CN112723400B - Method for melting calcium aluminate by synchronously activating, inerting, impurity removing and low-magnesium aluminum ash - Google Patents
Method for melting calcium aluminate by synchronously activating, inerting, impurity removing and low-magnesium aluminum ash Download PDFInfo
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- CN112723400B CN112723400B CN202011500535.7A CN202011500535A CN112723400B CN 112723400 B CN112723400 B CN 112723400B CN 202011500535 A CN202011500535 A CN 202011500535A CN 112723400 B CN112723400 B CN 112723400B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/164—Calcium aluminates
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/064—Dephosphorising; Desulfurising
- C21C7/0645—Agents used for dephosphorising or desulfurising
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for melting calcium aluminate by synchronously activating, inerting, impurity removing and roasting low-magnesium aluminum ash, which comprises the following steps of carrying out wet ball milling on a mixed raw material of the low-magnesium aluminum ash and a calcium-containing additive, and sequentially carrying out solid-liquid separation, drying and roasting on ball-milled materials to obtain a calcium aluminate product; the method takes low-magnesium aluminum ash slag generated in the aluminum smelting process as a raw material to prepare the calcium aluminate product which can be used for steel smelting desulphurization, not only realizes the comprehensive utilization of dangerous waste, but also can obtain higher economic value, and the method has the advantages of simple operation, low cost, environmental friendliness and meeting the requirement of industrial production.
Description
Technical Field
The invention relates to a preparation method of calcium aluminate, in particular to a method for melting calcium aluminate by taking low-magnesium aluminum ash as a raw material and removing impurities through synchronous activation and inerting, belonging to the field of regenerated metal and the field of comprehensive utilization of solid wastes.
Background
The aluminum ash slag is aluminum-containing waste slag formed in the production, processing and recycling processes of metal aluminum and aluminum alloy, and is divided into white slag and black slag. The white slag is aluminum slag generated on the upper layer of molten liquid in the casting process of electrolytic aluminum and secondary aluminum, the content of metallic aluminum in the white slag can reach 80 percent, and the white slag can be used as a secondary aluminum industrial raw material; the black slag is fine ash obtained by recovering metal aluminum from primary aluminum ash by using methods of ash frying, rotary kiln and the like, finely grinding and screening, and the main components of the black slag are aluminum oxide, AlN and Al4C3Metallic aluminum and fluoride, cyanide, NaCl, KCl and SiO2. In the electrolytic aluminum process, 30-50 kg of aluminum ash/ton of aluminum is generated by anode replacement, electrolytic bath overhaul, ingot casting and aluminum discharge; the metal aluminum generates 30-40 kg of aluminum ash/ton of aluminum in the processes of remelting, ingot casting, alloy preparation, casting of parts and the like; the waste aluminum is regenerated to produce 150-250 kg of aluminum ash/ton of aluminum.
Compared with the production process of primary aluminum, the recovery production process of secondary aluminum only needs 5 percent of energy consumption and only discharges 5 percent of greenhouse gas. With the vigorous development of the secondary aluminum industry, the recycling production of the secondary aluminum becomes the development trend of the future aluminum industry, and the yield of the secondary aluminum in China in 2019 reaches 715 ten thousand tons, which is increased by 2.88 percent on a year-by-year basis. In the secondary aluminum industry, raw materials are wide in source (aluminum processing leftover materials, beverage cans, foils, commercial wastes, turning, rolling or casting metals and the like), and the components are complex, and 15-25% of aluminum ash can be formed when one ton of secondary aluminum is produced. According to incomplete statistics, only in the secondary aluminum industry, the aluminum ash generated each year is up to more than 100 million tons.
The white slag mainly contains metal aluminum for recovery because of containing a large amount of metal aluminum. The black slag can adopt a method of separating soluble salt by water leaching to hydrolyze and deactivate partial nitride and carbide to be converted into alumina, and finally the high-alumina deactivated slag produced and converted can be used as raw materials of cement, ceramics, refractory materials, water purifying agents and the like. When the inerted aluminum ash is adopted to produce calcium aluminate as a desulfurizing agent for steelmaking, the content of MgO in the aluminum ash needs to be considered, because magnesium oxide can react with aluminum oxide at high temperature to generate a high-melting-point substance phase of magnesium aluminate spinel, and the magnesium aluminate spinel is more stable in property and more difficult to convert in the inerting process of the aluminum ash. Great difficulty is brought to the subsequent synthesis and purification of calcium aluminate, and the desulfurization performance of the calcium aluminate is obviously reduced by doping a large amount of high-melting-point magnesium aluminate spinel in a calcium aluminate system.
