CN115895340A - Production method of small-particle-size coated ceramic ink material - Google Patents
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Abstract
A production method of a small-particle-size coated ceramic ink material comprises the following steps of: s1: siO 2 And (3) construction of a wrapping layer: in alkaline solution, forming a uniform coating layer on the surface of the dispersed nano-scale pigment by using tetraethoxysilane, and drying to obtain porous SiO coated on the surface 2 The colorant particles of (a); s2 ZrSiO 4 And (3) construction of a wrapping layer: porous SiO of aqueous solutions of zirconium salts containing mineralizers 2 The coating pigment particles react at high temperature to form uniform ZrSiO 4 A coated colorant particle; s3, post-treatment of the wrapping type pigment: according to the property of the pigment, removing a small amount of incompletely-wrapped pigment powder through oxygen-enriched low-temperature roasting or acid washing, and mixing with a proper dispersant and buffer salt to disperse in a water-based or organic solvent to form a small-particle-size wrapped ceramic ink product. The invention can effectively improve the wrapped potteryThe coating rate of the ceramic ink material and the particle size control requirement of the ink-jet printed product avoid material loss caused by crushing and acid washing processes, and further greatly improve the yield of the coated ceramic ink product.
Description
Technical Field
The invention relates to the technical field of ceramic ink, in particular to a production method of a small-particle-size coated ceramic ink material.
Background
The encapsulated ceramic ink material is usually prepared by mixing medium-high temperatureIncorporation of a colorant unstable under conditions into ZrSiO having excellent physicochemical properties 4 And in the inclusion body, the inclusion type inorganic pigment greatly improves the thermal stability and the acid and alkali resistance of the material. Wherein zirconium silicate is coated with cadmium sulfoselenide scarlet pigment (CdS) x Se 1-x @ZrSiO 4 Also known as cadmium red) is the only bright red hue high temperature colorant that has been produced and used at present. The traditional pigment is generally refined after being calcined, and the particles with the particle size of 5-45 mu m generally account for more than 90 percent of the total number of the particles. The novel ink-jet printing equipment has higher requirements on inorganic pigments in ceramic ink: the particle size is less than 1.0 μm, preferably 300-600nm, and larger particles are not favorable for fine pattern and text presentation and can cause filter and nozzle clogging.
Due to ZrSiO 4 The formation conditions of the wrapping layer are relatively harsh, with SiO 2 And ZrO 2 Is used as raw material to form ZrSiO through solid phase reaction 4 The temperature of (2) is usually above 1500 ℃, and the synthesis temperature can be reduced to 600-1000 ℃ by replacing synthesis raw materials or adding mineralizer. ZrSiO can be obtained even though it has been reported that ZrSiO can be obtained by a low temperature hydrothermal reaction (150-250 ℃) and a prolonged synthesis time (24-48 h) 4 However, due to the migration of the silicon source and the slow directional growth of zirconium silicate under hydrothermal conditions, the separation of zirconium silicate from the pigment is likely to occur, and it is difficult to achieve complete and compact wrapping of the pigment. Therefore, the mixed powder or the dried gel is roasted at a high temperature of 700-1100 ℃, and the powdery material is subjected to coarse crushing and fine crushing from top to bottom to obtain a nearly compact massive sintered pigment due to high-temperature agglomeration and sintering, and finally the pigment exposed on the particle surface due to crushing is removed by strong acid cleaning, so that the method is a common method in the field. Usually, less than 10% of the fed pigment exists in the final product, which not only seriously affects the color generation effect of the pigment, but also causes a great deal of waste of raw materials and causes environmental pollution.
Therefore, it is necessary to design a method for producing small-particle-size coated ceramic ink materials, so as to avoid the problems of low coating rate and low product yield of the coated ceramic ink materials caused by the traditional crushing and pickling process.
Disclosure of Invention
The invention provides a production method of a small-particle-size coated ceramic ink material, which effectively avoids ZrSiO in the traditional process scheme by adopting a step-by-step coating and dispersed suspension high-temperature fluidization treatment technology 4 The coating layer is agglomerated and sintered at a high temperature, so that the coating rate of the coated ceramic ink and the particle size control requirement of the ink-jet printed product can be effectively improved, the material loss caused by crushing and acid washing procedures is avoided, the yield of the coated ceramic ink product is greatly improved, and good social, environmental and economic benefits are realized.
