CN111925223B - Preparation method of active magnesium aluminate spinel powder - Google Patents
Preparation method of active magnesium aluminate spinel powder Download PDFInfo
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- CN111925223B CN111925223B CN202010853130.5A CN202010853130A CN111925223B CN 111925223 B CN111925223 B CN 111925223B CN 202010853130 A CN202010853130 A CN 202010853130A CN 111925223 B CN111925223 B CN 111925223B
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- aluminate spinel
- magnesium aluminate
- aluminum
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- aluminum ash
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- 239000011777 magnesium Substances 0.000 title claims abstract description 45
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 45
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 45
- 239000011029 spinel Substances 0.000 title claims abstract description 45
- -1 magnesium aluminate Chemical class 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 55
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000000034 method Methods 0.000 claims abstract description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001301 oxygen Substances 0.000 claims abstract description 18
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 235000001055 magnesium Nutrition 0.000 claims description 41
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- 235000012245 magnesium oxide Nutrition 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 7
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 7
- 239000001095 magnesium carbonate Substances 0.000 claims description 7
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 235000012254 magnesium hydroxide Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 abstract description 3
- 239000002920 hazardous waste Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 3
- 159000000000 sodium salts Chemical class 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract description 2
- 229910001051 Magnalium Inorganic materials 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 8
- 239000001103 potassium chloride Substances 0.000 description 8
- 235000011164 potassium chloride Nutrition 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 7
- 239000002893 slag Substances 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 5
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 239000011819 refractory material Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical class [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009875 water degumming Methods 0.000 description 1
Images
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- 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
- 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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- 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
- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
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Abstract
The invention discloses a preparation method of active magnesium aluminate spinel powder, and aims to solve the technical problems that in the prior art, a preparation process of magnesium aluminate spinel is complex, energy consumption is high, and the performance of a prepared product is poor. The preparation method of the magnalium spinel powder comprises the following steps: taking the mass percent as 35-90%: 9-60%: 1-5% of aluminum ash, magnesium raw materials and an impurity removing agent to prepare a mixed material; grinding the obtained mixed material; calcining at 1100-1650 ℃ in an oxygen-enriched environment by taking air as a combustion-supporting medium to obtain the catalyst. The invention takes the aluminum ash as the aluminum raw material, thereby realizing the harmless treatment and resource utilization of the hazardous waste; the impurity removing agent can quickly remove impurities such as sodium salt, potassium salt and the like in the aluminum ash, and simultaneously, aluminum nitride in the aluminum ash is quickly oxidized and denitrified at high temperature to generate nontoxic and harmless nitrogen, so that the method is environment-friendly and pollution-free; in the oxygen-enriched high-temperature calcination process, the residual metallic aluminum in the aluminum ash is utilized to release heat in the combustion process, so that the energy consumption is low.
Description
Technical Field
The invention relates to the technical field of refractory materials, in particular to a preparation method of active magnesium aluminate spinel powder.
Background
The magnesia-alumina spinel is a high-quality alkaline refractory material, has high melting point, high strength, good thermal conductivity, good stability and good slag resistance, and is widely applied to the fields of ladle castables, ladle lining bricks, cement rotary kilns and the like. But the synthesis process is accompanied by volume expansion, and the densification requires higher temperature, large energy consumption and higher equipment requirement.
The aluminum ash is waste generated in the industrial production process of aluminum, mainly comprises simple substance aluminum, aluminum compounds, silicon oxide, magnesium oxide, sodium salt, potassium salt, fluoride salt, titanium oxide and the like, and has toxicity and inflammability. Scum generated on the surface of the melt in the processes of transferring, purifying and decontaminating the melt in the electrolytic aluminum process, scum (salt slag and aluminum ash) generated on the surface of the melt in the processes of transferring, purifying and decontaminating the waste aluminum smelting melt, and salt slag and secondary aluminum ash generated in the process of recovering metal aluminum from the aluminum ash and the aluminum slag by a molten salt method are listed in the 2019 edition of national hazardous waste records. According to statistics, each 1 ton of aluminum is produced, 15-30 kg of aluminum ash is probably generated, the domestic aluminum yield in 2019 is 3500 ten thousand tons, the generated aluminum ash is about 52.5-105 ten thousand tons, and the harmlessness and the recycling of the aluminum ash are problems which are urgently needed to be solved in the aluminum industrial production.
