CN114058195B - Preparation method of ceramic pigment and ceramic pigment - Google Patents
Preparation method of ceramic pigment and ceramic pigment Download PDFInfo
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- CN114058195B CN114058195B CN202111587571.6A CN202111587571A CN114058195B CN 114058195 B CN114058195 B CN 114058195B CN 202111587571 A CN202111587571 A CN 202111587571A CN 114058195 B CN114058195 B CN 114058195B
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
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Abstract
The invention discloses a preparation method of a ceramic pigment and the ceramic pigment, wherein the method comprises the following steps: step 1, providing aluminum ash; step 2, adding water into the aluminum ash, stirring, standing for a preset time, removing a supernatant, adding an alkali solution, fully stirring, and performing solid-liquid separation to obtain a solid-phase mixture; step 3, roasting the solid-phase mixture to obtain a roasted product; and 4, adding a doped ion source, a mineralizer and a stabilizer into the roasted product, and performing high-temperature solid-phase synthesis to obtain the ceramic pigment. According to the method provided by the embodiment of the invention, secondary utilization of solid hazardous waste aluminum ash can be realized, meanwhile, a solid phase method is combined, the harm to the environment is reduced, the resource utilization of the aluminum ash in the field of ceramic pigments is promoted, and the preparation method has the advantages of simple process, easiness in control, easiness in production, environmental friendliness and capability of greatly reducing the production cost.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a preparation method of a ceramic pigment and the ceramic pigment.
Background
The aluminum ash is a solid waste generated in the industrial production, use and recycling processes of aluminum such as electrolytic aluminum, cast aluminum and the like. The components of the aluminous ash vary with the production raw materials and the operation conditions of enterprises. The components are generally metallic aluminum, aluminum oxide, iron oxide, potassium, sodium, calcium, magnesium chloride, etc., and are related directly to the contaminants contained in the raw material, covering agent, slag former, refining agent, etc., and also to the atmosphere in the casting furnace.
At present, the aluminum ash is mainly stockpiled or buried, and toxic and harmful ions in the aluminum ash can permeate into the ground to pollute soil and underground water. In addition, when the weather is hot and humid, substances such as aluminum nitride and aluminum carbide in the aluminum ash react with water to generate gases such as ammonia gas and methane, and the air is polluted. Therefore, useful components in the aluminum ash are converted into high value-added products to obtain raw materials, and at the same time, the problem of pollution caused by landfill of harmful wastes is solved.
Disclosure of Invention
In view of this, the invention provides a preparation method of a ceramic pigment, which is simple in process and can utilize waste aluminum ash to obtain a ceramic pigment with higher added value.
The invention adopts the following technical scheme:
the preparation method of the ceramic pigment comprises the following steps:
step 1, providing aluminum ash;
step 2, adding water into the aluminum ash, stirring, standing for a preset time, removing a supernatant, adding an alkali solution into the mixture, fully stirring, and performing solid-liquid separation to obtain a solid-phase mixture;
step 3, roasting the solid-phase mixture to obtain a roasted product;
and 4, adding a doped ion source, a mineralizer and a stabilizer into the roasted product, and performing high-temperature solid-phase synthesis to obtain the ceramic pigment.
Preferably, the mass percentage of the aluminum ash is 30wt% to 85wt% with respect to the total amount of the aluminum ash, the dopant ion source, the mineralizer, and the stabilizer.
Preferably, in the step 2, the mass ratio of the aluminum ash to the water is 1: (1-7), wherein the mass ratio of the aluminum ash to the alkali solution is 1: (1-3).
Preferably, the alkali solution is an aqueous sodium hydroxide solution having a concentration of 0.5 to 40wt%.
Preferably, in the step 3, the roasting temperature is 500-1100 ℃.
Preferably, in the step 4, the high-temperature solid phase synthesis temperature is 1000-1350 DEG C
Preferably, in the step 4, the dopant ions contained in the dopant ion source are one or more of manganese ions, zinc ions, chromium ions and cobalt ions.
Preferably, the mass percentage of the mineralizer is 1-5wt%, and the mineralizer is one or more of compounds of sodium chloride, sodium fluoride and ammonium chloride.
Preferably, the weight percentage of the stabilizer is 1-10wt%, and the stabilizer is one or more of boric acid, calcium carbonate, calcium chloride and dipotassium hydrogen phosphate.
The invention also provides a ceramic pigment which is prepared by the preparation method of the ceramic pigment.
