CN117025027A - Aqueous yellow polymer ink and preparation method thereof - Google Patents
Aqueous yellow polymer ink and preparation method thereof Download PDFInfo
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- CN117025027A CN117025027A CN202311174173.0A CN202311174173A CN117025027A CN 117025027 A CN117025027 A CN 117025027A CN 202311174173 A CN202311174173 A CN 202311174173A CN 117025027 A CN117025027 A CN 117025027A
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- 229920000642 polymer Polymers 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 45
- 239000000919 ceramic Substances 0.000 claims abstract description 45
- 239000000049 pigment Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 239000002562 thickening agent Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 24
- 229920001223 polyethylene glycol Polymers 0.000 claims description 24
- 239000004584 polyacrylic acid Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 9
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 9
- 229920000058 polyacrylate Polymers 0.000 claims description 9
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical group [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 5
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 5
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 5
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical group 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000007639 printing Methods 0.000 abstract description 11
- 239000012855 volatile organic compound Substances 0.000 abstract description 10
- 239000003960 organic solvent Substances 0.000 abstract description 8
- 239000000976 ink Substances 0.000 description 64
- 239000002245 particle Substances 0.000 description 13
- 238000007641 inkjet printing Methods 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 238000005259 measurement Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000001052 yellow pigment Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
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- 239000005431 greenhouse gas Substances 0.000 description 1
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- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
-
- 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
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to the technical field of digital jet printing ink, in particular to water-based yellow polymer ink and a preparation method thereof. The raw materials of the water-based yellow polymer ink comprise a yellow ceramic pigment, a water-soluble polyacrylic acid polymer, a thickener, a surface tension mixture and water, wherein each cubic meter of the water-based yellow polymer ink contains 0.2-1.0 milligram of the water-soluble polyacrylic acid polymer, and each 100 parts of the water-based yellow polymer ink contains 13-16% of the yellow ceramic pigment by volume fraction; the thickener is contained in an amount of 0.01 to 15% by mass per 100 parts of the aqueous yellow polymer ink, and the surface tension mixture is contained in an amount of 0.01 to 0.1% by mass per 100 parts of the aqueous yellow polymer ink. The ink does not contain organic solvent and volatile organic compound, and the ink still has good dispersibility and jet printing property, so that the harm caused by the organic solvent and the volatile organic compound contained in the ink is improved.
Description
Technical Field
The invention relates to the technical field of digital jet printing ink, in particular to water-based yellow polymer ink and a preparation method thereof.
Background
Digital inkjet printing is a technique based on sending digitized pattern data to an inkjet printer and ejecting ink drops to print a pattern directly on a substrate. Compared with the traditional graphic printing technology, the digital ink-jet printing technology can easily create or customize a printed image, and a printing object does not need to be contacted with a printing head, so that various materials and objects with complex shapes can be used as the printing object. In addition, this printing technique can achieve higher ink efficiency because the ink is ejected only to the desired location using a digital inkjet printing method based on drop-on-demand.
Because of these advantages, ceramic inkjet printing has been the technology of choice in the tile decorating industry for the past decade. However, despite success, the industry has recently been under pressure for environmental problems such as global warming and air pollution. Since most of inks used in digital inkjet printing are based on organic solvents and contain Volatile Organic Compounds (VOCs) to ensure dispersion stability and printability thereof, such inks have the following disadvantages: 1) Affecting human health may lead to occupational hazards for operators, and prolonged or repeated exposure to high levels of VOCs may have serious health effects on the central nervous system, liver or kidneys; 2) Air pollution and environmental impact, VOCs released into the atmosphere can react with other pollutants and sunlight to form ozone, which adversely affects air quality and human health. When they are released into the soil or water, these resources may be contaminated, posing a threat to the plant, animal and aquatic ecosystem. In addition, VOCs emissions can also lead to the formation of greenhouse gases, exacerbating climate change.
It is therefore necessary to develop environmentally friendly and functional ceramic inks to replace organic solvent-based ink jet printing inks containing VOCs.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide an aqueous yellow polymer ink and a preparation method thereof. The ink provided by the embodiment of the invention does not contain organic solvents and volatile organic compounds, and still has good dispersibility and jet printing property, so that the harm caused by the organic solvents and volatile organic compounds contained in the ink is improved.
