CN110436498B - Method for recovering high-purity alumina from secondary aluminum ash at smelting end of secondary aluminum - Google Patents
Method for recovering high-purity alumina from secondary aluminum ash at smelting end of secondary aluminum Download PDFInfo
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- C22B21/00—Obtaining aluminium
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Abstract
The invention relates to the technical field of recovery of alumina, and discloses a method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting, which comprises the following steps: s1, grinding and screening the black ash to obtain fine ash; s2, mixing and stirring the fine ash in the S1 and a dissolving agent in a reaction chamber, absorbing overflowed gas by using an ammonia gas absorption tower, filtering and separating out residues, washing the residues, and mixing washing liquor into filtrate for later use; s3, adding a precipitator into the filtrate, wherein precipitates and gas are generated; s4, adding a purifying agent into the filtrate of S3, adjusting the pH value of the solution to 12-14, filtering and separating out precipitates, washing the precipitates, and mixing washing liquor into the filtrate for later use; s5, mixing CO2Introducing gas into the filtrate of S4 to generate precipitate, filtering, separating, washing and drying the precipitate; s6, and roasting the precipitate in the S5 to obtain the alumina product. The invention realizes the recycling of the aluminum ash and conforms to the sustainable scientific development.
Description
Technical Field
The invention relates to the technical field of recovery of alumina, in particular to a method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting.
Background
In the production process of primary aluminum and secondary aluminum, alloy elements in aluminum liquid, metal oxides, nitrides and complex compounds generated by the reaction of aluminum with oxygen, nitrogen, injected fuel gas and the like in air at high temperature are mixed with impurities in the aluminum liquid, salts in a solvent and aluminum water which does not separate from slag, and the slag is aluminum ash, so the aluminum ash usually contains metal aluminum, aluminum oxide, aluminum nitride, molten salt mixture and other components. In the production process of aluminum, the generation of aluminum ash cannot be avoided, mainly from three aspects, firstly, in the process of producing aluminum by electrolyzing aluminum oxide through molten salt, 3-5 kg of aluminum ash can be generated in each 100kg of electrolyzed aluminum; secondly, in the processing processes of casting, ingot casting, remelting for multiple times, alloy preparation and the like of aluminum parts, 3-4 kg of aluminum ash is generated when 100kg of aluminum or waste aluminum is processed averagely; thirdly, in the process of remelting and recovering aluminum scrap and recycling aluminum slag, 15-25 kg of aluminum ash is generated for each 100kg of regenerated aluminum.
The aluminum ash can be divided into primary aluminum ash and secondary aluminum ash, wherein the primary aluminum ash has higher aluminum content and is silver gray, also called white ash; the secondary aluminum ash has a low aluminum content and is black, also called black ash. The secondary aluminum ash comprises 10-30% of aluminum, 30-70% of aluminum oxide, about 10% of silicon dioxide, about 5% of ferric oxide and 10-30% of chloride (containing sodium, magnesium, potassium, calcium and the like). The recycling treatment of the secondary aluminum ash is a key and difficult point of the comprehensive utilization of the aluminum industrial waste, and the recycling of the aluminum ash at present can be mainly divided into four aspects: the recovery of metal aluminum in the aluminum ash, the recovery of salt in the aluminum ash, the recovery of aluminum oxide in the aluminum ash and the production of special aluminum oxide, and functional materials or auxiliary materials thereof can also be produced by utilizing the aluminum ash.
Although much research is carried out on aluminum ash, a mature method for recycling aluminum slag in a high-value and environment-friendly mode is not available at present, most black ash at the tail end of the aluminum industry is mainly stockpiled, land resources are occupied, and harmful substances in the ash can enter the environment through diffusion, so that the human health is harmed, and the ecological environment is broken. National records of hazardous waste (2016) specify: four kinds of waste residues, namely waste residue generated by maintenance and abandonment of an electrolytic cell in the aluminum electrolysis process, primary smelting waste residue generated in the aluminum pyrometallurgical process, salt slag and scum generated in the aluminum electrolysis process, and inflammable skimming slag generated in the aluminum pyrometallurgical process, belong to HW48 nonferrous metal smelting waste. Therefore, the effective recovery of valuable components in the aluminum ash, the improvement of the recovery rate of aluminum in the aluminum ash and the realization of the recycling and harmless comprehensive utilization of the aluminum ash are not only requirements for realizing energy conservation, emission reduction and circular sustainable scientific development, but also necessary guarantees for building green industry, civilized ecology and the like.
Disclosure of Invention
The invention aims to provide a method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting, and aims to achieve the aims of recycling the aluminum ash and sustainable scientific development.