The technical scheme of the invention has at least one of the following effects:
according to the preparation method of the ceramic pigment, solid hazardous waste aluminum ash is purified and converted into aluminum oxide or aluminum hydroxide, doping ions are introduced, a specific mineralizer is added to promote the solid phase reaction, a stabilizer is added to conceal the interference of elements such as calcium, magnesium, silicon and the like on the solid phase reaction, and the ceramic pigment and the preparation method thereof are prepared by adopting a solid phase synthesis method. The method realizes resource utilization of the aluminum ash in the field of ceramic pigments, avoids the harm of random treatment of the aluminum ash to the environment, greatly reduces the production cost of the traditional chemical process, has simple process and environmental protection, and meets the requirement of industrial production.
Description of the drawings:
FIG. 1 is a flow chart of a method for producing a ceramic pigment according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction chart of a red colorant powder according to example 1 of the present invention;
FIG. 3 is a physical appearance diagram of a red colorant powder in example 1 of the present invention;
FIG. 4 is an X-ray diffraction diagram of a pink colorant powder according to embodiment 2 of the present invention;
FIG. 5 is a diagram showing the appearance of a pink colorant powder in example 2 of the present invention;
FIG. 6 is an X-ray diffraction chart of a blue coloring material powder according to example 3 of the present invention;
FIG. 7 is a schematic external view of a blue coloring material powder according to example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the description of the embodiments of the invention given above, are within the scope of protection of the invention.
The ceramic pigment is an important component in the field of decoration of ceramic products, and is an important component in the colour-decorating agent of ceramic products and ceramic glaze or blank material, in which the aluminium series pigment is extensively used, mainly including manganese red pigment, chrome-aluminium red pigment and cobalt blue pigment, etc..
The aluminum ash mainly contains metallic aluminum, aluminum oxide, aluminum hydroxide and other substances. The inventor finds that alumina and aluminum hydroxide in the aluminous ash can be used as raw materials for preparing ceramic pigments, and particularly, the method for producing the ceramic pigments by using solid hazardous aluminous ash as the raw materials can obtain the high-value ceramic pigments and can better utilize the aluminous ash.
The method for preparing the ceramic coloring material and the ceramic coloring material according to the embodiment of the present invention are described in detail below.
As shown in FIG. 1, the preparation method of the ceramic pigment according to the embodiment of the present invention comprises the following steps:
and S110, providing aluminum ash.
In one embodiment of the present application, the aluminum ash is aluminum ash. Preferably, the aluminum ash is crushed and sieved, and the mesh of the sieving can be 80-325 meshes, and more preferably 80-140 meshes, so as to obtain the undersize aluminum ash. Therefore, impurities such as bulk metallic aluminum and the like are removed, particles with uniform particle size are obtained, and the uniformity and the stability of the pigment are improved.
During the screening process, the screened dust and the large metal aluminum can be further recycled.
And S120, adding water into the aluminum ash, stirring, standing for a preset time, removing a supernatant, adding an alkali solution into the mixture, fully stirring, and performing solid-liquid separation to obtain a solid-phase mixture.
That is, in this step, water is first added and sufficiently stirred, and left to stand for a certain period of time to allow soluble salts therein to be sufficiently dissolved and removed by solid-liquid separation (i.e., removal of supernatant). In the embodiment of the present invention, the ratio of the aluminum ash to the water may be 1 to 1, preferably 1. The proportion can effectively remove soluble salts in the aluminous ash.
In the aluminum ash, a certain amount of nitrogen element is usually mixed, and this nitrogen element is usually present in the form of AlN. The presence of nitrogen will affect the subsequent solid phase reaction and thus the stability of the colorant. In addition, a part of unreacted Al is mixed in the aluminum ash.
For this purpose, after removal of the soluble salts thereof, the aluminum therein is also hydrolyzed on the one hand by introducing an alkaline solution to form aluminum hydroxide.
On the other hand, nitrogen therein can be effectively removed by adding an alkali solution such as an aqueous sodium hydroxide solution. The reaction mechanism is as follows:
AlN+H 2 O→Al(OH) 3 +NH 3
AlN+NaOH+H 2 O→NaAlO 2 +NH 3
in one embodiment of the invention, the adding ratio of the aluminum ash to the alkali solution is 1. Preferably, it may be 1:2, the proportion can reach the optimal alkali addition amount for removing nitrogen elements, and the nitrogen removal rate is as high as 94.19 percent.
In one embodiment of the present invention, the alkaline solution may be sodium hydroxide solution with a concentration of 0.5-40%, which is effective for removing nitrogen element in the form of aluminum nitride from aluminum ash.
In some embodiments, the sodium hydroxide solution is slowly added to the aluminum ash from which the supernatant liquid is removed, and heated and stirred for a predetermined time, wherein the heating temperature is 50 to 125 ℃, and the predetermined time may be 2 to 4 hours. Heating and stirring for a preset time, and then carrying out solid-liquid separation to obtain a solid-phase mixture.
S130, roasting the solid-phase mixture to obtain a roasted product.