The invention provides a production method of a small-particle-size coated ceramic ink material, which comprises the following steps of:
S1：SiO 2 packaging layer construction (pigment pretreatment):
s1.1, dispersing a nano pigment and a surfactant in an alcohol solution, uniformly stirring, and adjusting the pH of the solution to 10-11 to obtain a solution A;
s1.2, preparing an alcoholic solution of TEOS, and adjusting the pH of the solution to 11-12 to obtain a solution B;
s1.3, injecting the solution B into the solution A for multiple times, performing hydrolytic condensation to generate precipitates, and separating and cleaning the precipitates to obtain slurry C;
s1.4, drying the slurry C to obtain the surface-coated porous SiO 2 The pigment particles of (1) are powder D;
S2：ZrSiO 4 and (3) packaging layer construction:
s2.1, adding a complexing agent and a mineralizing agent into a zirconium salt aqueous solution, uniformly stirring, and adjusting the pH of the solution to 8-10 to obtain an E solution;
s2.2, adding the powder D into the solution E according to the volume solid content of 15-30%, and uniformly stirring to obtain slurry F;
s2.3, carrying out high-temperature thermal decomposition spray drying on the slurry F, cooling and screening to obtain ZrSiO 4 The coated pigment particles are powder G;
s3: and (3) post-treatment of the wrapping type pigment:
s3.1, removing incompletely-wrapped pigment powder from the powder G by oxygen-enriched low-temperature roasting or acid washing, and then washing, filtering and drying to obtain ceramic ink powder H;
s3.2, mixing the powder H with an aqueous or organic solvent, and adding a dispersing agent and buffer salts to obtain the small-particle-size coated ceramic ink material product.
Preferably, the pH of the solution in step S1.1, step S1.2 and step S2.1 is adjusted by ammonia water with a concentration of 4-12wt%.
Preferably, in step S1.1, the colorant is CdS or CdS x Se 1-x 、Fe 2 O 3 Or modified carbon black, alcohol is ethanol, ethylene glycol or isopropanol, and surfactant is CTAB or PVP.
Preferably, the modified carbon black pigment is obtained by taking natural gas or high aromatic hydrocarbon oil as a raw material, performing incomplete combustion or pyrolysis, and performing surface hydrophilic modification treatment by at least one strong oxidant selected from concentrated nitric acid, potassium permanganate, concentrated sulfuric acid or hydrogen peroxide under a heating condition.
Preferably, in step S3.1, the powder G obtained by producing the modified carbon black pigment is subjected to oxygen-rich low-temperature roasting to remove incompletely-wrapped pigment powder, and the pigment powder G which is easily dissolved in acid is subjected to acid washing to remove incompletely-wrapped pigment powder.
Preferably, the volume ratio of alcohol to water in the alcoholic solution of step S1.1 is 0.2-2; the mass ratio of the nano pigment to the surfactant in the step S1.1 is 0.6-1.4; the volume ratio of alcohol to TEOS in the TEOS alcohol solution of the step S1.2 is 2-6.
Preferably, in step S1.3, solution B is injected into solution a in multiple portions, each at intervals of 4-8h.
Preferably, spray drying is performed on the slurry C in step S1.4 at the temperature of 300-350 ℃; the temperature of the high-temperature pyrolysis spray drying in step S2.3 is 700-900 ℃.
Preferably, in step S2.1, in the aqueous solution of zirconium salt, the concentration of zirconium salt is 2wt% to 10wt%, the concentration of complexing agent is 3wt% to 10wt%, and the concentration of mineralizer is 0.3wt% to 1wt%; wherein the complexing agent is citric acid, diethanolamine or phytic acid; the mineralizer is NaF or CaF 2 Or LiF; the zirconium salt is Zr (OCl) 2 ·8H 2 O or ZrCl 4 。
Preferably, in step S3.2, the dispersing agent is polyvinylpyrrolidone, polyvinyl butyral, polyethylene glycol, sodium tripolyphosphate or sodium carboxymethyl cellulose; the buffer salt is carbonate/bicarbonate, sodium monohydrogen phosphate/dihydrogen phosphate or monohydrogen phosphate/dihydrogen phosphate.
