CN109876929B - Flotation method for recycling aluminum electrolysis anode covering material - Google Patents
Flotation method for recycling aluminum electrolysis anode covering material Download PDFInfo
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Abstract
The invention belongs to the technical field of solid waste recovery in the aluminum electrolysis industry, and provides a flotation method for recovering aluminum electrolysis anode covering materials, which is characterized in that the powder of the aluminum electrolysis anode covering materials is subjected to size mixing by water, and flotation is carried out after a flotation reagent is added, wherein the flotation reagent comprises a collecting agent, a pH regulator and an inhibitor; collecting agent is one or more of sodium oleate, sodium linoleate, potassium oleate and potassium soyate, and pH regulator is one or more of sodium carbonate, sodium hydroxide and calcium oxide; the inhibitor is one or more of sodium carboxymethylcellulose and sodium methylenedinaphthalenesulfonate. The method can effectively separate the main components of cryolite and alumina in the aluminum electrolysis anode covering material, and the used medicament system is simple, foaming agents and dispersing agents are not required to be added, and the used medicaments are low in cost and easy to purchase. Therefore, the invention provides an economical and feasible method for treating the aluminum electrolysis anode covering material.
Description
Technical Field
The invention relates to the technical field of recycling of wastes in the electrolytic aluminum industry, in particular to a flotation method for recycling aluminum electrolysis anode covering materials.
Background
With the continuous increase of domestic electrolytic aluminum production capacity, more and more electrolytic aluminum solid wastes are generated, and the wastes pollute the environment and cause economic loss. The electrolytic aluminum anode covering material is a cryolite/alumina-based covering material, is used for protecting the anode, has the effects of reducing anodic oxidation, reducing iron-carbon pressure drop, preserving heat and the like, although the cryolite/alumina-based covering material can be recycled, in actual production, the electrode changing operation can lead a large amount of electrolyte to be taken out as the covering material, so that the more the waste covering materials of an electrolytic aluminum plant are accumulated, and the recycling is needed urgently. At present, the recycling of the covering materials has not attracted people's attention, but the huge amount cannot be ignored.
The main components of the waste covering material are alumina, cryolite, calcium fluoride, magnesium fluoride, potassium fluoride and the like with low content. No research has been made on the separation of coatings or similar component substances by flotation, and few research reports on the flotation agents for cryolite have been found; therefore, no collector or inhibitor for floating cryolite can be used for reference in the existing literature, so that the research on the flotation method of the anode covering material can solve the problem of comprehensive utilization of solid waste, can also research the flotation mechanism of cryolite, and provides a feasible scheme for the treatment of other electrolytic aluminum solid wastes.
Disclosure of Invention
Technical problem to be solved
The invention aims to provide a flotation method for recovering aluminum electrolysis anode covering materials, which treats the waste aluminum electrolysis anode covering materials by a flotation method, realizes the high separation of cryolite and alumina, and recovers the cryolite and the alumina.
(II) technical scheme
A flotation method for recovering aluminum electrolysis anode covering materials is characterized in that powder of the aluminum electrolysis anode covering materials is slurried with water, and subjected to flotation after a flotation reagent is added, wherein the flotation reagent comprises a pH regulator, an inhibitor and a collector; the pH regulator is one or more of sodium carbonate, sodium hydroxide and calcium oxide; the collecting agent is one or more of sodium oleate, sodium linoleate, potassium oleate and potassium soyate; the inhibitor is one or more of sodium carboxymethylcellulose and sodium methylene dinaphthalenesulfonate.
In a preferred embodiment of the invention, the flotation process comprises the following steps:
s1, preparing raw materials: crushing, grinding and screening the aluminum electrolysis anode covering material;
s2, mixing the prepared raw materials and water according to the mass ratio of 1:1.5-3.5, and performing size mixing to obtain ore pulp to be floated;
and S3, after the ore pulp to be floated is placed into a flotation tank, stirring is started, then a pH regulator is added to adjust the pH of the ore pulp to be floated to 7-10, then the inhibitor is added, stirring is continued, finally the collecting agent is added, and after stirring is fully performed, air flotation and foam scraping are performed.
In a preferred embodiment of the present invention, step S1 includes: and (3) crushing the blocky aluminum electrolysis anode covering material into small blocks, grinding the small blocks by using a ball mill, screening the small blocks by using a 200-mesh screen after grinding, and returning screened objects to the ball mill for regrinding after the screened objects enter the step S2.
The primary separation of cryolite and alumina is realized by grinding and screening, and the mutual coating and the influence on the flotation effect are avoided.
