CN109650415A - A method of extracting lithium carbonate from the lithium iron phosphate battery anode powder scrapped - Google Patents
A method of extracting lithium carbonate from the lithium iron phosphate battery anode powder scrapped Download PDFInfo
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- CN109650415A CN109650415A CN201811475655.9A CN201811475655A CN109650415A CN 109650415 A CN109650415 A CN 109650415A CN 201811475655 A CN201811475655 A CN 201811475655A CN 109650415 A CN109650415 A CN 109650415A
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- lithium
- powder
- chemical combination
- iron phosphate
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- 239000000843 powder Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 38
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 36
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 24
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 33
- 239000000126 substance Substances 0.000 claims description 33
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 24
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- 239000004411 aluminium Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- 239000011575 calcium Substances 0.000 claims description 16
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 15
- 239000011777 magnesium Substances 0.000 claims description 15
- 229910052749 magnesium Inorganic materials 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000002893 slag Substances 0.000 claims description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 12
- 229910052791 calcium Inorganic materials 0.000 claims description 12
- 238000005485 electric heating Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 239000011574 phosphorus Substances 0.000 claims description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000002386 leaching Methods 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 238000012797 qualification Methods 0.000 claims description 7
- 235000017550 sodium carbonate Nutrition 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 6
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 claims description 4
- ZSYNKHJUSDFTCQ-UHFFFAOYSA-N [Li].[Fe].P(O)(O)(O)=O Chemical compound [Li].[Fe].P(O)(O)(O)=O ZSYNKHJUSDFTCQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 239000002686 phosphate fertilizer Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 241001062472 Stokellia anisodon Species 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- 229910001414 potassium ion Inorganic materials 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 229910001415 sodium ion Inorganic materials 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 235000011121 sodium hydroxide Nutrition 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000003660 carbonate based solvent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- -1 diaphragm Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 229940032958 ferric phosphate Drugs 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 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
- 235000019738 Limestone Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- 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
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The method that the invention discloses a kind of to extract lithium carbonate from the lithium iron phosphate battery anode powder scrapped, including " preparation positive powder-circulating leaching-filtration washing etc. " eight steps.The method that the object of the present invention is to provide a kind of to extract lithium carbonate from the lithium iron phosphate battery anode powder scrapped, the process is environmental-friendly, low energy consumption, production cost is low, blowdown flow rate is few, efficiently realizes comprehensive utilization of resources, meets industrialized production.
Description
Technical field
The present invention relates to belong to secondary resource to recycle and circular economy technical field, and in particular to a kind of from scrapping
The method of lithium carbonate is extracted in lithium iron phosphate battery anode powder.
Background technique
As the highest secondary cell of energy density, lithium ion battery can having covered absolutely in scale application energy storage device
Most of mobile communication and digital product market, and important influence is produced to its technological progress, in recent years, with performance and
The raising of production technique, lithium ion battery start to be applied to energy storage industry, environmentally protective New-energy electric vehicle and other electricity
The dynamic vehicles become a very important product in New Energy Industry, international, demand of the domestic market to lithium ion battery
Amount has started in blowout situation.
The lithium ion battery needs scrapped with the application of lithium ion battery, after thering are a large amount of service life to expire every year
It is safe and environment-friendly, expeditiously handle.Useless lithium battery recycling is of great immediate significance to new energy sustainable development, waste and old
The recovery operation of lithium battery can not only mitigate influence of the waste lithium cell to environment, can also economize on resources, reduce battery
Production cost generates biggish economic benefit.
Since lithium battery recycling is the novel industry risen in recent years, past production practices and technological accumulation are almost one
Piece blank.Domestic technique personnel had applied for the patent of many waste lithium cells recycling one by one in recent years, such as application No. is
201410354162.5 Chinese patent, disassembled using the lithium iron phosphate battery anode scrapped into iron phosphate lithium electrode and graphite plate
Electrode is put into addition electrolyte in electrolytic cell and is electrolysed, and is detached from lithium ion and enters solution, then extracts lithium after solution is concentrated
Salt.The method is feasible in principle, actually performance difficulty, we are in the practice of dismantling lithium battery, most of phosphoric acid
The positive plate of iron lithium is substantially damaged during dismantling, packaging, transport, so cannot obtain from useless lithium battery
To iron phosphate lithium electrode piece, electrolysis, concentration lithium-containing solution energy consumption are huge, economically also infeasible, in production can not at all
Using.Also such as all used in these national patents of CN102280673A, CN104362468A and CN102751548A
Old ferric phosphate lithium piece (powder) is subjected to high-temperature calcination, removal organic matter, oxidation ferrous iron, then carries out ball milling, selection by winnowing, solvent leaching
Out, it cleans, precipitate to extract lithium.In these methods, it is all used in the step of LiFePO4 is separated with aluminium collector first
High-temperature roasting, due to there is fluorine-containing oiliness binder PVDF in pole piece, is also mixed with plastics in pole piece during high-temperature roasting
The substances such as diaphragm, carbonate-based solvent, when high-temperature roasting, these substances can generate fluoride and carcinogenic dioxin gas, sternly
Heavily contaminated environment and to human body generation seriously affect, national environmental protection is very stringent to this monitoring, and waste lithium cell is wanted to pass through high temperature
Roasting is difficult to pass through in environmental protection to incinerate the large amount of organic wherein contained.