By calcination, on the one hand, a small amount of residual metallic aluminum in the aluminum ash can be oxidized and carbon impurities oxidized, and on the other hand, part of the aluminum hydroxide can be dehydrated.
In the first embodiment of the invention, the roasted product is obtained by low-temperature oxygen-enriched roasting, wherein the oxygen-enriched roasting temperature is 500-1100 ℃, and preferably the temperature can be 500-850 ℃. The roasted product is a mixture of aluminum oxide and aluminum hydroxide.
S140, adding a doping ion source, a mineralizer and a stabilizer into the roasted product, and performing high-temperature solid-phase synthesis to obtain a ceramic pigment.
Wherein, the high temperature solid phase synthesis means that doping ions are doped into alumina crystal lattices at high temperature to form solid solution so as to form stable ceramic pigment. In one embodiment of the invention, the temperature for high temperature solid phase synthesis is between 1000-1350 ℃.
In one embodiment of the present invention, the dopant ions in the dopant ion source may be one or more of manganese ions, zinc ions, chromium ions, and cobalt ions, all of which are used as dopant elements or colorant formulation components. The dopant ion may be selected according to the color of the ceramic coloring material to be formed, and for example, a red coloring material may be formed by introducing a manganese ion, a pink coloring material may be formed by introducing a chromium ion, a blue coloring material may be formed by introducing a cobalt ion, or the like, and further, a plurality of dopant ions may be introduced at the same time.
In one embodiment of the invention, the mass percentage of the mineralizer may be 1-5wt%, and the mineralizer is one or more of the compounds sodium chloride, sodium fluoride and ammonium chloride.
In one embodiment of the invention, the weight percentage of the stabilizer is 1-10wt%, and the stabilizer is one or more of boric acid, calcium carbonate, calcium chloride and dipotassium hydrogen phosphate.
According to the preparation method of the ceramic pigment provided by the embodiment of the invention, the solid hazardous waste aluminum ash can be recycled, the harm to the environment is reduced by combining a solid phase method, and the resource utilization of the aluminum ash in the field of the ceramic pigment is promoted, so that the preparation method has the advantages of simple process, easiness in control, easiness in production, environmental friendliness and capability of greatly reducing the production cost.
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the following specific examples.
Example 1
1) Sieving aluminous ash (solid hazardous waste aluminous ash) by a 140-mesh sieve, and then mixing the aluminous ash with water-cement ratio of 5:1, mixing, stirring, standing and removing supernatant;
2) According to the alkali-ash ratio of 2:1, adding a sodium hydroxide solution with the mass fraction of 20% into the treated aluminum ash in the step 1), heating to 80 ℃, stirring for 2 hours, and cooling to obtain a solid-phase mixture;
3) Carrying out low-temperature oxygen-enriched roasting on the obtained solid-phase mixture at 700 ℃ to obtain a mixture of aluminum oxide and aluminum hydroxide;
4) Adding 87 parts by mass of mixture, 7 parts by mass of manganese carbonate, 2 parts by mass of sodium fluoride, 3 parts by mass of calcium chloride and 1 part by mass of ammonium chloride into the mixture obtained in the step 3), and performing high-temperature solid-phase synthesis at 1050 ℃ to obtain the red pigment powder.
The sample characterization results are shown in table 1:
TABLE 1 characterization results
The colorimetric values of the full-body ceramic tile sample plate with the red pigment addition amount of 5 percent after being calcined by a roller kiln are shown in Table 2:
TABLE 2 color value Table
Wherein, L, a, b in the table are indexes for evaluating the coloring material, and respectively represent a brightness value, a red-green value and a yellow-blue value; wherein, the bigger the value of L, the brighter the coloring material, the positive value of a indicates that the coloring material is red, and the negative value indicates that the coloring material is green, and the positive value of b indicates that the coloring material is yellow, and the negative value indicates that the coloring material is blue; the value of a in the data is greater than b, indicating that the sample is red; in the data, the values a and b are negative values, and the absolute value of the value a is less than the value b, so that the sample is blue. Therefore, the scheme of the invention can obtain the red ceramic tile with bright pigment.
FIG. 2 is a XRD pattern corresponding to the sample of example 1, with the XRD pattern of the manganese red material substantially corresponding to that of a PDF card, indicating successful doping of the alumina lattice with manganese ions. The physical map can be seen in FIG. 3.