In a preferred embodiment of the present invention, in step S1, the mixture is ground for 30 to 50 minutes by using a dry ball mill.
In a preferred embodiment of the present invention, in step S2, the prepared raw materials and water are mixed and slurried in a mass ratio of 1: 2.
In a preferred embodiment of the present invention, in step S3, when the inhibitor is sodium carboxymethyl cellulose, the amount is 0.05-0.4 kg/t; taking the raw materials as a reference, and when the inhibitor is sodium methylene dinaphthalene sulfonate, the dosage is 0.2-0.35 kg/t;
in step S3, when the raw material is taken as a reference and the collecting agent is sodium oleate, the dosage of the collecting agent is 0.2-1.2 kg/t; when the raw material is taken as a reference and the collecting agent is potassium oleate, the dosage of the collecting agent is 0.2-1.2 kg/t.
In a preferred embodiment of the present invention, in step S3, after the pH of the slurry to be floated is adjusted to 9, preferably by using CaO as a pH adjuster, sodium carboxymethylcellulose or sodium methylenedinaphthalene sulfonate as an inhibitor and sodium oleate as a collector are sequentially added to the flotation cell.
In a preferred embodiment of the invention, in step S3, the collector and the inhibitor are added to the flotation cell in the form of aqueous solution; the collecting agent is sodium oleate, the concentration of the aqueous solution of the collecting agent is 9-10%, the inhibitor is sodium carboxymethyl cellulose, and the mass concentration of the aqueous solution of the inhibitor is 1.5-3%.
More preferably, the mass concentration of the sodium hydroxide aqueous solution is 30%, the mass concentration of the sodium oleate aqueous solution is 10%, and the mass concentration of the sodium carboxymethyl cellulose aqueous solution is 2%.
In a preferred embodiment of the present invention, in step S3, pH adjuster, inhibitor and collector are added to the flotation cell in sequence, and after adding one agent each time, the mixture is stirred for 2-5 minutes before proceeding to the next step.
In a preferred embodiment of the present invention, in step S3, the aerated flotation froth scraping time is 4-7 minutes.
In a preferred embodiment of the invention, the flotation process further comprises a concentration step S4: and (4) diluting the bubbles scraped in the step (S3) with water, and then concentrating, wherein the flotation agent is not added in the concentration.
(III) advantageous effects
The invention has the beneficial effects that:
the invention firstly provides a flotation method for recovering the electrolytic aluminum anode covering material, and the main components of alumina and cryolite in the electrolytic aluminum anode covering material are separated, so that the covering material of an electrolytic aluminum plant is prevented from being wasted, the problem of comprehensive utilization of solid wastes of the aluminum electrolytic plant is solved, and a feasible scheme is provided for the treatment of other electrolytic aluminum solid wastes.
The flotation method can effectively separate the cryolite and the alumina, and the used medicament system is simple, foaming agents and dispersing agents are not required to be added, and the used medicaments are low in cost and easy to purchase, so that the method is economical and feasible for treating the aluminum electrolysis anode covering material.
Drawings
FIG. 1 is a schematic flow chart of a flotation method for recovering aluminum electrolysis anode covering material according to a preferred embodiment of the invention.
Detailed Description
As shown in fig. 1, a schematic flow chart of a flotation method for recovering aluminum electrolysis anode covering material according to a preferred embodiment of the present invention includes:
s1, preparing raw materials: crushing, grinding and screening the aluminum electrolysis anode covering material; the massive aluminum electrolysis anode covering material is crushed into small blocks, then is ground by a ball mill, and is sieved by a 200-mesh (below 0.074mm and capable of being sieved) screen after being ground, the undersize material enters the step S2, and the oversize material returns to the ball mill to be ground and sieved again.
Preferably, the mulch broken into small pieces is ground using a dry ball mill for 30-50 minutes.
The primary separation of cryolite and alumina is realized by grinding and screening, and the mutual coating and the influence on the flotation effect are avoided.
S2, size mixing: mixing the prepared raw materials and water according to the mass ratio of 1:1.5-3.5, and performing size mixing to obtain ore pulp to be floated, preferably according to the following raw materials: mixing and pulping water in a mass ratio of 1: 2.
S3, air flotation: and (2) after the ore pulp to be floated is placed into a flotation tank, stirring is started, then a pH regulator is added to adjust the pH of the ore pulp to be floated to 7-10, then the inhibitor is added, stirring is continued, finally a collecting agent is added, and after stirring is fully carried out, air flotation and foam scraping are carried out for 4-7 minutes.
