CN110127649B - Method for recycling waste cathode carbon blocks of electrolytic aluminum electrolysis cell - Google Patents
Method for recycling waste cathode carbon blocks of electrolytic aluminum electrolysis cell Download PDFInfo
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- CN110127649B CN110127649B CN201910373382.5A CN201910373382A CN110127649B CN 110127649 B CN110127649 B CN 110127649B CN 201910373382 A CN201910373382 A CN 201910373382A CN 110127649 B CN110127649 B CN 110127649B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01D5/06—Preparation of sulfates by double decomposition
- C01D5/08—Preparation of sulfates by double decomposition with each other or with ammonium sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
Abstract
The invention discloses a recycling method of waste cathode carbon blocks of an aluminum electrolytic cell, which comprises the steps of crushing, crushing and ball-milling the raw materials of the waste cathode carbon blocks of the aluminum electrolytic cell into powder, and adding hydrogen peroxide to remove cyanide; adding concentrated sulfuric acid to react to generate hydrogen fluoride gas, introducing the hydrogen fluoride gas into a condensation absorption tower, and circularly absorbing the hydrogen fluoride gas by using deionized water or a low-concentration hydrofluoric acid solution to obtain 25-40% hydrofluoric acid products; the carbon powder can be used as a raw material for processing a new cathode for recycling after being added with NaOH for neutralization, filtered and dried; finally, a large amount of sodium sulfate contained in the filtrate is concentrated to obtain sodium sulfate crystals. The invention has the advantages that: the process is advanced, the advantages are obvious, and zero emission of environmental pollutants in the recycling process is realized; the treated waste cathode carbon blocks can be used for processing new cathode carbon blocks repeatedly, and the main harmful component fluorine in the original waste cathode carbon blocks is converted into high-added value hydrogen fluoride, so that the fluorine can be recycled.
Description
Technical Field
The invention belongs to the technical field of electrolytic aluminum industrial solid waste comprehensive treatment. In particular to a method for harmlessly treating waste cathode carbon blocks of an electrolytic aluminum electrolysis cell and effectively recovering carbon and fluorine resources in the waste cathode carbon blocks.
Background
The aluminum electrolysis capacity of China is 4500 ten thousand tons, the actual yield exceeds 3600 ten thousand tons and accounts for more than 50 percent of the global aluminum electrolysis capacity in 2017. In the process of aluminum electrolysis production, the carbon cathode expands due to the permeation of fluorine-containing salt, and further causes the damage and the rejection of the electrolytic cell. General use of aluminum electrolysis cellsThe cell is stopped for overhaul after 4 to 6 years, all the waste cell lining materials (overhaul slag for short) are taken out, and the waste cathode carbon blocks account for about 50 percent of the overhaul slag. The overhaul slag is solid waste inevitable in the production process of electrolytic aluminum, and 10-30 kg of overhaul slag is generated for each 1 ton of electrolytic aluminum. The electrolytic aluminum overhaul slag is specified as dangerous solid waste (category: HW 48) in the national hazardous waste record, and the waste tank lining is listed as HW32 inorganic fluoride waste and HW33 inorganic cyanide waste in the national hazardous waste record. The carbon material in the waste cathode carbon block for aluminum electrolysis accounts for 30-70 percent, and the rest is electrolyte and mainly Na 3 [AlF 6 ]、NaF、CaF 2 、MgF 2 、LiF、AlF 3 、NaCN、 Na 4 [Fe(CN) 6 ]Etc., and also small amounts of Al and Al 4 C 3 AlN and Na, which are soluble and reactive with water to produce HF, HCN and H 2 、CH 4 、NH 3 And the harmful or flammable gases, fluorine-containing and cyanogen-containing compounds, which enter the environment, can cause great harm to the health and growth of human beings, animals and plants.
