CN110028042A - A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block - Google Patents
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block Download PDFInfo
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- CN110028042A CN110028042A CN201910373403.3A CN201910373403A CN110028042A CN 110028042 A CN110028042 A CN 110028042A CN 201910373403 A CN201910373403 A CN 201910373403A CN 110028042 A CN110028042 A CN 110028042A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/07—Preparation from the hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/06—Preparation with gaseous nitric acid or nitrogen oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention discloses a kind of recoverying and utilizing method of aluminum cell waste cathode carbon block, aluminum cell waste cathode carbon block raw material is obtained powdered carbon after broken, color sorting, crushing, ball milling by this method, then supplying accounts for the 5A type of 5~20wt% of powdered carbon quality and granularity less than 2mm or 10X type zeolite molecular sieve and is heat-treated 30~120min at a temperature of 800~1600 DEG C, 98wt% is added in obtained fluorine-containing solid product, the HF gas of generation is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product by 80~120 DEG C of hot concentrated sulfuric acids.The present invention is using zeolite molecular sieve as heat treatment reaction mass, play the role of catalyst and dispersing agent simultaneously, technique is advanced, with the obvious advantage, high added value hydrofluoric acid product, environmental benefit and remarkable in economical benefits are obtained under the premise of realizing pernicious gas " zero-emission ".
Description
Technical field
The invention belongs to Aluminium Industry solid waste technical field of comprehensive utilization.Specifically a kind of waste and old yin of electrolytic aluminium electrolytic tank
Pole carbon block harmless treatment and effectively the recycling wherein method of charcoal and fluorine resource.
Background technique
The Aluminium Industry in China is always maintained at higher growth rate since the 21th century certainly.The electricity of alumina eltrolysis
It is limited to solve groove life, an overhaul will be carried out within every 3~5 years, waste cathode carbon block is the main waste that electrolytic cell overhaul generates
One of, it is the fluorine-containing dangerous solid waste generated in electrolytic process.
To China in 2017 is completed about 45,000,000 tons of aluminium electroloysis production capacity, actual production is more than 36,000,000 tons, accounts for global electricity
Solve 50% or more of aluminium production capacity.During aluminum electrolysis, charcoal cathode due to fluorine-containing salts infiltration and expand, further cause
The breakage of electrolytic cell is scrapped.Aluminium cell generally just needed to stop groove overhaul using 4~6 years or so, took out all waste lining materials
Expect (referred to as slag from delining), waste cathode carbon block accounts for about the 50% of slag from delining.Slag from delining is inevitable during Aluminum Electrolysis Production
Solid waste, 1 ton of electrolytic aluminium of every production about generates the slag from delining of 10~30kg.Electrolytic aluminium slag from delining is in " National Hazard
Waste register " in be defined as dangerous solid waste (classification are as follows: HW48), waste lining has been put into " National Hazard waste register "
HW32 inorganic fluoride waste, HW33 inorganic cyanide waste.In aluminum electrolysis waste cathode carbon block, carbon materials account for 30%~
70%, remaining is electrolyte, is mainly Na3 [AlF6], NaF, CaF2, MgF2, LiF, AlF3, NaCN, Na4 [Fe (CN) 6] etc.,
There are also a small amount of Al, Al4C3, AlN, Na etc., these substances and water have soluble and reactivity, can generate HF, HCN,
H2, CH4, NH3 etc. be harmful or imflammable gas, it is fluorine-containing, enter containing cyanogen compound environment can health to the mankind and animals and plants with
Growth constitutes greatly harm.Therefore, the comprehensive utilization technique for studying aluminum cell waste cathode carbon block is both resource reclaim
The requirement of content and environmental protection meets the requirement of China's strategy of sustainable development.
