CN113540605B - Harmless treatment method for pyrolysis tail gas of retired old lithium battery - Google Patents

Harmless treatment method for pyrolysis tail gas of retired old lithium battery Download PDF

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CN113540605B
CN113540605B CN202110804377.2A CN202110804377A CN113540605B CN 113540605 B CN113540605 B CN 113540605B CN 202110804377 A CN202110804377 A CN 202110804377A CN 113540605 B CN113540605 B CN 113540605B
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tail gas
pyrolysis
lithium battery
retired
cobalt
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CN113540605A (en
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刘春力
米雪
刘鹏飞
姬海燕
罗旭彪
曾桂生
杨利明
邵鹏辉
石慧
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Nanchang Hangkong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8678—Removing components of undefined structure
    • B01D53/8687—Organic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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

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Abstract

The invention discloses a harmless treatment method for pyrolysis tail gas of retired old lithium batteries, which relates to the field of comprehensive recycling of the old lithium batteries and specifically comprises the following steps: the electrode material of the retired lithium battery is crushed and then placed into a pyrolysis furnace for air pyrolysis, pyrolysis oil is recovered from oil gas discharged by pyrolysis through condensation, tail gas passes through alkali liquor to intercept fluoride in the tail gas, the cobalt/manganese-based catalyst is prepared by utilizing active powder of the retired lithium battery for vulcanization roasting and water leaching, and then the tail gas treated by the alkali liquor enters a fixed bed catalytic oxidation reactor filled with the cobalt/manganese-based catalyst recovered from the retired lithium battery for catalytic degradation treatment. The catalyst prepared by the retired lithium battery is used for treating the organic waste gas generated by the pyrolysis treatment of the catalyst, so that the catalyst is suitable for treating various retired lithium batteries such as lithium cobaltate, lithium manganate and nickel cobalt lithium manganate, and has strong applicability; the organic waste gas harmless treatment process has the advantages of low temperature, simple process, good operation environment, easy control and amplification and the like.

