CN115160850A - Water-based ink for decorative paper and preparation method thereof - Google Patents
Water-based ink for decorative paper and preparation method thereof Download PDFInfo
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- CN115160850A CN115160850A CN202210886561.0A CN202210886561A CN115160850A CN 115160850 A CN115160850 A CN 115160850A CN 202210886561 A CN202210886561 A CN 202210886561A CN 115160850 A CN115160850 A CN 115160850A
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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
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to water-based ink for decorative paper and a preparation method thereof, belonging to the technical field of decorative materials and comprising the following raw materials in parts by weight: 50-55 parts of aqueous polyurethane solution, 10-15 parts of pigment, 5-8 parts of modified silicon dioxide, 1-3 parts of dispersing agent, 0.4-0.9 part of flatting agent, 0.5-1 part of defoaming agent and 50-60 parts of deionized water; the preparation steps are as follows: compared with the traditional polyurethane water-based ink, the water-based ink is prepared by adding the self-made modified silicon dioxide, wherein the modified silicon dioxide is an esterification product of pyridyl hyperbranched polyester and carboxylated silicon dioxide, so that the water resistance and wear resistance of the ink can be improved, the components of the ink can be uniform, and the performance is stable.
Description
Technical Field
The invention belongs to the technical field of decorative materials, and particularly relates to water-based ink for decorative paper and a preparation method thereof.
Background
The decorative paper mainly plays a role in providing decoration of patterns and covering for preventing bottom glue solution from seeping, generally, after decorative base paper is printed with patterns such as wood grains and stone grains through ink, a printed matter is impregnated with melamine resin or polyester resin solution and is formed into the decorative paper through hot pressing and pressing on a base material, therefore, the ink of the decorative paper is required to have good adhesive force to paper and certain high temperature resistance of an ink film, the water-based ink adopted by the conventional decorative paper at present generally adopts water-based polyurethane as a connecting material, the prepared printing ink has poor water resistance, poor printing effect, fuzzy color change when meeting water and even delamination, and therefore, the improvement of the water-based ink of the decorative paper with higher comprehensive performance is a technical problem to be solved at present.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a water-based ink for decorative paper and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the water-based ink for decorative paper comprises the following raw materials in parts by weight: 50-55 parts of aqueous polyurethane solution, 10-15 parts of pigment, 5-8 parts of modified silicon dioxide, 1-3 parts of dispersing agent, 0.4-0.9 part of flatting agent, 0.5-1 part of defoaming agent and 50-60 parts of deionized water;
the water-based ink for decorative paper is prepared by the following steps:
adding a dispersing agent into deionized water, then adding a pigment, modified silicon dioxide and a water-based polyurethane solution, stirring at a rotating speed of 250-300r/min for 20-30min, transferring into a grinding machine, grinding to a particle size of less than 10 mu m, adding a defoaming agent and a leveling agent, and uniformly mixing to obtain the water-based ink for decorative paper.
Further, the modified silica is prepared by the following steps:
step A1, adding pyridyl dibasic acid, fluorine-containing dihydric alcohol, p-toluenesulfonic acid and DMF (dimethyl formamide), heating to reflux reaction for 2-3h under the protection of nitrogen and normal pressure, then decompressing to 1.2kPa (kilopascal) and continuing to reflux reaction for 2-3h, cooling to room temperature after the reaction is finished, and decompressing and distilling to remove DMF to obtain pyridyl hyperbranched polyester, wherein the using amount ratio of the pyridyl dibasic acid to the fluorine-containing dihydric alcohol to the p-toluenesulfonic acid is 3.3-3.5g:4.6-5.1g:0.11-0.16g;
step A2, ultrasonically dispersing carboxylated silicon dioxide in DMF, adding pyridyl hyperbranched polyester and p-toluenesulfonic acid, heating to 100-120 ℃, stirring for reaction for 1-2 hours, after the reaction is finished, centrifugally separating, washing precipitates for 3-5 times by deionized water, and drying at 80 ℃ to constant weight to obtain modified silicon dioxide, wherein the mass ratio of the carboxylated silicon dioxide to the pyridyl hyperbranched polyester is 10:1.8-2.4, wherein the dosage ratio of the p-toluenesulfonic acid is 2% of the sum of the mass of the carboxylated silicon dioxide and the mass of the pyridyl hyperbranched polyester.