The waste cathode carbon block is a valuable resource rich in highly graphitized carbon and fluorine-containing electrolyte. Therefore, how to completely remove the harm of fluoride and cyanide in the aluminum electrolysis waste cathode carbon block and realize the harmless and resource recycling of the aluminum electrolysis waste cathode carbon block is an industry difficult to overcome, and experts in the industry and production front personnel carry out a plurality of years of research and study aiming at the difficult problem, such as adopting alkali leaching or ultrasonic-assisted flotation pressure alkali leaching (CN 106745137A, CN106077038A, CN106077040A, CN106587122A, CN101817521A, CN106086938A, CN 105821445A), acid treatment or ultrasonic-assisted flotation pressure acid treatment (CN 106077037A, CN106077036A, CN106180118A, CN 101984984A), combination of alkali leaching and acid leaching and fly ash (CN 107162061A), heat-preservation cyanogen-removal combined flotation to obtain carbon slag and electrolyte slag and heating to remove carbon (CN 106064813A, CN105964659A, CN 107313073A), high-temperature calcination (CN 102989744A, CN105964660A, CN106517209A, CN107904621A, CN106147910A, CN100542702C, CN101054693A, CN107628614A, CN105642649A, CN106185818A, CN 106269787A), water leaching (CN 105772486A, CN107377592A, CN105728440A, CN 106166560A) and chemical precipitation (CN 105327933A) for treatment.
From the prior technical results, the harmless and resource treatment and utilization of the waste cathode carbon block of the aluminum electrolytic cell are divided into two main categories of wet treatment and high-temperature treatment of aqueous solution. The wet treatment involves water washing (leaching), alkali treatment, acid-alkali combination, combined flotation process and the like, mainly aims at recovering electrolyte and carbon, and adopts an oxidant to decompose cyanide into harmless gas substances in the wet treatment. The high-temperature treatment technology mainly aims at harmlessness, and uses the waste cathode as fuel to burn, or adopts the combination of technologies such as high temperature, vacuum and the like to respectively recycle the electrolyte or the carbon material, so that the cyanogen-containing compound is oxidized and decomposed into harmless gas substances at high temperature.
From the prior technical achievements, the wet treatment and high-temperature treatment of the waste cathode carbon block of the aluminum electrolytic cell still have the following problems, such as that a large amount of salt-containing and fluorine-containing wastewater generated in the wet treatment is not effectively treated, and secondary pollution is caused; generated H 2 、CH 4 、NH 3 The gas is not controlled and utilized, and the generated HF causes serious pollution; the recovered electrolyte and carbon material have high impurity content and can not be directly utilized; the difficulty of process control is high due to the influence of factors such as the difference of the capacity and the age of the electrolytic aluminum tank, the fluctuation of components, the granularity of powder and the like; a large amount of tail gas carrying HF and dust is generated in the high-temperature treatment; the electrolyte is not completely recovered, and part of the electrolyte remains in the carbon material or the slag; the melting agglomeration of the electrolyte with low melting point occurs in the furnace, which causes the incomplete combustion residual quantity of the carbon material to be larger, and the melting agglomeration of the electrolyte in the furnace causes the deterioration of the production working condition and the poor production stability.
Disclosure of Invention
The invention aims to provide a new technical scheme aiming at the defects of the existing aluminum electrolysis waste cathode carbon block treatment scheme. The scheme combines high-temperature treatment and wet treatment, carries out harmless treatment on the aluminum electrolysis waste cathode carbon block aiming at the characteristic that the waste cathode carbon block mainly comprises carbon and fluoride salt, and can fully utilize substances obtained after waste treatment to obtain carbon fine powder and fluoride with high added value.
The technical scheme for solving the technical problems is as follows:
a method for recycling waste cathode carbon blocks of an electrolytic aluminum cell is characterized in that the treatment process comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 30wt% hydrogen peroxide into the carbon powder according to the weight ratio of 1: 1, and stirring at 80 ℃ and 50-200 rpm for 10-30 min to decompose cyanide and excessive hydrogen peroxide; adding 95-98 wt% concentrated sulfuric acid into the cyanide-removed material in an amount which is 5-7 times the weight of the raw carbon powder, and generating HF gas at 120 ℃ and a stirring speed of 100-200 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing the HF gas by using deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 25-40 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution to pH value of 5 to obtain precipitate, filtering, washing, and drying at 60 deg.C to obtain carbon powder for processing new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches about 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
The invention has the advantages that: the process is advanced, the advantages are obvious, and zero emission of environmental pollutants in the recycling process is realized; the treated waste cathode carbon blocks can be reused for processing new cathode carbon blocks, and the main harmful component fluorine in the original waste cathode carbon blocks is converted into high-added value hydrogen fluoride, so that the cyclic utilization of the fluorine is realized.