A series of problems that lithium encounters in production practice is mentioned for waste phosphoric acid lithium iron battery anode, we are in production practices
In constantly grope, improve, establish waste phosphoric acid iron lithium positive plate low temperature electric heating and rub mill separation, screening and cyclonic separation ferric phosphate with the hands
Lithium powder and aluminum shot, LiFePO4 powder directly use sulfuric acid dynamic circulation leach, leachate be separated by solid-liquid separation after, removing iron from solution, except aluminium, remove
Phosphorus filtering, filtrate add the simple process flow for adding sodium carbonate to precipitate lithium carbonate again by concentration after caustic soda deliming, magnesium.
Summary of the invention
The method that the object of the present invention is to provide a kind of to extract lithium carbonate from the lithium iron phosphate battery anode powder scrapped, should
Process is environmental-friendly, low energy consumption, production cost is low, blowdown flow rate is few, efficiently realizes comprehensive utilization of resources, meets industrialization
Production.
In order to achieve the above object, the technical solution adopted by the present invention is that: it is a kind of from the lithium iron phosphate battery anode powder scrapped
The middle method for extracting lithium carbonate, which comprises the steps of:
Step 1: preparation positive powder: the waste phosphoric acid lithium iron battery positive plate of dismantling being put into low temperature electric heating and rubs with the hands in grinding machine and will heat
Time is adjusted to 1~3 minute, and temperature is adjusted in the range of 150~300 DEG C, makes aluminium collector and phosphorus by screening and cyclone dust collection
Sour iron lithium powder separation；
Step 2: circulating leaching: the resulting iron phosphate lithium positive pole powder of step 1 being added to by the solid-to-liquid ratio of 1 ︰ 3.5~5 and is put into
In water or the circulation chemical combination bucket of filter residue washing lotion, the circulation chemical combination bucket is the steel lining anti-corrosion that two same volumes are 25m3~50m3
Ceramic tile, with stirring, drum with cover；Mounting height differs 300mm~1000mm, and the high bucket of installation site is known as chemical combination bucket I,
The bucket that installation position is set low is known as chemical combination bucket II；Chemical combination bucket I is connected with II top of chemical combination bucket with the PP pipe of ￠ 350mm；Chemical combination bucket II
Bottom be mounted with that a circulating pump is pumped into from I top of chemical combination bucket；It is added by the 30%~70% of positive powder weight from chemical combination bucket I dense
Sulfuric acid does not need to heat；Due to containing the aluminium powder of more organic matter and 2%~3% or so in positive powder, being added, the concentrated sulfuric acid is anti-
At once, chemical combination bucket top can generate a thick layer of thick foam, can constantly emit slot, constantly pass through ￠ from chemical combination bucket I
The PP pipe of 350mm flows to chemical combination bucket II, and foam and liquid pass through the circulating pump of II lower part of chemical combination bucket installation constantly from top again
It is pumped into chemical combination bucket I, entire reaction process recycles always, 2~6h of reaction time, and Paris white is added after detection is qualified by pH value tune
It is whole to 2~5；
Step 3: filtration washing: the slurry that step 2 is reacted is pumped into automatic chamber-type press filter filtering, and filtrate enters next work
Sequence, filter residue, which places into filter residue and stirs in cask washing to stir to wash, to be refiltered, and is stirred after washing filter 1~3 time, detection slag is containing solvable lithium less than 0.02%
When~0.1%, qualification is washed in wash heat, and cleaning solution is respectively put into liquid receiver, and slag is put into slag library, centralized processing；
Step 4: dephosphorization removes iron, removes aluminium: being added in removal of impurities bucket from the leachate that step 3 obtains and is heated to 60~90 DEG C, by every
Hydrogen peroxide oxidation 60~90 minutes of 5~30kg32% are added in cube leachate, then again plus Ca (OH) 2, pH value is transferred to 6~
