CN111499397B - Method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues - Google Patents
Method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues Download PDFInfo
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Abstract
The invention provides a method for preparing a reclaimed material of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues, which comprises the following steps: A) crushing the hardened anti-seepage material, the insulating brick and the refractory brick in the aluminum-silicon overhaul slag to obtain an initial raw material; B) mixing and reacting the initial raw material with an aqueous solution of an oxidant to remove cyanide in the initial raw material to obtain a treatment solution; C) and mixing the treatment solution with an inhibitor and a trapping agent for flotation, introducing bubbles, and sequentially performing bubble scraping, washing and drying to obtain the reclaimed materials of the aluminum oxide and the silicon oxide. The invention utilizes a flotation method to separate the cryolite from the alumina and the silicon oxide, and then takes the alumina and the silicon oxide as ingredients to prepare the dry type impermeable material, and simultaneously completes the direct recovery of the insulating brick and the refractory brick with relatively complete components and the regeneration treatment of the overhaul slag solid waste.
Description
Technical Field
The invention relates to the technical field of aluminum electrolysis overhaul residues, in particular to a method for preparing a reclaimed material of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues.
Background
China is a big country for manufacturing aluminum industry, and the yield of alumina and electrolytic aluminum accounts for more than 40 percent of the world. In the aluminum production process, a large amount of hazardous waste, commonly called overhaul residue, is generated. In recent years, with the continuous improvement of the national environmental protection requirement, the problem of processing a large amount of waste residues in the aluminum electrolysis industry becomes the first problem to be solved by related enterprises, and an economical and feasible new waste residue utilization technology is urgently needed to be provided. In the aluminum electrolysis industry at present, the common electrolytic bath overhaul residues are aluminum-silicon overhaul residues, and the sources of the aluminum-silicon overhaul residues are light castable, ceramic fiber plates, clay heat-insulating refractory bricks, dry type impermeable materials, high-aluminum refractory bricks, high-strength castable, impermeable bricks and other materials in the electrolytic bath. The overhaul slag contains a large amount of pollutant components, but also contains a plurality of useful components; for the aluminum-silicon overhaul slag, the solid waste contains SiO2、Al2O3、TiO2、Fe2O3The output of the waste residues is up to hundreds of millions of tons every year, the waste residues are not utilized and can only be treated by adopting a stacking method, and serious environmental pollution is caused.
In the aluminum electrolysis production, an anti-seepage material is required to be arranged in an aluminum electrolysis cell and is used for preventing the high-temperature aluminum liquid and electrolyte in the aluminum electrolysis from seepingThe leakage is also an important component of the refractory and heat-insulating material of the aluminum electrolysis cell. At present, the main components of the impermeable material adopted in the industry are SiO2And Al2O3The principle is that when electrolyte permeates and contacts with the impermeable material, the electrolyte reacts with the impermeable material to generate a compact vitreous body-shaped nepheline layer, so that electrolyte liquid and Na and NaF steam are prevented from continuously permeating, the heat-insulating layer is prevented from being damaged, the occurrence of leakage accidents is prevented, the safety production is guaranteed, the service life of the aluminum electrolytic cell is prolonged, and the economic benefit is improved.
Part of the seepage-proofing material in the aluminum-silicon solid waste reacts with electrolyte to form hard lumps, and the rest seepage-proofing material is well preserved with insulating bricks and refractory bricks, which are treated as dangerous waste to cause resource waste.
The scholars propose to regenerate the anti-seepage material by using the waste cell lining of the aluminum electrolysis cell, for example, the Chinese patent with the publication number of CN105130460A proposes a method for regenerating the anti-seepage material by using the waste cell lining of the aluminum electrolysis cell. The method sorts the waste cathode carbon blocks, refractory materials and waste cathode steel bars in the waste cell lining of the aluminum electrolytic cell according to the types, selects the refractory materials in the waste cathode carbon blocks, refractory materials and waste cathode steel bars, crushes the refractory materials into powder, and adds alumina, calcium oxide and the like to mix to prepare the regenerated anti-seepage material. However, the method does not remove the electrolyte in the waste refractory material, the content of the electrolyte is about 40-50%, and when the electrolyte is used as a raw material for manufacturing the anti-seepage material, the content of alumina and silicon oxide playing the role of anti-seepage is reduced, so that the anti-seepage effect is influenced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues, the method can realize the reuse of the overhaul residues and can prepare reclaimed materials of the aluminum oxide and the silicon oxide, and the reclaimed materials can be used as components of dry type impermeable materials.