Drawings
FIG. 1 is a process flow diagram of the method for recycling waste cathode carbon blocks of an electrolytic aluminum cell of the invention. The raw materials are waste cathode carbon blocks of an alumina electrolysis cell after overhaul in an electrolytic aluminum factory, and high-concentration hydrofluoric acid, carbon powder, alumina and mirabilite are respectively obtained after treatment.
Detailed Description
The present invention will be further described with reference to the following examples, but it should be noted that the scope of the present invention is not limited to these examples.
Example 1
A method for recycling waste cathode carbon blocks of an electrolytic aluminum cell comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 10g of hydrogen peroxide with the concentration of 30wt% into 10g of carbon powder according to the weight ratio of 1: 1, and stirring at 80 ℃ and 50rpm for 10min to decompose cyanide and excessive hydrogen peroxide; adding 50g of concentrated sulfuric acid with the concentration of 95wt% into the material without cyanide according to 5 times of the weight of the raw carbon powder, and generating HF gas at the temperature of 120 ℃ and the stirring speed of 100 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing by using deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 28.8 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution until the pH value is 5 to obtain a precipitate, filtering, washing and drying the precipitate at 60 ℃ to obtain the carbon powder for processing a new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
Example 2
A recycling method of waste cathode carbon blocks of an electrolytic aluminum electrolytic cell comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 10g of hydrogen peroxide with the concentration of 30wt% into 10g of carbon powder according to the weight ratio of 1: 1, and stirring for 20min at 80 ℃ and 100rpm to decompose cyanide and excessive hydrogen peroxide; adding 70g of concentrated sulfuric acid with the concentration of 95wt% into a material without cyanide according to the amount of 7 times of the weight of the raw carbon powder, and generating HF gas at the temperature of 120 ℃ and the stirring speed of 150 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing with deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrogen with concentration of 25.0wt%A fluoric acid; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution until the pH value is 5 to obtain a precipitate, filtering, washing and drying the precipitate at 60 ℃ to obtain the carbon powder for processing a new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
Example 3
A recycling method of waste cathode carbon blocks of an electrolytic aluminum electrolytic cell comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 10g of hydrogen peroxide with the concentration of 30wt% into 10g of carbon powder according to the weight ratio of 1: 1, and stirring for 30min at 80 ℃ and 100rpm to decompose cyanide and excessive hydrogen peroxide; adding 60g of concentrated sulfuric acid with the concentration of 98wt% into the material without cyanide according to 6 times of the weight of the raw carbon powder, and generating HF gas at the temperature of 120 ℃ and the stirring speed of 200 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing the HF gas by using deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 40.0 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution to pH value of 5 to obtain precipitate, filtering, washing, and drying at 60 deg.C to obtain carbon powder for processing new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
Example 4
A method for recycling waste cathode carbon blocks of an electrolytic aluminum cell comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 10g of hydrogen peroxide with the concentration of 30wt% into 10g of carbon powder according to the weight ratio of 1: 1, and stirring for 20min at 80 ℃ and 200rpm to decompose cyanide and excessive hydrogen peroxide; removing cyanide from the material as suchAdding 70g of concentrated sulfuric acid with the concentration of 95wt% into 7 times of the weight of the carbon powder, and generating HF gas at the temperature of 120 ℃ and the stirring speed of 150 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing the HF gas by using deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 32.5 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution until the pH value is 5 to obtain a precipitate, filtering, washing and drying the precipitate at 60 ℃ to obtain the carbon powder for processing a new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches about 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
