CN115304405B - Boehmite digital glaze ink and preparation method thereof - Google Patents
Boehmite digital glaze ink and preparation method thereof Download PDFInfo
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- CN115304405B CN115304405B CN202210905152.0A CN202210905152A CN115304405B CN 115304405 B CN115304405 B CN 115304405B CN 202210905152 A CN202210905152 A CN 202210905152A CN 115304405 B CN115304405 B CN 115304405B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses boehmite digital glaze ink and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Mixing a soluble aluminum salt solution, an alkali liquor, a niobium diselenide dispersion liquid and a surfactant under a stirring state, and performing a hydrothermal reaction to obtain a finished product slurry; (2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material; (3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder; (4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent, and grinding to obtain the boehmite digital glaze ink, wherein the boehmite digital glaze ink prepared by the method has full color development on the glaze surface formed after digital glaze spraying printing, and has high wear resistance.
Description
Technical Field
The invention belongs to the technical field of ceramic glaze, and particularly relates to boehmite digital glaze ink and a preparation method thereof.
Background
With the progress of ceramic digital glaze spraying technology and the popularization of products such as ceramic large plates, thin plates, rock plates and the like, the novel digital glaze spraying technology gradually replaces the traditional glaze spraying technology such as glaze spraying, glaze spraying and the like. The digital glaze spraying process can reduce the consumption of the glaze, meet the use requirement of the high-precision glaze surface, and highly cater to the market trend of large-sized ceramic tiles. Firstly, the glazing can be little and even. And secondly, digital printing, namely, accurately positioning printing according to the designed pattern, wherein the pattern can be different from one piece to another. Third, printing can be stacked, mold effects can be achieved, and the mold can be different from piece to piece, which is also not possible with conventional molds.
The boehmite digital glaze ink is a digital glaze ink commonly used in a digital glaze spraying process, and is mainly prepared by mixing boehmite powder serving as a raw material with a solvent, but the boehmite digital glaze ink prepared by the existing preparation process has poor color development of a glaze surface formed after digital glaze spraying printing and also has poor wear resistance.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the boehmite digital glaze ink and the preparation method thereof, and the boehmite digital glaze ink prepared by the preparation method has full color on the glaze surface formed after digital glaze spraying printing and has stronger wear resistance.
The technical aim of the invention is realized by the following technical scheme:
a preparation method of boehmite digital glaze ink comprises the following steps:
(1) Mixing a soluble aluminum salt solution, an alkali liquor, a niobium diselenide dispersion liquid and a surfactant under a stirring state, and performing a hydrothermal reaction to obtain a finished product slurry;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder;
(4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent and grinding to obtain the boehmite digital glaze ink.
Preferably, in the step (1), the temperature of the hydrothermal reaction is 100-150 ℃ and the reaction time is 10-15h.
Preferably, in step (1), the surfactant is at least one of polyethylene oxide or cetyltrimethylammonium bromide.
Preferably, in the step (1), the solid-to-liquid ratio g/mL of the surfactant to the soluble aluminum salt solution is (0.3-1): 100.
Preferably, in step (1), the soluble aluminum salt in the soluble aluminum salt solution is at least one of aluminum sulfate and aluminum chloride.
Preferably, in the step (1), the alkali solution is at least one of sodium hydroxide and potassium hydroxide.
Preferably, in the step (1), the concentration of aluminum ions in the soluble aluminum salt solution is 0.5-0.8mol/L, and the concentration of hydroxyl ions in the alkali liquor is 2.5-3mol/L.
Preferably, in the step (1), the volume ratio of the soluble aluminum salt solution to the alkali liquor is 1: (4-10).
Preferably, in step (1), the solid content of the niobium diselenide dispersion is 1% -3%, and the volume ratio of the niobium diselenide dispersion to the soluble aluminum salt solution is (0.1-0.5): 1.
Preferably, in the step (1), the niobium diselenide dispersion liquid is obtained by dispersing niobium diselenide in a dispersion liquid.
Preferably, in the step (1), the dispersion liquid is PVP solution with the mass concentration of 1.5% -3%.
Preferably, in the step (2), the drying temperature is 70-100 ℃ and the drying time is 2-5h.
Preferably, in the step (3), the heat treatment refers to treating the finished solid material at 450-550 ℃ for 3-6 hours.
Preferably, in step (3), the boehmite powder has a D90 value of less than 20 micrometers.
Preferably, in the step (4), the solvent includes white mineral oil, isooctyl laurate and a functional auxiliary agent.
A boehmite digital glaze ink is characterized in that: prepared by the preparation method.