In view of the above, the present application provides a method for preparing a reclaimed material of aluminum oxide and silicon oxide from an electrolytic bath aluminum-silicon overhaul slag, comprising the following steps:
A) crushing the hardened anti-seepage material, the insulating brick and the refractory brick in the aluminum-silicon overhaul slag to obtain an initial raw material;
B) mixing and reacting the initial raw material with an aqueous solution of an oxidant to remove cyanide in the initial raw material to obtain a treatment solution;
C) and mixing the treatment solution with an inhibitor and a trapping agent for flotation, introducing bubbles, and sequentially performing bubble scraping, washing and drying to obtain the reclaimed materials of the aluminum oxide and the silicon oxide.
Preferably, the particle size of the starting material is not greater than 200 μm.
Preferably, the particle size of the starting material is 150 to 200 μm.
Preferably, the aqueous solution of the oxidant contains sodium hydroxide and one or two of sodium hypochlorite and hydrogen peroxide, and the pH of the aqueous solution of the oxidant is more than 10; and the content of one or two of the sodium hypochlorite and the hydrogen peroxide in the oxidant aqueous solution is 20-30 wt%.
Preferably, the ratio of the starting material to the aqueous solution of the oxidizing agent is 1 g: (2-6) ml.
Preferably, the collector is selected from one or more of oxidized paraffin soap, dicarboxyethyl sulfosuccinamide tetrasodium salt and silicone oil, and the inhibitor is selected from one or more of sodium oxalate, sodium citrate and sodium carboxymethyl cellulose.
The application provides a dry impermeable material, which consists of a reclaimed material of alumina and silica, quartz sand, alumina, calcium oxide and magnesium oxide prepared by the method in the scheme.
Preferably, the reclaimed materials account for 30-55 wt%, the quartz sand accounts for 25-35 wt%, the alumina accounts for 10-20 wt%, the calcium oxide accounts for 5-10 wt%, and the magnesium oxide accounts for 3-8 wt%.
Preferably, the particle size of the reclaimed materials is less than 200 mu m, the particle size of the quartz sand is 2.5-5 mm, the particle size of the aluminum oxide is 0.5-2.5 mm, the particle size of the calcium oxide is 0.5-2.5 mm, and the content of the magnesium oxide is 0.5-2.0 mm.
The application provides a method for preparing a reclaimed material of alumina and silica by using electrolytic bath aluminum-silicon overhaul residues, which separates cryolite from the alumina and the silica in the overhaul residues by using a flotation method, thereby preparing the reclaimed material of the alumina and the silica. The reclaimed material can be used as a batching for further preparing a dry impermeable material. The method provided by the application not only prepares the anti-seepage material, but also solves the problems of environmental pollution caused by the overhaul slag solid waste and economic value generated by recycling the solid waste in the aluminum electrolysis industry.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The method for preparing the reclaimed materials of aluminum oxide and silicon oxide by using the electrolytic bath aluminum-silicon overhaul slag solves the problems of environmental pollution and solid waste reutilization caused by overhaul slag solid waste and impermeable materials in the aluminum electrolysis industry, and particularly, the method for preparing the reclaimed materials of aluminum oxide and silicon oxide by using the electrolytic bath aluminum-silicon overhaul slag comprises the following steps:
A) crushing the hardened anti-seepage material, the insulating brick and the refractory brick in the aluminum-silicon overhaul slag to obtain an initial raw material;
B) mixing and reacting the initial raw material with an aqueous solution of an oxidant to remove cyanide in the initial raw material to obtain a treatment solution;
C) and mixing the treatment solution with an inhibitor and a trapping agent for flotation, introducing bubbles, and sequentially performing bubble scraping, washing and drying to obtain the reclaimed materials of the aluminum oxide and the silicon oxide.
In the process of preparing the reclaimed materials of the alumina and the silica by using the aluminum-silicon overhaul residues of the electrolytic cell, firstly, a hardened anti-seepage material, a heat-insulating brick and a refractory brick in the aluminum-silicon overhaul residues are selected as raw materials of the reclaimed materials of the alumina and the silica, and the raw materials are mixed and crushed to obtain initial raw materials; in the present application, the particle size of the primary raw material is not greater than 200 μm, and in a specific embodiment, the particle size of the primary raw material is 150 to 200 μm. The crushing is a crushing method well known to those skilled in the art, and the present application is not particularly limited, and in a specific embodiment, the crushing is performed by using a ball mill.