Disclosure of Invention
The invention aims to provide a method for preparing a calcium aluminate product by using low-magnesium aluminum ash as a raw material and combining wet ball milling with high-temperature solid-phase reaction, aiming at solving the technical problems in the process of preparing the calcium aluminate desulfurizer for steel-making desulfurization by using the low-magnesium aluminum ash.
In order to achieve the technical purpose, the invention provides a method for melting calcium aluminate by synchronously activating, inerting, impurity removing and melting low-magnesium aluminum ash.
The technical scheme of the invention uses low-magnesium aluminum ash as a raw material, in order to realize harmless treatment of harmful components and comprehensive utilization and value-added processing of valuable components aluminum, a synergistic treatment process of inerting and impurity removal of wet ball milling, regulation and control of raw material components and high-temperature solid-phase reaction enhanced conversion is adopted, the removal of nitrogen, carbon and soluble salt and conversion and activation of useful aluminum components are realized in the wet ball milling process, active substances such as limestone, slaked lime and the like added in ingredients can promote the smooth solid-phase reaction in the calcium aluminate synthesis process, the synthesis temperature is finally reduced, and the decomposition rate of magnesium aluminate spinel and the generation rate of calcium aluminate are improved. The active calcium oxide generated in the high-temperature solid-phase reaction can replace magnesium oxide in spinel to form calcium aluminate, and the liberated magnesium oxide can be solid-melted into the calcium aluminate to form a composite oxide.
As a preferable scheme, the content of magnesium in the low magnesium aluminum ash is lower than 2.0% by mass, and the content of aluminum in the low magnesium aluminum ash is not lower than 40% by mass. The aluminum in the low-magnesium aluminum ash is a main valuable component, the phase compositions of the low-magnesium aluminum ash are metallic aluminum, aluminum oxide, aluminum nitride, aluminum carbide and the like, and the premise that the phases of the aluminum which can be utilized are converted into calcium aluminate is that the aluminum of the phases is converted into aluminum oxide; besides aluminum compounds, magnesia is also one of the important components of aluminum ash, which is derived from the oxidation of magnesium element in aluminum alloy and is easy to react with alumina to generate magnesia-alumina spinel under high temperature condition, both magnesia and magnesia-alumina spinel are high melting point substances, thus playing a bad role in melting calcium aluminate, and the magnesia-alumina spinel has stable structure and is difficult to decompose and convert; therefore, one of the technical difficulties in preparing calcium aluminate from low-magnesium aluminum ash is to regulate the conversion of magnesium aluminate spinel and magnesium oxide, promote the generation of low-melting-point substances and reduce the melting point of a material system. The higher the content of magnesium in the low-magnesium aluminum ash is, the more unfavorable the preparation process of calcium aluminate is, and the content of magnesium is preferably controlled to be less than 2.0 percent by mass, so that the calcium aluminate with better desulfurization performance can be obtained.
As a preferred embodiment, the calcium-containing additive is a mixture of limestone, slaked lime and quicklime. In the calcium aluminate synthesis process, limestone is one of the most commonly used calcium sources with low price, but limestone has poor reactivity and the decomposition process absorbs heat and forms a large amount of carbon dioxide gas; the active component of the calcined lime is free calcium oxide, the calcined lime is easy to convert and weakly dissociate in the solution under the wet chemical condition, the solution can be controlled to be alkalescent, and a large amount of heat is released; under an alkaline system, the synergistic conversion of metal aluminum, aluminum nitride and aluminum carbide can be promoted, the oxidation of the metal aluminum, the decomposition of the aluminum nitride and the aluminum carbide are enhanced, high-activity aluminum hydroxide is generated, and harmful elements of nitrogen and carbon in the aluminum nitride and the aluminum carbide are converted into gas; the slaked lime can improve the cohesion of materials and improve the reactivity of the raw materials, and by optimally proportioning the limestone, the slaked lime and the quick lime, the use cost of the additive can be reduced, the activity of the materials can be obviously improved, and the phase transformation of the magnesia-alumina spinel and the synthesis of calcium aluminate are promoted.