On the other hand, chinese patent document CN108585826a discloses a method for preparing magnesia-alumina spinel by using secondary aluminum ash, which is to calcine the secondary aluminum ash at 900-1200 ℃, remove impurities by water leaching, press balls, and then sinter or perform electric melting to prepare magnesia-alumina spinel, and has the disadvantages of complex treatment process, long process flow and large energy consumption; chinese patent document CN105294135A discloses a method for directly preparing an aluminum spinel refractory material by using aluminum ash and a material prepared by the method, wherein magnesium aluminate spinel directly prepared by using the aluminum ash is adopted, but the finished product has low density, high impurity content and poor slag corrosion resistance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of active magnesium aluminate spinel powder, so as to solve the technical problems of complex preparation process and high energy consumption of magnesium aluminate spinel in the prior art while realizing harmless and resource utilization of aluminum ash, and provide raw materials for synthesizing magnesium aluminate spinel by a two-step method.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the active magnesium aluminate spinel powder comprises the following steps:
(1) Mixing 35-90% of aluminum ash, 9-60% of magnesium raw material and 1-5% of impurity removing agent by mass percent to prepare a mixed material;
(2) Grinding the obtained mixed material;
(3) Calcining at 1100-1650 ℃ in an oxygen-enriched environment by taking air as a combustion-supporting medium to obtain the active magnesium aluminate spinel powder.
Preferably, in the step (1), the aluminum ash contains 5 to 15 mass% of Al and Al 2 O 3 50～75%、AlN 10～25%、SiO 2 ≤2%、Fe 2 O 3 ≤1.5%、CaO≤1%。
Preferably, in the step (1), the magnesian raw material is at least one of magnesite, light burned magnesite, periclase and magnesium hydroxide.
Preferably, in the step (1), the purity of the magnesium raw material is more than or equal to 98 percent, and the particle size is controlled to be 200-350 meshes.
Preferably, in the step (1), the impurity removing agent is at least one of ammonium fluoride, ammonium chloride, aluminum fluoride and ammonium carbonate.
Preferably, in the step (2), the particle size of the ground powder is controlled to be 150-325 meshes.
Preferably, in the step (3), the calcination time is controlled to be 0.5 to 1 hour.
Preferably, in the step (3), the oxygen content of the oxygen-rich gas is controlled to be 5-15%, and oxygen is provided for the combustion of the simple substance aluminum and the oxidation denitrification of the aluminum nitride.
In the implementation process of the method, the waste gas generated in each link can be collected by fully utilizing the means and equipment in the prior art, the waste heat of the waste gas is fully utilized, and the tail gas is subjected to harmless treatment and then is discharged after reaching the standard.
Compared with the prior art, the invention has the main beneficial technical effects that:
1. the raw material used in the method is aluminum ash, the aluminum raw material in the aluminum ash is utilized, part of magnesium raw material and impurity removing agent are added, and active magnesium aluminate spinel powder is prepared by high-temperature calcination, once a magnesium aluminate spinel crystal phase is formed, volume expansion can not be generated during secondary sintering, and the active magnesium aluminate spinel powder can be used as a raw material for synthesizing magnesium aluminate spinel by a two-step method, so that long-time high-temperature densification caused by volume expansion in the sintering process is avoided, the comprehensive energy consumption is reduced, and the service life of production equipment is prolonged; realizes the harmless treatment and resource utilization of the hazardous waste.