Example 2
1) Sieving the solid hazardous waste aluminum ash with a 140-mesh sieve, mixing the solid hazardous waste aluminum ash with water according to the water-ash ratio of 5.0, stirring and standing;
2) Adding 30 mass percent of sodium hydroxide solution into the treated aluminum ash according to the alkali ash ratio of 2.0, heating to 100 ℃, stirring for 3 hours, and cooling to obtain a solid phase mixture;
3) Carrying out low-temperature oxygen-enriched roasting on the obtained solid-phase mixture at 750 ℃ to obtain a mixture of aluminum oxide and aluminum hydroxide;
4) And adding 50 parts by mass of the mixture, 7 parts by mass of chromium oxide, 35 parts by mass of zinc oxide and 8 parts by mass of boric acid into the obtained mixture, and performing high-temperature solid-phase synthesis at 1250 ℃ to obtain the pink pigment powder.
The sample characterization results are shown in table 3:
TABLE 3 characterization results
The XRD pattern of example two can be seen in fig. 4, which shows the successful doping of chromium ions into alumina lattice in the following fig. 5.
The chromatic value of the whole ceramic tile sample plate with 5% of the peach red pigment is shown in Table 4 after being calcined by a roller kiln:
TABLE 4 color value Table
From Table 4, the scheme of the invention can obtain the pink ceramic tile with brighter pigment.
Example 3
1) And (3) sieving the solid dangerous waste aluminum ash by a 140-mesh sieve, and then mixing the solid dangerous waste aluminum ash with the solid dangerous waste aluminum ash according to a water-ash ratio of 5:1, mixing, stirring and standing for later use;
2) According to the alkali-ash ratio of 2:1, adding a sodium hydroxide solution with the mass fraction of 40% into the treated aluminum ash, heating to 120 ℃, stirring for 4 hours, and cooling to obtain a solid-phase mixture;
3) Carrying out low-temperature oxygen-enriched roasting on the obtained solid-phase mixture at 850 ℃ to obtain a mixture of aluminum oxide and aluminum hydroxide;
4) And adding 75 parts by mass of the mixture, 20 parts by mass of cobalt oxide and 5 parts by mass of boric acid into the obtained mixture, and performing high-temperature solid-phase synthesis at 1200 ℃ to obtain blue pigment powder.
The sample characterization results are shown in table 5:
TABLE 5 characterization results
Wherein, fig. 6 shows the XRD pattern of example three, illustrating the successful doping of cobalt ions into the alumina lattice, and the physical diagram can be seen in fig. 7 below.
The chroma value of the whole ceramic tile sample plate with 5% of the additive amount of the cobalt blue material after being calcined by a roller kiln is shown in Table 6:
TABLE 6 color value table
From Table 6, cobalt blue ceramic tiles were obtained according to the protocol of the present invention.
The composition analysis (XDF) of the aluminum ash in the above examples is shown in Table 7:
TABLE 7 aluminum ash composition analysis (XDF) results
The base ceramic of the full body ceramic tile template in the above examples is a ceramic formulation commonly used in ceramic factories, and its composition analysis (XDF) is shown in table 8:
TABLE 8 Whole body ceramic sample composition analysis (XDF) results
While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (8)
1. A method for preparing a ceramic pigment is characterized by comprising the following steps:
step 1, providing aluminum ash;
step 2, adding water into the aluminum ash, stirring, standing for a preset time, removing a supernatant, adding an alkali solution, fully stirring, and performing solid-liquid separation to obtain a solid-phase mixture, wherein the alkali solution is a sodium hydroxide aqueous solution, and the concentration of the sodium hydroxide aqueous solution is 0.5-40wt%;
step 3, roasting the solid-phase mixture to obtain a roasted product;
and 4, adding a doped ion source, a mineralizer and a stabilizer into the roasted product, and performing high-temperature solid-phase synthesis to obtain the ceramic pigment.
2. The method according to claim 1, wherein the mass percentage of the aluminum ash is 30wt% to 85wt% with respect to the total amount of the aluminum ash, the dopant ion source, the mineralizer, and the stabilizer.
3. The preparation method according to claim 1, wherein in the step 2, the mass ratio of the aluminum ash to the water is 1: (1-7), wherein the mass ratio of the aluminum ash to the alkali solution is 1: (1-3).
4. The production method according to any one of claims 1 to 3, wherein the baking temperature in the step 3 is 500 to 1100 ℃.
5. The method according to any one of claims 1 to 3, wherein the high temperature solid phase synthesis temperature in step 4 is 1000 to 1350 ℃.
6. The method according to claim 1, wherein in the step 4, the dopant ions contained in the dopant ion source are one or more of manganese ions, zinc ions, chromium ions, and cobalt ions.
7. The preparation method according to claim 1, characterized in that the mass percentage of the mineralizer is 1-5wt%, and the mineralizer is one or more of the compounds sodium chloride, sodium fluoride and ammonium chloride.
8. The method according to claim 1, wherein the stabilizer is one or more of boric acid, calcium carbonate, calcium chloride and dipotassium hydrogen phosphate, and the weight percentage of the stabilizer is 1-10 wt%.
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