The preparation method comprises the steps of taking pyridyl dibasic acid and fluorine-containing dihydric alcohol as raw materials, carrying out esterification reaction to obtain hyperbranched polyester, wherein the hyperbranched polyester contains terminal hydroxyl, F-C chains, benzene rings and pyridine groups, namely the pyridyl hyperbranched polyester, then taking the pyridyl hyperbranched polyester and carboxylated silicon dioxide as raw materials, carrying out esterification reaction again, and connecting the pyridyl hyperbranched polyester on the surface of the carboxylated silicon dioxide through chemical bonds to obtain the modified silicon dioxide.
The fluorine-containing dihydric alcohol is prepared by the following steps:
adding hexafluorobutyl methacrylate, diethanolamine and absolute ethyl alcohol into a three-neck flask, heating to reflux reaction for 8-9h, cooling to room temperature, and then carrying out reduced pressure distillation to remove the ethyl alcohol to obtain the fluorine-containing dihydric alcohol, wherein the dosage ratio of the hexafluorobutyl methacrylate, the diethanolamine and the absolute ethyl alcohol is 0.01mol:0.01mol:25-30mL.
The pyridyl diacid comprises the following steps:
adding p-aminobenzoic acid and DMF (dimethyl formamide) into a three-neck flask, controlling the reaction temperature to be 15-20 ℃, adding triethylamine, stirring for 20-30min at the temperature, then dropwise adding a DMF solution of 2, 6-pyridinedicarbonyl chloride, controlling the dropwise adding speed to be 1-2 drops/second, stirring and reacting for 10-12h after the dropwise adding is finished, heating to 80 ℃, keeping the temperature and reacting for 24h, cooling to room temperature after the reaction is finished, adding deionized water for washing, performing suction filtration, and performing vacuum drying on a filter cake at 60 ℃ to constant weight to obtain pyridyl dibasic acid, wherein the dosage ratio of the DMF solution of the p-aminobenzoic acid, the DMF, the triethylamine and the 2, 6-pyridinedicarbonyl chloride is 0.2mol:130-150mL:0.21mol:100mL of a solution of 2, 6-pyridinedicarbonyl chloride in DMF was prepared from 2, 6-pyridinedicarbonyl chloride and DMF according to a molar ratio of 0.1mol:100 mL.
The carboxylated silicon dioxide is prepared by the following steps:
mixing and stirring a silane coupling agent KH-550, succinic anhydride and DMF for 3h to obtain a modified solution, ultrasonically dispersing nano-silica in DMF, adding the modified solution and deionized water, stirring for 4-5h, after stirring, performing suction filtration, repeatedly washing a filter cake with absolute ethyl alcohol and distilled water, and finally drying at 80 ℃ to constant weight to obtain carboxylated silica;
wherein the dosage ratio of KH-550, succinic anhydride and DMF in the modified liquid is 0.01mol:0.01mol:25mL, and the dosage ratio of the nano silicon dioxide, the DMF, the modified liquid and the deionized water is 10g:100-120mL:2.1-2.5mL:3-5mL, firstly, performing amidation reaction on KH-550 and succinic anhydride to obtain a silane coupling agent containing amido bonds and terminal carboxyl groups, and further performing condensation reaction on a hydrolysate of the silane coupling agent and hydroxyl groups on the surface of the nano silicon dioxide to obtain carboxylated silicon dioxide with the surface rich in carboxyl groups and amido bonds.
Furthermore, the solid content of the aqueous polyurethane solution is 30-40%.
Further, the pigment is a color pigment and titanium dioxide according to the mass ratio of 1-5: 3-4.
Further, the dispersing agent is one or more of polyvinylpyrrolidone, TEGO Disper 750W and TEGO Disper 750W which are mixed according to any proportion.
Further, the flatting agent is HX-3313 flatting agent.
Further, the defoaming agent is BYK-011 or BYK-024.
