CN110938838A - Method for treating anode carbon slag of aluminum electrolysis cell by using NaCl molten salt extraction method - Google Patents

Method for treating anode carbon slag of aluminum electrolysis cell by using NaCl molten salt extraction method Download PDF

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CN110938838A
CN110938838A CN201911073837.8A CN201911073837A CN110938838A CN 110938838 A CN110938838 A CN 110938838A CN 201911073837 A CN201911073837 A CN 201911073837A CN 110938838 A CN110938838 A CN 110938838A
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nacl
molten salt
primary
carbon
carbon slag
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CN110938838B (en
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彭建平
梁诚
狄跃忠
魏征
王耀武
冯乃祥
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Northeastern University China
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/06Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
    • C25C3/18Electrolytes
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    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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Abstract

A method for treating anode carbon slag of an aluminum electrolysis cell by using a NaCl molten salt extraction method comprises the following steps; (1) crushing anode carbon slag of the aluminum electrolytic cell; (2) mixing the crushed carbon residue with NaCl; (3) putting the mixture into a crucible, and heating to 810-1020 ℃ to obtain mixture molten salt; (4) the mixture is condensed by molten salt; placing the mixture into water, stirring and dissolving to obtain suspension on the upper layer and primary precipitate on the bottom; (5) separating the suspension from the precipitate, and filtering to obtain filtrate and filter residue; (6) washing and drying filter residues to obtain primary carbon powder; evaporating and crystallizing the filtrate to obtain primary NaCl salt; (7) mixing the primary precipitate and primary NaCl salt, and repeating the steps (3) to (6) to respectively obtain secondary precipitate, secondary carbon powder and secondary NaCl salt; and drying the secondary precipitate to form electrolyte. The method of the invention saves a large amount of pretreatment time and cost; the raw materials are low in price, the treatment process is simple, and the environment-friendly effect is realized without toxic byproducts.