The invention is realized in the following way:
in a first aspect, the present invention provides an aqueous yellow polymer ink, which is prepared from a yellow ceramic pigment, a water-soluble polyacrylic acid polymer, a thickener, a surface tension admixture and water, wherein each cubic meter of the aqueous yellow polymer ink contains 0.2-1.0 mg of the water-soluble polyacrylic acid polymer, and each 100 parts of the aqueous yellow polymer ink contains 13-16% of the yellow ceramic pigment by volume fraction; the aqueous yellow polymer ink contains 0.01-15% by mass of a thickener per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of a surface tension admixture per 100 parts of the aqueous yellow polymer ink.
In an alternative embodiment, the thickener is selected from the group consisting of polyol polymers, preferably polyethylene glycol;
the surface tension mixture is selected from polysilanes.
In an alternative embodiment, the aqueous yellow polymer ink contains 0.2 to 1.0 milligrams of water-soluble polyacrylic acid polymer per cubic meter of the aqueous yellow polymer ink, and 13 to 16 percent by volume of the yellow ceramic pigment per 100 parts of the aqueous yellow polymer ink; 0.01-15% by mass of polyethylene glycol per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of polysilane per 100 parts of the aqueous yellow polymer ink.
In an alternative embodiment, the aqueous acrylic polymer is a polymer with polyacrylic acid as the main chain and polyethylene glycol methyl methacrylate as the side chain;
the solid content of the aqueous acrylic polymer is 10-30%.
In an alternative embodiment, the yellow ceramic pigment is selected from Pr doped ZrSiO 4 。
In an alternative embodiment, the Pr doped ZrSiO 4 The preparation process of (2) is as follows: the base material, mineralizer and solvent are wet mixed, then dried, calcined and micronized, wherein the base material is selected from silica, zirconia and praseodymium oxide.
In an alternative embodiment, the amount of silica in the base material is 30-40% by mass, the amount of zirconium dioxide is 55-65% by mass, and the amount of praseodymium oxide is 2-7% by mass;
the mineralizer is used in an amount of 2-4% of the base material.
In an alternative embodiment, the mineralizer is selected from sodium fluoride;
the drying temperature is 75-85 ℃, and the calcining temperature is 1000-1200 ℃.
In an alternative embodiment, the aqueous acrylic polymer is synthesized from polyacrylic acid, ammonium persulfate, hydroquinone monomethyl ether, and polyethylene glycol methyl methacrylate.
In a second aspect, the present invention provides a method for preparing the aqueous yellow polymer ink according to the foregoing embodiment, including: yellow ceramic pigment, aqueous polyacrylic acid polymer, thickener, surface tension mixture and water are mixed proportionally.
The invention has the following beneficial effects: according to the embodiment of the invention, the yellow ceramic pigment, the aqueous polyacrylic acid polymer, the thickener and the surface tension mixture are matched according to a specific proportion, so that the prepared aqueous yellow polymer ink still has good dispersibility and jet printing property even on the basis of no adoption of an organic solvent and a volatile compound, and can be widely applied to digital ink-jet printing. Meanwhile, the harm caused by organic solvents and volatile compounds in the existing digital ink-jet printing ink is avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a diagram showing the results of the test provided in test example 1 of the present invention;
FIGS. 2-3 are graphs showing the detection results provided in detection example 2 of the present invention;
FIG. 4 is a graph showing the results of the test provided in test example 3 of the present invention;
FIG. 5 is a graph showing the results of the X-ray and FE-SEM images provided in test example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention embodiment is a water-based yellow polymer ink, which is prepared from the following raw materials of yellow ceramic pigment, water-soluble polyacrylic acid polymer, thickener, surface tension mixing agent and water, wherein each cubic meter of the water-based yellow polymer ink contains 0.2-1.0 mg of the water-soluble polyacrylic acid polymer, and each 100 parts of the water-based yellow polymer ink contains 13-16% of the yellow ceramic pigment by volume fraction; the aqueous yellow polymer ink contains 0.01-15% by mass of a thickener per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of a surface tension admixture per 100 parts of the aqueous yellow polymer ink.
