CN113880554A - Method for preparing black ceramic material - Google Patents
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- CN113880554A CN113880554A CN202111217355.2A CN202111217355A CN113880554A CN 113880554 A CN113880554 A CN 113880554A CN 202111217355 A CN202111217355 A CN 202111217355A CN 113880554 A CN113880554 A CN 113880554A
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- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
- C04B33/1322—Red mud
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9661—Colour
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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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
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The invention discloses a method for preparing a black ceramic material, which comprises the following steps: adding an iron-containing material and an additive into a base material to form a ceramic raw material, and sintering the ceramic raw material to be black in an air atmosphere to obtain a black ceramic material; wherein, the additive contains one or more of Mn, Ni and Mg ions; based on the total weight of the ceramic raw material, the mixing amount of the iron-containing material is 30-70 wt%, and the mixing amount of the additive is 2-20 wt%. The method can directly utilize the 3-valent iron ions in the iron-containing material, does not need to reduce the 3-valent iron ions into 2-valent iron ions, and does not need non-oxidizing or reducing atmosphere, so that the 3-valent iron ions in the material can react with Mn, Ni and Mg ions of the additive to generate the required mineral phase, and the mineral phase directly acts on the ceramic material to blacken, thereby obviously reducing the preparation cost, having simple preparation process and good performance of the ceramic product. The invention is suitable for the fields of solid waste resource utilization and novel building material preparation.
Description
Technical Field
The invention belongs to the field of solid waste resource utilization and novel building material preparation, and particularly relates to a method for preparing a black ceramic material.
Background
Part of industrial solid wastes contain a large amount of iron oxide components, such as red mud, iron tailings, iron-containing dust and the like, and part of low-grade ores, inferior ores and muck contain a large amount of iron oxide components, so that the iron oxide components are difficult to be recycled at present. The common characteristics of the materials are that the mass percentage of the ferric oxide is more than 25 percent, and the main valence state of the iron ions is 3-valent iron.
The black ceramic material is a ceramic material with larger use amount in ceramic products and has high added value. If the iron-containing materials can be prepared into black ceramic raw materials, the added value and the market space of ceramic products can be improved. However, most of the iron ions and minerals having a valence of 3 are yellow, orange-yellow or brownish red, and ceramics fired in air containing a large amount of iron ions having a valence of 3 also exhibit yellow, orange-yellow or brownish red.
Since 2-valent iron is a black colorant, the industry typically reduces the 3-valent iron ions to 2-valent iron ions, which react with chromium, manganese, vanadium or other mineral ions to form black ceramics. However, these methods require non-oxidizing or reducing atmosphere, or add reducing agents such as coal dust, which results in higher cost; in addition, the prepared black ceramic has poor performance and is easy to foam, most of 3-valent iron still forms brown or yellow mineral phases such as hematite and the like, and is difficult to convert into black.
Disclosure of Invention
The technical problem solved by the invention is to provide a method for preparing the black ceramic material, the method does not need to reduce 3-valent iron ions into 2-valent iron ions, and non-oxidizing or reducing atmosphere is also not needed, so that the preparation cost is obviously reduced, the preparation process is simple, and the performance of the ceramic product is good.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of making a black ceramic material, the method comprising:
adding an iron-containing material and an additive into a base material to form a ceramic raw material, and sintering the ceramic raw material to be black in an air atmosphere to obtain a black ceramic material;
wherein, the additive contains one or more of Mn, Ni and Mg ions; based on the total weight of the ceramic raw material, the mixing amount of the iron-containing material is 30-70 wt%, and the mixing amount of the additive is 2-20 wt%.
As an embodiment of the invention, the iron-bearing material is a solid waste or mineral containing ferric iron and having an iron oxide mass content of more than 25% by weight;
the mass content of ferric ions in the iron-containing material is higher than that of ferrous ions;
the iron-containing material is one or more of iron tailings, red mud, iron-containing dust, cheap iron-containing minerals and muck.
As an embodiment of the invention, the additive is selected from one or more of a magnesium oxide-containing material, a manganese oxide-containing material and a nickel oxide-containing material; preferably, the additive is selected from one or more of tailings, smelting slag, waste battery materials and waste electrode materials; the sum of the contents of Mn, Ni and Mg elements in the additive is 5-40 wt%;
optionally, the additive is selected from one or more of chemical magnesium oxide, carbonate, manganese ore or ferromanganese ore, manganese oxide, carbonate and nickel oxide and carbonate, and the sum of the contents of Mn, Ni and Mg in the additive is 40-79 wt%.
In one embodiment of the present invention, the base material is a ceramic mixed material composed of one or more of a quartz-based ceramic material, a feldspar-based ceramic material, and a clay-based ceramic material.
