CN106077040A - A kind of method of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block - Google Patents
A kind of method of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block Download PDFInfo
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- CN106077040A CN106077040A CN201610499164.2A CN201610499164A CN106077040A CN 106077040 A CN106077040 A CN 106077040A CN 201610499164 A CN201610499164 A CN 201610499164A CN 106077040 A CN106077040 A CN 106077040A
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- alkali
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- cathode carbon
- leaching
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- 238000000034 method Methods 0.000 title claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 73
- 239000003513 alkali Substances 0.000 title claims abstract description 64
- 239000002699 waste material Substances 0.000 title claims abstract description 55
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000002386 leaching Methods 0.000 title claims abstract description 42
- 239000000706 filtrate Substances 0.000 claims abstract description 30
- 229910001610 cryolite Inorganic materials 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 21
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 11
- 239000008187 granular material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- CPRMKOQKXYSDML-UHFFFAOYSA-M rubidium hydroxide Chemical compound [OH-].[Rb+] CPRMKOQKXYSDML-UHFFFAOYSA-M 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 abstract description 11
- 239000004411 aluminium Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000002910 solid waste Substances 0.000 abstract description 3
- 238000002604 ultrasonography Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 8
- 238000010309 melting process Methods 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000009210 therapy by ultrasound Methods 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 5
- 238000005188 flotation Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011268 mixed slurry Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- 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
- C25C3/12—Anodes
- C25C3/125—Anodes based on carbon
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The method that the present invention relates to a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, belongs to aluminium electroloysis solid waste technical field of resource recovery.The present invention adds leaching in alkali liquor after broken for aluminum electrolysis waste cathode carbon block, is filtrated to get powdered carbon and the first filtrate;The dipped journey of alkali is carried out in ultrasonic environment;By CO2It is passed through the first filtrate, separates out crystal, be filtrated to get cryolite, alumag and the second filtrate, the second filtrate recycle.Present invention process is simple, operation is convenient, and ultrasound wave accelerates reaction rate with alkali leaching synergism, improves the purity of product powdered carbon, and the purity of gained powdered carbon is 97.92% to the maximum, production cycle 70min.
Description
Technical field
The method that the present invention relates to a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, belongs to aluminium electroloysis solid
Useless technical field of resource recovery.
Background technology
Internal lining of aluminium electrolytic bath is built in steel framework, by materials such as charcoal, carborundum, refractory brick, insulating brick, calcium silicate boards
Constitute.In production process, Pot Lining inevitably by the permeating corrosion of the materials such as high-temperature electrolysis matter and aluminum liquid, metallic sodium,
Causing inner lining structure to deform, rupture, aluminum liquid and electrolyte in groove spill from crack.General new electrolysis bath uses 3~6 years
After be accomplished by stopping groove overhaul, the waste lining of generation is topmost solid waste during aluminum electrolysis.Research shows, often
One ton of primary aluminum of electrolysis production can produce about 30kg waste lining.Chinese primary aluminum yield 31,410,000 tons in 2015, waste lining discharge capacity
Nearly million tons.
The waste lining that aluminum electrolysis is discharged is extremely harmful solid waste, and its soluble fluoride and cyanide content are tight
Heavily exceed standard.By wind, Exposure to Sunlight, the effect that drenches with rain, in waste lining, harmful substance will shift: enter air, penetrate into soil and
Subsoil water, damages ecological environment, has a strong impact on human health and animal and plant growth.
The processing method of waste lining, is divided into wet method and the big class of pyrogenic process two, has multinomial Patents.Waste lining pyrogenic attack skill
Art gradually develops into the dominant technology processing waste lining because of advantages such as short, simple to operate, the small investments of its technological process.
Patent CN101357367A provides a kind of method utilizing gangue process aluminum electrolytic groove waste lining, passes through: raw material
Broken, levigate, by gangue that addition is waste lining quality 10%~30% and the quick lime of waste lining quality 5%~35%
Mix homogeneously with waste lining;Under the conditions of temperature is 900 DEG C~1200 DEG C, roasting 40min~70min, calcining matter is levigate to grain
Degree less than 0.074mm, leaches remaining soluble fluorine ion with the lime water that concentration is 0.5%~5%, extraction time be 30~
60min, filters afterwards, uses it for anything else after filtrate collection, and filtering residue reclaims and is available thing.
