CN110775955B - Method for treating anode carbon slag of aluminum electrolysis cell by using NaOH molten salt method - Google Patents
Method for treating anode carbon slag of aluminum electrolysis cell by using NaOH molten salt method Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
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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
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
- C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
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Abstract
A method for treating anode carbon slag of an aluminum electrolysis cell by using a NaOH molten salt method comprises the following steps: (1) crushing anode carbon slag of an aluminum electrolytic cell; (2) mixing the crushed carbon residue with NaOH; (3) heating the mixed material to 400-1000 ℃ to melt; (4) Cooling the mixture molten salt along with the furnace, and mixing with water to obtain a suspension; (5) filtering the obtained filter residue and filtrate; adding hydrochloric acid into the filter residue to neutralize NaOH, washing with water, and drying to obtain carbon powder; (6) Introducing CO into the filtrate 2 Carbonizing, filtering to obtain secondary filter residue Al (OH) 3 (ii) a Evaporating and crystallizing the secondary filtrate to obtain Na 2 CO 3 And NaF. The method has the advantages of simple pretreatment process, easily obtained raw materials, lower melting temperature, no waste gas generation and capability of treating the anode carbon slag of the aluminum electrolytic cell on a large scale.
Description
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 electrolytic cell by using a NaOH molten salt method.
Background
The molten salt electrolysis method for producing metallic aluminum is the only method for producing industrial aluminum in the world today, and the method takes molten cryolite as a solvent and Al 2 O 3 Taking a carbon body as an anode and a cathode as raw materials, and electrolyzing at 920-950 ℃ to obtain molten metal aluminum; in the aluminum electrolysis productionIn the process, the anode carbon block is mainly formed by petroleum coke and pitch coke, and is fired by a series of procedures of crushing, calcining, blending, kneading and the like under the condition of coal pitch adhesion.
During the aluminum electrolysis production process, layered carbon slag is generated at the bottom of the anode of the electrolytic cell. The carbon residue is mainly generated as follows: (1) The selection of raw materials and the setting of process conditions in the production process of the carbon block are very strict, when the quality of the carbon block is unqualified, the anode can generate oxidation reaction, and carbon particles fall off the surface of the anode into an electrolytic bath to form carbon slag; (2) Na elements in the electrolyte can infiltrate into the cathode carbon block in the production process, so that stress is generated in the cathode carbon block, and the phenomenon of slag falling of the cathode carbon block is caused.
The carbon residue has an overproof F content, has great environmental pollution and needs to be recycled and harmlessly treated; in the past, the treatment mode of the carbon slag is landfill, which causes resource waste and serious damage to the surrounding environment. The existence of the carbon slag also has great influence on the aluminum electrolysis process: (1) the conductivity of the electrolyte is reduced, and the energy consumption is increased; (2) The heat stability of the electrolytic cell is damaged, the anode is easily wrapped, and the loss of equipment is large; (3) a large amount of manpower and material resources are consumed for fishing the carbon slag; the existing carbon slag treatment technology mainly comprises a flotation method and a roasting method, and mainly aims to realize the separation of C and electrolyte in the carbon slag; however, these methods generally have the problems of poor separation effect, low product purity, etc., and thus the electrolyte and carbon powder products cannot be effectively separated.
Disclosure of Invention
Aiming at various problems in the existing electrolytic cell anode carbon slag treatment technology, the invention provides a method for treating the anode carbon slag of an aluminum electrolytic cell by using a NaOH molten salt method, which comprises the steps of uniformly mixing NaOH solid powder and the anode carbon slag, heating to 400-1000 ℃ to enable the NaOH solid powder and the anode carbon slag to react, using the NaOH to react with an electrolyte in a molten state, converting the electrolyte into a soluble product, and enabling carbon not to participate in the reaction, thereby realizing the separation of the electrolyte and the carbon in the carbon slag.