Compared with the prior art, the invention has the following beneficial effects: the method effectively avoids ZrSiO in the traditional process scheme by adopting the step-by-step wrapping and dispersed suspension high-temperature fluidization treatment technology 4 The coating layer is agglomerated and sintered under the high-temperature condition, so that the general method of random coating and sintering-crushing is fundamentally changed, and the coating type ceramic ink material is a novel process design and production method for the coating type ceramic ink material; the coating rate of the coating type ceramic ink and the particle size control requirement of the ink-jet printed product can be effectively improved, the material loss caused by crushing and acid washing procedures is avoided, and the yield of the coating type ceramic ink product is greatly improved; can realize good social, environmental and economic benefits.
Drawings
FIG. 1 is an SEM image of a ceramic color obtained by the method for producing a small-particle-size-encapsulated ceramic ink material in example 1 of the present invention.
Detailed Description
Example 1
Preparing the heterocrystal coated CdS ceramic ink:
the method specifically comprises the following steps:
1. dispersing 100g CdS with the particle size range of 100-300nm in 5L ethanol solution (the ratio of alcohol to water is 1,v/v), adding 80g CTAB, ultrasonically dispersing and uniformly stirring, and adjusting the pH value of the solution to 11 by 6wt% ammonia water to obtain a color material mixed solution;
then dissolving 1L TEOS in 4L ethanol, and adjusting the pH of the solution to 12 by 10wt% ammonia water to obtain TEOS alcoholic solution;
and injecting the TEOS alcohol solution into the pigment mixed solution by a metering pump for 40min every time, wherein the feeding interval is 4h. And aging the mixed solution for 12h, then centrifugally separating a precipitate, washing with pure water for 3-4 times, and preparing slurry to obtain slurry with the volume solid content of 25%. Then spray drying at 350 deg.C to obtain core-shell structure CdS @ SiO 2 The powder of (4);
2. dissolving 80g of zirconium oxychloride octahydrate in 1L of water, adding 100g of citric acid and 10g of LiF, and uniformly stirring; slowly injecting 6wt% ammonia water to adjust the pH of the solution to 8.5 to obtain a zirconium salt solution;
3. 0.2L CdS @ SiO 2 Adding zirconium salt solution into the powder, stirring, spray drying the obtained slurry at 750 deg.C under 90% nitrogen (nitrogen: air =9, v/v) by high temperature pyrolysis spray dryer, cooling, sieving to obtain zirconium silicate coated pigment powder with particle size less than 1 μm, and HNO 3 Acid washing and pure water washing for 3-4 times, centrifugally separating, and drying at 120 deg.C to obtain coating pigment powder;
4. and adding 0.2L of butyl acetate, 50ml of isopropyl palmitate, 10g of PEG-2000 and 5g of CTAB into 100g of dried coating pigment powder, fully stirring and mixing, adding a sodium carbonate/sodium bicarbonate buffer solution, and adjusting the pH value to 9.3 to obtain a finished product of the zirconium silicate coated CdS ceramic printing ink.