Patent CN104984984A discloses a kind of aluminium cell slag from delining resource method for innocent treatment and system, should
Method includes: 1) mixed with sulphuric acid by slag from delining powder, and stirring leaches to obtain mixed slurry A;2) mixed slurry A is heated, negative
Make Blausure (German) escape and use alkaline solution absorption under the conditions of pressure, obtain mixed slurry B;3) in mixed slurry B, add flotation agent to enter
Row flotation, obtains bottom mud and top layer mud, and bottom mud obtains thick cryolite and mixed liquor A through solid-liquid separation;4) to mixed liquor A
After the stirring reaction of middle addition aluminium removal, solid-liquid separation obtains thick aluminium hydroxide and mixed liquid B;5) to flotation gained top layer mud with mixed
Close and liquid B is separately added into defluorinating agent stirring reaction, solid-liquid separation.
Patent CN1895803A discloses a kind of method of process aluminum electrolytic groove waste lining: crushed by waste lining, adds powder
Coal ash, quick lime uniformly mix, levigate to granularity less than briquetting after 0.074mm, at 900~1100 DEG C of roasting temperatures 30~90
Minute;After roasting, material is levigate is less than 0.074mm to granularity, leaches the solvable of remnants with the lime water that concentration is 0.5%~5%
F-Filtering, gained filtrate can be as soda industry and the raw material of aluminum oxide industry, and filtering residue can be as cement industry and refractory material
The raw material of industry.
Patent CN102161049A discloses the method for comprehensive utilization of a kind of aluminum cell waste cathode carbon block, its feature
It is: will be through sorting, broken, pulverizing, ash disposal and dried waste and old cathode carbon block as carbon block for blast furnace, electric furnace carbon block, electrolysis
Groove cathode carbon pieces, electrolysis bath side wall carbon block, electrolysis carbon block, self-calcining charcoal blocks or carbon paste production raw material use.
Patent CN102502641A discloses a kind of microwave heating red mud and waste cathode of aluminum electrolytic cell carbon block synthesizing silicon carbide
Method, production technology is: red mud ore grinding is processed the ratio accounting for entirety less than the part of 0.074mm to granularity and is not less than
40wt%, adds appropriate reducing agent and carries out magnetizing roast, and magnetic separation separation magnetic iron ore obtains siliceous solid material the most again;Will
Aluminium electroloysis waste cathode carbon block carries out pretreatment, and the ore grinding process to the granularity part less than 0.074mm accounts for the ratio of entirety and is not less than
40wt%, obtains powdered carbon after carrying out FLOTATION SEPARATION, soda acid remove impurity process;Siliceous solid material and powdered carbon mix homogeneously,
The microwave field of 2450MHz or 916MHz synthesizes 30~300min, obtains silicon carbide products.
Aluminium electroloysis waste lining processing method is more, but owing to its technology and economic benefit restrict, is applied to the big rule of industrialization
The technique that mould processes is less.How to reduce or to eliminate the impact on environment of the aluminium electroloysis waste lining harmful substance, being allowed to more reasonable
It is effectively realized refuse reclamation, is an important difficulty facing of current metallurgy of aluminium practitioner.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of ultrasonic assistant alkali leaching process aluminum electrolytic groove waste and old cathode carbon
The method of block.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, comprises the following steps:
Step one
Aluminum cell waste cathode carbon block is crushed, obtains standby granule;
Step 2
Standby powder step one obtained adds ultrasonic leaching in alkali liquor, filters after leaching, obtains powdered carbon and the first filter
Liquid;
Step 3
It is passed through CO to step 2 gained the first filtrate2, produce precipitation, filter to obtain cryolite, alumag and the
Two filtrates, the second filtrate returns step 2 recycling.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, in step one, described standby
With in granule, particle diameter accounts for the 50%-100% of standby granule gross mass less than the granule of 200 mesh.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, in step 2, in alkali liquor
At least one in NaOH, KOH, LiOH, RbOH of solute, prioritizing selection NaOH.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, in step 2, described alkali
OH in liquid—Concentration be 1-5mol/L, prioritizing selection 2-4mol/L.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, in step 2, by standby
When granule adds leaching in alkali liquor, controlling extraction temperature is 25-100 DEG C, preferred 70-90 DEG C, time 30-180min, preferred 60-
90min, liquid-solid ratio is 5-10:1, stir speed (S.S.) 400-1000r/min
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, in step 2, ultrasound wave
Frequency 25-40KHz, preferred 40KHz, power is 50-600W, preferred 150-300W, processes time 10-180min, preferred 20-
40min。
The present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block method, in step 3, described to
First filtrate is ventilated and is passed through CO by flow 5-100L/h, preferred 15-40L/h2, duration of ventilation 5-30min, preferred 10-
20min, produces precipitation, filters isolated cryolite, alumag and the second filtrate, and the second filtrate returns step 2
Recycle.
The method of the present invention a kind of ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, the purity of gained powdered carbon is
Greatly 97.92%.