Description

Harmless treatment method for pyrolysis tail gas of retired old lithium battery
Technical Field
The invention relates to the field of comprehensive recycling of waste lithium ion batteries, in particular to a harmless treatment method for pyrolysis tail gas of retired waste lithium batteries.
Background
Lithium ion batteries have become an attractive energy storage technology due to their advantages of high efficiency, high power, high energy density, and the like, and are undergoing expansion development. However, the service life of the lithium ion battery is only 2-3 years, and if a large number of lithium batteries are not properly disposed after being retired, toxic substances contained in the lithium ion batteries can cause serious environmental hazards. Meanwhile, the retired lithium battery contains a large amount of precious strategic metal resources. Therefore, the recycling of the retired lithium battery has double meanings of environmental protection and resource saving.
At present, the recovery methods of the retired lithium battery are various, and in order to reduce the influence of aluminum foil, copper foil, binder and the like in the electrode material on the recovery efficiency and value of competitive metals, most of the recovery processes comprise pyrolysis treatment of the electrode material so as to separate active substances of the electrode material from a current collector in advance. CN108666643A proposes a method and an apparatus for recovering a lithium ion battery positive electrode material, which is disclosed in the patent, wherein the method comprises the steps of crushing a lithium ion battery positive electrode material to be recovered, obtaining material powder, and then sorting the material powder through a sieving machine and a pneumatic shaker to obtain aluminum foil powder adhered with lithium cobaltate impurities. CN 111841232A proposes a method for purifying pyrolysis tail gas of a multi-stage furnace of a waste lithium battery, in the method, the tail gas discharged by the pyrolysis of the waste lithium battery is firstly treated by a cyclone separator, a flue gas cooler, a bag-type dust remover and a first/second/third-stage washing tower in sequence; and then burning the tail gas, sequentially spraying quicklime powder and activated carbon powder in a segmented manner to the discharged tail gas pipeline to remove fluoride, sulfide and dioxin in the tail gas, and finally, dedusting the discharged gas by a bag-type dust collector and then discharging the gas in a pollution-free manner.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a harmless treatment method for pyrolysis tail gas of an obsolete lithium battery.
The technical solution of the invention is as follows:
a method for harmlessly treating the pyrolysis tail gas of an old retired lithium battery comprises the steps of pyrolyzing an electrode material in the retired lithium battery material to obtain a mixture at least containing positive active powder and pyrolysis oil gas, recycling pyrolysis oil through condensation and backflow of the pyrolysis oil gas, treating the tail gas subjected to condensation and backflow through alkali liquor to intercept fluoride in the tail gas, preparing a cobalt/manganese-based catalyst by using the positive active powder, and performing catalytic degradation treatment on the tail gas subjected to alkali liquor treatment through the cobalt/manganese-based catalyst.
Preferably, the electrode material comprises a retired positive electrode material or a mixture of a retired positive electrode material and a retired negative electrode material.
Preferably, the retired positive electrode material comprises any one or a combination of at least two of lithium cobaltate, lithium nickel cobalt manganese oxide, lithium manganese oxide and lithium iron phosphate; the retired cathode material comprises any one or combination of at least two of a graphite cathode, a silicon cathode and a silicon-carbon cathode.
Preferably, the binder contained in the electrode material comprises any one of styrene-butadiene rubber, carboxymethyl cellulose, polyacrylic acid and polyacrylonitrile or a combination of at least two of the styrene-butadiene rubber, the carboxymethyl cellulose, the polyacrylic acid and the polyacrylonitrile.
Preferably, the exhaust temperature of the tail gas after the pyrolysis oil is recovered by condensing and refluxing is lower than 100 ℃.
Preferably, the lye comprises one or more of a potassium hydroxide solution, a sodium hydroxide solution and a calcium hydroxide solution.
Preferably, the specific preparation method of the cobalt/manganese-based catalyst comprises the following steps: mixing the positive active powder and sulfide according to the mass ratio of 0.25-4:1, roasting at 800 ℃ after mixing, carrying out water leaching treatment on a roasted product at normal temperature according to the solid-to-liquid ratio of 20-200g/L, and filtering and separating leached slurry to obtain a solid, wherein the solid is a cobalt/manganese-based catalyst.
Preferably, the sulphide comprises any one of sulphuric acid, sulphate, pyrosulphate or a combination of at least two thereof.
Preferably, the specific process of the catalytic degradation treatment is as follows: and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor with the filling amount of 50-100mg of cobalt/manganese-based catalyst at the flow rate of 50-100 ml/min.
The invention has the beneficial effects that:
according to the harmless treatment method for the pyrolysis tail gas of the obsolete lithium battery, the cobalt/manganese-based catalyst is prepared by using the active powder of the positive electrode in the obsolete lithium battery to treat the organic waste gas generated by the pyrolysis treatment of the cobalt/manganese-based catalyst, so that the method is suitable for treating various obsolete lithium batteries such as lithium cobaltate, lithium manganate and nickel cobalt lithium manganate and has strong applicability; the organic waste gas harmless treatment process has the advantages of low temperature, simple process, good operating environment, easiness in control and amplification and the like, is a brand new method for treating the waste lithium battery pyrolysis tail gas, and has very high removal rate of organic matters in the treated tail gas.
Drawings
FIG. 1 is a flow chart of the harmless treatment method of pyrolysis tail gas of the present invention.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
It should be noted that:
ex-service nickel cobalt lithium manganate battery material (the positive electrode is nickel cobalt lithium manganate, the negative electrode is graphite, and the binder is styrene butadiene rubber);