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 NaOH to prepare a mixed material, wherein the mass ratio of the NaOH to the crushed carbon slag in the mixed material is more than or equal to 2;
(3) The mixed material is filled into a crucible, then is put into an electric furnace to be heated to 400-1000 ℃, and when the mixed material is completely melted, naOH, naF and NaAlO are obtained 2 A mixture molten salt coexisting with carbon;
(4) Cooling the mixture molten salt to normal temperature along with the furnace to obtain a material consisting of upper foam and bottom molten salt; mixing the upper foam and the bottom molten salt with water, and stirring to dissolve water-soluble components to obtain a suspension;
(5) Filtering the suspension to obtain filter residue and filtrate; adding hydrochloric acid into the filter residue to neutralize NaOH in the filter residue, then washing with water until the washing liquid is neutral, drying to remove water, and preparing carbon powder;
(6) Introducing CO into the filtrate 2 Carbonizing to obtain Al (OH) 3 Precipitating; filtering the carbonized material to obtain secondary filter residue with solid component Al (OH) 3 (ii) a Evaporating and crystallizing the obtained secondary filtrate to obtain Na 2 CO 3 And NaF.
In the step (3), the mixture is put into an electric furnace and heated to 500-900 ℃.
In the step (3), the reaction formula of the main reaction of the NaOH and the carbon residue is as follows:
4NaOH+Na 3 AlF 6 ＝NaAlO 2 +6NaF+2H 2 O(g)。
in the step (6), the reaction formula of the carbonization reaction is:
2NaAlO 2 +CO 2 +3H 2 O＝Na 2 CO 3 +2Al(OH) 3 ；
when NaAlO is used 2 Al in the alloy is totally generated into Al (OH) 3 The reaction is complete.
The mass concentration of the hydrochloric acid is more than or equal to 30 percent.
In the step (6), the temperature of the evaporative crystallization is 400 to 1000 ℃.
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 Al 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 in the carbon powder is more than or equal to 80 percent.
In the method, the carbon powder contains more than or equal to 80 percent of C by mass percent.
Compared with the prior art, the invention has the following advantages: 1. the pretreatment process is simple, and the carbon slag is not required to be completely crushed into powder with the particle size of micron level, so that the carbon slag pretreatment time and cost are saved; 2. the raw material NaOH powder is easy to obtain, the melting point of NaOH is 318 ℃, the temperature required by the melting reaction is lower, and the energy consumption is reduced; 3. compared with the prior art such as a flotation method, a high-temperature roasting method and the like, the method has the advantages of no waste gas generation, environmental protection and large-scale treatment of the anode carbon slag of the aluminum electrolytic cell.
Drawings
FIG. 1 is a schematic flow chart of the method for treating anode carbon slag of an aluminum electrolysis cell by using a NaOH molten salt method;
FIG. 2 is an XRD pattern of anode carbon slag of the aluminum electrolytic cell in example 1 of the present invention;
FIG. 3 is an XRD pattern of the carbon powder in example 1 of the present invention.
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.
NaOH and hydrochloric acid adopted in the embodiment of the invention are all commercial products.
The crucible used in the embodiment of the invention is a corundum crucible.
The mass concentration of the hydrochloric acid adopted in the embodiment of the invention is more than or equal to 30 percent.
In the examples of the present invention, na was contained in the mixture 2 CO 3 The mass ratio of the carbon slag to the crushed carbon slag is = 3-5.
In the embodiment of the invention, the mixed material is heated to 500-900 ℃ in an electric furnace and then is kept warm for 20min.
In the embodiment of the invention, the washing liquid is washed by water until the washing liquid is neutral, and then the sodium chloride generated by neutralization is removed at the same time.
The following are preferred embodiments of the present invention.