Description

Method for treating anode carbon slag of aluminum electrolysis cell by using NaCl molten salt extraction method
Technical Field
The invention belongs to the technical field of metallurgy and environmental protection, and particularly relates to a method for treating anode carbon slag of an aluminum electrolysis cell by using a NaCl molten salt extraction method.
Background
The method for producing the metal aluminum by the molten salt electrolysis method is the only method for producing the industrial aluminum in the world at present, and the method takes the molten cryolite as a solvent, alumina as a raw material and a carbon body as an anode and a cathode, and metal aluminum liquid is obtained by electrolysis at 920-950 ℃. At present, the aluminium electrolysis prebaked anode is mainly made of aggregate (petroleum coke) and binder (asphalt), and in the production process of electrolytic aluminium, because the oxidation resistance of the aggregate and the binder in the carbon anode are inconsistent, and because of the corrosion and scouring of aluminium liquid and electrolyte, part of petroleum coke particles fall off from a matrix and enter molten salt electrolyte to form carbon slag.
The existence of the carbon slag in the electrolytic cell has great influence on the aluminum electrolysis production process. The carbon slag in the electrolytic cell is mainly powdery and granular, is mainly mixed in the electrolyte or suspended on the upper layer of the electrolyte, not only can influence the physical and chemical properties of the electrolyte, such as conductivity, fluidity and the like, but also can cause the reduction of the polar distance under the condition of constant cell voltage, aggravate the secondary dissolution loss of aluminum on the interface of the electrolyte and aluminum liquid, and finally cause the problems of current efficiency reduction and the like. Therefore, in order to ensure the normal operation of the aluminum electrolysis production process, carbon slag in the electrolyte of the aluminum electrolysis cell must be periodically salvaged by workers; in the process of fishing the carbon slag, a large amount of electrolytes adhered to the surface of the carbon slag are fished away together, and the proportion of the electrolytes is usually 60-80%; according to statistics, about 3-5 kg of carbon slag is generated in each 1t of raw aluminum, the yield of raw aluminum in China is 3227 ten thousand tons in 2017, the total amount of carbon slag generated by an aluminum electrolysis enterprise is about 29 ten thousand tons, and about 17.4 ten thousand tons of electrolyte is taken away by the carbon slag, so that a large amount of electrolyte waste is caused.
At present, the method for separating and recovering the anode carbon slag of the aluminum electrolytic cell mainly comprises the following steps: (1) a flotation method; adding water into the carbon slag, grinding the carbon slag to a certain concentration and granularity, adding a flotation reagent, stirring, and then introducing the carbon slag into a flotation machine and introducing air to form bubbles; the carbon powder floats upwards to the upper part of the ore pulp along with the bubbles and is taken out, and the electrolyte is discharged from the bottom flow of the flotation tank, thereby realizing the purpose of separating the carbon powder from the electrolyte in the carbon slag; although flotation has the advantages of low treatment cost, less labor, low labor intensity of workers, good production environment and the like, the recovery rate of electrolyte is low, the carbon content of the recovered electrolyte is high (about 5 percent), and the recovery is not beneficial to returning to the aluminum electrolysis production; the recycled carbon still contains about 20 percent of electrolyte, and the carbon slurry containing about 20 percent of electrolyte is still difficult to treat and recycle; the flotation wastewater contains fluorine ions, and wastewater treatment is needed, so that the recovery cost is increased; (2) a roasting method; roasting the carbon slag at a certain temperature to fully combust combustible substances such as carbon, hydrogen and the like in the carbon slag, wherein the obtained roasted product is electrolyte, so that the aim of separating the electrolyte from the carbon in the carbon slag is fulfilled; the disadvantage is that the high temperature roasting can cause secondary environmental protection problem; the roasting time is long, the production efficiency is low, and the large-scale treatment of the carbon slag is not facilitated; the labor intensity of workers is high, the working environment is bad, and the like; (3) a vacuum smelting method; grinding carbon slag into fine powder, adding a proper binder, pressing into a briquette, and then utilizing the volatile characteristic of electrolyte at high temperature in a vacuum furnace to cool and condense the electrolyte on the upper part of the vacuum furnace, and leaving carbon in a tank body, thereby achieving the purpose of separation; however, the method has low separation rate, the separation rate of the electrolyte is more than 83%, the carbon content in the residual carbon residue is about 74%, and harsh conditions such as certain vacuum degree are required, so that the large-scale application and popularization of the method are limited. Other methods, such as leaching the electrolyte in the carbon residue with acid solution or alkali solution, cannot completely separate the carbon residue from the electrolyte, and have complex process and high cost, which are not industrially applied.
Disclosure of Invention
Aiming at various problems in the existing electrolytic cell anode carbon residue treatment technology, the invention provides a method for treating the anode carbon residue of the aluminum electrolytic cell by using a NaCl molten salt extraction method, wherein NaCl and the anode carbon residue are uniformly mixed and then heated to 810-1020 ℃ to be molten, and then the separation of electrolyte and carbon is realized by using the physical characteristic that NaCl is easily dissolved in water, so that the separation cost is reduced and the separation efficiency of the electrolyte and the carbon is improved.
The method of the invention is carried out according to the following steps;
(1) crushing large blocks in the anode carbon slag of the aluminum electrolytic cell to prepare crushed carbon slag with the particle size of less than or equal to 20 mm;
(2) uniformly mixing the crushed carbon slag and NaCl to prepare a mixed material, wherein the mass ratio of the NaCl to the crushed carbon slag in the mixed material is more than or equal to 2;
(3) putting the mixed material into a crucible, then placing the crucible in an electric furnace, heating the crucible to 810-1020 ℃, and obtaining a mixture molten salt formed by NaCl, electrolyte and carbon when the mixed material is completely melted;
(4) cooling the mixture molten salt along with the furnace until the mixture molten salt is solidified to obtain solidified mixed salt; placing the coagulated mixed salt in water, stirring to dissolve the water-soluble components, wherein the upper layer of the obtained material is suspension, and the bottom of the obtained material is primary precipitation;
(5) pouring out the suspension, separating the suspension from the precipitate, and filtering the separated suspension to obtain filtrate and filter residue;