As a preferable scheme, the content of the calcium-containing additive in the quicklime is more than 50% by mass.
As a preferred scheme, the low magnesium aluminum ash and the calcium-containing additive are mixed to meet the following requirements: the molar ratio Al/(Ca + Mg) is 1 (1.15-1.21). In order to promote the decomposition and conversion of the magnesia-alumina spinel and promote the reaction of the magnesia-alumina spinel and calcium oxide, the magnesia-alumina spinel is converted into calcium aluminate by virtue of the replacement effect that the basicity of CaO is stronger than that of MgO, and the liberated magnesium oxide can be solid-melted into the calcium aluminate to form a composite oxide, and the melting point is lower than 1400 ℃. By means of the calcium-containing additive, the reaction which preferentially takes place is CaO + MgAl2O4＝CaAl2O4+ MgO, with increasing CaO content, the reaction proceeds more easily to the right, and calcium aluminate is more easily formed, and the final target product is calcium aluminate series.
Preferably, the liquid-solid ratio of the wet ball milling is 1mL: 0.3-0.9 g, the ball milling speed is 5-100 r/min, and the ball milling time is 6-12 h. The optimized ball milling rotation speed is 10-50 r/min, on one hand, the conversion and decomposition of aluminum-containing substances are strengthened through mechanical activation by wet ball milling, on the other hand, the activity of products of aluminum oxide and aluminum hydroxide is improved, the contact and particle size matching of calcium-containing substances and aluminum oxide are improved, and the solid phase reaction is facilitated; in addition, impurity elements such as soluble salt and the like in the aluminum ash can be separated in the process of grinding and leaching and solid-liquid separation in the wet ball milling process, so that the deep impurity removal of the aluminum ash is realized. The wet ball milling adopts water as a ball milling medium.
As a preferable scheme, the roasting is a two-stage roasting process in an air atmosphere, the temperature of the first-stage roasting is 400-800 ℃, and the temperature of the second-stage roasting is 1350-1450 ℃. On one hand, the invention adopts a two-stage roasting method to strengthen the oxidation of unreacted and sufficient metal aluminum simple substances in the aluminum ash by one-stage low-temperature roasting and promote the decomposition and conversion of partial calcium-containing flux such as limestone, slaked lime and the like; and the two-stage high-temperature roasting realizes the solid-phase reaction, thereby ensuring the conversion of the components of aluminum, magnesium and calcium in the materials and the generation of calcium aluminate.
As a preferable scheme, the roasting time is 2-4 h; the time of the second-stage roasting is 2-3 h.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) the technical scheme of the invention takes the low-magnesium aluminum ash as the raw material, realizes value-added processing while performing harmless treatment, prepares a calcium aluminate product which can be used as a steelmaking desulfurizer, and has higher economic value;
2) according to the technical scheme, decomposition and removal of harmful substances in the aluminum ash and separation of soluble salt are realized through ball milling inerting and deep activation by a wet method, the inerted product is high-activity aluminum hydroxide with a large specific surface area, and a large amount of calcium hydroxide is formed after quicklime is hydrated, so that inerting conversion of an aluminum-containing compound can be promoted.
3) According to the invention, through regulation and control of raw material components and control of high-temperature roasting conditions, the inerted product can be fully converted into calcium aluminate, a small amount of magnesia-alumina spinel is synergistically converted into calcium-magnesia-alumina composite oxide, the generation of calcium aluminate series substances is enhanced, the system synthesis temperature is reduced, and the conversion rate is improved.
The technical scheme of the invention has the advantages of simple operation, mild synthesis conditions, high utilization rate of raw materials in the low-magnesium aluminum ash, low production cost and environmental friendliness, and meets the requirements of industrial production.
Drawings
FIG. 1 is an XRD pattern of a calcium aluminate product prepared in comparative example 1;
figure 2 is the XRD pattern of the calcium aluminate product prepared in example 1.
Detailed Description
The following examples are intended to further illustrate the present disclosure, but not to limit the scope of the claims.