10, it after detecting iron in solution, aluminium, phosphorus qualification, is filtered with filter press, filter residue enters slag library and is uniformly processed excessively, and solution enters next work
Sequence；
Step 5: solution deliming, magnesium: the filtrate that step 4 is obtained is put into removal of impurities bucket, is heated to 75~90 DEG C, adds piece alkali by PH
Value is transferred to 12 or more；Reaction 30~after sixty minutes, it is refiltered after detection calcium, magnesium all qualifications, filter residue enters slag library and is uniformly processed, filtrate
Into subsequent processing；
Step 6: removal of impurities liquid concentration: the removal of impurities liquid pump that step 5 obtains being entered into liquid storage tank, is concentrated by evaporation in four-effect evaporator, only
When change liquid is concentrated into 40~60 g/l of oxide containing lithium, cooling, precipitating is put into settling tank；
Step 7: precipitating lithium carbonate product: after step 6 concentration, the solution after standing for 24 hours in sedimentation basin is extracted from top
Clear liquid is added in sinker kettle, then after extraordinarily entering food-grade soda ash solid powder by the 1.1~1.6 of lithium molar ratio into kettle, then
Complexing agent EDETATE SODIUM is added in kettle in the ratio that 0.5~2kg is added in every cube of liquid, is warming up to 70~95 DEG C, stir 60~
150 minutes, after sampling is qualified, lithium carbonate product was obtained after dehydration, washing, drying；
Step 8: the processing of sinker tail water: step 7 sinker tail washings, washing water being pumped into MVR evaporator high temperature crystallization, produce anhydrous sodium sulphate
Product, condensed water return step three are used as slurry；
Further, in the step 1, the LiFePO4 powder mesh number isolated in grinding machine is rubbed with the hands from low temperature electric heating and reaches 300-
400 mesh account for 85%, aluminium content≤3%.
Further, in the step 2, the filter residue washing lotion oxide containing lithium being put into circulation chemical combination bucket reaches 3.5~
4.5g/l, the oxidation lithium content of last leachate is in 17~18g/l.
Further, in the step 3, slag and the reverse-flow washing of wash water, the amount and leaching of cleaning solution are used when residue washing
The amount of liquid is equal out, keeps water system balance, water system is avoided to expand.
Further, in the step 4, the Ca (OH) 2 of addition is manufactured emulsion.
Further, in the step 5, when adding piece alkali removing calcium and magnesium, if pH value is at 12 or more, calcium and magnesium is also below standard,
20% sodium carbonate liquor can be added, additive amount is added by 1.5 times of the sum of calcium, magnesium mole.
Further, in the step 7, in lithium carbonate washing operation, in order to by sodium ion, potassium ion, sulfate radical, chlorine
The solable matters such as root washing it is up to standard, using it is secondary stir wash, three times automatic centrifuge dehydration operating process.
Further, leached mud can be used as production phosphate fertilizer and smelt the raw material of ferrophosphorus.
The beneficial effects of the present invention are:
1, the present invention rubs mill separation LiFePO4 and aluminium collector with the hands using low temperature electric heating when positive plate of lithium battery is scrapped in processing
Innovative technology, heating and temperature control just fails in fluorine-containing binder PVDF, and the Undec temperature range of fluorine, at this
Within temperature range, while guaranteeing that plastic diaphragms and carbonate-based solvent also do not decompose, which solves positive plate of lithium battery height
Temperature roasting generates harmful fluoro-gas, generates the problem that carcinogenic dioxin gas endangers environment and the physical and mental health of people.
2, in order to emit slot when solving iron phosphate lithium positive pole powder acidleach, the problem that leaching operation can not carry out devises circulation
The innovative technology of leaching, it is ensured that normal production.
3, entire process design is with process is short, energy saving, production cost is low, the lithium rate of recovery is high, good product quality
Feature: lithium comprehensive recovery is greater than 92%, is higher by 8% or so than current domestic average level；Product quality reaches LITHIUM BATTERY carbonic acid
The standard of lithium.