The invention has the beneficial effects that:
compared with the traditional polyurethane water-based ink, the polyurethane water-based ink prepared by the invention is added with self-made modified silicon dioxide, the modified silicon dioxide is an esterification product of pyridyl hyperbranched polyester and carboxylated silicon dioxide, namely nano silicon dioxide with pyridyl hyperbranched polymer grafted on the surface through a chemical bond, the hyperbranched polyester contains terminal hydroxyl, F-C chains, benzene rings and pyridine groups, the modified silicon dioxide is added into a polyurethane solution, the hydroxyl of the pyridyl hyperbranched polyester can participate in the crosslinking and curing reaction of polyurethane to form a transition layer in the nano silicon dioxide and polyurethane molecules, so that the interface defect is reduced, the nano silicon dioxide fully exerts the wear resistance and heat resistance, the F-C chains of the pyridyl hyperbranched polyester exist, and the low surface energy characteristic based on fluorine elements is adopted, the hydrophobic property of an ink curing film can be improved, the water resistance is further improved, the heat resistance of the ink is improved due to the introduction of rigid benzene rings, more remarkably, the pyridyl hyperbranched polyester on the surface of the modified silicon dioxide can be used as a transition layer to improve the connectivity between the silicon dioxide and an ink base material, and the wear resistance, the heat resistance and the water resistance of the ink are improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A fluorine-containing diol is prepared by the following steps:
adding 0.01mol of hexafluorobutyl methacrylate, 0.01mol of diethanolamine and 25mL of absolute ethanol into a three-neck flask, heating to reflux reaction for 8h, cooling to room temperature, and carrying out reduced pressure distillation to remove ethanol to obtain the fluorine-containing dihydric alcohol.
Example 2
A fluorine-containing diol is prepared by the following steps:
adding 0.01mol of hexafluorobutyl methacrylate, 0.01mol of diethanolamine and 30mL of absolute ethanol into a three-neck flask, heating to reflux reaction for 9h, cooling to room temperature, and carrying out reduced pressure distillation to remove ethanol to obtain the fluorine-containing dihydric alcohol.
Example 3
A pyridyl diacid, which is prepared by the following steps:
adding 0.2mol of p-aminobenzoic acid and 130mL of DMF into a three-neck flask, controlling the reaction temperature to be 15 ℃, adding 0.21mol of triethylamine, stirring for 20min at the temperature, then dropwise adding a DMF solution of 2, 6-pyridinedicarbonyl chloride, controlling the dropwise adding speed to be 1 drop/second, stirring and reacting for 10h after the dropwise adding is finished, heating to 80 ℃, keeping the temperature and reacting for 24h, cooling to room temperature after the reaction is finished, adding deionized water for washing, performing suction filtration, and performing vacuum drying on a filter cake at 60 ℃ to constant weight to obtain pyridyl dibasic acid, wherein the DMF solution of the 2, 6-pyridinedicarbonyl chloride is prepared from the 2, 6-pyridinedicarbonyl chloride and the DMF according to the mol ratio of 0.1: 100 mL.
Example 4
A pyridyl diacid, which is prepared by the following steps:
adding 0.2mol of p-aminobenzoic acid and 150mL of DMF into a three-neck flask, controlling the reaction temperature to be 20 ℃, adding 0.21mol of triethylamine, stirring for 30min at the temperature, then dropwise adding a DMF solution of 2, 6-pyridinedicarbonyl chloride, controlling the dropwise adding speed to be 2 drops/second, stirring for reacting for 12h after the dropwise adding is finished, heating to 80 ℃, keeping the temperature for reacting for 24h, cooling to room temperature after the reaction is finished, adding deionized water for washing, performing suction filtration, and performing vacuum drying on a filter cake at 60 ℃ to constant weight to obtain a pyridyl dibasic acid, wherein the DMF solution of the 2, 6-pyridinedicarbonyl chloride is prepared from the 2, 6-pyridinedicarbonyl chloride and the DMF according to the following mole ratio of 0.1: 100 mL.
Example 5
A modified silica made by the steps of:
step A1, adding 3.3g of pyridyl dibasic acid of example 3, 4.6g of fluorine-containing dihydric alcohol of example 1, 0.11g of p-toluenesulfonic acid and 80mL of DMF (dimethyl formamide) into a three-neck flask, heating to reflux reaction for 2 hours under the protection of nitrogen and normal pressure, then continuing reflux reaction for 2 hours under reduced pressure of 1.2kPa, cooling to room temperature after the reaction is finished, and removing DMF (dimethyl formamide) through reduced pressure distillation to obtain pyridyl hyperbranched polyester;
step A2, ultrasonically dispersing 10g of carboxylated silicon dioxide into 100mL of DMF (dimethyl formamide), adding 1.8g of pyridyl hyperbranched polyester and p-toluenesulfonic acid, heating to 100 ℃, stirring for reaction for 1 hour, after the reaction is finished, centrifugally separating, washing precipitates for 3 times by using deionized water, and drying at 80 ℃ to constant weight to obtain modified silicon dioxide, wherein the use ratio of the p-toluenesulfonic acid is 2% of the sum of the mass of the carboxylated silicon dioxide and the pyridyl hyperbranched polyester;
the carboxylated silicon dioxide is prepared by the following steps:
mixing and stirring 0.01mol of silane coupling agent KH-550, 0.01mol of succinic anhydride and 25mL of DMF for 3h to obtain a modified solution, ultrasonically dispersing 10g of nano-silica in 100mL of DMF, adding 2.1mL of the modified solution and 3mL of deionized water, stirring for 4h, after stirring, carrying out suction filtration, repeatedly washing a filter cake with absolute ethyl alcohol and distilled water, and finally drying at 80 ℃ to constant weight to obtain the carboxylated silica.