Example 2
The preparation method of the heterocrystal coated carbon black ceramic printing ink comprises the following steps:
the method specifically comprises the following steps:
1. dispersing 60g of carbon black powder subjected to surface hydrophilic modification in 5L of isopropanol solution (the ratio of alcohol to water is 1,v/v), adding 80g of PVP, performing ultrasonic dispersion and uniformly stirring, and adjusting the pH value of the solution to 11 by 6wt% of ammonia water to obtain a pigment mixed solution;
then dissolving 1L TEOS in 4L isopropanol, and adjusting the pH of the solution to 12 by 8wt% ammonia water to obtain a TEOS alcoholic solution;
the TEOS alcohol solution is evenly injected into the pigment mixed solution for three times by a metering pump for 40min each time, and the feeding interval is 6h. And aging the mixed solution for 12h, then centrifugally separating a precipitate, washing with pure water for 3-4 times, and preparing slurry to obtain slurry with the volume solid content of 30%. Then spray drying treatment is carried out at 320 ℃ in nitrogen atmosphere to obtain the core-shell structure C @ SiO 2 The powder of (4);
2. dissolving 80g of zirconium oxychloride octahydrate in 1L of water, adding 70ml of diethanolamine and 10g of NaF, and uniformly stirring; slowly injecting 10wt% ammonia water to adjust the pH of the solution to 8.5 to obtain a zirconium salt solution;
3. 0.2L of C @ SiO 2 Adding zirconium salt solution into the powder, stirring uniformly, performing spray drying heat treatment on the obtained slurry at 900 ℃ in a high-purity nitrogen atmosphere by using a high-temperature pyrolysis spray dryer, cooling the obtained powder, screening to reserve zirconium silicate coated pigment powder with the particle size of less than 1 mu m, cleaning for 3-4 times in an atmosphere of 80% oxygen (oxygen: nitrogen =4, v/v) at 350 ℃ and pure water, performing centrifugal separation, and drying at 120 ℃ to obtain the coated pigment powder;
4. and adding 0.15L of propylene glycol and 0.1L of diethylene glycol, 10g of SRE-4026X and 5g of PVP into 90g of dried coating pigment powder, fully stirring and mixing, adding a sodium monohydrogen phosphate/sodium dihydrogen phosphate buffer solution, and adjusting the pH value to 7.2 to obtain a finished product of the zirconium silicate coated carbon black ceramic printing ink.
Example 3
Heterocrystal coated CdS x Se 1-x Preparation of ceramic ink:
the method specifically comprises the following steps:
1. changing the pigment raw material into nano CdS x Se 1-x Core-shell CdS were obtained by the same procedure and conditions as in example 1 x Se 1-x @SiO 2 The powder of (4);
2. dissolving 95g of zirconium tetrachloride in 1L of water, adding 70ml of diethanolamine and 10g of LiF, and uniformly stirring; slowly injecting 5wt% ammonia water to adjust the pH of the solution to 8.5 to obtain a zirconium salt solution;
3. adding 0.2L CdS x Se 1-x @SiO 2 Adding zirconium salt solution into the powder, stirring, spray drying the obtained slurry at 850 deg.C under 95% argon (argon: air =20, v/v) atmosphere in a pyrolysis spray dryer, cooling, sieving to obtain zirconium silicate coated pigment powder with particle size less than 1 μm, and HNO 3 Acid washing and pure water washing for 3-4 times, centrifugally separating, and drying at 120 deg.C;
4. adding 0.2L of butyl acetate and 50ml of isopropyl palmitate, 6g of sodium carboxymethylcellulose and 5g of CTAB into 100g of dried coating pigment powder, fully stirring and mixing, and adding sodium carbonate/sodium bicarbonateAdjusting the pH value of the buffer solution to 9.3 to obtain zirconium silicate coated CdS x Se 1-x And (5) ceramic printing ink finished product.
Example 4
Heterocrystal coated Fe 2 O 3 The preparation method of the ceramic printing ink comprises the following steps:
the method specifically comprises the following steps:
1. changing the pigment raw material into nano Fe 2 O 3 Core-shell structure Fe was obtained in the same manner and conditions as in example 2 2 O 3 @SiO 2 The powder of (4);
2. 80g of zirconium oxychloride octahydrate are dissolved in 1L of water, 100g of diethanolamine and 10g of LiF are added, and the mixture is stirred uniformly. Slowly injecting 8wt% ammonia water to adjust the pH of the solution to 10 to obtain a zirconium salt solution;
3. 0.2L of Fe 2 O 3 @SiO 2 Adding zirconium salt solution into the powder, stirring, spray drying the obtained slurry at 800 deg.C under 80% argon (argon: air =4, v/v) atmosphere by pyrolysis spray dryer, cooling the obtained powder, sieving to obtain zirconium silicate coated pigment powder with particle size less than 1 μm, and HNO 3 Acid washing and pure water washing for 3-4 times, centrifugally separating, and drying at 120 deg.C;
4. adding 0.2L of propylene glycol methyl ether acetate and 50ml of diethylene glycol methyl ether, 6g of sodium dodecyl sulfate and 4g of PVB into 100g of dried coating color powder, fully stirring and mixing, adding a sodium carbonate/sodium bicarbonate buffer solution to adjust the PH to 9.3, and obtaining the zirconium silicate coated Fe 2 O 3 And (5) ceramic printing ink finished product.
