CN107196004B - A method of recycling valuable metal from applying waste lithium ionic power battery - Google Patents
A method of recycling valuable metal from applying waste lithium ionic power battery Download PDFInfo
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- CN107196004B CN107196004B CN201710336679.5A CN201710336679A CN107196004B CN 107196004 B CN107196004 B CN 107196004B CN 201710336679 A CN201710336679 A CN 201710336679A CN 107196004 B CN107196004 B CN 107196004B
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- sulfuric acid
- mixed powder
- power battery
- filtrate
- hydroxide
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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
- 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
Abstract
The method that the invention discloses a kind of from waste and old lithium ion power power battery recycles valuable metal, including applying waste lithium ionic power battery through overdischarge, disassemble, isolate positive plate;Positive plate is calcined under nitrogen atmosphere, crushed and is sieved, the mixed powder of LFP and NCM are obtained;Sulfuric acid is sequentially added into mixed powder and hydrogen peroxide is reacted, and leachate adjusts pH with ammonium hydroxide and refilters after filtering, and filtrate adjusts pH with alkali and refilters, and second level filtrate is extracted with phosphoric acid kind of extractants, is then allowed to stand, is isolated organic phase and water phase;Solid sodium carbonate is added to water phase, precipitates to obtain lithium carbonate;Into organic phase plus dilute sulfuric acid is stripped, then adjusts its pH after adjusting nickel cobalt manganese ratio;Finally it is aged to obtain nickel cobalt manganese hydroxide.The step of recovery method of the invention is simple, handles simultaneously to ternary and iron lithium cell, reduces battery sorting, is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of recovery methods of waste and old lithium ion battery, in particular to a kind of from applying waste lithium ionic power electric
The method of valuable metal is recycled in pond.
Background technique
Lithium ion battery has many advantages, such as that energy density is high, has extended cycle life, self discharge is small, memory-less effect, from commodity
Since change, has received widespread attention and applied.The positive electrode of lithium-ion-power cell has LiFePO4 (LFP) or nickel cobalt manganese
(NCM) the advantages that material etc., lithium iron phosphate positive material is safe and environment-friendly with its, stability is good, has very big in power battery market
Advantage.Explosive growth is presented in China's electric car within 2014, and waste battery is also increasing at the same time, how to handle this
A little old and useless batterys have become social issues that need special attention;In addition with the fast development of ternary battery material, the following ternary material
It is also considerable that material scraps market.
It about most of recycling of waste and old lithium ion battery is respectively processed to LFP battery and NCM battery at present, this
Kind process is sorted firstly the need of to waste and old power battery, separately carries out processing recycling, this method recovery efficiency is low
And process flow is complicated, economic benefit is not significant.
Summary of the invention
To solve the above problems, there is technique letter the invention discloses a kind of method for handling LFP Yu NCM battery simultaneously
It is single, recovery efficiency is high, the advantages that economizing on resources, be suitble to large-scale production.
The present invention is achieved through the following technical solutions:
The method of valuable metal is recycled in a kind of applying waste lithium ionic power battery, comprising the following steps:
(1) applying waste lithium ionic power battery disassembles decladding after overdischarge, then the dismantling of resulting battery roll core is isolated
Positive plate;
(2) positive plate is calcined under nitrogen atmosphere, then crushes and cross 80 meshes, obtains the mixing of LFP and NCM
Powder;
(3) sulfuric acid being sequentially added to mixed powder and hydrogen peroxide being reacted, being filtered to product must except after carbon elimination slag
Leachate;
(4) adjusting the pH value of leachate with ammonium hydroxide is 2-2.5, filters to obtain sediment ferric phosphate and filtrate;
(5) filtrate in step (4) is adjusted pH value with alkali is 5-6, after being filtered to remove a small amount of remaining iron and aluminium, obtains two
Grade filtrate;
(6) it will be extracted through step (5) treated second level filtrate with phosphoric acid kind of extractants, and be then allowed to stand, isolate
Organic phase and water phase;
(7) solid sodium carbonate is added to water phase, precipitates to obtain lithium carbonate;
(8) add dilute sulfuric acid to be stripped into organic phase, nickel source, cobalt source or manganese source is added into strip liquor then to adjust
Save nickel cobalt manganese ratio, make nickel, cobalt, the manganese element molar ratio 1:1:1 in strip liquor, then plus alkali adjust its pH value as 11-12;Most
After be aged to obtain nickel cobalt manganese hydroxide.
Further scheme, the temperature that positive plate is calcined under nitrogen atmosphere in the step (2) is 400-600 DEG C, calcining
Time is 2-4h.
Further scheme, the concentration of sulfuric acid is 2.5-4mol/L, the matter of the mixed powder and sulfuric acid in the step (3)
Amount volume ratio g:mL is 1:(6-10), the additional amount of the hydrogen peroxide is that 2-4mL is added in every gram of mixed powder.