Wherein the thickener is selected from polyol polymers, preferably polyethylene glycol; polyol polymers such as polyethylene glycol are commercially available materials, and are commercially available from, for example, the biosciences of Aibisin (Shanghai).
The surface tension mixture is selected from polysilanes. Polysilanes are also commercially available materials available today, for example from Shanghai Seiyaku Biotechnology Inc.
Thus, the aqueous yellow polymer ink contains 0.2-1.0 milligrams of water-soluble polyacrylic acid polymer per cubic meter, and 13-16% volume fraction of yellow ceramic pigment per 100 parts of the aqueous yellow polymer ink; 0.01-15% by mass of polyethylene glycol per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of polysilane per 100 parts of the aqueous yellow polymer ink.
For example, the water-soluble polyacrylic acid polymer in the aqueous yellow polymer ink may contain 0.2 mg, 0.3 mg, 0.4 mg, 0.5mg, 0.6 mg, 0.7 mg, 0.8 mg, 0.9 mg, 1.0 mg, etc. of any value or any range of values between any two values between 0.2 and 1.0 mg per cubic meter.
The volume fraction of the yellow ceramic pigment is any value or any range of values formed by any two values between 13% and 16%, such as 13%, 14%, 15% and 16%.
The mass fraction of polyethylene glycol is any value or range of values formed by any two values between 0.01 and 15% such as 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, 0.5%, 1%, 5%, 10% and 15%.
The mass fraction of polysilane is any value or range of values formed by any two values between 0.01% and 0.1%, such as 0.01%, 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 0.1%, etc.
Wherein, the crystal structure of the yellow ceramic pigment adopted in the embodiment of the invention is ZrSiO doped with Pr 4 。ZrSiO 4 SiO with edge sharing 4 Tetrahedra and ZrO 8 The main building block of a triangular dodecahedron, which contains empty octahedral voids. The yellow ceramic pigment may be self-made or commercially available, for example, from Shandong Nernst Biotechnology Inc.
The embodiment of the invention also provides a preparation process of the yellow ceramic pigment, in particular ZrSiO 4 The synthesis process is as follows:
SiO 2 +4NaF→SiF 4 (g)+2Na 2 O
SiF 4 →Si 4+ +4e - +2F 2
Si 4+ +4e - +ZrO 2 +O 2 →ZrSiO 4
specifically: the base material, mineralizer, alumina balls and solvent (e.g., ethanol) are wet-mixed together for 3 hours to form a mixed powder, and then the mixed powder is dried at 75-85 deg.c, followed by calcination at 1000-1200 deg.c for 1-2 hours in an oxidizing environment (oxygen-containing atmosphere). Then, the obtained yellow ceramic pigment is micronized by using a bead mill, the particle size of the powder obtained after micronization is less than one fiftieth of the diameter of a nozzle for inkjet printing, and the average particle size is generally less than 300nm so as to prevent the nozzle of an inkjet printing head from being blocked.
Wherein, the mineralizer is selected from NaF, and the dosage of the mineralizer is 2-4% of the dosage of the base material.
The silicon dioxide is used in an amount of 30-40% by mass, the zirconium dioxide is used in an amount of 55-65% by mass and the praseodymium oxide is used in an amount of 2-7% by mass. The total amount of silica, zirconia and praseodymia was 100%.
The solid content of the aqueous acrylic polymer is 10-30%.
The water-based acrylic acid polymer is a polymer taking polyacrylic acid as a main chain and polyethylene glycol methyl methacrylate as a side chain. Specifically, the modified acrylic acid is synthesized from polyacrylic acid, ammonium persulfate, hydroquinone monomethyl ether and polyethylene glycol methyl methacrylate.
The present examples select polyacrylic acid as the backbone to ensure electrostatic repulsion and polyethylene glycol methyl methacrylate as the side chain to provide steric hindrance. When the effects of electrostatic repulsion and steric hindrance are combined, high dispersion stability of pigment particles in the aqueous ceramic ink can be achieved.