Wherein: the pH regulator is one or more of sodium carbonate, sodium hydroxide and calcium oxide; the collecting agent is one or more of sodium oleate, sodium linoleate, potassium oleate and potassium soyate; the inhibitor is one or more of sodium carboxymethylcellulose and sodium methylenedinaphthalenesulfonate.
After the flotation tank is started to stir, the raw materials can be fully dispersed in water, firstly, a pH regulator is added to adjust the pH to 7-10, then, an inhibitor is added, after full stirring, a collecting agent is finally added, and after stirring for 2-3 minutes, aeration flotation and foam scraping are started.
The sodium oleate is used as a collecting agent, and the dosage of the sodium oleate is 0.2-1.2kg/t by taking the weight of the raw materials as a reference. Before use, water is added for dilution, and sodium oleate and water are prepared into an aqueous solution according to the mass ratio of 1: 9.
When sodium carboxymethylcellulose is selected as an inhibitor, the dosage of the sodium carboxymethylcellulose is 0.05-0.4kg/t based on the weight of the raw materials, and water is added to prepare an aqueous solution with the mass concentration of 1.5-3% before use; when the sodium methylene dinaphthalenesulfonate is selected as the inhibitor, the dosage of the sodium methylene dinaphthalenesulfonate is 0.2-0.35 kg/t.
The pH regulator is one or more of sodium carbonate, sodium hydroxide and calcium oxide; adjusting the pH value of the ore pulp to 7-10 by using an adjusting agent. Preferably, sodium hydroxide is used as a pH regulator, and an aqueous solution with the mass concentration of 28-32% is prepared before use.
S4: selecting: and (4) diluting the roughing bubbles scraped in the step (S3) with water, and then carrying out concentration, wherein the flotation agent is not added in the concentration.
The features and technical effects of the present invention are further described below with reference to specific examples.
The raw materials adopted in the following examples are all the same covering material, and the main components of the covering material comprise about 31 wt% of alumina, 53 w% of cryolite, 14 wt% of other fluorides and 2 wt% of carbon blocks.
Example 1
The embodiment provides a flotation method for recovering aluminum electrolysis anode covering materials, which comprises the following steps:
(1) crushing the aluminum electrolysis anode covering material, grinding for 30 minutes by using a dry ball mill, screening by using a 200-mesh vibrating screen after grinding, checking screen underflow, and returning screen overflow for grinding again.
(2) The raw materials are prepared and then are mixed with water, warm water is added into the raw materials according to the mass ratio of 1:2 of the raw materials to the water, and the temperature of the uniformly mixed slurry is about 30 ℃, preferably 33-38 ℃.
(3) Preparing a flotation reagent: preparing the flotation reagents into an aqueous solution, wherein: the mass concentration of the inhibitor sodium carboxymethyl cellulose aqueous solution is 2%, the mass concentration of the collecting agent sodium oleate aqueous solution is 10%, and the mass concentration of the pH regulator sodium hydroxide aqueous solution is 30%.
(4) And (3) putting the slurry obtained in the step (2) into a flotation tank of a flotation machine, opening a main shaft, stirring for 2 minutes, fully dispersing, adding a sodium hydroxide solution to adjust the pH value of the slurry to 9, adding an inhibitor sodium carboxymethyl cellulose solution with the dosage of 200g/t (calculated by solute sodium carboxymethyl cellulose), adding a collector sodium oleate with the dosage of 800g/t (calculated by solute sodium oleate), stirring for 2 minutes, then starting inflation and foam scraping, and scraping for 4 minutes.
(5) Adding water into the roughly selected bubbles until the roughly selected bubbles are diluted to 1L, and then finely selecting the bubbles without adding a flotation agent.
Through 4 times of experiments, the content of alumina in the rough concentrate is about 29.04%, and the content of cryolite in the rough concentrate is about 54.37%. The content of cryolite in the tailings is about 32.76 percent, and the content of cryolite is 52.45 percent. The concentration concentrate has an alumina content of about 30.28% and a cryolite content of about 55.23%.
Example 2
The flotation process of this example differs from that of example 1 in that: calcium oxide powder is used as a pH regulator, the pH is still adjusted to 9, and the use amount of sodium oleate is reduced to 200 g/t.
After 4 flotation passes, the alumina content in the concentrate was found to be about 25.57% and the cryolite content was found to be about 56.76%, the alumina content in the rougher tailings was found to be about 37.38% and the cryolite content was found to be about 47.07%. Wherein the roughing yield is about 63% and the beneficiating yield is about 25%.