The beneficial effects of the invention are as follows:
according to the preparation method of the boehmite digital glaze ink, the niobium diselenide dispersion liquid is added into the preparation raw materials, so that the niobium diselenide dispersion liquid is inserted into boehmite crystals in the process of generating boehmite crystals through hydrothermal reaction, and atomic-level mixing is formed, so that boehmite powder can be modified, and finally prepared boehmite digital glaze ink is full in color development of glaze after digital glaze spraying printing, and meanwhile, the boehmite digital glaze ink has high wear resistance.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1:
a preparation method of boehmite digital glaze ink is characterized by comprising the following steps: the method comprises the following steps:
(1) Under the stirring state, mixing an aluminum chloride solution, a sodium hydroxide solution, a niobium diselenide dispersion liquid and polyethylene oxide, and then carrying out hydrothermal reaction to obtain a finished product slurry, wherein the temperature of the hydrothermal reaction is 100 ℃, the reaction time is 15h, the solid-to-liquid ratio g/mL of the polyethylene oxide and the sodium hydroxide solution is 0.3:100, the concentration of aluminum ions in the aluminum chloride solution is 0.5mol/L, the concentration of hydroxyl ions in the sodium hydroxide solution is 2.5mol/L, and the volume ratio of the aluminum chloride solution to the sodium hydroxide solution is 1:4, the solid content of the niobium diselenide dispersion liquid is 1%, and the volume ratio of the niobium diselenide dispersion liquid to the aluminum chloride solution is 0.1:1; the niobium diselenide dispersion liquid is obtained by dispersing niobium diselenide into PVP solution with the concentration of 1.5 percent;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material, wherein the drying temperature is 70 ℃ and the drying time is 5 hours;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder, wherein the heat treatment means that the finished product solid material is treated for 6 hours at 450 ℃, and the D90 value of the obtained boehmite powder is smaller than 20 microns;
(4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent, and grinding to obtain the boehmite digital glaze ink, wherein the solvent comprises 20 parts of mineral oil, 20 parts of isopropyl laurate, 3 parts of Shanghai tri-n CH6 and 0.01 part of BYK-055, and the solid-liquid ratio g/mL of the boehmite powder to the solvent is 4:6.
The boehmite digital glaze ink is prepared by the preparation method.
Example 2:
a preparation method of boehmite digital glaze ink is characterized by comprising the following steps: the method comprises the following steps:
(1) Under the stirring state, mixing an aluminum chloride solution, a sodium hydroxide solution, a niobium diselenide dispersion liquid and hexadecyl trimethyl ammonium bromide, and performing a hydrothermal reaction to obtain a finished product slurry, wherein the temperature of the hydrothermal reaction is 150 ℃, the reaction time is 10 hours, the solid-to-liquid ratio g/mL of the hexadecyl trimethyl ammonium bromide and the sodium hydroxide solution is 1:100, the concentration of aluminum ions in the aluminum chloride solution is 0.8mol/L, the concentration of hydroxide ions in the sodium hydroxide solution is 3mol/L, and the volume ratio of the aluminum chloride solution to the sodium hydroxide solution is 1:10, the solid content of the niobium diselenide dispersion liquid is 3%, and the volume ratio of the niobium diselenide dispersion liquid to the aluminum chloride solution is 0.5:1; the niobium diselenide dispersion liquid is obtained by dispersing niobium diselenide into PVP solution with the concentration of 3 percent;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material, wherein the drying temperature is 100 ℃ and the drying time is 2 hours;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder, wherein the heat treatment means that the finished product solid material is treated for 3 hours at 550 ℃, and the D90 value of the obtained boehmite powder is smaller than 20 microns;
(4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent, and grinding to obtain the boehmite digital glaze ink, wherein the solvent comprises 20 parts of mineral oil, 20 parts of isopropyl laurate, 3 parts of Shanghai tri-n CH6 and 0.01 part of BYK-055, and the solid-liquid ratio g/mL of the boehmite powder to the solvent is 4:6.
The boehmite digital glaze ink is prepared by the preparation method.
Example 3:
a preparation method of boehmite digital glaze ink is characterized by comprising the following steps: the method comprises the following steps:
(1) Under the stirring state, mixing an aluminum chloride solution, a sodium hydroxide solution, a niobium diselenide dispersion liquid and polyethylene oxide, and then carrying out hydrothermal reaction to obtain a finished product slurry, wherein the temperature of the hydrothermal reaction is 120 ℃, the reaction time is 12h, the solid-to-liquid ratio g/mL of the polyethylene oxide and the sodium hydroxide solution is 0.5:100, the concentration of aluminum ions in the aluminum chloride solution is 0.6mol/L, the concentration of hydroxyl ions in the sodium hydroxide solution is 2.8mol/L, and the volume ratio of the aluminum chloride solution to the sodium hydroxide solution is 1:6, the solid content of the niobium diselenide dispersion liquid is 2%, and the volume ratio of the niobium diselenide dispersion liquid to the aluminum chloride solution is 0.3:1; the niobium diselenide dispersion liquid is obtained by dispersing niobium diselenide into PVP solution with the concentration of 2 percent;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material, wherein the drying temperature is 90 ℃ and the drying time is 3 hours;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder, wherein the heat treatment means that the finished product solid material is treated for 5 hours at 500 ℃, and the D90 value of the obtained boehmite powder is smaller than 20 microns;
(4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent, and grinding to obtain the boehmite digital glaze ink, wherein the solvent comprises 20 parts of mineral oil, 20 parts of isopropyl laurate, 3 parts of Shanghai tri-n CH6 and 0.01 part of BYK-055, and the solid-liquid ratio g/mL of the boehmite powder to the solvent is 4:6.