Example 6
A modified silica made by the steps of:
step A1, adding 3.5g of pyridyl dibasic acid of example 4, 5.1g of fluorine-containing dihydric alcohol of example 2, 0.16g of p-toluenesulfonic acid and 100mL of DMF (dimethyl formamide) into a three-neck flask, heating to reflux reaction for 3h under the protection of nitrogen and normal pressure, then continuing reflux reaction for 3h under reduced pressure of 1.2kPa, cooling to room temperature after the reaction is finished, and removing DMF (dimethyl formamide) through reduced pressure distillation to obtain pyridyl hyperbranched polyester;
step A2, ultrasonically dispersing 10g of carboxylated silicon dioxide into 120mL of DMF, adding 2.4g of pyridyl hyperbranched polyester and p-toluenesulfonic acid, heating to 120 ℃, stirring for reaction for 2 hours, after the reaction is finished, centrifugally separating, washing the precipitate for 5 times by using deionized water, and drying at 80 ℃ to constant weight to obtain modified silicon dioxide, wherein the using amount ratio of the p-toluenesulfonic acid is 2% of the sum of the mass of the carboxylated silicon dioxide and the pyridyl hyperbranched polyester;
the carboxylated silicon dioxide is prepared by the following steps:
mixing and stirring 0.01mol of silane coupling agent KH-550, 0.01mol of succinic anhydride and 25mL of DMF for 3h to obtain a modified solution, ultrasonically dispersing 10g of nano-silica in 120mL of DMF, adding 2.5mL of the modified solution and 5mL of deionized water, stirring for 5h, after stirring, carrying out suction filtration, repeatedly washing a filter cake with absolute ethyl alcohol and distilled water, and finally drying at 80 ℃ to constant weight to obtain the carboxylated silica.
Comparative example 1
The fluorine-containing dihydric alcohol in the example 5 is substituted for pentaerythritol with equal mass, and the rest of the raw materials and the preparation process are the same as the example 5.
Comparative example 2
The same materials and preparation process as in example 6 were used except that the same mass of p-aminobenzoic acid was replaced with the pyridyl dibasic acid in example 6.
Comparative example 3
A modified silica made by the steps of:
ultrasonically dispersing 10g of nano silicon dioxide in 120mL of DMF, adding 0.3g of silane coupling agent KH-550 and 5mL of deionized water, stirring for 5 hours, after stirring, carrying out suction filtration, repeatedly washing a filter cake with absolute ethyl alcohol and distilled water, and drying at 80 ℃ to constant weight to obtain the modified silicon dioxide.
Example 7
The water-based ink for decorative paper comprises the following raw materials in parts by weight: 50 parts of aqueous polyurethane solution, 10 parts of pigment, 5 parts of modified silicon dioxide in example 5, 1 part of dispersing agent, 0.4 part of flatting agent, 0.5 part of defoaming agent and 50 parts of deionized water;
the water-based ink for decorative paper is prepared by the following steps:
adding a dispersing agent into deionized water, then adding a pigment, modified silicon dioxide and a water-based polyurethane solution, stirring for 20min at a rotating speed of 250r/min, transferring into a grinding machine, grinding to a granularity of less than 10 mu m, adding a defoaming agent and a leveling agent, and uniformly mixing to obtain the water-based ink for decorative paper.
Wherein the solid content of the aqueous polyurethane solution is 30%, and the pigments are DPP254 red pigment and titanium dioxide according to the mass ratio of 1:3, the dispersant is polyvinylpyrrolidone, the flatting agent is HX-3313, and the defoaming agent is BYK-011.