Example 3
This example differs from example 2 in that: sodium methylenedinaphthalenesulfonate was used as an inhibitor in an amount of 0.35 kg/t.
After 4 flotation passes, the alumina content in the concentrate was found to be about 28.37% and the cryolite content was found to be about 56.97%, the alumina content in the rougher tailings was found to be about 37.71% and the cryolite content was found to be about 45.65%. Wherein the roughing yield is about 70% and the beneficiating yield is about 62%.
Among them, the flotation separation effect of the embodiment 3 is quite equivalent to that of the embodiment 2, and is obviously better than that of the embodiment 1. From this, when calcium oxide was used as a pH adjuster to adjust the pH to 9 and sodium oleate was used as a collector, the flotation separation effect obtained was excellent when either sodium carboxymethylcellulose or sodium methylenedinaphthalene sulfonate was used as an inhibitor.
Example 4
This example differs from example 3 only in that the roughing lather time was adjusted from 4 minutes to 7 minutes.
After 5 flotation passes, the alumina content in the rougher concentrate was found to be about 27.96%, the cryolite content was found to be about 54.20%, the alumina content in the rougher tailings was found to be about 36.93%, the cryolite content was found to be about 44.17%, the alumina content in the cleaner concentrate was found to be about 26.87%, and the cryolite content was found to be about 57.04%. Wherein the roughing yield is about 82% and the beneficiating yield is about 55%.
Therefore, the bubble scraping time of the aerated flotation is prolonged, and the roughing yield is favorably improved. The roughing efficiency of the embodiment is optimal.
Example 5
In this example, sodium carbonate was used as a pH adjuster, adjusted to pH 8, sodium oleate was used in an amount of 1200g/t, and the inhibitor was sodium carboxymethylcellulose was used in an amount of 200g/t, in comparison with example 1.
After 4 flotation passes, the alumina content in the rougher concentrate was found to be about 30.32%, the cryolite content was found to be about 54.98%, the alumina content in the rougher tailings was found to be about 33.41%, the cryolite content was found to be about 49.17%, the alumina content in the cleaner concentrate was found to be about 30.09%, and the cryolite content was found to be about 55.31%. Wherein the rougher yield is about 75% and the cleaner yield is about 63%.
Example 6
In this example, sodium carbonate was used as a pH adjuster to adjust the pH to 9, potassium oleate was used as a collector in an amount of 200g/t, and sodium methylenedinaphthalenesulfonate was used as an inhibitor in an amount of 200g/t, in comparison with example 1.
After 4 flotation passes, the rougher tailings were found to have an alumina content of about 33.78% and a cryolite content of about 48.67%, the cleaner concentrates had an alumina content of about 30.84% and a cryolite content of about 55.82%. Wherein the roughing yield is about 73% and the beneficiating yield is about 62%.
Example 7
In this example, sodium carbonate was used as a pH adjuster to adjust the pH to 9, potassium oleate was used as a collector in an amount of 1200g/t, and sodium methylenedinaphthalenesulfonate was used as an inhibitor in an amount of 200g/t, in comparison with example 1.
After 4 flotation passes, the alumina content in the rougher tailings was found to be about 34.32%, the cryolite content was found to be about 48.54%, the alumina content in the cleaner concentrate was found to be about 29.87%, and the cryolite content was found to be about 55.85%. Wherein the roughing yield is about 73 percent and the concentrating yield is about 60 percent.
Example 8
This example compares to example 1 using CaO powder as pH adjuster, adjusted to pH 9, sodium linoleate used in an amount of 350g/t, and inhibitor sodium carboxymethylcellulose used in an amount of 400 g/t.
After 4 flotation passes, the alumina content in the rougher tailings was determined to be about 35.38%, the cryolite content was determined to be about 46.65%, the alumina content in the cleaner concentrate was determined to be about 27.92%, and the cryolite content was determined to be about 56.82%. Wherein the roughing yield is about 70% and the beneficiating yield is about 62%.
Example 9
This example compares to example 1 using CaO powder as a pH adjuster to a pH of 9, potassium soyate in an amount of 800g/t, and the inhibitor sodium carboxymethyl cellulose in an amount of 50 g/t.
After 4 flotation passes, the alumina content in the rougher tailings was found to be about 34.06% and the cryolite content was found to be about 48.53%, the alumina content in the cleaner concentrate was found to be about 30.18% and the cryolite content was found to be about 55.91%. Wherein the roughing yield is about 73 percent and the concentrating yield is about 63 percent.
