CN111690282A - Preparation method of blue pigment for coating/ink-jet printing/nano zirconia ceramic - Google Patents
Preparation method of blue pigment for coating/ink-jet printing/nano zirconia ceramic Download PDFInfo
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- CN111690282A CN111690282A CN202010758848.6A CN202010758848A CN111690282A CN 111690282 A CN111690282 A CN 111690282A CN 202010758848 A CN202010758848 A CN 202010758848A CN 111690282 A CN111690282 A CN 111690282A
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- ink
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
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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
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
Abstract
The invention discloses a preparation method of a blue pigment for coating/ink-jet printing/nano zirconia ceramics, which comprises a preparation method of synthesizing the blue pigment by adopting a semi-liquid semi-solid phase process. The preparation method comprises the following steps: metal salts such as cobalt, aluminum and the like and alkali or alkali metal salts are simultaneously dropped into water, a nano precursor is obtained after filter pressing, washing and drying, and the blue pigment for coating/ink-jet printing/nano zirconia ceramics is obtained by uniformly mixing the precursor, rare earth compounds such as doped stability-assisting yttrium and the like, white carbon black and mineralizer according to a certain mass ratio and then calcining at 900-1000 ℃. According to the invention, through nanocrystallization of the precursor, the high-temperature crystal transformation temperature is reduced to 900-1000 ℃ from the original 1280 ℃, the materials after crystal transformation can directly reach within 2 microns without mechanical refining of D50, the integrity, high specific surface and stable chemical property of the materials are maintained, and the performance requirements in the fields of coating, ink-jet printing, zirconia ceramics and the like are met.
Description
Technical Field
The invention relates to preparation of a pigment, in particular to a preparation method of a blue pigment for coating/ink-jet printing/nano zirconia ceramics.
Background
The blue pigment is generally cobalt-aluminum blue or cobalt-silicon blue, and the solid phase method is the most commonly used method, but the method has the problems of high energy consumption, large particles, wide particle size distribution, uneven color development and the like, and the blue pigment prepared by the prior art has very high cobalt content. In 2017, the popularity of modern antique bricks makes black and white gray tones become the mainstream of development, so that the dosage of blue pigments is increased, and in addition, cobalt is used as a raw material of a positive electrode material such as lithium cobaltate and the like, so that the dosage of cobalt is increased rapidly, and finally, cobalt oxide is increased from 16 ten thousand/ton to 50 ten thousand/ton in 2017. Therefore, it is necessary to prepare a blue pigment having a strong coloring ability.
In recent years, colored zirconia ceramics have been used in the dental ceramics, jewelry and ceramic back plates for mobile phones industry. Compared with the traditional metal and plastic mobile phone back plate, the colorful ceramic back plate well avoids the interference of the metal back plate to mobile phone signals, and simultaneously, the strength, toughness, color and texture of the colorful ceramic back plate can reach the application level. At present, the cobalt-aluminum blue pigment and the cobalt-silicon blue pigment on the market have the problems of non-uniform color generation, poor color stability and the like in zirconia ceramics.
Disclosure of Invention
The invention aims to provide a preparation method of a blue pigment, which is suitable for coating/ink-jet printing/zirconia ceramics. The common synthesis method of the blue pigment is a solid phase method, the pigment synthesized by the method has large particles and wide particle size distribution, further ball milling is needed to be carried out to a nanometer level, and the problems of extremely non-uniform pigment grain size, different appearance, influence on tinting strength and the like are easily caused after ball milling. The invention adopts several commercially available blue pigments for paint/ceramic to be applied to the zirconium ceramic at the beginning, but the blue color cannot be presented in the zirconium ceramic, and the blue pigments are found to be unstable in structure through analysis, and the cobalt cannot be presented in the blue color in the zirconium ceramic. Therefore, the invention adopts a process of combining semi-solid semi-liquid, doped yttrium and other rare earth elements and compounding a small amount of chromium with silicon which has multiple functions to prepare the blue pigment with strong color development, small particles, narrow particle size distribution and strong chemical stability.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a blue pigment for coating/ink-jet printing/nano zirconia ceramics comprises the following steps:
(1) in molar ratio Co2+:Cr3+:Al3+:Zn2+= 0.7 to 1.0: (0.01-0.02): (1.4-2.0): (0.02-0.03), respectively weighing metal salts of cobalt salt, chromium salt, aluminum salt and zinc salt, and then dissolving the metal salts in water to be marked as A;
(2) weighing alkali or alkali metal salt, and dissolving in water, and marking as B;
(3) dissolving a dispersant in water to be marked as C;
(4) dripping A, B into C, stirring, and controlling pH as D;
(5) after dripping, washing D with water until no ions are washed out;
(6) drying at 100-150 ℃ and marking as E;
(7) adding a rare earth compound, a mineralizer and a silica material, and crushing the mixture to pass through a sieve of 100-1000 meshes, wherein the mark is F;
(8) and putting the F into a crucible at 900-1000 ℃, calcining for 60-120 minutes, washing with water, drying, and then crushing with air flow to obtain the blue pigment for the coating/ink-jet printing/nano zirconia ceramic, which is marked as G.