As an embodiment of the present invention, the sintering conditions are: the temperature is 1000 ℃ and 1200 ℃;
the black ceramic material comprises one or more of ceramic tiles, black bricks, rock plates, stone-like ceramic thick bricks, sintered bricks, archaized bricks, ancient bricks, sintered tiles and ceramic plates.
As an embodiment of the present invention, a spinel mineral in which ferric ions are present and one or more ions of manganese, magnesium and nickel are present at the same time in the black ceramic material;
the spinel mineral comprises MnFe2O4，NiFe2O4，(Mg,Mn)(Fe,Al)2O4And MgFe2O4One or more of them.
As an embodiment of the present invention, the black ceramic material contains a pyroxene mineral or/and a calcium iron garnet mineral having two or more ions of solid-solution iron, manganese, magnesium and nickel;
the pyroxene mineral comprises (Mg, Mn, Fe, Ca, Ni) (Fe, Ni, Mg, Mn) Si2O6,Na(Al,Fe)Si2O6，Ca(Fe,Al)(Si,Al)2O6One or more of the above;
the calcium iron garnet mineral comprises Mn3Fe2[SiO4]3、Fe3Fe2[SiO4]3And (Ca, Mg)3Fe2[SiO4]3One or more of them.
The technical scheme provided by the invention at least brings the following beneficial effects:
the method can directly utilize the 3-valent iron ions in the iron-containing material, does not need to reduce the 3-valent iron ions into 2-valent iron ions, and does not need non-oxidizing or reducing atmosphere, so that the 3-valent iron ions in the material can react with Mn, Ni and Mg ions of the additive to generate the required mineral phase, and the mineral phase directly acts on the ceramic material to blacken, thereby obviously reducing the preparation cost, having simple preparation process and good performance of the ceramic product.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in further detail below.
Example 1: adding red mud ceramic containing manganese ore with mass purity of 64.7%, wherein the red mud content in the ceramic raw material is 40 wt%, and adding manganese ore raw material containing manganese oxide 64.7 wt% into the ceramic raw materialThe content of the porcelain raw material is 5 wt%. The red mud ceramic is sintered in air at the sintering temperature of 1130-1190 ℃ and is dark black. The mineral phase contains spinel minerals such as MnFe spinel2O4) And magnesium titanium ore (MgTi)2O5) Hematite, quartz, etc. The spinel mineral contains Mn2+、Fe3+And O2-And ions which have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic had an iron oxide content of 14.9 wt%, a magnesium oxide content of 2.4 wt%, and a manganese oxide content of 8.7 wt%.
Example 2: red mud ceramic added with nickel oxide (chemical purity) with mass purity of 98%
The red mud content in the ceramic raw material is 40 wt%, and the nickel oxide chemical pure raw material which contains 98 wt% of manganese oxide is added into the ceramic raw material, and the content in the ceramic raw material is 10 wt%. The red mud ceramic is sintered in air at the sintering temperature of 1130-1190 ℃ and is black in color. The mineral phase contains spinel minerals such as nickel magnetite (NiFe)2O4) And calspodumene (CaFeSi)2O6) Hematite, quartz, nitinol (NiTiO)3) And the like. These minerals contain Ca2+、、Fe3+、Ni2+And O2-And plasma, wherein the ions have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic has an iron oxide content of about 14.9 wt.% and a nickel oxide content of about 9.8 wt.%.
Example 3: red mud ceramic added with talc
The red mud content in the ceramic raw material is 40 wt%, and the talc raw material, which contains 16 wt% of magnesium oxide, is added into the ceramic raw material, and the content in the ceramic raw material is 10 wt%. The red mud ceramic is sintered in a roller kiln at the sintering temperature of 1160-1180 ℃ and is brownish black in color. The ore phase contains spinel (Mg (Al, Fe) with magnesium, aluminum and iron solid solution2O4Forsterite (Mg)2SiO4) And hematite and anorthite. These minerals contain Mg2+、Fe3+、Al3+And O2-The plasma is generated by the plasma generation device,the ions have the function of making the red mud ceramic black after solid solution or reaction. However, the spinel formed was a solid solution, and the black color of the sample was reduced, and the color was slightly shifted to brown, but the whole color was still pale black. The red mud ceramic has an iron oxide content of about 15.3 wt%, a magnesium oxide content of about 4.5 wt%, and an aluminum oxide content of about 19.4 wt%.