2. The invention uses the impurity removing agent to gasify NaCl and KCl in the aluminum ash and separate the gasified NaCl and KCl from the aluminum ash, so that the impurities such as sodium salt, sylvite and the like in the aluminum ash can be rapidly and thoroughly removed, and the prepared active magnesium aluminate spinel powder has low impurity content; the NaCl and the KCl are gasified and condensed to become solid for recycling, and the solid can be compounded into an aluminum water refining agent for recycling after being recycled; simultaneously, the aluminum nitride in the aluminum ash is quickly oxidized and denitrified at high temperature to generate nontoxic and harmless nitrogen (4AlN + 3O) 2 =2Al 2 O 3 +2N 2 ) And is environment-friendly and pollution-free.
3. In the oxygen-enriched high-temperature calcination process, the combustion heat release of the metal aluminum remained in the aluminum ash is utilized, the energy consumption is low, namely, the metal aluminum simple substance is combusted to generate a large amount of heat, and a heat source is provided for the calcination: 4Al 3O 2 =2Al 2 O 3 。
4. In the traditional technology, oxygen-enriched combustion replaces air with pure oxygen to carry out fuel combustion, the fuel combustion speed is high, the combustion is sufficient, the flame temperature is high, the smoke is low in black toxicity, and part of smoke is required to be recycled; the invention uses air as combustion-supporting medium, provides enough surplus oxygen in the fuel combustion process to make the fuel fully burn, and simultaneously the excess oxygen makes the solid carbon in the carbon slag fully burn, thereby greatly reducing the production cost.
Drawings
FIG. 1 is an XRD pattern of active magnesium aluminate spinel powder prepared in example 1.
Detailed Description
The following examples are intended to illustrate the present invention in detail and should not be construed as limiting the scope of the present invention in any way.
The starting materials referred to in the following examples are, unless otherwise specified, all commercially available conventional starting materials; the assays or detection methods referred to are conventional, unless otherwise specified.
Example 1: method for preparing active magnesium aluminate spinel powder
Preparing active magnesium aluminate spinel powder by using aluminum ash and light-burned magnesia, wherein the aluminum ash comprises the following components: 7% of Al, al 2 O 3 55%、AlN 20%、SiO 2 1.4%、Fe 2 O 3 0.5 percent of CaO, 0.8 percent of NaCl and KCl, 9 percent of fluoride, 3 percent of granularity, 140 meshes of granularity, 98.5 percent of purity of light-burned magnesia and 325 meshes of granularity; mixing 70 parts of aluminum ash and 30 parts of light-burned magnesia, adding 1 part of ammonium fluoride, and uniformly mixing; grinding to 325 meshes; calcining the powder at 1380 ℃ for 2.5h to obtain active magnesium-aluminum spinel powder, wherein the oxygen content in the calcining process is 10%.
Example 2: method for preparing active magnesium aluminate spinel powder
Selecting aluminum ash (components: al 5%, al) 2 O 3 62%、AlN 15%、SiO 2 0.7%、Fe 2 O 3 1.5 percent of CaO, 1.0 percent of NaCl and KCl, 8 percent of fluoride and 180 meshes of granularity and periclase (the content of magnesium oxide is 98.5 percent and the granularity is 200 meshes) to prepare active magnesium aluminate spinel powder; 80 parts of aluminum ash and 20 parts of periclase are mixed, and then 2 parts of ammonium carbonate is added and mixed uniformly.
Grinding to 200 meshes, calcining at 1450 ℃ for 1h, wherein the oxygen content in the calcining process is 8 percent, and the oxygen content in the calcining process is controlled to be 8 percent.
Example 3: method for preparing active magnesium aluminate spinel powder
Selecting aluminum ash (components: al 10%, al) 2 O 3 50%、AlN 15%、SiO 2 0.5%、Fe 2 O 3 1.5 percent of CaO, 0.8 percent of NaCl and KCl, 8.7 percent of fluoride, 10 percent of fluoride and 180 meshes of granularity and magnesium hydroxide (98 percent of purity and 200 meshes) to prepare active magnesium aluminate spinel powder; 85 parts of aluminum ash and 15 parts of magnesium hydroxide are mixed, and then 2 parts of a mixed remover (comprising ammonium fluoride and ammonium chloride in a weight ratio of 1:1) is added to be uniformly mixed.