Example 5
Heterocrystal coated CdS x Se 1-x Preparation of ceramic ink:
the method comprises the following specific steps:
1. the same procedure and conditions as in example 3 gave CdS with core-shell structure x Se 1-x @SiO 2 The powder of (4);
2. changing the type and the dosage of zirconium salt, dissolving 120g of zirconium oxychloride octahydrate in 1L of water, adding 100g of diethanolamine and 10g of LiF, and uniformly stirring; slowly injecting 6wt% ammonia water to adjust the pH of the solution to 7.5 to obtain a zirconium salt solution;
3. the subsequent steps and conditions were the same as in example 3.
Example 6
The preparation method of the heterocrystal coated carbon black ceramic printing ink comprises the following steps:
the method comprises the following specific steps:
1. dispersing 60g of carbon black powder subjected to surface hydrophilic modification in 5L of isopropanol solution (the ratio of alcohol to water is 1,v/v), adding 80g of PVP, performing ultrasonic dispersion and uniformly stirring, and adjusting the pH value of the solution to 11 by 6wt% of ammonia water to obtain a pigment mixed solution;
then 2L of TEOS is dissolved in 5L of isopropanol, and the pH value of the solution is adjusted to 12 by 12wt% of ammonia water to obtain a TEOS alcoholic solution;
and injecting the TEOS alcohol solution into the pigment mixed solution by a metering pump for 40min every time, wherein the feeding interval is 8h. Aging the mixed solution for 12h, then centrifugally separating a precipitate, washing with pure water for 3-4 times, and preparing slurry to obtain slurry with the volume solid content of 30%; then spray drying treatment is carried out at 320 ℃ in nitrogen atmosphere to obtain the core-shell structure C @ SiO 2 The powder of (4);
2. 160g of zirconium oxychloride octahydrate are dissolved in 2L of water, 140ml of diethanolamine and 15g of CaF are added 2 Uniformly stirring; slowly injecting 8wt% ammonia water to adjust the pH of the solution to 8.5 to obtain a zirconium salt solution;
3. the subsequent steps and conditions were the same as in example 2.
The physical and chemical properties of the ceramic ink powder of examples 1 to 6 were characterized, wherein the average particle size was measured with a full-automatic laser particle size analyzer; the morphology of the nanoparticles is observed by SEM; stability is measured by the time the ink is allowed to stand until significant coagulation occurs, and the results are as follows:
it can be seen that the zirconium silicate coated ceramic ink obtained by the method of the invention has no special raw material limitation, and can realize the expression of various tones. Average particle size of the obtained coated ceramic ink particlesThe diameter D90 is less than 800nm, which meets the requirement of the ceramic nozzle on the particle size range of the ink particles. In addition, the particle size distribution of the pigment particles of the product and the thickness of the coating layer can be accurately regulated and controlled by controlling the particle size of the raw material pigment and the feeding amount of TEOS and zirconium salt. The invention avoids ZrSiO in the traditional technical scheme by adopting the step-by-step wrapping and suspension fluidization high-temperature treatment technology 4 The agglomeration and sintering of the wrapping layer under the high-temperature condition and the subsequent crushing treatment process avoid the material loss caused by the crushing and acid washing processes, and obviously improve the wrapping rate of pigment particles and the product yield. Compared with the prior art in the field, the method can realize lower pollution emission, higher raw material utilization efficiency and economic benefit.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A production method of a small-particle-size coated ceramic ink material is characterized by comprising the following steps of:
S1：SiO 2 and (3) construction of a wrapping layer:
s1.1, dispersing a nano pigment and a surfactant in an alcohol solution, uniformly stirring, and adjusting the pH of the solution to 10-11 to obtain a solution A;
s1.2, preparing an alcoholic solution of TEOS, and adjusting the pH of the solution to 11-12 to obtain a solution B;
s1.3, injecting the solution B into the solution A for multiple times, performing hydrolytic condensation to generate precipitates, and separating and cleaning the precipitates to obtain slurry C;
s1.4, drying the slurry C to obtain the surface-coated porous SiO 2 The pigment particles are powder D;
S2：ZrSiO 4 and (3) construction of a wrapping layer:
s2.1, adding a complexing agent and a mineralizing agent into a zirconium salt aqueous solution, uniformly stirring, and adjusting the pH of the solution to 8-10 to obtain an E solution;
s2.2, adding the powder D into the solution E according to the volume solid content of 15-30%, and uniformly stirring to obtain slurry F;
s2.3, carrying out high-temperature thermal decomposition spray drying on the slurry F, cooling and screening to obtain ZrSiO 4 The coated pigment particles are powder G;
s3: and (3) coating type pigment post-treatment:
s3.1, removing incompletely-wrapped pigment powder from the powder G by oxygen-enriched low-temperature roasting or acid washing, and then washing, filtering and drying to obtain ceramic ink powder H;
s3.2, mixing the powder H with an aqueous or organic solvent, and adding a dispersing agent and buffer salts to obtain the small-particle-size coated ceramic ink product.