Further, the aqueous acrylic polymer may be self-made or purchased as a finished product, such as from Beijing Cheng Weihua chemical Co.
This example provides the following illustrative preparation steps: polyacrylic acid and polyethylene glycol methyl methacrylate (molar ratio of both = 1.5-2.0) were mixed with hydroquinone monomethyl ether (0.5-1.0% of total monomer weight) in deionized water. After complete dissolution, the polyacrylic acid solution and ammonium persulfate (0.5-1.0% by weight of the total monomer weight) were added dropwise to deionized water in the reactor to form a mixture. The reactor was equipped with a reflux condenser, a feed inlet and an air inlet pipe. The mixture was stirred and heated at 75-95 ℃ for 4-6 hours. After that, the reaction solution was cooled to room temperature, and the pH was adjusted to 5-6 with NaOH (40-60% by weight aqueous solution). Finally, a brown transparent polymeric surfactant is obtained.
It should be noted that the preparation methods of the yellow ceramic pigment and the aqueous polyacrylic acid polymer provided in the embodiments of the present invention are merely examples of the embodiments of the present invention.
According to the embodiment of the invention, the agglomeration of yellow ceramic pigment particles in the ink is prevented by adopting the aqueous polyacrylic acid polymer, so that the nozzle is prevented from being blocked during ink-jet printing. The yellow ceramic pigment can be distributed more uniformly, and the jet printing property is improved. The addition of the thickener and the surface tension mixture can adjust the rheological specification of the ink, and further improve the performance of the ink.
In a second aspect, the present invention provides a method for preparing the aqueous yellow polymer ink according to the foregoing embodiment, including: yellow ceramic pigment, aqueous polyacrylic acid polymer, thickener, surface tension mixture and water are mixed proportionally.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
The detection instrument adopted by the invention is as follows: viscosity measurement was performed using a rotary rheometer (HAAKE MARS III, thermo Fisher Scientific, U.S.), surface tension was performed using a surface tension analyzer (DST-60,Surface Electro Optics, korea), sedimentation and dispersibility were performed using a turbo can (turbo LAB, formula, france), and hydrodynamic radius and surface charge were measured using a particle size analyzer (VASCO, cordouan, france) and Zeta potential analyzer (ELS-Z, otsuka Electronics, japan).
Example 1
The embodiment of the invention provides water-based yellow polymer ink, which comprises 16% of yellow ceramic pigment with the volume fraction of 0.5mg/m 2 The aqueous polyacrylic acid polymer (molecular weight 950), polyethylene glycol (molecular weight 1800) with a mass fraction of 12%, polysilane with a mass fraction of 0.08% and water.
Among them, polyethylene glycol (molecular weight 1800) was purchased from the company of biosciences, inc. of Arbitraria (Shanghai). Polysilanes were purchased from Shanghai Seiyaka Biotechnology Co.
The preparation of the aqueous acrylic polymer is as follows:
polyacrylic acid and polyethylene glycol methyl methacrylate (molar ratio of both = 2.0) were mixed with hydroquinone monomethyl ether (1.0% of the total monomer weight) in deionized water. After complete dissolution, the polyacrylic acid solution and ammonium persulfate (0.5% of the total monomer weight) were added dropwise to deionized water in the reactor to form a mixture. The reactor was equipped with a reflux condenser, a feed inlet and an air inlet pipe. The mixture was stirred and heated at 85 ℃ for 5 hours. Thereafter, the reaction solution was cooled to room temperature, and the pH was adjusted to 5.5 with NaOH (50% by weight aqueous solution). Finally, a brown transparent polymeric surfactant (20% by weight of the solids content in the aqueous solution) was obtained.
The yellow ceramic pigment was prepared as follows:
the base material (60% ZrO by weight) 2 35% by weight of SiO 2 5% by weight Pr 6 O 11 ) And mineralizer (added to the mixture of the base material by weight of 3% NaF) were wet-mixed with alumina balls and ethanol for 3 hours, after which the mixed powder was dried in an oven at 80℃and then sintered at 1100℃for 1 hour in an oxidizing atmosphere. The yellow ceramic pigment obtained was then micronized using a bead mill.