(6) washing the filter residue with water to remove NaCl component, and then drying to remove moisture to obtain primary carbon powder; evaporating and crystallizing the filtrate to obtain primary NaCl salt;
(7) mixing the primary precipitate with primary NaCl salt, and repeating the steps (3) to (6) on the obtained secondary mixed material to respectively obtain secondary precipitate, secondary carbon powder and secondary NaCl salt; wherein the secondary precipitate is dried to remove moisture and form electrolyte.
In the method, the secondary NaCl salt is returned to the step (2) to be recycled as NaCl.
The element components of the anode carbon slag of the aluminum electrolytic cell comprise 29.7 percent of C, 16.6 percent of Na, 11.3 percent of All and 34.1 percent of F by mass percent; wherein Na, Al and F are electrolyte components.
In the method, the recovery rate of C of the primary carbon powder and the secondary carbon powder is more than or equal to 85 percent.
In the method, the mixture of the primary carbon powder and the secondary carbon powder contains more than or equal to 85 percent of C by mass percent.
In the method, the mass ratio of NaCl to the crushed carbon slag is 2-4, and the mixed material is placed in an electric furnace and heated to 880-950 ℃.
In the method, the larger the mass ratio of NaCl to the crushed carbon slag is, the lower the temperature rise in the electric furnace can be, and the better the separation effect of the carbon and the electrolyte is.
In the step (4), the suspension is immediately poured out after the stirring is stopped, so that carbon in the suspension is prevented from settling.
Compared with the prior art, the invention has the following advantages: 1. the pretreatment process is simple, and the powder is not required to be completely crushed into micron-level powder, so that a large amount of pretreatment time and cost are saved; 2. the raw material NaCl is low in price, easy to obtain, low in consumption and capable of being recycled; 3. compared with the prior art such as a flotation method, a high-temperature roasting method, a vacuum distillation method and the like, the method has the advantages of simple treatment process, no harsh reaction conditions, low cost, environmental protection, no toxic by-product generation and capability of quickly treating a large amount of aluminum cell anode carbon slag.
The method of the invention extracts carbon components by using a large amount of NaCl molten salt at high temperature, separates the electrolyte originally combined with the carbon from the carbon, and then realizes the separation and recovery of the electrolyte and the carbon by utilizing the physical characteristic that the NaCl salt is easy to dissolve in water.
Drawings
FIG. 1 is a schematic flow chart of the method for treating anode carbon slag of an aluminum electrolysis cell by using a NaCl molten salt extraction method according to the invention;
FIG. 2 is an XRD pattern of the primary carbon powder in example 1 of the present invention;
FIG. 3 is an XRD pattern of secondary carbon powder in example 1 of the present invention;
fig. 4 is an XRD pattern of the electrolyte in example 1 of the present invention;
FIG. 5 is an XRD pattern of a secondary NaCl salt according to the invention in example 1.
Detailed Description
In the examples of the present invention, filtration was carried out by suction filtration using a buchner funnel.
The X-ray diffraction model adopted in the embodiment of the invention is X Pertpro.
The water used in the embodiment of the invention is deionized water.
NaCl used in the examples of the present invention was a commercially available product.
The crucible adopted in the embodiment of the invention is a corundum crucible.
The following are preferred embodiments of the present invention.
The purity of the electrolyte obtained in the embodiment of the invention is more than or equal to 88 percent.
In the embodiment of the invention, the drying temperature of the secondary precipitation is 100 +/-5 ℃, and the time is at least 10 min.
In the embodiment of the invention, the mixed material is heated to 810-1020 ℃ in an electric furnace and then is kept warm for 20 min.
Example 1
The flow is shown in figure 1;
crushing large blocks in the anode carbon slag of the aluminum electrolytic cell to prepare crushed carbon slag with the particle size of less than or equal to 20 mm; the aluminum cell anode carbon slag comprises 29.7 percent of C, 16.6 percent of Na, 11.3 percent of Al and 34.1 percent of F according to mass percent; wherein Na, Al and F are electrolyte components;
uniformly mixing the crushed carbon slag and NaCl to prepare a mixed material, wherein the mass ratio of the NaCl to the crushed carbon slag in the mixed material is 4;
putting the mixed material into a crucible, then putting the crucible into an electric furnace, heating the crucible to 880 ℃, and obtaining a mixture molten salt formed by NaCl, electrolyte and carbon when the mixed material is completely melted;
cooling the mixture molten salt along with the furnace until the mixture molten salt is solidified to obtain solidified mixed salt; placing the coagulated mixed salt in water, stirring to dissolve water soluble components, wherein the upper layer of the obtained material is suspension, the bottom is primary precipitate, and XRD pattern is shown in FIG. 2;
pouring out the suspension, separating the suspension from the precipitate, and filtering the separated suspension to obtain filtrate and filter residue;
washing the filter residue with water to remove NaCl component, and then drying to remove moisture to obtain primary carbon powder; evaporating and crystallizing the filtrate to obtain primary NaCl salt;
mixing the primary precipitate and primary NaCl salt to obtain a secondary mixed material, and then repeating the steps of preparing a mixture molten salt, adding water for dissolution, filtering, drying filter residue and carrying out evaporative crystallization to respectively obtain a secondary precipitate, secondary carbon powder and secondary NaCl salt; the XRD pattern of the secondary NaCl salt is shown in figure 5, and the secondary NaCl salt is recycled as NaCl; the XRD pattern of the secondary carbon powder is shown in figure 3;
drying the secondary precipitate to remove water to form electrolyte, wherein an XRD (X-ray diffraction) pattern is shown in figure 4, and the purity of the electrolyte is 88.5%;
the recovery rate of C of the primary carbon powder and the secondary carbon powder is 86 percent; the mixture of the primary carbon powder and the secondary carbon powder contains C87% by mass.
Example 2
The method is different from the embodiment in that:
(1) the mass ratio of NaCl to the crushed carbon slag in the mixed material is 2;
(2) heating the mixed material to 900 ℃ to melt;
(3) the electrolyte purity is 90.3%; the recovery rate of C of the primary carbon powder and the secondary carbon powder is 85 percent; the mixture of the primary carbon powder and the secondary carbon powder contains 88% of C by mass percent.
Example 3
The method is different from the embodiment in that:
(1) the mass ratio of NaCl to the crushed carbon slag in the mixed material is 3;
(2) heating the mixed material to 950 ℃ for melting;
(3) the electrolyte purity is 90.6%; the recovery rate of C of the primary carbon powder and the secondary carbon powder is 86 percent; the mixture of the primary carbon powder and the secondary carbon powder contains 86% of C by mass percent.