4, production technology of the invention is environmental-friendly, and what is generated in entire production passes through acid mist spray column containing sour waste gas on a small quantity
Qualified discharge after spray, waste water extract anhydrous sodium sulphate after closed cycle, waste residue due to contain a large amount of phosphorus and iron, be production phosphate fertilizer and
The raw material of ferrophosphorus.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Fig. 2 is that implementation result compares figure to the present invention in a specific embodiment.
Specific embodiment
Table 1. scraps lithium iron phosphate battery anode powder chemical analysis (%)
| Li2O | Al | PVDF | Acetylene black | Carbonate-based solvent | Fe | PO4 | Other |
| 8.20 | 2.75 | 1.95 | 1.45 | 0.34 | 30 | 52 | 3.31 |
Embodiment one
Step 1: by 2kg scrap iron phosphate lithium positive pole piece be put into electric heating rub with the hands grinding machine separation positive powder and aluminium, electric heating time be
1.5 minutes, heating temperature was 220 DEG C, and iron phosphate lithium positive pole powder mesh number is -400 to account for 87%, iron phosphate lithium positive pole Fen ︰ aluminum shot=
80 ︰ 20, the weight of iron phosphate lithium positive pole powder are 1.6kg, and aluminum shot is 0.4 kg.Composition is shown in Table 1.
Step 2: obtaining iron phosphate lithium positive pole powder 1.6kg, be added in reactor tank and be tuned into the solid-liquid ratio of 1 ︰ 4.5 with water
After slurry, then in the ratio of the Zheng Ji Fen ︰ acid ︰ of (weight ratio)=1 0.4 it is slowly added to the concentrated sulfuric acid (attention emits slot, and acid addition time control exists
1h or more) it is not added thermal response, then plus agstone (CnCO3 >=90%) solution pH value is transferred to 4 by reaction time 4h, then
It is filtered, filter residue water counter current washes are secondary, and leaching requirement after wash water is collected, is used for next time by 4.5 times of meterings of positive powder amount
It leaches and uses.Leached mud does 1.5 times that agent slag rate is positive powder.
Step 3: leachate is added the hydrogen peroxide of the ratio addition 32% of 10kg in 1m3 liquid, adds to 80 DEG C, constant temperature stirs 70 points
Clock, then plus milk of lime pH value is transferred to 7.5, sample detection iron ion, aluminium ion, phosphate anion are respectively less than mistake after 0.008g/l
Filter.
Step 4: the solution of step 3 is heated to 85 DEG C, solid sodium hydroxide is added, solution pH value is transferred to 12 or more,
After forty minutes, sample detection calcium, magnesium are less than qualification after 0.01g/l for reaction, calculate by the sum of calcium, magnesium molar ratio, add 20% carbon
Acid sodium solution, until being filtered after calcium, magnesium are qualified.
Step 5: the solution that step 4 is filtered is concentrated by evaporation to original 1/2.5, is put into settling box cooling, precipitating
24h。
Step 6: taking supernatant to be put into sinker reactor tank the solution for precipitating 24 h, by the extraordinarily food of lithium molar ratio 1.25
After grade sodium carbonate, then by the EDETATE SODIUM of every 1m3 solution addition 0.8kg, 90 DEG C are warming up to, reacted 120 minutes, the carbon of precipitating
Sour lithium filters, and twice with the elution of 500ml deionized water, drying obtains lithium carbonate product.As a result see Fig. 2.
Embodiment two
It is compared with embodiment one, 2kg is scrapped into iron phosphate lithium positive pole piece in step 2 and rubs the 1.6kg that grinding machine is isolated with the hands through electric heating
Iron phosphate lithium positive pole powder, difference are, are added in reactor tank and are sized mixing by the solid-to-liquid ratio of 1 ︰ 3 with water, front and back process as in the first embodiment,
As a result see Fig. 2.
Embodiment three
It is compared with embodiment one, 2kg is scrapped into iron phosphate lithium positive pole piece in step 2 and rubs the 1.6kg that grinding machine is isolated with the hands through electric heating
Iron phosphate lithium positive pole powder is distinguished and is to be slowly added to the concentrated sulfuric acid in the ratio of Zheng Ji Fen ︰ acid=1 ︰ 0.65, and leached mud does agent slag rate
It is 2.2 times of positive powder, front and back process is as in the first embodiment, result is shown in Fig. 2.
