CN112919512B - Method for preparing aluminum oxide and potassium sulfate by using brown corundum dust-removing ash - Google Patents
Method for preparing aluminum oxide and potassium sulfate by using brown corundum dust-removing ash Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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Abstract
The invention discloses a method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust, which comprises the following steps: 1) Mixing brown corundum dust and potassium pyrosulfate or potassium bisulfate, grinding, and roasting to obtain clinker; 2) Dissolving clinker with water, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag; 3) Respectively obtaining aluminum sulfate and potassium sulfate by evaporating and crystallizing by utilizing the difference of the solubility of the aluminum sulfate and the potassium sulfate; 4) The aluminum sulfate is roasted to obtain an aluminum oxide product, so that the recovery of potassium and aluminum in the brown alumina dust is realized. The invention has the characteristics of simple process, high recovery rate of aluminum and potassium and low recovery cost.
Description
Technical Field
The invention relates to a method for recovering valuable components in brown corundum dust, in particular to a method for preparing aluminum oxide and potassium sulfate by using brown corundum dust.
Background
A large amount of dust substances can be generated in the smelting process of brown fused alumina, if serious air pollution is caused by the fact that the dust substances cannot be effectively treated, the pollution of the brown fused alumina to air and water bodies is mainly reduced in a collecting and accumulating mode by a brown fused alumina production enterprise at present, and the brown fused alumina cannot be effectively utilized.
Because of the difference of smelting raw material sources and smelting processes, the brown corundum dust-removing ash has more complex components, and the main components comprise about 40 percent of silicon dioxide, 20-30 percent of aluminum oxide and 10-20 percent of potassium oxide, if the aluminum and the potassium in the brown corundum dust-removing ash can be effectively recovered, and silicon is enriched in residues, the problem of brown corundum dust-removing ash accumulation pollution can be solved, and the added value of products can be improved. Researchers have conducted extensive research with respect to recovery of valuable components from brown alumina fly ash.
The patent publication No. CN103060573A discloses a comprehensive recovery process of valuable components in corundum smelting dust containing gallium and potassium, wherein the corundum dust is subjected to pretreatment, acid leaching, neutralization, alkali dissolution, seed and electrolysis and other procedures to comprehensively recover the components such as gallium, potassium, aluminum hydroxide and the like, but the problems of overlarge alkali consumption and the like caused by the fact that neutralization and alkali dissolution are needed after acid leaching due to a plurality of operation steps are limited, and the large-scale industrial application of the corundum dust is limited.
The method is simple and low in energy consumption, and can separate out part of potassium elements, but the dissolution rate of potassium is not high, and the recovery of aluminum cannot be realized, so that the method has no popularization value in actual industrial production.
Disclosure of Invention
The invention aims to provide a method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust. The invention has the characteristics of simple process, high recovery rate of aluminum and potassium and low recovery cost.
The technical scheme of the invention is as follows: a method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust removal ash comprises the following steps:
1) Mixing brown corundum dust and potassium pyrosulfate or potassium bisulfate, grinding, and roasting to obtain clinker;
2) Dissolving clinker with water, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag;
3) Respectively obtaining aluminum sulfate and potassium sulfate by evaporating and crystallizing by utilizing the difference of the solubility of the aluminum sulfate and the potassium sulfate;
4) The aluminum sulfate is roasted to obtain an aluminum oxide product, so that the recovery of potassium and aluminum in the brown alumina dust is realized.
In the aforementioned method for preparing aluminum oxide and potassium sulfate by using brown alumina dust, in the step 1), the molar ratio of the aluminum oxide to potassium pyrosulfate, potassium bisulfate or concentrated sulfuric acid in the brown alumina dust is 1:3-8.
In the aforementioned method for preparing aluminum oxide and potassium sulfate by using brown corundum dust, in the step 1), the roasting temperature is 210-380 ℃ and the roasting time is 30-360min.
In the step 2), the clinker is dissolved in water at 20-100 ℃ for 30-180min, and the liquid-solid ratio is 3-15.