Example 2
The embodiment of the invention provides water-based yellow polymer ink, which comprises 15% of yellow ceramic pigment with the volume fraction of 0.35mg/m 2 The water-based polyacrylic acid polymer comprises 12% of polyethylene glycol (molecular weight 1800), 0.08% of polysilane and water.
Among them, polyethylene glycol (molecular weight 1800) was purchased from the company of biosciences, inc. of Arbitraria (Shanghai). Polysilanes were purchased from Shanghai Seiyaka Biotechnology Co. Yellow ceramic pigments were purchased from Shandong Nepal Biotechnology Inc.
Example 3
The embodiment of the invention provides water-based yellow polymer ink, which comprises 13% of yellow ceramic pigment by volume fraction, 0.35mg/m 2 The water-based polyacrylic acid polymer comprises 10% of polyethylene glycol (molecular weight 1800), 0.08% of polysilane and water.
Among them, polyethylene glycol (molecular weight 1800) was purchased from the company of biosciences, inc. of Arbitraria (Shanghai). Polysilanes were purchased from Shanghai Seiyaka Biotechnology Co. Yellow ceramic pigments were purchased from Shandong Nepal Biotechnology Inc.
Test case
Viscosity depends on interactions between particles, in particular, weak interactions result in low viscosity, while strong interactions result in high viscosity, and viscosity measurements also reflect the dispersibility of the ink, i.e., lower viscosity, more dispersed ink, and uniform and stable dispersion.
Therefore, sodium Dodecyl Sulfate (SDS) (purchased from shenzhen vibro biotechnology limited), polyacrylic acid (purchased from beijing Cheng Weihua chemical engineering limited) and the aqueous polyacrylic acid polymer provided in example 1 of the present invention were used as a surfactant, and inks were prepared at different concentration gradients and the viscosity of the inks was measured, respectively. The yellow ceramic powder, polyethylene glycol and polysilane content of the ink were the same as in example 1.
The results are shown in FIG. 1. As can be seen from fig. 1, the viscosity of the ink can be significantly reduced by using the aqueous polypropylene polymer in the embodiment of the present invention, and the aqueous polypropylene polymer can be sufficiently adsorbed to the surface of the ceramic particles, thereby effectively blocking the interaction between the ceramic particles. In particular when the content of the aqueous polypropylene polymer is 0.5mg/m 2 The viscosity of the ink was 1.15 mPas, at which point the viscosity was optimal.
Detection example 2
The water-soluble polyacrylic acid polymer in example 1 was replaced with polyacrylic acid (available from Sank materials technologies Co., ltd. Of Hubei), and the water-soluble polyacrylic acid polymer was not used, and the zeta potential, hydrodynamic radius and sedimentation velocity of 3 inks were then tested.
The results are shown in fig. 2 and 3. As can be seen from FIG. 2, the zeta potential of the aqueous polymer ink was-18.7 mV without the surfactant, and the zeta potential after the addition of the polyacrylic acid and the aqueous polyacrylic acid polymer was-39.4 mV and-42.1 mV, thus indicating an improvement in the dispersion stability of the ink. In general, zeta potentials between 0 and-30 mV are considered to represent low dispersion stability, while exceeding-30 mV represents good dispersion stability. Furthermore, the hydrodynamic radius of the aqueous polymer ink was 265nm without surfactant, and 315nm and 365nm, respectively, measured under polyacrylic acid and aqueous polyacrylic acid polymers.
As can be seen from FIG. 3, the sedimentation rates of the samples containing no surfactant and polyacrylic acid were 0.78mm/h and 0.67mm/h, respectively, whereas the sedimentation rate of the ink sample using the aqueous polyacrylic acid polymer as the surfactant was 0.29mm/h, which was 56.7% slower than the ink sample containing polyacrylic acid. Further, the dispersion stability of the aqueous yellow polymer ink provided by the embodiment of the invention is obviously improved.
Detection example 3
The yellow ceramic pigment of example 1 was changed to pigment yellow 81 yellow pigment (available from the company of pharmaceutical chemicals, inc. of the same flying, hubei) and tested for ink jet morphology and printability.