Grinding to 325 meshes, calcining at 1400 ℃ for 5h to obtain the active magnesium aluminate spinel powder, wherein the oxygen content is controlled to be 12% in the calcining process.
Example 4: method for preparing active magnesium aluminate spinel powder
Selecting aluminum ash (components: al 10%, al) 2 O 3 65%、AlN 7%、SiO 2 0.5%、Fe 2 O 3 1.5 percent of CaO, 0.5 percent of NaCl and KCl, 4.1 percent of fluoride, 10 percent of granularity 180 meshes) and magnesite (the content of magnesium carbonate is 98.2 percent, and the granularity is 200 meshes) to prepare active magnesium aluminate spinel powder; 60 parts of aluminum ash and 40 parts of magnesite are mixed, 1.5 parts of ammonium chloride is added, and the mixture is uniformly mixed.
Grinding to 325 meshes, and calcining at 1350 ℃ for 10h to obtain the active magnesium aluminate spinel powder, wherein the oxygen content in the calcining process is 12%.
Test example:
taking the active magnesium aluminate spinel powder prepared in the examples 1 to 4, and detecting Al of the active magnesium aluminate spinel powder 2 O 3 、MgO、CaO、Na 2 O+K 2 The content of O. The detection standard is GB/T5069 chemical analysis method for magnesium-aluminum series refractory materials.
The results are shown in Table 1.
TABLE 1 index for active magnesium aluminate spinel powder
As can be seen from Table 1, the magnesium-aluminum alloy product has the advantages of more than 90 percent of magnesium-aluminum alloy content, less impurity components and no more than 0.3 percent of alkali metal oxide content, and meets the component requirements of GBT26564-2011 magnesium-aluminum spinel.
The present invention is described in detail with reference to the examples above; however, those skilled in the art will understand that various changes may be made in the specific parameters of the embodiments described above, or equivalent substitutions of related steps and materials may be made without departing from the spirit of the invention, so as to form a plurality of specific embodiments, which are common variations of the invention and will not be described in detail herein.
Claims (7)
1. The preparation method of the active magnesium aluminate spinel powder is characterized by comprising the following steps:
(1) Mixing 35-90% of aluminum ash, 9-60% of magnesium raw material and 1-5% of impurity removing agent by mass percent to prepare a mixed material; the impurity removing agent is at least one of ammonium fluoride, ammonium chloride and ammonium carbonate;
(2) Grinding the obtained mixed material;
(3) Calcining at 1100-1650 ℃ in an oxygen-enriched environment by taking air as a combustion-supporting medium to obtain the active magnesium aluminate spinel powder.
2. The method for preparing active magnesium aluminate spinel powder according to claim 1, wherein in the step (1), the aluminum ash contains 5-15% of Al and 5-15% of Al in percentage by mass 2 O 3 50～75%、AlN 10～25%、SiO 2 ≤2%、Fe 2 O 3 ≤1.5%、CaO≤1%。
3. The method for preparing active magnesium aluminate spinel powder according to claim 1, wherein in the step (1), the magnesium raw material is at least one of magnesite, light burned magnesite, periclase and magnesium hydroxide.
4. The method for preparing the active magnesium aluminate spinel powder according to claim 1, wherein in the step (1), the purity of the magnesium raw material is more than or equal to 98%, and the particle size is controlled to be 200-350 meshes.
5. The method for preparing active magnesium aluminate spinel powder according to claim 1, wherein in the step (2), the particle size of the ground powder is controlled to be 150-325 meshes.
6. The method for preparing the magnesium aluminate spinel powder according to claim 1, wherein in the step (3), the calcination time is controlled to be 0.5 to 1 hour.
7. The method for preparing magnesium aluminate spinel powder according to claim 1, wherein in the step (3), the oxygen content in the oxygen-rich environment is controlled to be 5-15%.
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