Further scheme, the reaction temperature in the step (3) are 60-90 DEG C.
Further scheme, the alkali in the step (5) and step (8) are one in sodium hydroxide, potassium hydroxide or ammonium hydroxide
Kind is several.
Further scheme, phosphoric acid kind of extractants is one of P204, P507, Cyanex272 or several in the step (6)
Kind.
Further scheme, the concentration of the dilute sulfuric acid in the step (7) are 0.1mol/L-1mol/L.
P204, P507, Cyanex272 in the present invention are the extractants that American Cyanamid Company is used as Separation of nickel and cobalt, are these
The common extractant in field.
The beneficial effects of the present invention are:
1, recovery process method of the invention is simple, directly handles applying waste lithium ionic electrical core of power battery, reduces
The step of cell classification, is suitable for large-scale production;
2, recovery process of the invention can be recycled simultaneously LFP battery and NCM battery, and by gold therein
Belong to element to be recycled respectively with ferric phosphate, lithium carbonate and nickel cobalt manganese hydroxide form, removal process is simple and efficient, and is had
Considerable economic benefit.
Detailed description of the invention
Fig. 1 is the flow chart that valuable metal is recycled from applying waste lithium ionic power battery.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1
A kind of method that valuable metal is recycled in applying waste lithium ionic power battery, as shown in Figure 1, comprising the following steps:
(1) applying waste lithium ionic power battery is obtained into battery roll core after overdischarge carries out dismantling decladding;
(2) positive plate is isolated into battery roll core dismantling;
(3) positive plate 400 calcines 4h, binder PVDF and diaphragm in pyrolytic battery roll core under nitrogen atmosphere;
(4) battery roll core obtained in step (3) is smashed it through into 80 meshes, extracting screen underflow obtains LFP and NCM mixed powder
Material;
(5) sulfuric acid of 4mol/L and hydrogen peroxide/every gram of material of 2ml, reaction temperature 90 are sequentially added into mixed powder
DEG C, the mass volume ratio 1/10(kg/L of added mixed powder and sulfuric acid), it is filtered to remove carbon slag and obtains leachate;
(6) leachate to pH=2 are adjusted with ammonium hydroxide and is settled out ferric phosphate, filtered to get filtrate;
(7) leachate is adjusted with sodium hydroxide and precipitate a small amount of remaining iron and aluminium to pH=5, filter to get filtrate;
(8) filtrate obtained in step (7) is extracted with P204 and removes nickel cobalt manganese metal ion, settle and separate go out organic phase and
Water phase.
(9) sodium carbonate solid is added into water phase obtained in step (8), obtains lithium carbonate precipitating;
(10) it is added to the dilute sulfuric acid that concentration is 0.1mol/L to organic obtained in step (8) and is stripped, obtain anti-
Extract liquid;
(11) nickel source is added into strip liquor, cobalt source or manganese source adjust nickel cobalt manganese ratio, make nickel in strip liquor, cobalt,
Manganese element molar ratio is 1:1:1, then adjusts pH=11 with sodium hydroxide and be aged to obtain nickel cobalt manganese hydroxide.
Embodiment 2
(1) applying waste lithium ionic power battery is obtained into battery roll core after overdischarge carries out dismantling decladding;
(2) positive plate is isolated into battery roll core dismantling;
(3) positive plate 500 DEG C of calcining 3h under nitrogen atmosphere, binder PVDF in pyrolytic battery roll core and every
Film;
(4) battery roll core obtained in step (3) is smashed it through into 80 meshes, extracting screen underflow obtains LFP and NCM mixed powder
Material;
(5) sulfuric acid of 3mol/L and hydrogen peroxide/every gram of material of 4ml, reaction temperature 80 are sequentially added into mixed powder
DEG C, the mass volume ratio 1/8(kg/L of added mixed powder and sulfuric acid), it is filtered to remove carbon slag and obtains leachate;
(6) leachate to pH=2 are adjusted with ammonium hydroxide and is settled out ferric phosphate, filtered to get filtrate;
(7) leachate is adjusted with potassium hydroxide and precipitate a small amount of remaining iron and aluminium to pH=6, filter to get filtrate;
(8) filtrate obtained in step (7) is extracted with P507 and removes nickel cobalt manganese metal ion, settle and separate go out organic phase and
Water phase.
(9) sodium carbonate solid is added into water phase obtained in step (8), lithium is recycled in the form of lithium carbonate;
(10) it is added to the dilute sulfuric acid that concentration is 0.5mol/L to organic obtained in step (8) and is stripped, obtain anti-
Extract liquid;
(11) nickel source is added into strip liquor, cobalt source or manganese source adjust nickel cobalt manganese ratio, make nickel in strip liquor, cobalt,
Manganese element molar ratio is 1:1:1, then adjusts pH=11.5 with potassium hydroxide and be aged to obtain nickel cobalt manganese hydroxide.