The technical purpose of the invention is realized by the following technical scheme: a method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting comprises the following steps:
s1, recovering metal aluminum: grinding and screening the black ash, and stacking the screened fine ash for later use;
s2, dissolved alumina: mixing and stirring the fine ash in the S1 and a dissolving agent in a reaction chamber, absorbing overflowed gas by using an ammonia gas absorption tower, filtering and separating out residues, washing the residues, and mixing washing liquor into filtrate for later use;
s3, metal ion coprecipitation: adding a precipitator into the filtrate, wherein precipitation and gas are generated;
s4, purifying and removing impurities: adding a purifying agent into the filtrate of S3, adjusting the pH value of the solution to 12-14, filtering and separating out precipitate, washing the precipitate, and mixing washing liquor into the filtrate for later use;
s5, aluminum oxide reprecipitation: introducing CO2Introducing gas into the filtrate of S4 to generate precipitate, filtering, separating, washing and drying the precipitate;
s6, roasting: and roasting the precipitate in S5 to obtain an alumina product.
The invention is further provided with: the screen sieved in the S1 is 60 meshes.
The invention is further provided with: the dissolving agent in the S2 is one or a mixture of more of hydrochloric acid, sulfuric acid and nitric acid, the concentration of hydrogen ions is 4-6 mol/L, the dissolving temperature is 70-90 ℃, and the mass ratio of the acid solution to the aluminum ash in the S1 is 15-25: 1, the dissolution time is 100-200 min.
The invention is further provided with: the ammonia gas absorbed in the S2 is applied to the recovery of ammonium salt, and the residue is applied to refractory materials, building materials or auxiliary materials thereof.
The invention is further provided with: and the precipitant added in the S3 is one or a mixture of more of sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate, and the S3 retention time is 120-180 min.
The invention is further provided with: and the purifying agent added in the S4 is sodium hydroxide, potassium hydroxide or a mixture thereof, and the time for adding the purifying agent is 100-180 min.
The invention is further provided with: CO used in said S52And part or all of the gas is derived from the gas generated in the S3, the filtered solution can be reused in the S3, and the reprecipitation time is 150-250 min.
The invention is further provided with: the roasting temperature in the S6 is 700-800 ℃, and the time is 120-180 min.
The invention is further provided with: and putting the metal aluminum particles which are not sieved in the S1 into a smelting furnace to recover aluminum.
The invention has the beneficial effects that: the production method is simple and easy to implement, has low requirements on equipment and production sites, requires low temperature, is carried out at normal pressure, recycles waste liquid and waste gas, avoids environmental pollution, efficiently recovers valuable components in aluminum ash, obtains an active aluminum oxide product with high purity and fine granularity, and can be used in industries such as catalysis, adsorption or biological materials; meanwhile, the waste gas can be used for recovering ammonium salt, and the residue can be used for producing refractory materials, building materials or auxiliary materials thereof, so that the aluminum ash is recycled, and the requirements of sustainable development are met.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow diagram of an embodiment of the method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
A method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting comprises the following steps:
s1, recovering metal aluminum: further grinding the black ash fried by the rotary kiln, separating fine aluminum particles and residual ash by using a 60-mesh sieve, putting unseparated metal aluminum particles into a smelting furnace to recover aluminum, and stacking the separated fine ash for later use;
s2, dissolved alumina: mixing and stirring the fine ash and a dissolving agent in a reaction chamber for dissolving, wherein the dissolving agent is a hydrochloric acid solution, the concentration of hydrogen ions is 4mol/L, the dissolving temperature is 70 ℃, and the mass ratio of the acid solution to the aluminum ash in S1 is 15: 1, the dissolving time is 100min, the dissolving process is carried out under normal pressure, overflowed gas is absorbed by an ammonia absorption tower and can be used for recovering ammonium salt, residues are filtered and separated out, the residues are washed, the residues can be used for producing refractory materials, building materials or auxiliary materials thereof, and washing liquor is mixed into filtrate for standby;
s3, metal ion coprecipitation: adding a precipitator into the filtrate, wherein the precipitator is sodium carbonate, keeping the pH value of the solution at 4.3 for 120min after adding the precipitator, simultaneously generating precipitate and gas, and leading out the gas through a gas collecting device;
s4, purifying and removing impurities: adding a purifying agent into the reaction chamber, wherein the added purifying agent is sodium hydroxide, the time of keeping the added sodium hydroxide is 100min, the pH value of the solution is 12.5, most of the precipitate is dissolved, a small amount of the precipitate is remained and cannot be dissolved, filtering and separating the precipitate, washing the precipitate, and mixing washing liquor into the filtrate for later use;
s5, aluminum oxide reprecipitation: introducing sufficient carbon dioxide gas derived from S3 into the filtrate to generate a large amount of precipitate, filtering, separating, washing the precipitate, drying, treating the filtrate mixed with washing liquid (such as adding precipitant), recycling into S3, and standing for 150 min;
s6, roasting: the precipitate in S5 was calcined at 700 deg.C for 120min to give an alumina product with a purity of 98.3% and a recovery of alumina of 92.1%.