Further, the metal salt in the step (1) is chloride, nitrate or sulfate corresponding to metal ions.
Further, the alkali or alkali metal salt in the step (2) is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium carbonate hydroxide, and the molar ratio of the alkali or alkali metal salt to the metal salt is 1.1-1.3: 1.
Further, the dispersant in the step (3) is polyethylene glycol-1000, polyethylene glycol-2000 or sodium dodecyl benzene sulfonate, and the dosage of the dispersant is 0.05-0.2% of the total mass of the metal salt.
Further, the pH value in the step (4) is preferably 6-9.
Further, in the step (7), the silica is white carbon black or silicon micro powder, the mesh number of the white carbon black and the silicon micro powder is required to be more than 1000 meshes, and the using amount of the silica is 2-5% of the mass of the E.
Further, in the step (7), the mineralizing agent is one or more than two of boric acid, borax, diammonium hydrogen phosphate or sodium hexafluoroaluminate, and the using amount of the mineralizing agent is 0.5-2% of the mass of the E.
Further, in the step (7), the rare earth compound is one or more of yttrium and neodymium, has a high specific surface area, and is used in an amount of 0.1-1% of the mass of E.
Compared with the prior art, the invention has the following advantages:
the invention adopts a technique of combining semi-solid semi-liquid, rare earth elements such as yttrium and the like and a small amount of chromium compounded with silicon and having multiple functions to prepare the blue pigment, and the obtained pigment has the advantages of strong color development, small particles, narrow particle size distribution, strong chemical stability and the like, and can generate color in a coating/ink-jet printing matrix and can generate color stably in zirconia ceramics.
Drawings
FIG. 1 is a block diagram of the process of the present invention.
Detailed Description
The present invention will be further described with reference to specific examples, but the embodiments of the present invention are not limited thereto, and the process parameters not specifically described may be performed by referring to the conventional techniques.
Example 1
A preparation method of a blue pigment for coating/ink-jet printing/nano zirconia ceramics comprises the following steps:
(1) 5.75g of CrCl was taken3 .6H2O，237.5g CoCl2 .6H2O，502.5g AlCl3 .6H2O，4.2gZnCl2Dissolving in 5000mL of water to obtain solution A; 250 g of Na2CO3Dissolving in 5000mL of water to obtain solution B; 0.5g of polyethylene glycol-1000 is dissolved in 2000mL of water to obtain C; dropping A and B into C, keeping pH at 8 to obtain solution D, stirring for 1 hr, washing with water until D has no ion, oven drying at 120 deg.C, and pulverizing to obtain powder E with 200 mesh; 0.5 wt% of yttrium and neodymium rare earth compounds, 1 wt% of borax, 2.5 w% of white carbon black and E are uniformly mixed and put into a crucible, calcined for 120 minutes at 900 ℃, washed by water and crushed by air flow.