Waste cathode carbon block is a kind of valuable resource rich in high-graphitized carbon and fluorine-containing electrolyte.Therefore, how thoroughly
The harm of fluoride and cyanide in aluminium electroloysis waste cathode carbon block is released, realizes the innoxious and resource of aluminium electroloysis waste cathode carbon block
Change that recycle be the industry difficulty for needing to capture, expert scholar and production line personnel have carried out more for this problem
Year unremitting exploratory development, such as taken using alkali leaching or ultrasonic wave secondary flotation alkaline pressure of oxygen leaching (CN106745137A,
CN106077038A、CN106077040A、CN106587122A、CN101817521A、CN106086938A、
CN105821445A), acid processing or ultrasonic wave secondary flotation pressurization acid processing (CN106077037A, CN106077036A,
CN106180118A, CN101984984A), alkali leaching combine with Ore Leaching and flyash (CN107162061A), keep the temperature remove
Cyanogen combination flotation obtain breeze and electrolyte slag and heat go charcoal (CN106064813A, CN105964659A, CN107313073A),
High-temperature calcination (CN102989744A, CN105964660A, CN106517209A, CN107904621A, CN106147910A,
CN100542702C、CN101054693A、CN107628614A、CN105642649A、CN106185818A、
CN106269787A), water logging (CN105772486A, CN107377592A, CN105728440A, CN106166560A) and change
The methods of precipitating (CN105327933A) is learned to be handled.
From the point of view of existing technological achievement, the innoxious of waste cathode of aluminum electrolytic cell carbon block, recycling treatment are utilized and are divided into
Two major class of wet-treating and high-temperature process of aqueous solution.Wet-treating further relates to washing (leaching), alkali process, acid processing, Acid-Base
Joint and combination floatation process etc. use oxidant by cyanogen mainly for the purpose of recycling electrolyte and carbon in wet-treating
Compound resolves into harmless gaseous matter.High-temperature process technology is mainly for the purpose of innoxious, using useless cathode as fuel combustion,
Or using the technologies such as high temperature, vacuum combine, utilizations is separately recovered in electrolyte or carbon materials, contain cyanogen compound at high temperature by
Oxygenolysis is at harmless gaseous matter.
From the point of view of existing technological achievement, the wet-treating of waste cathode of aluminum electrolytic cell carbon block and high-temperature process still have with
Lower problem causes secondary pollution if a large amount of saliferous generated in wet-treating, fluoride waste are not effectively addressed；Institute
The H of generation2、CH4、NH3Gas is not under control and utilizes, and generated HF causes serious pollution；The electrolyte of recycling and
Carbon materials impurity content is excessively high, cannot directly utilize；The difference in aluminum electrolytic tank capacity and slot age, the fluctuation of ingredient, powder grain
The influence of the factors such as degree, causes technique controlling difficulty big；The tail gas of a large amount of entrainment HF and dust can be generated in high-temperature process；Electricity
Solution matter recycling is not thorough, and partially remains in carbon materials or clinker；The electrolyte of low melting point occurs vitreous clinker in furnace, leads
Cause the incomplete residual quantity of Carbon Materials oxidizing fire larger, electrolyte vitreous clinker in furnace causes production status to deteriorate, production is steady
Qualitative difference.
Summary of the invention
The purpose of the present invention is to the existing shortcomings to aluminium electroloysis waste cathode carbon block processing scheme, provide one
Cover new technical solution.Program combination pyrogenic attack and wet-treating, for containing the spy of fluoride in waste cathode carbon block
Property, aluminum cell waste cathode carbon block is subjected to harmless treatment and resource utilization, is realizing pernicious gas " zero-emission "
Under the premise of obtain high added value hydrofluoric acid product, further solve such solid waste environmental issue and generate considerable economic benefit.