Example 2
A method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting comprises the following steps:
s1, recovering metal aluminum: further grinding the black ash fried by the rotary kiln, separating fine aluminum particles and residual ash by using a 60-mesh sieve, putting unseparated metal aluminum particles into a smelting furnace to recover aluminum, and stacking the separated fine ash for later use;
s2, dissolved alumina: mixing and stirring the fine ash and a dissolving agent in a reaction chamber for dissolving, wherein the dissolving agent is a mixed solution of sulfuric acid and nitric acid with equal molar concentration, the concentration of hydrogen ions in the mixed solution is 6mol/L, the dissolving temperature is 90 ℃, and the mass ratio of the acid solution to the aluminum ash in S1 is 25: 1, the dissolving-out time is 200min, the dissolving-out process is carried out under normal pressure, overflowed gas is absorbed by an ammonia absorption tower and can be used for recovering ammonium salt, residues are filtered and separated out, the residues are washed, the residues can be used for producing refractory materials, building materials or auxiliary materials thereof, and washing liquor is mixed into filtrate for standby;
s3, metal ion coprecipitation: adding a precipitator into the filtrate, wherein the precipitator is a mixture of sodium bicarbonate and potassium carbonate with equal mass, keeping the solution for 180min after the precipitator is added, the pH value of the solution is 4.6, precipitates and gas are generated simultaneously, and the gas is led out through a gas collecting device;
s4, purifying and removing impurities: adding a purifying agent into the reaction chamber, continuously adjusting the pH value of the solution, wherein the added purifying agent is potassium hydroxide, the time for keeping the added potassium hydroxide is 180min, the pH value of the solution is 13.2, most of the precipitate is dissolved, a small amount of the precipitate is remained and cannot be dissolved, filtering to separate out the precipitate, washing the precipitate, and mixing washing liquor into filtrate for later use;
s5, aluminum oxide reprecipitation: introducing sufficient carbon dioxide gas derived from S3 into the filtrate to generate a large amount of precipitate, filtering, separating, washing the precipitate, drying, treating the filtrate mixed with washing liquid (such as adding precipitant), recycling into S3, and allowing the precipitation process to last for 250 min;
s6, roasting: the precipitate in S5 was calcined at 800 ℃ for 180min to give an alumina product with a purity of 98.7% and a recovery of alumina of 92.6%.
Example 3
A method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting comprises the following steps:
s1, recovering metal aluminum: further grinding the black ash fried by the rotary kiln, separating fine aluminum particles and residual ash by using a 60-mesh sieve, putting unseparated metal aluminum particles into a smelting furnace to recover aluminum, and stacking the separated fine ash for later use;
s2, dissolved alumina: mixing and stirring the fine ash and a dissolving agent in a reaction chamber for dissolving, wherein the dissolving agent is a mixed solution of hydrochloric acid, sulfuric acid and nitric acid with equal molar concentration, the concentration of hydrogen ions in the mixed solution is 5mol/L, the dissolving temperature is 80 ℃, and the mass ratio of the acid solution to the aluminum ash in S1 is 20: 1, the dissolution time is 150min, the dissolution process is carried out under normal pressure, an ammonia absorption tower is used for absorbing overflowed gas, the ammonia absorption tower can be used for recovering ammonium salt, residues are filtered and separated out, the residues are washed, the residues can be used for producing refractory materials, building materials or auxiliary materials thereof, and washing liquor is mixed into filtrate for standby;
s3, metal ion coprecipitation: adding precipitant which is equal mass of mixed potassium carbonate and potassium bicarbonate into the filtrate, and keeping for 150min after adding the precipitant. At the moment, the pH value of the solution is 5.2, precipitation and gas are generated at the same time, and the gas is led out through a gas collecting device;
s4, purifying and removing impurities: adding a purifying agent into the reaction chamber, wherein the added purifying agent is sodium hydroxide and potassium hydroxide which are mixed by equal mass, the time for adding the purifying agent is 140min, the pH value of the solution is 13.5, most of precipitate is dissolved, a small amount of precipitate is remained and cannot be dissolved, filtering to separate out the precipitate, washing the precipitate, and mixing washing liquor into filtrate for later use;
s5, aluminum oxide reprecipitation: introducing sufficient carbon dioxide gas derived from S3 into the filtrate to generate a large amount of precipitate, filtering, separating, washing the precipitate, drying, treating the filtrate mixed with washing liquid (such as adding precipitant), recycling into S3, and standing for 200 min;
s6, roasting: the precipitate in S5 was calcined at 700 deg.C for 150min to yield an alumina product with a purity of 99.1% and a recovery of alumina of 93.5%.