Example 8
The water-based ink for decorative paper comprises the following raw materials in parts by weight: 52 parts of aqueous polyurethane solution, 13 parts of pigment, 7 parts of modified silicon dioxide in example 6, 2 parts of dispersing agent, 0.5 part of flatting agent, 0.8 part of defoaming agent and 55 parts of deionized water;
the water-based ink for decorative paper is prepared by the following steps:
adding a dispersing agent into deionized water, then adding a pigment, modified silicon dioxide and a water-based polyurethane solution, stirring for 25min at the rotation speed of 280r/min, transferring into a grinding machine, grinding to a particle size of less than 10 mu m, adding a defoaming agent and a leveling agent, and uniformly mixing to obtain the water-based ink for decorative paper.
Wherein the solid content of the aqueous polyurethane solution is 35%, and the pigment is phthalocyanine blue and titanium dioxide according to the mass ratio of 2:3, the dispersing agent is TEGO Disper 750W, the flatting agent is HX-3313, and the defoaming agent is BYK-011.
Example 9
The water-based ink for decorative paper comprises the following raw materials in parts by weight: 55 parts of aqueous polyurethane solution, 15 parts of pigment, 8 parts of modified silicon dioxide in example 5, 3 parts of dispersing agent, 0.9 part of flatting agent, 1 part of defoaming agent and 60 parts of deionized water;
the water-based ink for decorative paper is prepared by the following steps:
adding a dispersing agent into deionized water, then adding a pigment, modified silicon dioxide and a water-based polyurethane solution, stirring for 30min at the rotation speed of 300r/min, transferring into a grinding machine, grinding to a particle size of less than 10 mu m, adding a defoaming agent and a leveling agent, and uniformly mixing to obtain the water-based ink for decorative paper.
Wherein the solid content of the aqueous polyurethane solution is 40%, and the pigment is phthalocyanine green and titanium dioxide according to the mass ratio of 5:4, the dispersant is TEGO Disper 750W, the flatting agent is HX-3313, and the defoaming agent is BYK-024.
Comparative example 4
The modified silica of example 7 was substituted for the material of comparative example 1, and the remaining raw materials and preparation were the same as in example 7.
Comparative example 5
The modified silica of example 8 was substituted for the material of comparative example 2 and the remaining raw materials and preparation were the same as in example 7.
Comparative example 6
The modified silica of example 9 was substituted for the material of comparative example 3, and the remaining raw materials and preparation were the same as in example 9.
The aqueous inks prepared in examples 7 to 9 and comparative examples 4 to 6 were transferred onto the surface of base paper, dried at 100 ℃, and then tested: ink adhesion fastness was performed with reference to GB/T13217.7-2009, abrasion resistance: the wear-resistant grade is tested by referring to the standard GB/T4893.4-2013 furniture surface paint film physical and chemical property test, part 8, wear resistance testing method sand 100# (rubber grinding wheel, 1000g weight); moisture and heat resistance: standing at 65 ℃ and 96% humidity for 24h, and observing the surface state of the ink layer; storage stability: the inks of each group were stored at 25 ℃ for 6 months, observed for settling and delamination, and the test results are shown in table 1:
TABLE 1
| Item | Fastness to adhesion (%) | Wear rating | Moisture and heat resistance | Stability in storage |
| Example 7 | 95 | 4 stage | Without change | No precipitation and no delamination |
| Example 8 | 96 | Grade 5 | Without change | No precipitate, noDelamination of layers |
| Example 9 | 94 | Grade 5 | Without change | No precipitation and no delamination |
| Comparative example 4 | 90 | 4 stage | Having micro-bubbles on the surface | No precipitation and no delamination |
| Comparative example 5 | 88 | 4 stage | Without change | No precipitation, with stratification |
| Comparative example 6 | 85 | 4 stage | Having bubbles on the surface | With precipitation and demixing |
As can be seen from Table 1, the water-based inks prepared in examples 7 to 9 have high adhesion fastness, wear resistance, resistance to humidity and heat, storage stability and the like, and have a wide application prospect compared with those prepared in comparative examples 4 to 6.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (9)
1. The water-based ink for decorative paper is characterized by comprising the following raw materials in parts by weight: 50-55 parts of aqueous polyurethane solution, 10-15 parts of pigment, 5-8 parts of modified silicon dioxide, 1-3 parts of dispersing agent, 0.4-0.9 part of flatting agent, 0.5-1 part of defoaming agent and 50-60 parts of deionized water;
the modified silica is prepared by the following steps:
a1, mixing pyridyl dibasic acid, fluorine-containing dihydric alcohol, p-toluenesulfonic acid and DMF, carrying out reflux reaction for 2-3h under the condition of normal pressure under the protection of nitrogen, and continuously carrying out reflux reaction for 2-3h by reducing the pressure to 1.2kPa to obtain pyridyl hyperbranched polyester;
step A2, dispersing the carboxylated silicon dioxide in DMF (dimethyl formamide) by ultrasonic, adding pyridyl hyperbranched polyester and p-toluenesulfonic acid, and stirring at 100-120 ℃ for reaction for 1-2 hours to obtain modified silicon dioxide.