In the step 3), the evaporating crystallization is to raise the evaporating crystallization temperature to 80-100 deg.c, evaporating and concentrating to separate out potassium sulfate crystal until the concentration of aluminum sulfate reaches 731-890g/L, adding new aluminum-potassium containing sulfate solution, cooling to room temperature, collecting crystallized aluminum sulfate, and repeating the steps to separate aluminum from potassium.
In the aforementioned method for preparing aluminum oxide and potassium sulfate by using brown alumina dust, in the step 4), the roasting temperature of aluminum sulfate is 770-950 ℃.
In the method for preparing aluminum oxide and potassium sulfate by using brown alumina dust, the hot sulfur trioxide gas generated by roasting in the step 4) reacts with part of potassium sulfate prepared in the step 3), so that the regeneration of potassium pyrosulfate or potassium bisulfate is realized, and the potassium pyrosulfate or potassium bisulfate is reused for the treatment of the brown alumina dust.
The beneficial effects of the invention are that
The invention is characterized in that the brown corundum dust-removing ash is ground, mixed and roasted with potassium pyrosulfate or potassium bisulfate, so that potassium and aluminum in the dust-removing ash react with the potassium pyrosulfate or the potassium bisulfate to generate water-soluble sulfate, then the aluminum sulfate and the potassium bisulfate are utilized to separate crystallization and precipitation by utilizing the difference of solubility properties, aluminum sulfate is roasted at high temperature to obtain an aluminum oxide product, and the potassium sulfate can be directly used for fertilizer production and the like. The whole process is simple, the energy consumption is low, no alkali is consumed, and the cost for recovering valuable elements from the brown alumina dust is greatly reduced.
In addition, the potassium sulfate obtained by the invention can also react with hot sulfur trioxide gas generated during aluminum sulfate roasting to realize the regeneration of potassium pyrosulfate or potassium bisulfate and is reused for the production of brown alumina dust, thereby omitting the external addition of potassium pyrosulfate or potassium bisulfate, further reducing the cost, realizing the full utilization of substances and being suitable for wide popularization in industry.
The invention extracts and recovers the aluminum and the potassium through the process steps of additive mixing roasting, water leaching, crystallization separation and the like, and has the advantage of high recovery rate, wherein the recovery rate of the potassium is more than 90 percent, and the recovery rate of the aluminum is more than 85 percent.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
Embodiments of the invention
The recovery rate of aluminum and potassium according to the invention is calculated by adopting a formula (1):
wherein eta is the recovery rate of potassium or aluminum, m 1 The quality (g), omega of the filter residue 1 Content of potassium or aluminum (wt.%) in the filter residue, m 0 Omega is the mass (g) of the brown corundum dust 0 Is the content (wt.%) of potassium or aluminum in the fly ash.
Example 1
A method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust removal ash comprises the following specific steps:
1) Grinding and uniformly mixing brown corundum dust-removing ash and potassium pyrosulfate in a molar ratio of 1:4, and roasting at 360 ℃ for 150min to obtain roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching at 85 ℃ for 60min with a liquid-solid ratio of 4, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 90 ℃, the potassium sulfate crystal is evaporated and concentrated until the concentration of aluminum sulfate reaches 731-890g/L, then a new aluminum potassium sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 800 ℃ to obtain an aluminum oxide product, reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate, regenerating potassium pyrosulfate, and re-using the regenerated potassium pyrosulfate for the treatment of brown alumina dust.
In this example, the potassium and aluminum recovery rates were 96.1% and 91.2%, respectively.
Example 2
A method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust removal ash comprises the following specific steps:
1) Grinding and mixing brown corundum dust-removing ash and potassium pyrosulfate uniformly in a molar ratio of aluminum oxide to potassium ammonium pyrosulfate of 1:5, roasting at 300 ℃ for 180min, and obtaining roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching for 40min at 90 ℃ with a liquid-solid ratio of 6, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 80 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 850 ℃ to obtain an aluminum oxide product, reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate, regenerating potassium pyrosulfate, and re-using the regenerated potassium pyrosulfate for the treatment of brown alumina dust.
In this experiment, the potassium and aluminum recovery rates were 96.5% and 94.2%, respectively.