The method of the present invention a kind of ultrasonic assistant flotation alkaline pressure of oxygen leaching synthetical recovery aluminum electrolysis waste cathode carbon block, whole
The cycle of technique is 70min (not including pulverizing melting process).When industrial applications, the whole cycle can foreshorten to 1 hour.
The method of the present invention a kind of ultrasonic assistant flotation alkaline pressure of oxygen leaching synthetical recovery aluminum electrolysis waste cathode carbon block, passes through
Each technique and the synergism of conditional parameter, achieve beyond thought effect, especially ultrasonic frequency be 40KHz,
When ultrasonic power is 200W, ultrasonic leaching 10min in alkali liquor;The response rate of carbon is more than or equal to 97.05%.
Detailed description of the invention
It is described further below in conjunction with specific embodiment, but the present invention is not therefore subject to any restriction.
Embodiment 1
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 60.9, Al
12.23, O 9.55, F 5.38, Na 4.57, is crushed to-200 mesh and accounts for 90%, by liquid-solid ratio 8:1, broken powder is added NaOH
In the alkali liquor of concentration 2mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 90 DEG C, mixing speed 700rpm, alkali
Leaching time 60min, ultrasonic frequency 40KHz, power 200W, ultrasonic treatment time 30min;It is filtrated to get powdered carbon and filtrate,
Obtain the powdered carbon of 6.22g purity 97.89% after drying.
Alkali lixivium is passed through CO by 25L/h2Gas, ventilate 10min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 70min (not including broken melting process), and gained powdered carbon purity is 97.89%.
Comparative example
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 60.9, Al
12.23, O 9.55, F 5.38, Na 4.57, is crushed to-200 mesh and accounts for 90%, by liquid-solid ratio 8:1, broken powder is added NaOH
In the alkali liquor of concentration 2mol/L, the dipped journey of alkali is incubated in water-bath and carries out, constant temperature 90 DEG C, mixing speed 700rpm, during alkali leaching
Between 60min;It is filtrated to get powdered carbon and filtrate, obtains the powdered carbon of 7.04g purity 86.46% after drying.
Alkali lixivium is passed through CO by 25L/h2Gas, ventilate 10min, is filtrated to get electrolyte powder body.
Whole process cycle is 70min (not including broken melting process), and gained powdered carbon purity is 86.46%.
Embodiment 2
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 60.9, Al
12.23, O 9.55, F 5.38, Na 4.57, is crushed to-200 mesh and accounts for 50%, by liquid-solid ratio 10:1, broken powder is added NaOH
In the alkali liquor of concentration 3mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 100 DEG C, mixing speed 700rpm, alkali
Leaching time 90min, ultrasonic frequency 40KHz, power 50W, ultrasonic treatment time 50min;It is filtrated to get powdered carbon and filtrate, dry
The powdered carbon of 6.26g purity 97.31% is obtained after dry.
Alkali lixivium is passed through CO by 50L/h2Gas, ventilate 12min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 100min (not including broken melting process), and products therefrom powdered carbon purity is 97.31%.
Embodiment 3
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 60.9, Al
12.23, O 9.55, F 5.38, Na 4.57, is crushed to-200 mesh and accounts for 90%, by liquid-solid ratio 8:1, broken powder is added NaOH
In the alkali liquor of concentration 5mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 90 DEG C, mixing speed 1000rpm, alkali
Leaching time 180min, ultrasonic frequency 25KHz, power 600W, ultrasonic treatment time 180min;It is filtrated to get powdered carbon and filter
Liquid, obtains the powdered carbon of 6.22g purity 97.92% after drying.
Alkali lixivium is passed through CO by 5L/h2Gas, ventilate 30min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 210min (not including broken melting process), and gained powdered carbon purity is 97.92%.
Embodiment 4
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 48.86, Al
14.02, O 15.97, F 10.08, Na 4.58, is crushed to-200 mesh and accounts for 90%, added by broken powder by liquid-solid ratio 5:1
In the alkali liquor of NaOH concentration 1mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 90 DEG C, mixing speed
400rpm, alkali leaching time 60min, ultrasonic frequency 40KHz, power 150W, ultrasonic treatment time 30min;It is filtrated to get charcoal
Powder and filtrate, obtain the powdered carbon of 5.1g purity 97.61% after drying.
Alkali lixivium is passed through CO by 10L/h2Gas, ventilate 30min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 90min (not including broken melting process), and gained powdered carbon purity is 97.61%.
Embodiment 5
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 48.86, Al
14.02, O 15.97, F 10.08, Na 4.58, is crushed to-200 mesh and accounts for 100%, added by broken powder by liquid-solid ratio 7:1
In the alkali liquor of NaOH concentration 2mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 80 DEG C, mixing speed
600rpm, alkali leaching time 10min, ultrasonic frequency 40KHz, power 200W, ultrasonic treatment time 10min;It is filtrated to get charcoal
Powder and filtrate, obtain the powdered carbon of 5.59g purity 87.38% after drying.
