUAACER539 and step (1), after mixing, discharging, obtained environment-friendly type aqueous blue ink, technical indicator is in table 4.
In the environment-friendly type aqueous ink of gained, the content of each component is: the content of acrylic resin aqueous solution is 17wt%, the content of polyacrylate dispersion A is 26wt%, the content of polyacrylate dispersion B is 27.5wt%, the content of phthalocyanine blue is 12.5wt%, the content of Silok-7111 is 1.3wt%, the content of BYK-034 is the content of 0.6wt%, AQUAACER539 is 1.1wt%, and the content of deionized water is 14wt%.
The technical indicator of the environment-friendly type aqueous blue ink of table 4
| Project | Technical indicator | Examination criteria |
| Color | Standard is blue | GB/T13217.1-2009 |
| Viscosity | 31s(is coated with 4 glasss, 25 DEG C) | GB/T13217.4-2008 |
| Attachment fastness | 97% | GB/T13217.7-2009 |
| First dryness | 38mm/30s，25℃ | GB/T13217.5-2008 |
| Fineness | ≤9μm | GB/T13217.3-2008 |
Embodiment 5
1. the preparation of polyacrylate dispersion A
(1) 22kg ethyl propenoate, 18kg vinyl toluene, 4kgN-n-methylolacrylamide, 3.2kg diacetone-acryloamide(DAA), 0.816kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.476kg ammonium lauryl sulfate and 10.72kg deionized water are joined in emulsifying kettle, with 800 revs/min of stirring and emulsifying 45 minutes, obtained pre-emulsion;
(2) 0.5kg Sodium Persulfate is dissolved in 3.18kg deionized water, obtained initiator solution;
(3) 36.1kg deionized water, 0.384kg polyoxyethylene sorbitan alcohol fatty acid ester, 0.224kg ammonium lauryl sulfate and 0.4kg sodium bicarbonate are joined in reactor, by room temperature to 80 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 2.5 hours, and initiator solution dropwised in 3.5 hours; After pre-emulsion and initiator solution dropwise, to continue at 80 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is the polyacrylate dispersion A of 50wt%.
2. the preparation of polyacrylate dispersion B
(1) 20kg butyl acrylate, 20kg vinyl laurate, 4.5kg glycidyl acrylate, 2.5kg citraconic acid two hydrazides, 0.96kg Voranol EP 2001,0.576kg cetyl benzenesulfonic acid sodium and 13.04kg deionized water are joined in emulsifying kettle, with 1100 revs/min of stirring and emulsifying 40 minutes, obtained pre-emulsion;
(2) 0.5kg Potassium Persulphate is dissolved in 3.16kg deionized water, obtained initiator solution;
(3) 33.8kg deionized water, 0.54kg Voranol EP 2001,0.324kg cetyl benzenesulfonic acid sodium and 0.1kg Sodium phosphate dibasic are joined in reactor, by room temperature to 70 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; Pre-emulsion dropwised in 3 hours, and initiator solution dropwised in 4 hours; After pre-emulsion and initiator solution dropwise, to continue at 70 DEG C insulation reaction 3 hours, cooling discharge, obtained solid content is the polyacrylate dispersion B of 50wt%.
3. the preparation of acrylic resin aqueous solution
Be 9000 by 10kg deionized water and 10kg number-average molecular weight, acid number is that 240mgKOH/g solid propenoic acid resin joins in reactor, by room temperature to 65 DEG C, continue to drip triethylamine under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is the acrylic resin aqueous solution of 46wt%.
4. the preparation of environment-friendly aqueous black ink
(1) in Scattered Kettle, add above-mentioned acrylic resin aqueous solution, 0.55kgDISPERBYK-193 and the 0.35kg BYK-094 prepared of 15.5kg, 11kg carbon black and 20kg deionized water is added after stirring, after abundant dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) add the 25.5kg above-mentioned polyacrylate dispersion A for preparing and 26kg polyacrylate dispersion B in a reservoir and add mill base prepared by 1.1kgAQUAACER552 and step (1), after mixing, discharging, obtained environment-friendly aqueous black ink, technical indicator is in table 5.