Example 3
A method for preparing aluminum oxide and potassium sulfate by utilizing brown alumina dust removal ash comprises the following specific steps:
1) Grinding and uniformly mixing brown corundum dust-removing ash and potassium pyrosulfate in a molar ratio of aluminum oxide to potassium ammonium pyrosulfate of 1:3.5, roasting at 380 ℃ for 120min, and obtaining roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching at 85 ℃ for 60min with a liquid-solid ratio of 4, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 85 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 880 ℃ to obtain an aluminum oxide product, reacting the byproduct hot sulfur trioxide gas with the crystallized and separated potassium sulfate, and regenerating potassium pyrosulfate, so that the aluminum oxide product can be reused for treating brown alumina dust.
In this experiment, potassium and aluminum recovery rates were 93.3% and 86.4%, respectively.
Example 4
A method for efficiently recycling aluminum and potassium in brown corundum dust ash comprises the following specific steps:
1) Grinding and mixing brown corundum dust-removing ash and potassium bisulfate uniformly in a molar ratio of aluminum oxide to potassium bisulfate of 1:6, and roasting at 240 ℃ for 300min to obtain roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching for 60min at 95 ℃ with a liquid-solid ratio of 8, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 95 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 800 ℃ to obtain an aluminum oxide product, reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate, and regenerating potassium bisulfate, so that the potassium bisulfate can be reused for the treatment of brown alumina dust.
In this experiment, potassium and aluminum recovery rates were 94.6% and 92.1%, respectively.
Example 5
A method for efficiently recycling aluminum and potassium in brown corundum dust ash comprises the following specific steps:
1) Grinding and mixing brown corundum dust-removing ash and potassium bisulfate uniformly in a molar ratio of aluminum oxide to potassium bisulfate of 1:7, roasting at 280 ℃ for 150min, and obtaining roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching at 85 ℃ for 60min with a liquid-solid ratio of 6, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 100 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 850 ℃ to obtain an aluminum oxide product, reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate, regenerating potassium pyrosulfate, and re-using the regenerated potassium pyrosulfate for the treatment of brown alumina dust.
In this experiment, the potassium and aluminum recovery rates were 95.6% and 93.1%, respectively.
Example 6
A method for efficiently recycling aluminum and potassium in brown corundum dust ash comprises the following specific steps:
1) Grinding and mixing brown corundum dust-removing ash and potassium bisulfate uniformly in a molar ratio of aluminum oxide to potassium bisulfate of 1:8, roasting at 370 ℃ for 30min, and obtaining roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching for 30min at 100 ℃ with a liquid-solid ratio of 15, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 80 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 900 ℃ to obtain an aluminum oxide product, reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate, and regenerating potassium bisulfate, so that the potassium bisulfate can be reused for the treatment of brown alumina dust.
Example 7
A method for efficiently recycling aluminum and potassium in brown corundum dust ash comprises the following specific steps:
1) Grinding and mixing brown corundum dust and concentrated sulfuric acid uniformly in a molar ratio of alumina to concentrated sulfuric acid of 1:3, roasting at 210 ℃ for 360min, and obtaining roasting clinker after the reaction is completed;
2) Dissolving clinker in water, leaching for 180min at 20 ℃ with a liquid-solid ratio of 3, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the silicon-rich slag can be used for producing siliceous products;
3) Crystallization separation of aluminum sulfate and potassium sulfate by utilizing the difference of solubility properties of aluminum sulfate and potassium sulfate; the evaporating crystallization is that the evaporating crystallization temperature is firstly increased to 100 ℃, potassium sulfate crystals are separated out by evaporating concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, thus the purpose of separating aluminum from potassium can be achieved;
4) Roasting aluminum sulfate at 770 ℃ to obtain an aluminum oxide product, and reacting the by-product hot sulfur trioxide gas with the crystallized and separated potassium sulfate to regenerate potassium pyrosulfate which can be reused for the treatment of brown alumina dust.