Example 5
A method for recycling waste cathode carbon blocks of an electrolytic aluminum cell comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 10g of hydrogen peroxide with the concentration of 30wt% into 10g of carbon powder according to the weight ratio of 1: 1, and stirring for 30min at 80 ℃ and 200rpm to decompose cyanide and excessive hydrogen peroxide; adding 70g of concentrated sulfuric acid with the concentration of 95wt% into a material without cyanide according to the amount of 7 times of the weight of the raw carbon powder, and generating HF gas at the temperature of 120 ℃ and the stirring speed of 150 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing with deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 39.2 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution to pH value of 5 to obtain precipitate, filtering, washing, and drying at 60 deg.C to obtain carbon powder for processing new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches about 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
Claims (1)
1. A recycling method of waste cathode carbon blocks of an electrolytic aluminum electrolytic cell is characterized in that the treatment process comprisesThe method comprises the following steps: crushing and grinding waste cathode carbon blocks of an electrolytic aluminum electrolysis cell to carbon powder with a particle size of less than 45 meshes; adding 30wt% hydrogen peroxide into the carbon powder according to the weight ratio of 1: 1, and stirring at 80 ℃ and 50-200 rpm for 10-30 min to decompose cyanide and excessive hydrogen peroxide; adding 95-98 wt% concentrated sulfuric acid into the cyanide-removed material in an amount which is 5-7 times the weight of the raw carbon powder, and generating HF gas at 120 ℃ and a stirring speed of 100-200 rpm; introducing HF gas into a hydrogen fluoride condensation absorption tower, and circularly absorbing by using deionized water or low-concentration hydrofluoric acid to obtain high-concentration hydrofluoric acid with the concentration of 25-40 wt%; cooling the carbon powder after removing fluorine to room temperature, adding 40wt% NaOH aqueous solution until the pH value is 5 to obtain a precipitate, filtering, washing and drying the precipitate at 60 ℃ to obtain the carbon powder for processing a new cathode carbon block; adding 40wt% NaOH solution into the filtrate until pH reaches about 7, filtering, washing, drying at 80 deg.C to obtain aluminum hydroxide precipitate, and calcining at 1000 deg.C to obtain aluminum oxide; evaporating and concentrating the filtrate in the last step to obtain Na 2 SO 4 ·10H 2 O (mirabilite).
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| CN110791779B (en) * | 2019-12-05 | 2021-08-10 | 中南大学 | Method for preparing carbon cathode for aluminum electrolysis by using waste cathode of aluminum electrolysis cell |
| US11697594B2 (en) | 2020-01-19 | 2023-07-11 | Central South University | Method for recycling spent carbon cathode of aluminum electrolysis |
| CN111170299B (en) * | 2020-01-19 | 2021-06-22 | 中南大学 | Method for recovering waste cathode carbon blocks from aluminum electrolysis |
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| CN111909728A (en) * | 2020-08-13 | 2020-11-10 | 山东魏桥铝电有限公司 | System, method and application for gasification treatment of waste cathode carbon blocks of aluminum electrolysis cell and cooperation of coal oxygen-enriched combustion |
| CN112897502A (en) * | 2021-01-21 | 2021-06-04 | 郑州大学 | Method for treating waste cathode carbon blocks by using steel pickling wastewater |
| CN113443643B (en) * | 2021-05-25 | 2022-04-01 | 昆明理工大学 | Method for cooperatively treating aluminum ash, carbon slag and desulfurized gypsum slag |
| CN113426807B (en) * | 2021-06-29 | 2022-05-17 | 云南云铝润鑫铝业有限公司 | Method for combined treatment and comprehensive utilization of resources of dangerous waste residues generated in aluminum electrolysis |
| CN113426808B (en) * | 2021-06-29 | 2022-05-17 | 云南云铝润鑫铝业有限公司 | Method for recovering fluoride salt from aluminum electrolysis overhaul residues through pressurized alkaline leaching |
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