In the environment-friendly type aqueous ink of gained, the content of each component is: the content of acrylic resin aqueous solution is 15.5wt%, the content of polyacrylate dispersion A is 25.5wt%, the content of polyacrylate dispersion B is 26wt%, the content of carbon black is 11wt%, the content of DISPERBYK-193 is 0.55wt%, the content of BYK-094 is the content of 0.35wt%, AQUAACER552 is 1.1wt%, and the content of deionized water is 20wt%.
The technical indicator of table 5 environment-friendly aqueous black ink
| Project | Technical indicator | Examination criteria |
| Color | Standard black | GB/T13217.1-2009 |
| Viscosity | 29s(is coated with 4 glasss, 25 DEG C) | GB/T13217.4-2008 |
| Attachment fastness | 99% | GB/T13217.7-2009 |
| First dryness | 34mm/30s，25℃ | GB/T13217.5-2008 |
| Fineness | ≤8μm | GB/T13217.3-2008 |
Claims (10)
1. an environment-friendly type aqueous ink, is characterized in that: composition and the content of described environment-friendly type aqueous ink are:
The T of described polyacrylate dispersion A
git is 30 ~ 40 DEG C; Described polyacrylate dispersion A is prepared by following methods:
(1) be the diacetone-acryloamide(DAA) of 2 ~ 4wt% by the active function monomer that is 2 ~ 7wt% at the vinyl monomer preparing (methyl) acrylate that the content in polyacrylate dispersion A is 15 ~ 25wt%, content is 15 ~ 25wt%, content, content, and content be the nonionic emulsifying agent of 60 ~ 70wt% in the nonionic emulsifying agent of 0.5 ~ 2wt%, content is that the anionic emulsifier of 60 ~ 70wt% in the anionic emulsifier of 0.2 ~ 1wt% and deionized water join in emulsifying kettle, stirring and emulsifying, obtained pre-emulsion;
(2) will be that the initiator of 0.1 ~ 0.7wt% is dissolved in deionized water preparing the content in polyacrylate dispersion A, obtained initiator solution;
(3) buffer reagent being 0.1 ~ 0.5wt% by deionized water and remaining nonionic emulsifying agent, anionic emulsifier and the content when preparing polyacrylate dispersion A joins in reactor, by room temperature to 60 ~ 85 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; After pre-emulsion and initiator solution dropwise, to continue at 60 ~ 85 DEG C insulation reaction 2 ~ 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion A of 50%;
The T of described polyacrylate dispersion B
gfor-30 ~ 0 DEG C; Described polyacrylate dispersion B is prepared by following methods:
(1) nonionic emulsifying agent of 60 ~ 70wt% that to be the two hydrazides monomers of 2 ~ 4wt% and content by the active function monomer that is 2 ~ 7wt% at the vinyl monomer preparing (methyl) acrylate that the content in polyacrylate dispersion B is 15 ~ 25wt%, content is 15 ~ 25wt%, content, content be in the nonionic emulsifying agent of 0.5 ~ 2wt%, content are that the anionic emulsifier of 60 ~ 70wt% in the anionic emulsifier of 0.2 ~ 1wt% and deionized water join in emulsifying kettle, stirring and emulsifying, obtained pre-emulsion;
(2) will be that the initiator of 0.1 ~ 0.7wt% is dissolved in deionized water preparing the content in polyacrylate dispersion B, obtained initiator solution;
(3) by deionized water and remaining nonionic emulsifying agent, anionic emulsifier be that the buffer reagent of 0.1 ~ 0.5wt% joins in reactor preparing the content in polyacrylate dispersion B, by room temperature to 60 ~ 85 DEG C under whipped state, start to drip pre-emulsion prepared by step (1) and initiator solution prepared by step (2) simultaneously; After pre-emulsion and initiator solution dropwise, to continue at 60 ~ 85 DEG C insulation reaction 2 ~ 4 hours, cooling discharge, obtained solid content is the polyacrylate dispersion B of 50%;
Described active function monomer is selected from the mixture of one or more in hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, Propylene glycol monoacrylate, hy-droxybutyl, acrylamide, N hydroxymethyl acrylamide, vinylformic acid, glycidyl acrylate, vinyl cyanide.