Example 2
5.75g of CrCl was taken3 .6H2O，237.5g CoCl2 .6H2O，502.5g AlCl3 .6H2O，4.2gZnCl2Dissolved in 5000mL of water to obtain A1Liquid; 250 g of Na2CO3Dissolved in 5000mL of water to form B1Liquid; 0.5g of polyethylene glycol-1000 dissolved in 2000mL of water is C1(ii) a A is to be1And B1Co-dropping in C to maintain pH at 8 to obtain D1Stirring for 1 hr, washing with water to D1Until no ion is washed out, drying at 120 deg.C, pulverizing, and sieving with 200 mesh sieve E1(ii) a 0.5 wt% of yttrium and neodymium rare earth compounds, 1 wt% of borax, 2.5 w% of white carbon black and E1Mixing, loading in crucible, calcining at 1000 deg.C for 60 min, washing with water and jet pulverizing.
Example 3
5.75g of CrCl was taken3 .6H2O，237.5g CoCl2 .6H2O，502.5g AlCl3 .6H2O，4.2gZnCl2Dissolved in 5000mL of water to obtain A2Liquid; 250 g of Na2CO3Dissolved in 5000mL of water to form B2Liquid; 0.5g of polyethylene glycol-1000 dissolved in 2000mL of water is C2(ii) a A is to be2And B2Co-dropping in C to maintain pH at 8 to obtain D2Stirring for 1 hr, washing with water to D2Until no ion is washed out, drying at 120 deg.C, pulverizing, and sieving with 200 mesh sieve E2(ii) a 2.5 w% of white carbon black and E2Mixing, loading in crucible, calcining at 1000 deg.C for 60 min, washing with water and jet pulverizing.
Example 4
5.75g of CrCl was taken3 .6H2O，237.5g CoCl2 .6H2O，502.5g AlCl3 .6H2O，4.2gZnCl2Dissolved in 5000mL of water to obtain A3Liquid; 250 g of Na2CO3Dissolved in 5000mL of water to form B3Liquid; 0.5g of polyethylene glycol-1000 dissolved in 2000mL of water is C3(ii) a A is to be3And B3Is dropped on C3Maintaining the pH at 8 to obtain D3Stirring for 1 hr, washing with water to D3Until no ion is washed out, drying at 120 deg.C, pulverizing, and sieving with 200 mesh sieve E3(ii) a 0.5 wt% of yttrium and neodymium rare earth compounds, 2 wt% of borax, 2.5 w% of white carbon black and E3Mixing, loading in crucible, calcining at 900 deg.C for 120 min, washing with water and jet pulverizing.
Example 5
Taking 5.8g Cr (NO)3)3 .9H2O，200g Co(NO3)2 .6H2O，538g Al(NO3)3 .9H2O，6.4g Zn(NO3)2 .6H2Dissolving O in 5000mL of water to obtain A4Liquid; 94 g of NaOH dissolved in 5000mL of water is B4Liquid; 0.5g polyethylene glycol-2000 dissolved in 2000mL water is C4(ii) a Dropping A and B together on C4Maintaining the pH at 8 to obtain D4Stirring for 1 hr, washing with water to D4Until no ion is washed out, drying at 120 deg.C, pulverizing, and sieving with 200 mesh sieve E4(ii) a 0.5 wt% of yttrium and neodymium rare earth compounds, 1 wt% of boric acid, 2.5 w% of white carbon black and E4Mixing, loading in crucible, calcining at 1000 deg.C for 60 min, washing with water and jet pulverizing.
Example 6
Taking 6.3g Cr (NO)3)3 .9H2O，208.3g CoSO4 .7H2O，527g Al2(SO4)3，3.7g ZnSO4Dissolved in 5000mL of water to obtain A5Liquid; 197.4 g NaHCO3Dissolved in 5000mL of water to form B5Liquid; 0.5g sodium dodecylbenzenesulfonate dissolved in 2000mL water is C5(ii) a A is to be5And B5Is dropped on C5Maintaining the pH at 8 to obtain D5Stirring for 1 hr, washing with water to D5Washing until no ion is eluted, oven drying at 120 deg.C, and pulverizingSieving with 200 mesh sieve to obtain E5(ii) a 0.5 wt% of yttrium and neodymium rare earth compounds, 1 wt% of sodium hexafluoroaluminate, 2.5 w% of white carbon black and E5Mixing, loading in crucible, calcining at 1000 deg.C for 60 min, washing with water and jet pulverizing.