The main ingredient of zeolite molecular sieve is SiO2And Al2O3The compound of equal sieve and silica-sesquioxides, with carbon block can occur with
Lower reaction:
C(NaF)+O2→NaF+CO2↑ (1)
2NaCN+(2X+5)/2O2→2Na2O+2CO2↑+2NOx↑ (2)
2CaO+SiO2→Ca2SiO4 (3)
2NaF+CaO+2SiO2+Al2O3→CaF+2NaAlSiO4 (4)
2NaF+3CaO+SiO2+11Al2O3→Ca2SiO4·CaF2+2NaAl11O17 (5)
The technical scheme to solve the above technical problems is that
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, which is characterized in that its treatment process includes following
Step: waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh using crusher and ball mill, charcoal is added in powdered carbon
5~20wt% of silty amount and granularity are less than the 5A type or 10X type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；It will mix
Solid powder is closed at a temperature of 800~1600 DEG C, 30~120min of high-temperature heat treatment；It is heat-treated the CO generated2、NOxGas is passed through
10%NaOH solution is absorbed, and Na is obtained2CO3、NaNO3Salting liquid and recycled；What is obtained after heat treatment is fluorine-containing solid
80~120 DEG C of the 98wt% concentrated sulfuric acid is added in body object can obtain three solids, mixing salt solution and HF gas products, wherein
Solid product is powdered carbon, for recycling；Liquid is mixing salt solution, is added after 20%NaOH solution adjusting pH value of solution is 7 and obtains
To Na2SO4Solution is simultaneously recycled；HF gas is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product.
In the present invention, used zeolite molecular sieve is 5A type zeolite molecular sieve.
The present invention plays the role of catalyst and dispersing agent using zeolite molecular sieve as heat treatment reaction mass, work
Skill is advanced, with the obvious advantage, and high added value hydrofluoric acid product, environmental benefit are obtained under the premise of realizing pernicious gas " zero-emission "
And remarkable in economical benefits.
Detailed description of the invention
Fig. 1 is the recoverying and utilizing method process flow chart of aluminum cell waste cathode carbon block of the present invention.Raw material is aluminium electroloysis
Slot waste and old cathode carbon block；Hybrid solid is the powdered carbon and the solid material of zeolite molecular sieve after mixing crushed, after ball milling；
Solid is fluorine-containing solid product after heat treatment；Gas is the mixed gas that heat treatment generates；Liquid is that the concentrated sulfuric acid of addition heat is wet
The mixing salt solution obtained after method processing.
Specific embodiment
The present invention is further detailed below with reference to embodiment, but it should be noted that application range of the invention not
It is confined to these embodiments.
Embodiment 1
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, treatment process is the following steps are included: using broken
Waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh by broken machine and ball mill, and powdered carbon quality is added in 10g powdered carbon
5wt%, i.e. 0.5g and granularity are less than the 5A type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；By hybrid solid powder
At 800 DEG C, high-temperature heat treatment 30min；It is heat-treated the CO generated2、NOxGas is passed through 10%NaOH solution and is absorbed, and obtains
Na2CO3、NaNO3Salting liquid and recycled；It is dense that 80 DEG C of 98wt% is added in the fluorine-containing solids obtained after heat treatment
Sulfuric acid can obtain three solids, mixing salt solution and HF gas products, wherein solid product is powdered carbon, for recycling；Liquid
For mixing salt solution, it is added after 20%NaOH solution adjusting pH value of solution is 7 and obtains Na2SO4Solution is simultaneously recycled；By HF gas
It is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product, the fluorine rate of recovery is 81.3% in carbon block of giving up.
Embodiment 2
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, treatment process is the following steps are included: using broken
Waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh by broken machine and ball mill, and powdered carbon quality is added in 10g powdered carbon
20wt%, i.e. 2.0g and granularity are less than the 10X type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；By hybrid solid powder
End is at a temperature of 1600 DEG C, high-temperature heat treatment 120min；It is heat-treated the CO generated2、NOxGas is passed through the progress of 10%NaOH solution
It absorbs, obtains Na2CO3、NaNO3Salting liquid and recycled；120 DEG C are added in the fluorine-containing solids obtained after heat treatment
The 98wt% concentrated sulfuric acid can obtain three solids, mixing salt solution and HF gas products, wherein solid product is powdered carbon, for return
Receipts are used again；Liquid is mixing salt solution, is added after 20%NaOH solution adjusting pH value of solution is 7 and obtains Na2SO4Solution is simultaneously returned
It receives；HF gas is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product, the fluorine rate of recovery is 82.7% in carbon block of giving up.