2. The water based ink for decorative paper according to claim 1, wherein the ratio of the amount of the pyridyl dibasic acid to the amount of the fluorine-containing diol to the amount of the p-toluenesulfonic acid is 3.3 to 3.5g:4.6-5.1g:0.11-0.16g.
3. The water-based ink for decorative paper, as claimed in claim 1, wherein the mass ratio of the carboxylated silica to the pyridyl hyperbranched polyester is 10:1.8-2.4, and the dosage ratio of the p-toluenesulfonic acid is 2 percent of the sum of the mass of the carboxylated silicon dioxide and the mass of the pyridyl hyperbranched polyester.
4. The water-based ink for decorative paper, according to claim 1, is characterized in that the fluorine-containing glycol is prepared by the following steps:
mixing hexafluorobutyl methacrylate, diethanolamine and absolute ethyl alcohol, and carrying out reflux reaction for 8-9h to obtain fluorine-containing dihydric alcohol, wherein the dosage ratio of the hexafluorobutyl methacrylate to the diethanolamine to the absolute ethyl alcohol is 0.01mol:0.01mol:25-30mL.
5. An aqueous ink for decorative papers as claimed in claim 1, wherein said pyridyl dibasic acid is prepared by the steps of:
mixing p-aminobenzoic acid and DMF, adding triethylamine at 15-20 ℃, dropwise adding a DMF solution of 2, 6-pyridine dicarbonyl chloride after stirring, stirring for reaction for 10-12h after dropwise adding, and keeping the temperature at 80 ℃ for reaction for 24h to obtain the pyridyl dibasic acid.
6. An aqueous ink for decorative paper according to claim 5, wherein the ratio of the amount of the DMF solution of p-aminobenzoic acid, DMF, triethylamine and 2, 6-pyridinedicarbonyl chloride is 0.2mol:130-150mL:0.21mol:100mL of a DMF solution of 2, 6-pyridinedicarbonyl chloride was prepared from 2, 6-pyridinedicarbonyl chloride and DMF in a molar ratio of 0.1mol:100 mL.
7. A water based ink for decorative papers according to claim 1, characterized in that said carboxylated silica is prepared by the following steps:
mixing and stirring a silane coupling agent KH-550, succinic anhydride and DMF to obtain a modified solution, ultrasonically dispersing nano-silica in DMF, adding the modified solution and deionized water, and stirring for 4-5h to obtain carboxylated silica.
8. The water-based ink for decorative paper of claim 7, wherein the amount ratio of KH-550, succinic anhydride and DMF in the modifying liquid is 0.01mol:0.01mol:25mL, wherein the dosage ratio of the nano silicon dioxide, the DMF, the modification solution and the deionized water is 10g:100-120mL:2.1-2.5mL:3-5mL.
9. The preparation method of the water-based ink for decorative paper, which is characterized by comprising the following steps of:
adding a dispersing agent into deionized water, adding a pigment, modified silicon dioxide and a water-based polyurethane solution, stirring, transferring to a grinding machine, grinding to a particle size of less than 10 mu m, adding a defoaming agent and a leveling agent, and uniformly mixing to obtain the water-based ink for decorative paper.
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| CN117659643A (en) * | 2023-11-28 | 2024-03-08 | 扬州君禾薄膜科技有限公司 | Polyester material resistant to wet heat aging and preparation method thereof |
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| CN117659643A (en) * | 2023-11-28 | 2024-03-08 | 扬州君禾薄膜科技有限公司 | Polyester material resistant to wet heat aging and preparation method thereof |
| CN117659643B (en) * | 2023-11-28 | 2024-05-24 | 扬州君禾薄膜科技有限公司 | Polyester material resistant to wet heat aging and preparation method thereof |
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| Publication number | Publication date |
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| CN115160850B (en) | 2023-07-21 |
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