Results referring to fig. 4, fig. 4 shows a comparison of the spray pattern and printability of different yellow pigment inks, where a is the yellow ceramic pigment employed in the examples of the present invention and b is pigment yellow 81. From fig. 4, it can be seen that pigment yellow 81 observed longer tail and satellite ink droplets, and also found dripping after the initial ink droplets were ejected, the print dot area was not uniform in size, and the print quality was affected.
Detection example 4
X-ray and SEM electron scan test of the yellow ceramic pigment prepared in example 1, see FIG. 5, wherein table a in FIG. 5Showing the X-ray diffraction (XRD) pattern of the yellow ceramic pigment; b represents an electron field emission scanning electron microscope (FE-SEM) image. As can be seen from FIG. 5, the main phase of the yellow ceramic pigment of the present invention is ZrSiO 4 . As is clear from FIG. 5, the yellow ceramic pigment has an irregular particle shape with rough edges, a particle diameter of about 50 to 900nm, a D90 particle diameter of 647nm, and an average particle diameter of 289nm. This shape is due to the high mechanical energy of the ceramic particles being decomposed during micronization.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An aqueous yellow polymer ink is characterized in that the raw materials of the aqueous yellow polymer ink comprise a yellow ceramic pigment, a water-soluble polyacrylic acid polymer, a thickener, a surface tension mixture and water, wherein each cubic meter of the aqueous yellow polymer ink contains 0.2-1.0 milligram of the water-soluble polyacrylic acid polymer, and each 100 parts of the aqueous yellow polymer ink contains 13-16% of the yellow ceramic pigment by volume fraction; the aqueous yellow polymer ink contains 0.01-15% by mass of a thickener per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of a surface tension admixture per 100 parts of the aqueous yellow polymer ink.
2. The aqueous yellow polymer ink according to claim 1, wherein the thickener is selected from the group consisting of polyol polymers, preferably polyethylene glycol;
the surface tension mixture is selected from polysilanes.
3. The aqueous yellow polymer ink of claim 1 containing from 0.2 to 1.0 milligrams of water-soluble polyacrylic acid polymer per cubic meter of said aqueous yellow polymer ink and from 13 to 16% by volume of a yellow ceramic pigment per 100 parts of said aqueous yellow polymer ink; 0.01-15% by mass of polyethylene glycol per 100 parts of the aqueous yellow polymer ink and 0.01-0.1% by mass of polysilane per 100 parts of the aqueous yellow polymer ink.
4. The aqueous yellow polymer ink according to any one of claims 1 to 3, wherein the aqueous acrylic polymer is a polymer having polyacrylic acid as a main chain and polyethylene glycol methyl methacrylate as a side chain;
the solid content of the aqueous acrylic polymer is 10-30%.
5. The aqueous yellow polymer ink according to any one of claims 1 to 3, wherein the yellow ceramic pigment is selected from Pr doped ZrSiO 4 。
6. The aqueous yellow polymer ink of claim 5 wherein the Pr-doped ZrSiO 4 The preparation process of (2) is as follows: the base material, mineralizer and solvent are wet mixed, then dried, calcined and micronized, wherein the base material is selected from silica, zirconia and praseodymium oxide.
7. The aqueous yellow polymer ink according to claim 6, wherein the amount of the silica in the base material is 30 to 40% by mass, the amount of the zirconium dioxide is 55 to 65% by mass, and the amount of the praseodymium oxide is 2 to 7% by mass;
the mineralizer is used in an amount of 2-4% of the base material.
8. The aqueous yellow polymer ink of claim 6 wherein the mineralizer is selected from sodium fluoride;
the drying temperature is 75-85 ℃, and the calcining temperature is 1000-1200 ℃.
9. The aqueous yellow polymer ink of claim 4 wherein the aqueous acrylic polymer is synthesized from polyacrylic acid, ammonium persulfate, hydroquinone monomethyl ether, and polyethylene glycol methyl methacrylate.
10. A method of preparing the aqueous yellow polymer ink of claim 1, comprising: yellow ceramic pigment, aqueous polyacrylic acid polymer, thickener, surface tension mixture and water are mixed proportionally.
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