2. environment-friendly type aqueous ink according to claim 1, is characterized in that: described acrylic resin aqueous solution is prepared by following methods:
By etc. the deionized water of mass parts and solid propenoic acid resin join in reactor, by room temperature to 60 ~ 70 DEG C, continue to drip aminating agent under whipped state, the pH value of solution in reactor is made to remain 8 ~ 9, until the solid propenoic acid resin in reactor all dissolves, cooling, discharging, obtained solid content is the acrylic resin aqueous solution of 45 ~ 50wt%;
The number-average molecular weight of described solid propenoic acid resin is 5000 ~ 10000, and acid number is 190 ~ 250mgKOH/g;
Described aminating agent is selected from the mixture of one or more in Monoethanolamine MEA BASF, diethanolamine, trolamine, ammoniacal liquor, triethylamine.
3. environment-friendly type aqueous ink according to claim 1, is characterized in that: described (methyl) acrylate is selected from the mixture of one or more in methyl methacrylate, methyl acrylate, ethyl propenoate, butyl methacrylate, butyl acrylate, Isooctyl acrylate monomer;
Described vinyl monomer is selected from the mixture of one or more in vinylbenzene, vinyl toluene, vinyl-acetic ester, propionate, vinyl butyrate, 2 ethyl hexanoic acid vinyl acetate, vinyl laurate, acetic acid-1-ethylene methacrylic ester, vinyl pivalate.
4. environment-friendly type aqueous ink according to claim 1, is characterized in that: described nonionic emulsifying agent is selected from the mixture of one or more in Voranol EP 2001, polyoxyethylene alkyl phenyl ether, polyoxyethylene alkylallyl ether, polyoxyethylene sorbitan alcohol fatty acid ester, polyoxyethylene sorbitol fatty acid ester, glycerol fatty acid ester;
Described anionic emulsifier is selected from the mixture of one or more in ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate, cetyl benzenesulfonic acid sodium, B-53.
5. environment-friendly type aqueous ink according to claim 1, is characterized in that: described initiator is selected from the mixture of one or more in ammonium persulphate, Potassium Persulphate, Sodium Persulfate;
Described buffer reagent is selected from the mixture of one or more in sodium carbonate, sodium bicarbonate, sodium phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, bicarbonate of ammonia.
6. environment-friendly type aqueous ink according to claim 1, is characterized in that: two described hydrazides monomers are selected from the mixture of one or more in Malaysia acid dihydrazide, fumaric acid two hydrazides, methylene-succinic acid two hydrazides, citraconic acid two hydrazides.
7. environment-friendly type aqueous ink according to claim 1, is characterized in that: described pigment is selected from the mixture of one or more in phthalocyanine blue, phthalein viridescent, permanent bordeaux, diarylide yellow, carbon black, titanium dioxide.
8. environment-friendly type aqueous ink according to claim 1, is characterized in that: described wetting dispersing agent is selected from the mixture of one or more in DISPERBYK-182, DISPERBYK-190, DISPERBYK-193, Silok-7111, Silok-7116W, Silok-7117;
Described defoamer is selected from the mixture of one or more in BYK-012, BYK-016, BYK-017, BYK-024, BYK-034, BYK-044, BYK-094;
Described wax slurry is AQUAACER539, AQUAACER552 or their mixture.
9. environment-friendly type aqueous ink according to claim 1, is characterized in that: the time for adding of described pre-emulsion is 2 ~ 3 hours; The time for adding of described initiator solution is 3 ~ 4 hours.
10. a preparation method for the environment-friendly type aqueous ink described in claim 1 ~ 9 any one, is characterized in that: described preparation method comprises the following steps:
(1) in Scattered Kettle, add acrylic resin aqueous solution, wetting dispersing agent and defoamer, after stirring, add pigment and deionized water, fully after dispersion, be ground to fineness through sand mill and be less than 10 μm, obtained mill base;
(2) add mill base prepared by polyacrylate dispersion A, polyacrylate dispersion B, wax slurry and step (1) in a reservoir, after mixing, discharging, obtains described environment-friendly type aqueous ink; Wherein the content of acrylic resin aqueous solution is 15 ~ 20wt%, the content of polyacrylate dispersion A is 25 ~ 30wt%, the content of polyacrylate dispersion B is 25 ~ 30wt%, the content of pigment is 10 ~ 15wt%, the content of wetting dispersing agent is 0.5 ~ 1.5wt%, the content of defoamer is 0.3 ~ 0.7wt%, and the content of wax slurry is 1 ~ 3wt%, and the content of deionized water is 10 ~ 20wt%.
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