Comparative example one
It compares with embodiment one, in step 1,2kg is scrapped into iron phosphate lithium positive pole piece and rubs separation of phosphorus in grinding machine with the hands through electric heating
Sour iron lithium positive powder and aluminium, electric heating time are 3 minutes, and heating temperature is 320 DEG C, and iron phosphate lithium positive pole powder mesh number is -400 mesh
92% is accounted for, iron phosphate lithium positive pole Fen ︰ aluminium=86 ︰ 14, i.e. positive powder 1.72kg, aluminium 0.28kg.Li2O content changes in the composition of table 1
Become 7.79%, Al content changes into 3.50%, and less, influence factor can be ignored for other composition variations.Subsequent process is the same as implementation
Example one, is as a result shown in Fig. 2.
Comparative example two
It compares with embodiment one, difference is in step 2, and pulverized limestone (CaCO3 >=90%), which will be added, makes solution pH value be transferred to 4
It is changed to make solution pH value be transferred to 4 with NaOH, leached mud does 1.2 times that agent rate is positive powder, and front and back process is as in the first embodiment, result
See Fig. 2.
Comparative example three
It compares with embodiment one, difference is that solid sodium hydroxide is added in step 4, and solution pH value is transferred to 12 or more and is changed to
Solid sodium carbonate is added, solution pH value is transferred to 12 or more, front and back process is as in the first embodiment, result is shown in Fig. 2.
As shown in Figure 2, the content, solid-to-liquid ratio of aluminium, sulphuric acid in iron phosphate lithium positive pole powder, except aluminium, except iron, remove
The series of factors such as the selection of pH value adjustment agent of phosphorus, removing calcium and magnesium produce the rate of recovery of the lithium of iron phosphate lithium positive pole powder, lithium carbonate
Product impurities affect is than more significant.
It should be noted that, in this document, the terms "include", "comprise" or its any other variant are intended to non-row
His property includes, so that the process, method, article or equipment for including a series of elements not only includes those elements, and
And further include other elements that are not explicitly listed, or further include for this process, method, article or equipment institute it is intrinsic
Element.
Used herein a specific example illustrates the principle and implementation of the invention, the explanation of above example
It is merely used to help understand method and its core concept of the invention.The above is only a preferred embodiment of the present invention, it answers
When pointing out due to the finiteness of literal expression, and objectively there is unlimited specific structure, for the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement, retouching or variation can also be made, can also incited somebody to action
Above-mentioned technical characteristic is combined in the right way；These improve retouching, variation or combination, or the not improved structure by invention
Think and technical solution directly applies to other occasions, is regarded as protection scope of the present invention.
Claims (8)
1. a kind of method for extracting lithium carbonate from the lithium iron phosphate battery anode powder scrapped, which is characterized in that including walking as follows
It is rapid:
Step 1: preparation positive powder: the waste phosphoric acid lithium iron battery positive plate of dismantling being put into low temperature electric heating and rubs with the hands in grinding machine and will heat
Time is adjusted to 1~3 minute, and temperature is adjusted in the range of 150~300 DEG C, makes aluminium collector and phosphorus by screening and cyclone dust collection
Sour iron lithium powder separation；
Step 2: circulating leaching: the resulting iron phosphate lithium positive pole powder of step 1 being added to by the solid-to-liquid ratio of 1 ︰ 3.5~5 and is put into
In water or the circulation chemical combination bucket of filter residue washing lotion, the circulation chemical combination bucket is that two same volumes are 25m3~50m3Steel lining anti-corrosion
Ceramic tile, with stirring, drum with cover；Mounting height differs 300mm~1000mm, and the high bucket of installation site is known as chemical combination bucket I,
The bucket that installation position is set low is known as chemical combination bucket II；Chemical combination bucket I is connected with II top of chemical combination bucket with the PP pipe of ￠ 350mm；Chemical combination bucket II
Bottom be mounted with that a circulating pump is pumped into from I top of chemical combination bucket；It is added by the 30%~70% of positive powder weight from chemical combination bucket I dense
Sulfuric acid does not need to heat；Due to containing the aluminium powder of more organic matter and 2%~3% or so in positive powder, being added, the concentrated sulfuric acid is anti-
At once, chemical combination bucket top can generate a thick layer of thick foam, can constantly emit slot, constantly pass through ￠ from chemical combination bucket I