Embodiment 3
(1) applying waste lithium ionic power battery is obtained into battery roll core after overdischarge carries out dismantling decladding;
(2) positive plate is isolated into battery roll core dismantling;
(3) positive plate 600 DEG C of calcining 2h under nitrogen atmosphere, binder PVDF in pyrolytic battery roll core and every
Film;
(4) battery roll core obtained in step (3) is smashed it through into 80 meshes, extracting screen underflow obtains LFP and NCM mixed powder
Material;
(5) sulfuric acid of 2.5mol/L and hydrogen peroxide/every gram of material of 3ml are sequentially added into mixed powder, reaction temperature is
60 DEG C, the mass volume ratio 1/6(kg/L of added mixed powder and sulfuric acid), it is filtered to remove carbon slag and obtains leachate;
(6) it is settled out ferric phosphate with adjusting leachate to pH=2.5 in ammonium hydroxide, filtered to get filtrate;
(7) it with leachate is adjusted in ammonium hydroxide to a small amount of remaining iron of the precipitating of pH=6 and aluminium, filters to get filtrate;
(8) filtrate obtained in step (7) is extracted with Cyanex272 and removes nickel cobalt manganese metal ion, settle and separate goes out to have
Machine phase and water phase.
(9) sodium carbonate solid is added into water phase obtained in step (8), lithium is recycled in the form of lithium carbonate;;
(10) to obtained in step (8) it is organic be added to concentration be 1mol/L dilute sulfuric acid be stripped, be stripped
Liquid;
(11) nickel source is added into strip liquor, cobalt source or manganese source adjust nickel cobalt manganese ratio, make nickel in strip liquor, cobalt,
Manganese element molar ratio is 1:1:1, then adjusts pH=12 with sodium hydroxide and be aged to obtain nickel cobalt manganese hydroxide.
Above-described embodiment is further explanation for the content of present invention using as the explaination to the technology of the present invention content, but
Substantive content of the invention is not limited in described in following embodiments, those skilled in the art can with and should know appoint
What simple change or replacement based on true spirit should belong to protection scope of the presently claimed invention.
Claims (6)
1. recycling the method for valuable metal in a kind of applying waste lithium ionic power battery, it is characterised in that: the following steps are included:
(1) applying waste lithium ionic power battery disassembles decladding after overdischarge, then anode is isolated in the dismantling of resulting battery roll core
Piece;
(2) positive plate is calcined under nitrogen atmosphere, then crushes and cross 80 meshes, obtains the mixed powder of LFP and NCM
Material;
(3) sulfuric acid is sequentially added into mixed powder and hydrogen peroxide is reacted, and product is filtered except must soak after carbon elimination slag
Liquid out;
(4) adjusting the pH value of leachate with ammonium hydroxide is 2-2.5, filters to obtain sediment ferric phosphate and filtrate;
(5) filtrate in step (4) is adjusted pH value with alkali is 5-6, after being filtered to remove a small amount of remaining iron and aluminium, obtains second level filter
Liquid;
(6) will be extracted through step (5) treated second level filtrate with phosphoric acid kind of extractants, be then allowed to stand, isolate it is organic
Phase and water phase;Wherein phosphoric acid kind of extractants is one or more of P204, P507, Cyanex272;
(7) solid sodium carbonate is added to water phase, precipitates to obtain lithium carbonate;
(8) add dilute sulfuric acid to be stripped into organic phase, nickel source, cobalt source or manganese source is added into strip liquor then to adjust nickel
Cobalt manganese ratio, makes nickel, cobalt, manganese element molar ratio 1:1:1 in strip liquor, then plus alkali to adjust its pH value be 11-12;It is last old
Change to obtain nickel cobalt manganese hydroxide.
2. according to the method described in claim 1, it is characterized by: positive plate is calcined under nitrogen atmosphere in the step (2)
Temperature be 400-600 DEG C, calcination time 2-4h.
3. according to the method described in claim 1, it is characterized by: in the step (3) sulfuric acid concentration be 2.5-4mol/L,
The mass volume ratio g:mL of the mixed powder and sulfuric acid is 1:(6-10);The additional amount of the hydrogen peroxide is every gram of mixed powder
Middle addition 2-4mL.
4. according to the method described in claim 1, it is characterized by: the reaction temperature in the step (3) is 60-90 DEG C.
5. according to the method described in claim 1, it is characterized by: the alkali in the step (5) and step (8) is hydroxide
One or more of sodium, potassium hydroxide or ammonium hydroxide.
6. according to the method described in claim 1, it is characterized by: the concentration of the dilute sulfuric acid in the step (8) is 0.1mol/
L-1mol/L。
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