Claims (8)
1. A preparation method of a blue pigment for coating/ink-jet printing/nano zirconia ceramics is characterized by comprising the following steps:
(1) in molar ratio Co2+:Cr3+:Al3+:Zn2+= 0.7 to 1.0: (0.01-0.02): (1.4-2.0): (0.02-0.03), respectively weighing metal salts of cobalt salt, chromium salt, aluminum salt and zinc salt, and then dissolving the metal salts in water to be marked as A;
(2) weighing alkali or alkali metal salt, and dissolving in water, and marking as B;
(3) dissolving a dispersant in water to be marked as C;
(4) dripping A, B into C, stirring, and controlling pH as D;
(5) after dripping, washing D with water until no ions are washed out;
(6) drying at 100-150 ℃ and marking as E;
adding a rare earth compound, a mineralizer and a silica material, and crushing the mixture to pass through a sieve of 100-1000 meshes, wherein the mark is F;
(8) and putting the F into a crucible at 900-1000 ℃, calcining for 60-120 minutes, washing with water, drying, and then crushing with air flow to obtain the blue pigment for the coating/ink-jet printing/nano zirconia ceramic, which is marked as G.
2. The method for preparing the blue pigment for coating/ink-jet printing/nano zirconia ceramics according to claim 1, wherein the metal salt in the step (1) is chloride, nitrate or sulfate corresponding to metal ions.
3. The preparation method of the blue pigment for coating/ink-jet printing/nano zirconia ceramics according to claim 1, characterized in that the alkali or alkali metal salt in the step (2) is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium carbonate hydroxide, and the molar ratio of the alkali or alkali metal salt to the metal salt is 1.1-1.3: 1.
4. The method for preparing the blue pigment for coating/ink-jet printing/nano zirconia ceramics according to claim 1, wherein the dispersant in the step (3) is polyethylene glycol-1000, polyethylene glycol-2000 or sodium dodecyl benzene sulfonate, and the dosage of the dispersant is 0.05-0.2% of the total mass of the metal salt.
5. The method for preparing the blue pigment for coating/ink-jet printing/nano zirconia ceramics according to claim 1, wherein the pH in the step (4) is 6 to 9.
6. The preparation method of the blue pigment for the coating/ink-jet printing/nano zirconia ceramic according to claim 1, wherein the silica in the step (7) is white carbon black or silica powder, the mesh number of the white carbon black and the silica powder is more than 1000 meshes, and the usage amount of the blue pigment is 2-5% of the mass E.
7. The method for preparing the blue pigment for the coating/ink-jet printing/nano zirconia ceramic according to claim 1, wherein the mineralizing agent in the step (7) is one or more of boric acid, borax, diammonium hydrogen phosphate or sodium hexafluoroaluminate, and the amount of the mineralizing agent is 0.5 to 2 percent of the mass E.
8. The preparation method of the blue pigment for coating/ink-jet printing/nano zirconia ceramic according to claim 1, wherein the rare earth compound in the step (7) is one or more of yttrium and neodymium, has a high specific surface area, and is used in an amount of 0.1-1% of the mass of E.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113105755A (en) * | 2021-04-06 | 2021-07-13 | 包头中科世纪科技有限责任公司 | Novel inorganic blue pigment of rare earth oxide doped indium and transition metal oxide and preparation method thereof |
| CN113800905A (en) * | 2021-09-30 | 2021-12-17 | 江西金环颜料有限公司 | Preparation method of black pigment for nano zirconia ceramic |
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| CN105838110A (en) * | 2016-03-31 | 2016-08-10 | 江西金环颜料有限公司 | Preparation method for high-temperature black ceramic pigment used for laser 3D printing |
| CN110204926A (en) * | 2019-06-14 | 2019-09-06 | 佛山市华意陶瓷颜料有限公司 | A kind of Vanadium zirconium blue ceramic pigment, Vanadium zirconium blue ceramic ink and preparation method thereof |
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| CN113105755A (en) * | 2021-04-06 | 2021-07-13 | 包头中科世纪科技有限责任公司 | Novel inorganic blue pigment of rare earth oxide doped indium and transition metal oxide and preparation method thereof |
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