Comparative example 1
In the comparative example, on the basis of example 2, sodium carbonate is used as a pH regulator, the pH is adjusted to 9, a collector is dodecylamine and is used in an amount of 120g/t, and an inhibitor is sodium carboxymethylcellulose and is used in an amount of 200 g/t.
After 4 flotation passes, the rougher concentrate was found to have an alumina content of about 15.02%, a cryolite content of about 33.85%, and a rougher yield of about 20%. From the above comparison, it is understood that the flotation separation effect of comparative example 1 is poor.
The embodiment shows that the flotation method can effectively separate the cryolite and the alumina, and the medicament system of the invention is simple, foaming agents and dispersing agents are not required to be added, and the used medicaments have low cost and are easy to purchase. Therefore, the invention provides an economical and feasible method for treating the aluminum electrolysis anode covering material.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations. In addition, any combination of the technical features in the above embodiments is also included in the present invention when the combination of the features is not contradictory.
Claims (8)
1. A flotation method for recovering aluminum electrolysis anode covering materials is characterized in that the flotation method comprises the steps of mixing powder of the aluminum electrolysis anode covering materials with water to obtain slurry, adding a flotation reagent, and then carrying out flotation, wherein the flotation reagent comprises a pH regulator, an inhibitor and a collector; the pH regulator is one or more of sodium carbonate, sodium hydroxide and calcium oxide; the collecting agent is one or more of sodium oleate, sodium linoleate, potassium oleate and potassium soyate; the inhibitor is one or more of sodium carboxymethylcellulose and sodium methylene dinaphthalene sulfonate;
the flotation method comprises the following steps:
s1, preparing raw materials: crushing, grinding and screening the aluminum electrolysis anode covering material;
s2, mixing the prepared raw materials and water according to the mass ratio of 1:1.5-3.5, and performing size mixing to obtain ore pulp to be floated;
s3, after the ore pulp to be floated is placed into a flotation tank, stirring is started, then a pH regulator is added to adjust the pH of the ore pulp to be floated to 7-10, then the inhibitor is added, stirring is continued, finally a collecting agent is added, and after stirring is fully carried out, air flotation and foam scraping are carried out;
in step S3, when the raw materials are taken as the reference and the inhibitor is sodium carboxymethyl cellulose, the dosage is 0.05-0.4 kg/t; taking the raw materials as a reference, and when the inhibitor is sodium methylene dinaphthalene sulfonate, the dosage is 0.2-0.35 kg/t;
in step S3, when the raw material is taken as a reference and the collecting agent is sodium oleate, the dosage of the collecting agent is 0.2-1.2 kg/t; when the raw material is taken as a reference and the collecting agent is potassium oleate, the dosage of the collecting agent is 0.2-1.2 kg/t.
2. The flotation method according to claim 1, wherein step S1 includes: and (3) crushing the blocky aluminum electrolysis anode covering material into small blocks, grinding the small blocks by using a ball mill, screening the small blocks by using a 200-mesh screen after grinding, and returning screened objects to the ball mill for regrinding after the screened objects enter the step S2.
3. A flotation method according to claim 1, wherein in step S2, the prepared raw material is mixed with water and size-mixed according to a mass ratio of 1: 2.
4. A flotation process according to claim 1 or 2, characterized in that in step S3, after the pH of the slurry to be floated is adjusted to 9, preferably using CaO as a pH adjuster, sodium carboxymethylcellulose or sodium methylene bis naphthalene sulfonate as an inhibitor and sodium oleate as a collector are added to the flotation cell in sequence.
5. The flotation method according to claim 1 or 2, wherein in step S3, the collector and the inhibitor are added into the flotation tank in the form of aqueous solution; the collecting agent is sodium oleate, the concentration of the aqueous solution of the collecting agent is 9-10%, the inhibitor is sodium carboxymethyl cellulose, and the mass concentration of the aqueous solution of the inhibitor is 1.5-3%.
6. A flotation process according to claim 1 or 2, wherein in step S3, the pH adjuster, the depressor and the collector are added to the flotation cell in sequence, and each time one agent is added, the mixture is stirred for 2-5 minutes before the next step.
7. The flotation process according to claim 1 or 2, wherein in step S3, the aerated flotation froth is scraped for 4 to 7 minutes.
8. The flotation process according to claim 1 or 2, further comprising a concentration step S4: and (4) diluting the bubbles scraped in the step (S3) with water, and then concentrating, wherein the flotation agent is not added in the concentration.
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