Alkali lixivium is passed through CO by 100L/h2Gas, ventilate 10min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 20min (not including broken melting process), and gained powdered carbon purity is 87.38%.
Embodiment 6
Taking domestic certain factory aluminum cell waste cathode carbon block 10g, essential element content is (wt%): C 48.86, Al
14.02, O 15.97, F 10.08, Na 4.58, is crushed to-200 mesh and accounts for 80%, added by broken powder by liquid-solid ratio 8:1
In the alkali liquor of NaOH concentration 2mol/L, the dipped journey of alkali is incubated in ultrasonic environment and carries out, constant temperature 25 DEG C, mixing speed
700rpm, alkali leaching time 60min, ultrasonic frequency 25KHz, power 200W, ultrasonic treatment time 10min;It is filtrated to get charcoal
Powder and filtrate, obtain the powdered carbon of 5.05g purity 94.22% after drying.
Alkali lixivium is passed through CO by 100L/h2Gas, ventilate 5min, is filtrated to get electrolyte powder body, filtrate recycle.
Whole process cycle is 65min (not including broken melting process), and gained powdered carbon purity is 97.05%.
Claims (10)
1. the method for a ultrasonic assistant alkali leaching process aluminum electrolytic waste and old cathode carbon block, it is characterised in that comprise the following steps:
Step one
Aluminum cell waste cathode carbon block is crushed, obtains standby granule;
Step 2
Standby powder step one obtained adds ultrasonic leaching in alkali liquor, filters, obtain powdered carbon and the first filtrate after leaching;
Step 3
It is passed through CO to step 2 gained the first filtrate2, produce precipitation, filter to obtain cryolite, alumag and the second filter
Liquid, the second filtrate returns step 2 recycling.
The method of a kind of ultrasonic assistant alkali the most according to claim 1 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levying and be: in step one, in described standby granule, particle diameter accounts for the 50%-of standby granule gross mass less than the granule of 200 mesh
100%.
The method of a kind of ultrasonic assistant alkali the most according to claim 2 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levy and be: in step 2, at least one in NaOH, KOH, LiOH, RbOH of solute in alkali liquor.
The method of a kind of ultrasonic assistant alkali the most according to claim 3 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levy and be: in step 2, OH in described alkali liquor—Concentration be 1-5mol/L.
The method of a kind of ultrasonic assistant alkali the most according to claim 4 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levy and be: in step 2, when standby granule is added leaching in alkali liquor, control extraction temperature and be 25-100 DEG C, time 30-
180min, liquid-solid ratio is 5-10:1, stir speed (S.S.) 400-1000r/min.
The method of a kind of ultrasonic assistant alkali the most according to claim 5 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levying and be: in step 2, the frequency of ultrasonic leaching is 25-40KHz, and ultrasonic power is 50-600W, ultrasonic leaching time 10-
180min。
The method of a kind of ultrasonic assistant alkali the most according to claim 6 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levy and be: in step 3, described CO2Ventilating and be passed through filtrate by ventilation 5-100L/h, ventilation 5-30min produces precipitation, filters
Isolated cryolite, alumag and the second filtrate, the second filtrate returns step 2 and recycles.
The method of a kind of ultrasonic assistant alkali the most according to claim 7 leaching process aluminum electrolytic waste and old cathode carbon block, it is special
Levy and be: when ultrasonic frequency be 40KHz, ultrasonic power be 200W time, ultrasonic leaching 10min in alkali liquor;Product powdered carbon
Purity be 97.05%.
9. soak process aluminum electrolytic waste and old cathode carbon block according to a kind of ultrasonic assistant alkali described in claim 1-7 any one
Method, it is characterised in that: the purity of gained powdered carbon is 97.92% to the maximum.
10. soak process aluminum electrolytic waste and old cathode carbon block according to a kind of ultrasonic assistant alkali described in claim 1-7 any one
Method, it is characterised in that: the cycle of whole technique is 70min.
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CN108558223A (en) * | 2018-06-07 | 2018-09-21 | 沈阳银海再生资源科技有限公司 | Aluminium electroloysis waste lining prepares the method and system of rock wool |
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CN112322076B (en) * | 2020-11-04 | 2021-10-01 | 中南大学 | Method for preparing carbon black |
CN112322076A (en) * | 2020-11-04 | 2021-02-05 | 中南大学 | Method for preparing carbon black |
CN112808755A (en) * | 2021-02-01 | 2021-05-18 | 湖南绿脉环保科技股份有限公司 | Comprehensive utilization method of high-iron low-silicon red mud |
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