The application then mixes and reacts the initial raw material with the aqueous solution of the oxidant to remove the cyanide in the initial raw material; the oxidant is used for removing cyanide in the initial raw material; in a specific embodiment, the aqueous solution of the oxidant contains sodium hydroxide and one or two of sodium hypochlorite and hydrogen peroxide, and the pH of the aqueous solution of the oxidant is more than 10; the content of one or two of the sodium hypochlorite and the hydrogen peroxide in the oxidant aqueous solution is 20-30 wt%; the sodium hydroxide in the aqueous solution of the oxidizing agent is used to adjust the pH of the aqueous solution to a pH above 10 to ensure cyanide oxidation.
Mixing the treated solution with an inhibitor and a trapping agent for flotation, introducing bubbles, and sequentially performing bubble scraping, washing and drying to obtain a reclaimed material of aluminum oxide and silicon oxide; in the flotation process, the trapping agent is used for enabling the surface of the mineral to be easily combined with the bubbles, improving the floatability of the mineral and enabling the mineral to be easily attached to the bubbles. The inhibitor is used for inhibiting the combination of non-target minerals and bubbles, and reducing the floatability of the minerals. The inhibitor and the capture agent are obtained by analyzing the physical and chemical properties of the electrolyte and the carbon powder; the collector is selected from one or more of oxidized paraffin soap, dicarboxyethyl succinamide tetrasodium salt and silicone oil, and the inhibitor is selected from one or more of sodium oxalate, sodium citrate and sodium carboxymethyl cellulose. The above-mentioned processes of foam scraping, water washing and drying are technical means well known to those skilled in the art, and the present application is not particularly limited.
After the reclaimed materials of the alumina and the silicon oxide are obtained, the reclaimed materials are used as the components of the dry impermeable material and are mixed with quartz sand, the alumina, the calcium oxide and the magnesium oxide to obtain the dry impermeable material.
Because the main component of the anti-seepage material is SiO2And Al2O3Reacting with an electrolyteGeneration of Na2O·Al2O3·2SiO2Therefore, in order to maximize the effect of the anti-seepage material, SiO in the materials2With Al2O3The proportion should be in the range of 2: around 1. In view of this, the reclaimed material is 30 to 55wt%, the quartz sand is 25 to 35wt%, the alumina is 10 to 20wt%, the calcium oxide is 5 to 10wt%, and the magnesium oxide is 3 to 8 wt%.
The particle sizes of the reclaimed materials of the alumina and the silicon oxide, the quartz sand, the alumina, the calcium oxide and the magnesium oxide also influence the seepage-proofing effect of the seepage-proofing material; in a specific embodiment, the particle size of the reclaimed material is less than 200 μm, the particle size of the quartz sand is 2.5-5 mm, the particle size of the aluminum oxide is 0.5-2.5 mm, the particle size of the calcium oxide is 0.5-2.5 mm, and the content of the magnesium oxide is 0.5-2.0 mm.
The application provides a novel treatment method of overhaul residues, namely a method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues, which comprises the steps of firstly removing well-preserved impermeable materials, insulating bricks and refractory bricks by a flotation method and recycling; and crushing the other part of the overhaul slag, and then adding a reagent for treatment to obtain a dry anti-seepage material raw material for preparing the anti-seepage material.
For further understanding of the present invention, the method for preparing a barrier material by using an electrolytic bath aluminum siliceous overhaul slag provided by the present invention is described in detail below with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
1) Selecting hardened anti-seepage materials positioned at the lower part of a cathode in the aluminum-silicon overhaul residues, well-preserved insulating bricks and refractory bricks, and crushing the materials by using a ball mill until the particle size of the powder is 150-200 microns;
2) preparing an aqueous solution with the sodium hypochlorite content of 25%, and simultaneously adding NaOH into the aqueous solution to ensure that the pH value of the aqueous solution is about 13 to obtain an oxidant aqueous solution;
3) mixing the particles obtained in step 1) with the aqueous solution of an oxidizing agent obtained in step 2) in a ratio of 1: 3, proportioning, mixing and stirring for two hours; NaOH is added into the aluminum silicon overhaul slag during stirring to ensure that the pH value is always above 10 in the whole process, and the purpose of the step is to remove cyanide in the aluminum silicon overhaul slag;
4) adding an inhibitor and a trapping agent into the treated solution, wherein the collecting agent is oxidized paraffin soap, the inhibitor is sodium oxalate, stirring uniformly, introducing bubbles, and sequentially scraping, washing and drying to obtain an aluminum oxide and silicon oxide reclaimed material; the recovered material contains about 53% of silicon oxide, 96.5% of aluminum oxide and silicon oxide, and 3.5% of impurities
5) Mixing the prepared reclaimed materials with quartz sand, aluminum oxide, calcium oxide and magnesium oxide according to a proportion, wherein the specific proportion and the granularity requirement are as follows:
and pouring the materials into a stirrer, and uniformly mixing to obtain the dry impermeable material.