Comparative example 1
Taking aluminum ash (aluminum content is 63.6 percent and oxygen content is 1.8 percent) of an aluminum smelting plant as a raw material, firstly, mixing aluminum ash slag with a calcium-containing additive, wherein the calcium-containing additive is a mixture of limestone, slaked lime and quick lime (limestone: slaked lime: quick lime is 40 percent and 10 percent and 50 percent), and finally, putting the uniformly mixed sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the first-stage roasting temperature is 800 ℃, and the roasting time is 2 hours; the second stage roasting temperature is 1450 ℃, the roasting time is 3 hours, and the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of the calcium aluminate of the product is detected to be 36.3 percent, and the melting point of the product is 1588 ℃. No wet ball milling stage, no activation of aluminum ash, difficult solid phase reaction in the sintering process, low conversion rate of calcium aluminate and high melting point of the product. As shown in figure 1, a large number of spinel diffraction peaks remained in the product.
Comparative example 2
Taking aluminum ash (aluminum content is 63.6 percent and oxygen content is 1.8 percent) of a certain aluminum smelting plant as a raw material, firstly, mixing aluminum ash slag with a calcium-containing additive, wherein the calcium-containing additive is limestone, and the ratio of the aluminum ash and the calcium-containing additive is controlled within the range of Al (Ca + Mg) ═ 1: 1.15; performing wet ball milling on the uniformly mixed material, wherein the ball milling liquid-solid ratio is 1:0.9, the ball milling rotation speed is 20r/min, and the ball milling time is 6 h; after the ball milling is finished, washing the materials, carrying out solid-liquid separation, and finally placing the dried sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the roasting temperature in one stage is 800 ℃, and the roasting time is 2 hours; the second-stage roasting temperature is 1450 ℃, and the roasting time is 2 hours, so that the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of the calcium aluminate of the product is detected to be 50.3 percent, and the melting point of the product is 1583 ℃. In the wet ball milling stage, the calcium source is only suitable for limestone, the solid phase reaction in the sintering process is difficult, the conversion rate of calcium aluminate is low, and the melting point of the product is high.
Example 1
Aluminum ash (aluminum content is 63.6 percent and oxygen content is 1.8 percent) of an aluminum smelting plant is used as a raw material, the method firstly mixes the aluminum ash slag with a calcium-containing additive, the calcium-containing additive is limestone, slaked lime and a quicklime mixture (limestone: slaked lime: quicklime: 40 percent: 10 percent: 50 percent), and the ratio of the aluminum ash to the calcium-containing additive is controlled within the range of Al (Ca + Mg): 1: 1.15; performing wet ball milling on the uniformly mixed material, wherein the ball milling liquid-solid ratio is 1:0.9, the ball milling rotation speed is 20r/min, and the ball milling time is 6 h; after the ball milling is finished, washing the materials, carrying out solid-liquid separation, and finally placing the dried sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the roasting temperature in one stage is 800 ℃, and the roasting time is 2 hours; the second-stage roasting temperature is 1450 ℃, and the roasting time is 2 hours, so that the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of the calcium aluminate product is 88.7 percent and the melting point of the product is 1405 ℃. As shown in fig. 2, only the calcium aluminate diffraction peak (heptaaluminum dodecacalcium) is present in the product.
Example 2
Aluminum ash (aluminum content 63.6% and oxygen content 1.8%) in certain aluminum smelting plant is used as a raw material, the method comprises the steps of firstly mixing aluminum ash slag with a calcium-containing additive, wherein the calcium-containing additive is a mixture of limestone, slaked lime and quicklime (limestone: slaked lime: quicklime: 20%: 60%), and the ratio of the aluminum ash to the calcium-containing additive is controlled within the range of Al (Ca + Mg): 1: 1.21; performing wet ball milling on the uniformly mixed material, wherein the ball milling liquid-solid ratio is 1:0.3, the ball milling rotation speed is 10r/min, and the ball milling time is 12 h; after the ball milling is finished, washing the materials, carrying out solid-liquid separation, and finally placing the dried sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the roasting temperature in one stage is 400 ℃, and the roasting time is 4 hours; the second-stage roasting temperature is 1350 ℃, and the roasting time is 3 hours, so that the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of the calcium aluminate of the product is detected to be 90.3 percent, and the melting point of the product is 1402 ℃.