Example 4: red mud ceramic added with manganese-containing tailings
The red mud content in the ceramic raw material is 40 wt%, and meanwhile, the manganese-containing tailing raw material which contains 16.9 wt% of manganese oxide is added into the ceramic raw material, and the content in the ceramic raw material is 10 wt%. The red mud ceramic is sintered in air at the sintering temperature of 1130-1190 ℃ and is black in color. The mineral phase contains spinel minerals such as MnFe spinel2O4) Calcium iron garnet mineral (Ca)3Fe2(SiO4)3) And the like. The spinel minerals and calcium iron garnet minerals contain Mn2+、Fe3+、Ca2+And O2-And plasma, wherein the ions have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic contains about 16.9 wt% of iron oxide, about 1.9 wt% of manganese oxide and about 5.7 wt% of calcium oxide.
Example 5: red mud ceramic added with manganese-containing tailings
The red mud content in the ceramic raw material is 40 wt%, and meanwhile, the manganese-containing tailing raw material which contains 16.9 wt% of manganese oxide is added into the ceramic raw material, and the content in the ceramic raw material is 20 wt%. The red mud ceramic is sintered in air at the sintering temperature of 1130-1190 ℃ and is dark black. The mineral phase contains spinel minerals such as MnFe spinel2O4) And manganese spinel (MnAl)2O4) Calcium iron garnet mineral (Ca)3Fe2(SiO4)3) And hematite, quartz, anorthite, etc. The spinel minerals and calcium iron garnet minerals contain Mn2+、Fe3+、Ca2+And O2-And plasma, wherein the ions have the function of making the red mud ceramic black after solid solution or reaction. Oxidation in red mud ceramicsThe iron content was about 19.5 wt%, the manganese oxide content was about 3.8 wt%, and the calcium oxide content was about 6.2 wt%.
Example 6: red mud ceramic added with silicomanganese smelting slag
The red mud content in the ceramic raw material is 40 wt%, and meanwhile, the silicomanganese smelting slag (abbreviated as silicomanganese slag) raw material which contains 9.4 wt% of manganese oxide is added into the ceramic raw material, and the content of the red mud in the ceramic raw material is 10 wt%. The red mud ceramic is sintered in the air, the sintering temperature is 1130-1180 ℃, and the color is brownish black. The mineral phase contains spinel minerals such as MgFe2O4) Manganese-iron spinel (MnFe)2O4) And hematite, quartz, anorthite, etc. The spinel mineral contains Mn2+、Mg2+、Fe3+And O2-And ions which have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic contains about 14.4 wt% of iron oxide, about 1.2 wt% of manganese oxide and about 4.7 wt% of magnesium oxide.
Example 7: red mud ceramic added with ferronickel smelting slag
The red mud content in the ceramic raw material is 40 wt%, and meanwhile, ferronickel smelting slag (nickel-iron slag for short) raw material which contains 2.6 wt% of nickel oxide and 16.4 wt% of magnesium oxide is added into the ceramic raw material, and the content of the red mud in the ceramic raw material is 10 wt%. The red mud ceramic is sintered in air at the sintering temperature of 1130-1180 ℃ and is light black in color. The mineral phase contains spinel minerals such as MgFe2O4) Nickel-iron spinel (NiFe)2O4) And hematite, quartz, anorthite, etc. The generated spinel mineral contains Mg2+、Ni2+、Fe3+And O2-And ions which have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic contains about 15.2 wt% of iron oxide, about 0.3 wt% of nickel oxide and about 2.4 wt% of magnesium oxide.
Example 8: adding iron tailing ceramic containing manganese oxide
The tailing content in the ceramic raw material is 30 wt%, and simultaneouslyThe chemical pure manganese oxide material is added into the ceramic material, and the chemical pure manganese oxide material contains 98 wt% of manganese oxide and 10 wt% of manganese oxide. The tailing ceramic is sintered in air at the sintering temperature of 1130-1190 ℃ and the color is black. The mineral phase contains spinel minerals such as MnFe spinel2O4) And manganese spinel (MnAl)2O4) And hematite, quartz, and the like. These minerals contain Mn2+、Fe3+、Ca3+、Si4+And O2-And plasma, wherein the ions have the function of making the tailing ceramic black after solid solution or reaction. The tailings ceramic had an iron oxide content of about 11.4 wt%, a manganese oxide content of about 8.7 wt%, and an alumina content of about 21.5 wt%.
Example 9: red mud ceramic added with black slag
The red mud content in the ceramic raw material was 40 wt%, and the black slag raw material, which contains 4.08 wt% of manganese oxide and 2.66 wt% of magnesium oxide, was added to the ceramic raw material, and the content in the ceramic raw material was 17 wt%. The red mud ceramic is sintered in air at 1150-1170 ℃ and is black in color. The mineral phase contains spinel minerals such as MgFe2O4) Manganese-iron spinel (MnFe)2O4) And hematite, quartz, anorthite, etc. The spinel mineral contains Mn2+、Mg2+、Fe3+And O2-And ions which have the function of making the red mud ceramic black after solid solution or reaction. The red mud ceramic contains about 23.6 wt% of iron oxide, about 0.9 wt% of manganese oxide and about 4.2 wt% of magnesium oxide.