Example 1
The flow is shown in figure 1;
(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 electrolytic cell anode carbon residue comprises 29.7 percent of C, 16.6 percent of Na, 11.3 percent of Al and 34.1 percent of F by mass percent; wherein Na, al and F are electrolyte components; the XRD pattern is shown in figure 2;
(2) Uniformly mixing the crushed carbon residue with NaOH to prepare a mixed material, wherein the mass ratio of the NaOH to the crushed carbon residue in the mixed material is =3;
(3) Loading the mixture into crucible, heating to 500 deg.C in electric furnace, and melting the mixture to obtain the final product composed of NaOH, naF, and NaAlO 2 A mixture molten salt coexisting with carbon;
(4) Cooling the mixture molten salt to normal temperature along with the furnace to obtain a material consisting of upper foam and bottom molten salt; mixing the upper foam and the bottom molten salt with water, and stirring to dissolve water-soluble components to obtain a suspension;
(5) Filtering the suspension to obtain filter residue and filtrate; adding hydrochloric acid into the filter residue to neutralize NaOH in the filter residue, then washing with water until the washing liquid is neutral, drying to remove water, and preparing carbon powder; the XRD pattern is shown in figure 3;
(6) Introducing CO into the filtrate 2 Carbonizing to obtain Al (OH) 3 Precipitating; filtering the carbonized material to obtain secondary filter residue with solid component Al (OH) 3 (ii) a Evaporating and crystallizing the obtained secondary filtrate at 500 deg.C to obtain Na 2 CO 3 And NaF;
the recovery rate of C in the carbon powder is 81 percent; the carbon powder contains 84.4 percent of C by mass percent;
Na 2 CO 3 and the impurity content in the mixture of NaF is less than or equal to 1 percent.
Example 2
The method is the same as the embodiment and is different from the embodiment;
(1) The mass ratio of NaOH to the crushed carbon slag in the mixed material is =4;
(2) Heating to 650 deg.C in an electric furnace;
(3) The temperature of evaporative crystallization is 700 ℃;
(4) The recovery rate of C in the carbon powder is 82 percent; the carbon powder contains C87.8% by mass percentage.
Example 3
The method is the same as the embodiment and is different from the embodiment;
(1) The mass ratio of NaOH to the crushed carbon slag in the mixed material is =5;
(2) Putting the mixture in an electric furnace, and heating to 900 ℃;
(3) The temperature of evaporative crystallization is 900 ℃;
(4) The recovery rate of C in the carbon powder is 80 percent; the carbon powder contains 86.4 percent of C by mass percent.
Claims (5)
1. A method for treating anode carbon slag of an aluminum electrolysis cell by using a NaOH molten salt 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 NaOH to prepare a mixed material, wherein the mass ratio of the NaOH to the crushed carbon slag in the mixed material is more than or equal to 2;
(3) The mixed material is filled into a crucible, then the crucible is placed into an electric furnace, the temperature is raised to 400 to 1000 ℃, and when the mixed material is completely melted, naOH, naF and NaAlO are obtained 2 A mixture molten salt coexisting with carbon;
(4) Cooling the mixture molten salt to normal temperature along with the furnace to obtain a material consisting of upper foam and bottom molten salt; mixing the upper foam and the bottom molten salt with water, and stirring to dissolve water-soluble components to obtain a suspension;
(5) Filtering the suspension to obtain filter residue and filtrate; adding hydrochloric acid into the filter residue to neutralize NaOH in the filter residue, then washing with water until the washing liquid is neutral, drying to remove water, and preparing carbon powder;
(6) Introducing CO into the filtrate 2 Carbonizing to obtain Al (OH) 3 Precipitating; filtering the carbonized material to obtain solid component Al (OH) 3 (ii) a The obtained secondary filtrate is evaporated and crystallized to obtain Na 2 CO 3 And NaF;
the selected element components of the anode carbon residue of the aluminum electrolytic cell comprise 29.7 percent of C, 16.6 percent of Na, 11.3 percent of Al and 34.1 percent of F by mass percent; wherein Na, al and F are electrolyte components.
2. The method for processing the anode carbon slag of the aluminum electrolytic cell by using the NaOH molten salt method according to claim 1, wherein in the step (3), the temperature is raised to 500 to 900 ℃ in an electric furnace.
3. The method for treating the anode carbon slag of the aluminum electrolytic cell by using the NaOH molten salt method as claimed in claim 1, wherein the hydrochloric acid has a mass concentration of not less than 30%.
4. The method for processing the anode carbon slag of the aluminum electrolytic cell by using the NaOH molten salt method according to claim 1, wherein in the step (6), the temperature of evaporative crystallization is 400 to 1000 ℃.
5. The method for treating the anode carbon residue of the aluminum electrolytic cell by using the NaOH molten salt method according to claim 1, wherein the recovery rate of C in the carbon powder is more than or equal to 80%.
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