SiO in the impermeable material prepared by the method2And Al2O3The content is more than 85%, the tap density is 1.97g/cm3, the bulk density is 1.60g/cm3, the electrolyte permeation resistance is within 15mm under the experimental condition of 96h, and the thermal conductivity is 0.43W/m at 600 ℃.
Example 2
1) Selecting hardened anti-seepage materials positioned at the lower part of a cathode in the aluminum-silicon overhaul residues, well-preserved insulating bricks and refractory bricks, and crushing the materials by using a ball mill until the particle size of the powder is 150-200 microns;
2) preparing an aqueous solution with the hydrogen peroxide content of 20%, and simultaneously adding NaOH into the aqueous solution to ensure that the pH value is about 12 to obtain an oxidant aqueous solution;
3) mixing the particles obtained in step 1) with an aqueous solution of an oxidizing agent in a ratio of 1: 6, proportioning, mixing and stirring for two hours; NaOH is added into the aluminum silicon overhaul slag during stirring to ensure that the pH value is always above 11 in the whole process, and the purpose of the step is to remove cyanide in the aluminum silicon overhaul slag;
4) adding an inhibitor and a trapping agent into the treated solution, wherein the collecting agent is dicarboxyethyl succinamide sulfide tetrasodium salt, the inhibitor is sodium oxalate and sodium carboxymethyl cellulose, uniformly stirring, introducing bubbles, and sequentially scraping, washing and drying to obtain an aluminum oxide and silicon oxide reclaimed material; the content of silicon oxide is about 56 percent, the total purity of aluminum oxide and silicon oxide is 97.2 percent, and the content of impurities is 2.8 percent
5) Mixing the prepared reclaimed materials with quartz sand, aluminum oxide, calcium oxide and magnesium oxide according to a proportion, wherein the specific proportion and the granularity requirement are as follows:
and pouring the materials into a stirrer, and uniformly mixing to obtain the dry impermeable material.
SiO in the impermeable material prepared by the method2And Al2O3The content is more than 85%, the tap density is 1.87g/cm3, the bulk density is 1.51g/cm3, the electrolyte permeation resistance is within 15mm under the experimental condition of 96h, and the thermal conductivity is 0.37W/m at 600 ℃.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A method for preparing reclaimed materials of aluminum oxide and silicon oxide by using electrolytic bath aluminum-silicon overhaul residues comprises the following steps:
A) crushing the hardened anti-seepage material, the insulating brick and the refractory brick in the aluminum-silicon overhaul slag to obtain an initial raw material;
B) mixing and reacting the initial raw material with an aqueous solution of an oxidant to remove cyanide in the initial raw material to obtain a treatment solution;
C) mixing the treatment solution with an inhibitor and a trapping agent for flotation, introducing bubbles, and sequentially performing bubble scraping, washing and drying to obtain a reclaimed material of aluminum oxide and silicon oxide;
the aqueous solution of the oxidant contains sodium hydroxide and one or two of sodium hypochlorite and hydrogen peroxide, and the pH value of the aqueous solution of the oxidant is more than 10;
the trapping agent is selected from one or more of oxidized paraffin soap, dicarboxyethyl succinamide tetrasodium salt and organic silicone oil, and the inhibitor is selected from one or more of sodium oxalate, sodium citrate and sodium hydroxymethyl cellulose.
2. The method of claim 1, wherein the particle size of the starting material is no greater than 200 μm.
3. The method according to claim 1 or 2, wherein the particle size of the starting material is 150 to 200 μm.
4. The method according to claim 1, wherein the content of one or both of the sodium hypochlorite and the hydrogen peroxide in the aqueous oxidant solution is 20 to 30 wt%.
5. The method according to claim 4, characterized in that the ratio of the initial charge to the aqueous solution of the oxidizing agent is 1 g: (2-6) ml.
6. A dry type impermeable material, which consists of reclaimed materials of alumina and silica prepared by the method of any one of claims 1 to 5, quartz sand, alumina, calcium oxide and magnesium oxide; the recycled material content is 30-55 wt%, the quartz sand content is 25-35 wt%, the alumina content is 10-20 wt%, the calcium oxide content is 5-10 wt%, and the magnesium oxide content is 3-8 wt%; the particle size of the reclaimed materials is less than 200 mu m, the particle size of the quartz sand is 2.5-5 mm, the particle size of the aluminum oxide is 0.5-2.5 mm, the particle size of the calcium oxide is 0.5-2.5 mm, and the content of the magnesium oxide is 0.5-2.0 mm.
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