Embodiment 3
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, treatment process is the following steps are included: using broken
Waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh by broken machine and ball mill, and powdered carbon quality is added in 20g powdered carbon
10wt%, i.e. 2.0g and granularity are less than the 5A type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；By hybrid solid powder
End is at a temperature of 1000 DEG C, high-temperature heat treatment 80min；It is heat-treated the CO generated2、NOxGas is passed through 10%NaOH solution and is inhaled
It receives, obtains Na2CO3、NaNO3Salting liquid and recycled；110 DEG C are added in the fluorine-containing solids obtained after heat treatment
The 98wt% concentrated sulfuric acid can obtain three solids, mixing salt solution and HF gas products, wherein solid product is powdered carbon, for recycling
It uses again；Liquid is mixing salt solution, is added after 20%NaOH solution adjusting pH value of solution is 7 and obtains Na2SO4Solution is simultaneously recycled；
HF gas is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product, the fluorine rate of recovery is 84.1% in carbon block of giving up.
Embodiment 4
A kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, treatment process is the following steps are included: using broken
Waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh by broken machine and ball mill, and powdered carbon quality is added in 30g powdered carbon
8wt% and granularity are less than the 10X type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；By hybrid solid powder 1200
At a temperature of DEG C, high-temperature heat treatment 60min；It is heat-treated the CO generated2、NOxGas is passed through 10%NaOH solution and is absorbed, and obtains
Na2CO3、NaNO3Salting liquid and recycled；It is dense that 100 DEG C of 98wt% is added in the fluorine-containing solids obtained after heat treatment
Sulfuric acid can obtain three solids, mixing salt solution and HF gas products, wherein solid product is powdered carbon, for recycling；Liquid
For mixing salt solution, it is added after 20%NaOH solution adjusting pH value of solution is 7 and obtains Na2SO4Solution is simultaneously recycled；By HF gas
It is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product, the fluorine rate of recovery is 83.5% in carbon block of giving up.
Claims (2)
1. a kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block, which is characterized in that its treatment process include with
Lower step: waste and old cathode carbon block is crushed to powdered carbon of the granularity less than 45 mesh using crusher and ball mill, is added in powdered carbon
5~20wt% of powdered carbon quality and granularity are less than the 5A type or 10X type zeolite molecular sieve of 2mm, obtain uniformly mixed solid powder；It will
Hybrid solid powder is at a temperature of 800~1600 DEG C, 30~120min of high-temperature heat treatment；It is heat-treated the CO generated2、NOxGas is logical
Enter 10%NaOH solution to be absorbed, obtains Na2CO3、NaNO3Salting liquid and recycled；What is obtained after heat treatment is fluorine-containing
80~120 DEG C of the 98wt% concentrated sulfuric acid is added in solids can obtain three solids, mixing salt solution and HF gas products,
In, solid product is powdered carbon, for recycling；Liquid is mixing salt solution, after addition 20%NaOH solution adjusting pH value of solution is 7
Obtain Na2SO4Solution is simultaneously recycled；HF gas is passed through after deionized water carries out absorption condensation and obtains hydrofluoric acid product.
2. a kind of recoverying and utilizing method of electrolytic aluminium electrolytic tank waste and old cathode carbon block according to claim 1, feature exist
In the zeolite molecular sieve is 5A type zeolite molecular sieve.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408959A (en) * | 2019-07-25 | 2019-11-05 | 中南大学 | The method of charcoal and electrolyte is recycled in a kind of aluminum electrolysis waste cathode carbon block |
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| CN110408959B (en) * | 2019-07-25 | 2021-03-26 | 中南大学 | Method for recovering carbon and electrolyte from aluminum electrolysis waste cathode carbon blocks |
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