Claims (6)

1. A method for treating anode carbon slag of an aluminum electrolysis cell by using a NaCl molten salt extraction method is characterized by comprising the following steps;
(1) crushing large blocks in the anode carbon slag of the aluminum electrolytic cell to prepare crushed carbon slag with the particle size of less than or equal to 20 mm;
(2) uniformly mixing the crushed carbon slag and NaCl to prepare a mixed material, wherein the mass ratio of the NaCl to the crushed carbon slag in the mixed material is more than or equal to 2;
(3) putting the mixed material into a crucible, then placing the crucible in an electric furnace, heating the crucible to 810-1020 ℃, and obtaining a mixture molten salt formed by NaCl, electrolyte and carbon when the mixed material is completely melted;
(4) cooling the mixture molten salt along with the furnace until the mixture molten salt is solidified to obtain solidified mixed salt; placing the coagulated mixed salt in water, stirring to dissolve the water-soluble components, wherein the upper layer of the obtained material is suspension, and the bottom of the obtained material is primary precipitation;
(5) pouring out the suspension, separating the suspension from the precipitate, and filtering the separated suspension to obtain filtrate and filter residue;
(6) washing the filter residue with water to remove NaCl component, and then drying to remove moisture to obtain primary carbon powder; evaporating and crystallizing the filtrate to obtain primary NaCl salt;
(7) mixing the primary precipitate with primary NaCl salt, and repeating the steps (3) to (6) on the obtained secondary mixed material to respectively obtain secondary precipitate, secondary carbon powder and secondary NaCl salt; wherein the secondary precipitate is dried to remove moisture and form electrolyte.
2. The method for treating the anode carbon slag of the aluminum electrolytic cell by using the NaCl molten salt extraction method according to claim 1, wherein the secondary NaCl salt is returned to the step (2) to be recycled as NaCl.
3. The method for treating the anode carbon slag of the aluminum electrolysis cell by using the NaCl molten salt extraction method according to claim 1, wherein the anode carbon slag of the aluminum electrolysis cell comprises the selected element components of, by mass, 29.7% of C, 16.6% of Na, 11.3% of Al and 34.1% of F; wherein Na, Al and F are electrolyte components.
4. The method for treating the anode carbon slag of the aluminum electrolysis cell by using the NaCl molten salt extraction method as claimed in claim 1, wherein the C recovery rate of the primary carbon powder and the secondary carbon powder is more than or equal to 85%.
5. The method for treating anode carbon slag of the aluminum electrolysis cell by using the NaCl molten salt extraction method as claimed in claim 1, wherein the mixture of the primary carbon powder and the secondary carbon powder contains C more than or equal to 85% by mass.
6. The method for treating the anode carbon slag of the aluminum electrolysis cell by using the NaCl molten salt extraction method according to claim 1, wherein in the step (2), the mass ratio of NaCl to the crushed carbon slag is 2-4, and the mixture is placed in an electric furnace and heated to 880-950 ℃.
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