The boehmite digital glaze ink is prepared by the preparation method.
Comparative example 1: (in comparison with example 3, no niobium diselenide dispersion was added in the hydrothermal reaction step)
A preparation method of boehmite digital glaze ink is characterized by comprising the following steps: the method comprises the following steps:
(1) Under the stirring state, mixing an aluminum chloride solution, a sodium hydroxide solution and polyethylene oxide, and then carrying out hydrothermal reaction to obtain a finished product slurry, wherein the temperature of the hydrothermal reaction is 120 ℃, the reaction time is 12 hours, the solid-to-liquid ratio g/mL of the polyethylene oxide and the sodium hydroxide solution is 0.5:100, the concentration of aluminum ions in the aluminum chloride solution is 0.6mol/L, the concentration of hydroxyl ions in the sodium hydroxide solution is 2.8mol/L, and the volume ratio of the aluminum chloride solution to the sodium hydroxide solution is 1:6, preparing a base material;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material, wherein the drying temperature is 90 ℃ and the drying time is 3 hours;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder, wherein the heat treatment means that the finished product solid material is treated for 5 hours at 500 ℃, and the D90 value of the obtained boehmite powder is smaller than 20 microns;
(4) And (3) mixing the boehmite powder obtained in the step (3) with a solvent, and grinding to obtain the boehmite digital glaze ink, wherein the solvent comprises 20 parts of mineral oil, 20 parts of isopropyl laurate, 3 parts of Shanghai tri-n CH6 and 0.01 part of BYK-055, and the solid-liquid ratio g/mL of the boehmite powder to the solvent is 4:6.
The boehmite digital glaze ink is prepared by the preparation method.
Test example:
the boehmite digital glaze ink of the examples 1-3 and the comparative example 1 is printed on a ceramic substrate in an inkjet way and then fired to obtain a glaze with the glazing amount of 35g/m 2 Then, respectively performing performance test on the glaze, wherein the test standard is referred to national standard (GB/T3810.7-2006) in the seventh part of the ceramic tile test method: measurement of the abrasion resistance of glazed brick surfaces. The test results are shown in Table 1.
Table 1: glazing Performance test results
As can be seen from Table 1, the boehmite digital glaze ink prepared by the preparation method of the boehmite digital glaze ink provided by the invention can effectively enhance the wear resistance and color development of the glaze, the wear resistance level of the boehmite digital glaze ink reaches more than 3 levels, and meanwhile, the transmittance or the penetration color development can be excellent and the color development of the glaze is full.
In addition, as is clear from comparative example 3 and comparative example 1, the absence of the niobium diselenide dispersion in the hydrothermal reaction step results in poor color development of the final glaze and also poor abrasion resistance (grade 1 only) without changing other conditions.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (7)
1. A preparation method of boehmite digital glaze ink is characterized by comprising the following steps: the method comprises the following steps:
(1) Mixing a soluble aluminum salt solution, an alkali liquor, a niobium diselenide dispersion liquid and a surfactant under a stirring state, and performing a hydrothermal reaction to obtain a finished product slurry;
(2) Washing the finished product slurry obtained in the step (1), and drying to obtain a finished product solid material;
(3) Carrying out heat treatment on the finished product solid material obtained in the step (2), and grinding to obtain boehmite powder;
(4) Mixing the boehmite powder obtained in the step (3) with a solvent and grinding to obtain the boehmite digital glaze ink;
in the step (1), the temperature of the hydrothermal reaction is 100-150 ℃, the reaction time is 10-15h, and the volume ratio of the soluble aluminum salt solution to the alkali liquor is 1: (4-10) the solid content of the niobium diselenide dispersion liquid is 1-3%, and the volume ratio of the niobium diselenide dispersion liquid to the soluble aluminum salt solution is (0.1-0.5): 1.
2. The method for preparing the boehmite digital glaze ink according to claim 1, which is characterized in that: in the step (1), the surfactant is at least one of polyethylene oxide or cetyltrimethylammonium bromide.
3. The method for preparing the boehmite digital glaze ink according to claim 1, which is characterized in that: in the step (1), the concentration of aluminum ions in the soluble aluminum salt solution is 0.5-0.8mol/L, and the concentration of hydroxyl ions in the alkali liquor is 2.5-3mol/L.
4. The method for preparing the boehmite digital glaze ink according to claim 1, which is characterized in that: in the step (2), the drying temperature is 70-100 ℃ and the drying time is 2-5h.
5. The method for preparing the boehmite digital glaze ink according to claim 1, which is characterized in that: in the step (3), the heat treatment refers to treating the finished solid material for 3-6 hours at 450-550 ℃.
6. The method for preparing the boehmite digital glaze ink according to claim 1, which is characterized in that: in the step (4), the solvent comprises white mineral oil, isooctyl laurate and a functional auxiliary agent.
7. A boehmite digital glaze ink is characterized in that: is prepared by the preparation method according to any one of claims 1 to 6.
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2022
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