The PP pipe of 350mm flows to chemical combination bucket II, and foam and liquid pass through the circulating pump of II lower part of chemical combination bucket installation constantly from top again
It is pumped into chemical combination bucket I, entire reaction process recycles always, 2~6h of reaction time, and Paris white is added after detection is qualified by pH value tune
It is whole to 2~5；
Step 3: filtration washing: the slurry that step 2 is reacted is pumped into automatic chamber-type press filter filtering, and filtrate enters next work
Sequence, filter residue, which places into filter residue and stirs in cask washing to stir to wash, to be refiltered, and is stirred after washing filter 1~3 time, detection slag is containing solvable lithium less than 0.02%
When~0.1%, qualification is washed in wash heat, and cleaning solution is respectively put into liquid receiver, and slag is put into slag library, centralized processing；
Step 4: dephosphorization removes iron, removes aluminium: being added in removal of impurities bucket from the leachate that step 3 obtains and is heated to 60~90 DEG C, by every
Hydrogen peroxide oxidation 60~90 minutes of 5~30kg32% are added in cube leachate, then again plus Ca (OH)2, pH value is transferred to 6~
10, it after detecting iron in solution, aluminium, phosphorus qualification, is filtered with filter press, filter residue enters slag library and is uniformly processed excessively, and solution enters next work
Sequence；
Step 5: solution deliming, magnesium: the filtrate that step 4 is obtained is put into removal of impurities bucket, is heated to 75~90 DEG C, adds piece alkali by PH
Value is transferred to 12 or more；Reaction 30~after sixty minutes, it is refiltered after detection calcium, magnesium all qualifications, filter residue enters slag library and is uniformly processed, filtrate
Into subsequent processing；
Step 6: removal of impurities liquid concentration: the removal of impurities liquid pump that step 5 obtains being entered into liquid storage tank, is concentrated by evaporation in four-effect evaporator, only
When change liquid is concentrated into 40~60 g/l of oxide containing lithium, cooling, precipitating is put into settling tank；
Step 7: precipitating lithium carbonate product: after step 6 concentration, the solution after standing for 24 hours in sedimentation basin is extracted from top
Clear liquid is added in sinker kettle, then after extraordinarily entering food-grade soda ash solid powder by the 1.1~1.6 of lithium molar ratio into kettle, then
Complexing agent EDETATE SODIUM is added in kettle in the ratio that 0.5~2kg is added in every cube of liquid, is warming up to 70~95 DEG C, stir 60~
150 minutes, after sampling is qualified, lithium carbonate product was obtained after dehydration, washing, drying；
Step 8: the processing of sinker tail water: step 7 sinker tail washings, washing water being pumped into MVR evaporator high temperature crystallization, produce anhydrous sodium sulphate
Product, condensed water return step three are used as slurry.
2. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 1, rubs the LiFePO4 powder mesh number isolated in grinding machine with the hands from low temperature electric heating and reach 300-400
Mesh accounts for 85%, aluminium content≤3%.
3. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 2, the filter residue washing lotion oxide containing lithium being put into circulation chemical combination bucket reaches 3.5~4.5g/l, finally
The oxidation lithium content of leachate is in 17~18g/l.
4. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 3, slag and the reverse-flow washing of wash water, the amount of cleaning solution and the amount of leachate is used when residue washing
It is equal, water system balance is kept, water system is avoided to expand.
5. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 4, the Ca (OH) of addition2For manufactured emulsion.
6. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 5, when adding piece alkali removing calcium and magnesium, if pH value is at 12 or more, calcium and magnesium is also below standard, can be added
20% sodium carbonate liquor, additive amount are added by 1.5 times of the sum of calcium, magnesium mole.
7. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, in the step 7, in lithium carbonate washing operation, in order to which sodium ion, potassium ion, sulfate radical, chlorine root etc. is solvable
Property matter detergent it is up to standard, using it is secondary stir wash, three times automatic centrifuge dehydration operating process.
8. a kind of method that lithium carbonate is extracted from the lithium iron phosphate battery anode powder scrapped according to claim 1,
It is characterized in that, leached mud can be used as production phosphate fertilizer and smelt the raw material of ferrophosphorus.
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Denomination of invention: A Method for Extracting Lithium Carbonate from Scrapped Lithium Iron Phosphate Battery Positive Electrode Powder Effective date of registration: 20231027 Granted publication date: 20230210 Pledgee: Hunan Jinshi Rural Commercial Bank Co.,Ltd. Yaopodu Sub branch Pledgor: HUNAN TIANTAI TIANRUN NEW ENERGY TECHNOLOGY CO.,LTD. Registration number: Y2023980062988 |