2. The method for producing a small-particle-size encapsulated ceramic ink material as claimed in claim 1, wherein: in step S1.1, step S1.2 and step S2.1, the pH of the solution is adjusted by ammonia water, and the concentration of the ammonia water is 4-12wt%.
3. The method for producing a small-particle-size encapsulated ceramic ink material as claimed in claim 1, wherein: in step S1.1, the colorant is CdS or CdS x Se 1-x 、Fe 2 O 3 Or modified carbon black, alcohol is ethanol, ethylene glycol or isopropanol, and surfactant is CTAB or PVP.
4. The method for producing a small-particle-diameter-coated ceramic ink material as claimed in claim 3, wherein: the modified carbon black pigment is obtained by taking natural gas or high aromatic hydrocarbon oil as a raw material, carrying out incomplete combustion or pyrolysis, and carrying out surface hydrophilic modification treatment by at least one strong oxidant in concentrated nitric acid, potassium permanganate, concentrated sulfuric acid or hydrogen peroxide under the heating condition.
5. The method for producing a small-particle-diameter-coated ceramic ink material as claimed in claim 3, wherein: in the step S3.1, the powder G obtained by producing the modified carbon black pigment is subjected to oxygen-enriched low-temperature roasting to remove the pigment powder G which is not completely wrapped in the powder G, and the pigment powder G which is easy to dissolve in acid is subjected to acid washing to remove the pigment powder G which is not completely wrapped in the pigment powder G.
6. The method for producing a small-particle-size encapsulated ceramic ink material as claimed in claim 1, wherein: the volume ratio of the alcohol to the water in the alcohol solution in the step S1.1 is 0.2-2; the mass ratio of the nano pigment to the surfactant in the step S1.1 is 0.6-1.4; the volume ratio of alcohol to TEOS in the TEOS alcohol solution of the step S1.2 is 2-6.
7. The method for producing a small-particle-size encapsulated ceramic ink material as claimed in claim 1, wherein: in step S1.3, the solution B is injected into the solution A for multiple times, and the interval is 4-8h every time.
8. The method for producing a small-particle size encapsulated ceramic ink material as claimed in claim 1, wherein: in the step S1.4, spray drying is carried out on the slurry C at the temperature of 300-350 ℃; the temperature of the high-temperature pyrolysis spray drying in step S2.3 is 700-900 ℃.
9. The method for producing a small-particle size encapsulated ceramic ink material as claimed in claim 1, wherein: in the step S2.1, the concentration of the zirconium salt in the aqueous solution of the zirconium salt is 0.3wt% -1wt%; wherein the complexing agent is citric acid, diethanolamine or phytic acid; the mineralizer is NaF or CaF 2 Or LiF; the zirconium salt is Zr (OCl) 2 ·8H 2 O or ZrCl 4 。
10. The method for producing a small-particle-size encapsulated ceramic ink material as claimed in claim 1, wherein: in the step S3.2, the dispersing agent is polyvinylpyrrolidone, polyvinyl butyral, polyethylene glycol, sodium tripolyphosphate or sodium carboxymethyl cellulose; the buffer salt is carbonate/bicarbonate, sodium monohydrogen phosphate/dihydrogen phosphate or monohydrogen phosphate/dihydrogen phosphate.
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