Example 3
Taking aluminum ash (aluminum content is 70.6 percent and oxygen content is 1.0 percent) of an aluminum smelting plant as a raw material, firstly, mixing aluminum ash slag with a calcium-containing additive, wherein the calcium-containing additive is a mixture of limestone, slaked lime and quicklime (limestone: slaked lime: quicklime is 20 percent and 30 percent and 50 percent), and the ratio of the aluminum ash to the calcium-containing additive is controlled within the range of Al (Ca + Mg) being 1: 1.18; performing wet ball milling on the uniformly mixed material, wherein the ball milling liquid-solid ratio is 1:0.7, and the ball milling time is 8h, and the ball milling rotating speed is 30 r/min; after the ball milling is finished, washing the materials, carrying out solid-liquid separation, and finally placing the dried sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the roasting temperature in one stage is 800 ℃, and the roasting time is 4 hours; the second-stage roasting temperature is 1350 ℃, and the roasting time is 2 hours, so that the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of the calcium aluminate of the product is detected to be 92.3 percent, and the melting point of the product is 1395 ℃.
Example 4
Taking aluminum ash (aluminum content is 70.6 percent and oxygen content is 1.0 percent) of an aluminum smelting plant as a raw material, firstly, mixing aluminum ash slag with a calcium-containing additive, wherein the calcium-containing additive is a mixture of limestone, slaked lime and quicklime (limestone: slaked lime: quicklime: 10 percent: 80 percent), and the ratio of the aluminum ash to the calcium-containing additive is controlled within the range of Al (Ca + Mg): 1: 1.17; performing wet ball milling on the uniformly mixed material, wherein the ball milling liquid-solid ratio is 1:0.9, and the ball milling time is 10 hours at the ball milling rotating speed of 15 r/min; after the ball milling is finished, washing the materials, carrying out solid-liquid separation, and finally placing the dried sample in an air atmosphere to carry out two-stage temperature-controlled roasting, wherein the roasting temperature in one stage is 700 ℃, and the roasting time is 4 hours; the second-stage roasting temperature is 1390 ℃, and the roasting time is 2 hours, so that the obtained product is the calcium aluminate product which can be used for steel-making desulphurization. The theoretical content of calcium aluminate in the product is 91.0 percent and the melting point of the product is 1398 ℃.
Claims (5)
1. A method for melting calcium aluminate by synchronously activating, inerting, impurity removing and low-magnesium aluminum ash is characterized by comprising the following steps: carrying out wet ball milling on the mixed raw material of the low-magnesium aluminum ash and the calcium-containing additive, and sequentially carrying out solid-liquid separation, drying and roasting on the ball-milled material to obtain a calcium aluminate product;
the mass percent of magnesium in the low-magnesium aluminum ash is lower than 2.0 percent, and the mass percent of aluminum in the low-magnesium aluminum ash is not lower than 40 percent; the calcium-containing additive is a mixture of limestone, slaked lime and quicklime;
wherein, the mixed raw materials of the low-magnesium aluminum ash and the calcium-containing additive meet the following requirements: the molar ratio Al/(Ca + Mg) is 1 (1.15-1.21).
2. The method for melting calcium aluminate by synchronously activating, inerting, impurity removing and according to claim 1, characterized in that: the calcium-containing additive contains quicklime with the mass percentage of more than 50%.
3. The method for melting calcium aluminate by synchronously activating, inerting, impurity removing and according to claim 1, characterized in that: the liquid-solid ratio of the wet ball milling is 1mL: 0.3-0.9 g, the ball milling speed is 5-100 r/min, and the ball milling time is 6-12 h.
4. The method for melting calcium aluminate by synchronously activating, inerting, impurity removing and according to claim 1, characterized in that: the roasting is a two-stage roasting process in an air atmosphere, the temperature of the first-stage roasting is 400-800 ℃, and the temperature of the second-stage roasting is 1350-1450 ℃.
5. The method for melting calcium aluminate by synchronously activating, inerting, impurity removing and according to claim 4, characterized in that: roasting for 2-4 hours; the time of the second-stage roasting is 2-3 h.
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