Comparative example: mineral or solid waste without addition of one or more components selected from manganese oxide, magnesium oxide, zinc oxide and nickel oxide
The red mud contains 34.1 wt% of Fe2O3The main mineral phases are hematite, quartz, calcium iron garnet, calcium magnesium garnet and perovskite, the iron ions mainly comprise ferric iron ions, and the color is orange red. The red mud content in the red mud ceramic is 40 wt%. Sintering the red mud ceramic in air at the sintering temperature of 1130 DEG CAt-1190 deg.C, brown red, quartz, hematite, calcium iron ore, rutile and albite, and Fe3+、Si4+、Ca2+、Na+、O2-And (3) plasma. The red mud ceramic contains about 15.7 wt% of iron oxide, about 1.2 wt% of magnesium oxide, and about 4.4 wt% of sodium oxide.
In the invention, raw materials rich in manganese, nickel and magnesium, such as manganese-containing tailings, nickel-iron slag and the like, which are added in research and analysis, can be mixed with Fe in red mud or tailings3+The reaction is combined to generate spinel minerals, or one of garnet group minerals and pyroxene minerals, such as ferromanganese spinel, nickel magnetite, pleonaste, calcium iron garnet and the like, can simultaneously occur, and the generation of the materials can make the red mud ceramic show black under the reflection of visible light. And the degree of black color varies depending on the content of the substances. The research idea of converting the red mud material rich in ferric ions into the spinel material is provided, the additional values and the market competition space of the red mud or iron tailing ceramic are improved, and the method has the advantages of low production cost, simple process, obvious effect and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method of preparing a black ceramic material, the method comprising:
adding an iron-containing material and an additive into a base material to form a ceramic raw material, and sintering the ceramic raw material to be black in an air atmosphere to obtain a black ceramic material;
wherein, the additive contains one or more of Mn, Ni and Mg ions; based on the total weight of the ceramic raw material, the mixing amount of the iron-containing material is 30-70 wt%, and the mixing amount of the additive is 2-20 wt%.
2. The method of claim 1, wherein the iron-bearing material is a solid waste or mineral containing ferric iron and having an iron oxide mass content of more than 25% by weight;
the mass content of ferric ions in the iron-containing material is higher than that of ferrous ions;
the iron-containing material is one or more of iron tailings, red mud, iron-containing dust, cheap iron-containing minerals and muck.
3. The method of claim 1, wherein the additive is selected from one or more of a magnesium oxide-containing material, a manganese oxide-containing material, and a nickel oxide-containing material; preferably, the additive is selected from one or more of tailings, smelting slag, waste battery materials and waste electrode materials; the sum of the contents of Mn, Ni and Mg elements in the additive is 5-40 wt%;
optionally, the additive is selected from one or more of chemical magnesium oxide, carbonate, manganese ore or ferromanganese ore, manganese oxide, carbonate and nickel oxide and carbonate, and the sum of the contents of Mn, Ni and Mg in the additive is 40-79 wt%.
4. The method according to claim 1, wherein the base material is a ceramic mixed raw material composed of one or more of a quartz-based ceramic raw material, a feldspar-based ceramic raw material, and a clay-based ceramic raw material.
5. The method according to claim 1, wherein the sintering conditions are: the temperature is 1000 ℃ and 1200 ℃;
the black ceramic material comprises one or more of ceramic tiles, black bricks, rock plates, stone-like ceramic thick bricks, sintered bricks, archaized bricks, ancient bricks, sintered tiles and ceramic plates.
6. The method according to claim 1, characterized in that a spinel mineral of ferric ions and one or more of manganese, magnesium and nickel ions is present in the black ceramic material;
the spinel mineral comprises MnFe2O4，NiFe2O4，(Mg,Mn)(Fe,Al)2O4And MgFe2O4One or more of them.
7. The method according to claim 1, characterized in that pyroxene minerals or/and calcium iron garnet minerals in which ferric ions are present and one or more of manganese, magnesium and nickel are present simultaneously in the black ceramic material;
the pyroxene mineral comprises (Mg, Mn, Fe, Ca, Ni) (Fe, Ni, Mg, Mn) Si2O6,Na(Al,Fe)Si2O6，Ca(Fe,Al)(Si,Al)2O6One or more of the above;
the calcium iron garnet mineral comprises Mn3Fe2[SiO4]3、Fe3Fe2[SiO4]3And (Ca, Mg)3Fe2[SiO4]3One or more of them.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115572149A (en) * | 2022-10-18 | 2023-01-06 | 广西欧神诺陶瓷有限公司 | Colored ceramic tile prepared from tailings and preparation method thereof |
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