The pH value of the solution after the metal ion coprecipitation is completed in S3 needs to be kept between 4 and 6, the pH value of the solution after the purification and impurity removal is completed in S4 needs to be between 12 and 14, and the first to third examples only represent data shown in three practical experiments, but not represent only the data.
It should be noted that, in the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments may be referred to each other.
The above description is only for the purpose of describing the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention, and any variations and modifications made by those skilled in the art based on the above disclosure are within the scope of the appended claims.
Claims (5)
1. A method for recovering high-purity alumina from secondary aluminum ash at the smelting end of secondary aluminum is characterized by comprising the following steps: the method comprises the following steps:
s1, recovering metal aluminum: grinding and screening the black ash, and stacking the screened fine ash for later use;
s2, dissolved alumina: mixing and stirring the fine ash in the S1 and a dissolving agent in a reaction chamber, absorbing overflowed gas by using an ammonia gas absorption tower, filtering and separating out residues, washing the residues, and mixing washing liquor into filtrate for later use;
s3, metal ion coprecipitation: adding a precipitator into the filtrate, wherein precipitation and gas are generated at the moment, and the pH value of the solution is required to be kept between 4 and 6 after the metal ion coprecipitation is completed;
s4, purifying and removing impurities: adding a purifying agent into the filtrate of S3, adjusting the pH value of the solution to 12-14, filtering and separating out precipitate, washing the precipitate, and mixing washing liquor into the filtrate for later use;
s5, aluminum oxide reprecipitation: introducing CO2Introducing gas into the filtrate of S4 to generate precipitate, filtering, separating, washing and drying the precipitate;
s6, roasting: roasting the precipitate in the S5 to obtain an alumina product;
the dissolving agent in the S2 is one or a mixture of more of hydrochloric acid, sulfuric acid and nitric acid, the concentration of hydrogen ions is 4-6 mol/L, the dissolving temperature is 70-90 ℃, and the mass ratio of the acid solution to the aluminum ash in the S1 is 15-25: 1, the dissolving time is 100-200 min;
the precipitator added in the S3 is one or a mixture of more of sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate, and the S3 retention time is 120-180 min;
the purifying agent added in the S4 is sodium hydroxide, potassium hydroxide or a mixture thereof, and the time for adding the purifying agent is 100-180 min;
CO used in said S52And part or all of the gas is derived from the gas generated in the S3, the filtered solution can be reused in the S3, and the reprecipitation time is 150-250 min.
2. The method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting according to claim 1, wherein the method comprises the following steps: the screen sieved in the S1 is 60 meshes.
3. The method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting according to claim 1, wherein the method comprises the following steps: the ammonia gas absorbed in the S2 is applied to the recovery of ammonium salt, and the residue is applied to refractory materials, building materials or auxiliary materials thereof.
4. The method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting according to claim 1, wherein the method comprises the following steps: the roasting temperature in the S6 is 700-800 ℃, and the time is 120-180 min.
5. The method for recovering high-purity alumina from secondary aluminum ash at the tail end of secondary aluminum smelting according to claim 1, wherein the method comprises the following steps: and putting the metal aluminum particles which are not sieved in the S1 into a smelting furnace to recover aluminum.
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| CN111607709A (en) * | 2020-05-29 | 2020-09-01 | 重庆新格环保科技有限公司 | Method for performing harmless treatment on hazardous waste electrolytic aluminum ash |
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| CN111519033A (en) * | 2020-05-29 | 2020-08-11 | 重庆新格环保科技有限公司 | Method for performing harmless treatment on hazardous waste raw material secondary aluminum ash |
| CN113441510A (en) * | 2021-07-01 | 2021-09-28 | 格尔木弘钜环保科技有限公司 | Landfill method for treating waste by waste through treating aluminum ash with industrial waste acid |
| WO2023039490A1 (en) * | 2021-09-10 | 2023-03-16 | Hydrova Inc. | Obtaining valuable solids and combustible gas from aluminum remelting waste |
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