While the invention has been described with reference to the preferred embodiments, it should be understood that the invention is not limited to the embodiments described above, but is intended to cover modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (4)
1. The method for preparing the aluminum oxide and the potassium sulfate by using the brown alumina dust is characterized by comprising the following steps of:
1) Mixing brown corundum dust and potassium pyrosulfate, potassium bisulfate or concentrated sulfuric acid, grinding, and roasting to obtain clinker, wherein the roasting temperature is 210-380 ℃ and the roasting time is 30-360min;
2) Dissolving clinker in water, and separating liquid from solid to obtain aluminum-potassium-containing sulfate solution and silicon-rich slag, wherein the dissolving temperature of the clinker in water is 20-100 ℃, the dissolving time is 30-180min, and the liquid-solid ratio is 3-15;
3) By utilizing the difference of solubility of aluminum sulfate and potassium sulfate, firstly, the temperature of aluminum-potassium-containing sulfate solution is raised to 80-100 ℃, potassium sulfate crystals are separated out by evaporation and concentration until the concentration of aluminum sulfate reaches 731-890g/L, then new aluminum-potassium-containing sulfate solution is added, after the temperature is reduced to room temperature, the crystallized aluminum sulfate is collected, and then the steps are repeated, so that the purpose of aluminum-potassium separation can be achieved, and aluminum sulfate and potassium sulfate are respectively obtained;
4) The aluminum sulfate is roasted to obtain an aluminum oxide product, so that the recovery of potassium and aluminum in the brown alumina dust is realized.
2. The method for preparing aluminum oxide and potassium sulfate by using brown alumina fly ash according to claim 1, wherein: in the step 1), the molar ratio of the alumina to the potassium pyrosulfate, the potassium bisulfate or the concentrated sulfuric acid in the brown corundum dust is 1:3-8.
3. The method for preparing aluminum oxide and potassium sulfate by using brown alumina fly ash according to claim 1, wherein: in the step 4), the roasting temperature of aluminum sulfate is 770-950 ℃.
4. The method for preparing aluminum oxide and potassium sulfate by using brown alumina fly ash according to claim 1, wherein: and (3) reacting the hot sulfur trioxide gas generated by roasting in the step (4) with part of potassium sulfate prepared in the step (3) to realize the regeneration of potassium pyrosulfate or potassium bisulfate, and reusing the potassium pyrosulfate or potassium bisulfate in the treatment of brown alumina dust.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3484196A (en) * | 1966-04-04 | 1969-12-16 | Pechiney Prod Chimiques Sa | Process for treatment of coal schists for recovery of contained aluminum,iron and potassium |
| CN102515221A (en) * | 2011-12-02 | 2012-06-27 | 吉林大学 | Method for extracting alumina and amorphous silica from fly ash or coal gangue |
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| CN104058434B (en) * | 2014-04-30 | 2016-06-01 | 清华大学 | Produce the method for aluminum oxide |
| CN104445325B (en) * | 2014-12-05 | 2016-06-01 | 福州大学 | A kind of from containing the method extracting aluminium hydroxide potassium, aluminum ore |
| CN106477606B (en) * | 2016-10-12 | 2018-03-20 | 北京矿冶研究总院 | Method for extracting aluminum oxide from fly ash based on sulfuric acid curing |
| CN106477609B (en) * | 2016-10-12 | 2018-06-15 | 北京矿冶研究总院 | Method for producing alumina by coal ash sulfuric acid curing |
| CN110510648B (en) * | 2019-09-24 | 2021-01-01 | 中国科学院过程工程研究所 | Method for separating and recovering aluminum, potassium and ammonium from mixed solution containing aluminum sulfate, potassium sulfate and ammonium sulfate |
| CN113024285A (en) * | 2021-03-01 | 2021-06-25 | 贵州大学 | Method for recovering potassium and aluminum from brown corundum dust |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3484196A (en) * | 1966-04-04 | 1969-12-16 | Pechiney Prod Chimiques Sa | Process for treatment of coal schists for recovery of contained aluminum,iron and potassium |
| CN102515221A (en) * | 2011-12-02 | 2012-06-27 | 吉林大学 | Method for extracting alumina and amorphous silica from fly ash or coal gangue |
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