a material of a retired lithium manganate battery (a positive electrode: lithium manganate, a negative electrode: graphite, a binder: carboxymethyl cellulose);
the material of the retired cobalt acid lithium battery (the positive electrode: lithium cobaltate, the negative electrode: silicon carbon, and the binder: polyacrylonitrile).
The following examples can be referred to in fig. 1.
Example 1
Performing air pyrolysis on the decommissioned nickel cobalt lithium manganate battery material obtained by discharging and disassembling, mixing the positive active powder in the pyrolysis material with potassium pyrosulfate according to the mixing mass ratio of 1:2, roasting at 700 ℃, leaching the roasted product with pure water at normal temperature according to the solid-to-liquid ratio of 50g/L, and filtering to obtain a solid cobalt/manganese-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a calcium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 60mg of cobalt/manganese-based catalyst at a rate of 50ml/min for catalytic degradation treatment at a temperature of 200 ℃.
Example 2
Performing air pyrolysis on the retired lithium manganate battery material obtained by discharging and disassembling, uniformly mixing the positive active powder in the pyrolysis material with sulfuric acid according to the mixing mass ratio of 4:1, roasting at 750 ℃, leaching the roasted product with pure water at normal temperature according to the solid-liquid ratio of 100g/L, and filtering to obtain a solid manganese-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a sodium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 80mg of cobalt/manganese-based catalyst at a rate of 70ml/min for catalytic degradation treatment at a temperature of 250 ℃.
Example 3
Carrying out air pyrolysis on the retired cobalt acid lithium battery material obtained by discharging and disassembling, mixing the positive active powder and sodium pyrosulfate in the pyrolysis material according to the mixing mass ratio of 1:3, roasting at 600 ℃, leaching the roasted product with pure water at normal temperature according to the solid-liquid ratio of 50g/L, and filtering to obtain a solid cobalt-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a calcium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 90mg of cobalt-based catalyst at a rate of 80ml/min, and performing catalytic degradation treatment at 150 ℃.
Example 4
Performing air pyrolysis on the mixed material of the retired nickel cobalt lithium manganate and the cobalt acid lithium battery obtained by discharging and disassembling, mixing the positive active powder and potassium pyrosulfate in the pyrolysis material according to the mixing mass ratio of 1:2, roasting at 800 ℃, performing water leaching treatment on a roasted product at normal temperature according to the solid-to-liquid ratio of 150g/L, and filtering to obtain a solid cobalt/manganese-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a calcium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 100mg of cobalt/manganese-based catalyst at a rate of 100ml/min for catalytic degradation treatment at the temperature of 300 ℃.
Example 5
Performing air pyrolysis on the retired nickel cobalt lithium manganate battery obtained by discharging and disassembling and a lithium manganate mixed material, mixing positive active powder and potassium pyrosulfate in the pyrolysis material according to the mixing mass ratio of 1:2, roasting at 500 ℃, performing water leaching treatment on a roasted product at normal temperature according to the solid-to-liquid ratio of 20g/L, and filtering to obtain a solid cobalt/manganese-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a calcium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 100mg of cobalt/manganese-based catalyst at a rate of 100ml/min for catalytic degradation treatment at the temperature of 300 ℃.
Example 6
Performing air pyrolysis on the ex-service lithium manganate and lithium cobaltate battery mixed material obtained by discharging and disassembling, mixing the positive active powder and potassium pyrosulfate in the pyrolysis material according to the mixing mass ratio of 1:4, roasting at 700 ℃, performing water leaching treatment on a roasted product at normal temperature according to the solid-to-liquid ratio of 200g/L, and filtering to obtain a solid cobalt/manganese-based catalyst; tail gas discharged by pyrolysis is condensed to recover pyrolysis oil, and fluoride in the tail gas is intercepted through a calcium hydroxide solution; and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor filled with 90mg of cobalt/manganese-based catalyst at a rate of 90ml/min for catalytic degradation treatment at a temperature of 80 ℃.
Comparative example 1
Tail gas discharged by pyrolysis of a decommissioned lithium cobaltate battery material is treated by sequentially passing through a cyclone separator, a flue gas cooler, a bag-type dust collector and a primary/secondary/tertiary washing tower; and then burning the tail gas, sequentially spraying quicklime powder and activated carbon powder in a segmented manner into a discharged tail gas pipeline, and finally discharging the discharged gas after dedusting by a bag-type dust collector.
The tail gas treated by the above examples and comparative examples was analyzed by GC-MS. Calculating the organic matter removal rate, wherein the calculation method comprises the following steps: (organic matter content before catalytic treatment-organic matter content after catalytic treatment)/organic matter content before treatment, and whether fluoride is detected, are shown in the following table.
TABLE 1 Performance test values of examples and comparative examples
Test specimen Removal ratio of hydrocarbon organic matters (%) Fluoride (Yes or No)
Example 1 98.2 Whether or not
Example 2 97.3 Whether or not
Example 3 98.4 Whether or not
Example 4 96.7 Whether or not
Example 5 99.0 Whether or not
Example 6 96.6 Whether or not
Comparative example 1 81.4 Is provided with
As can be seen from the above table, the embodiment of the invention has the advantages of simple process, mild conditions, good operating environment and easy control compared with the comparative example, is a brand-new method for treating the pyrolysis tail gas of the waste lithium battery, is suitable for treating various retired lithium batteries such as lithium cobaltate, lithium manganate, nickel cobalt lithium manganate and the like, and has strong applicability; and the removal rate of organic matters in the treated tail gas is very high, and no fluoride is discharged. The method in the comparative example has complex treatment flow and difficult practical application, organic waste gas needs to be incinerated, the treatment cost is high, the comparative example adopts spraying alkali liquor, and tail gas is directly introduced into the alkali liquor in the embodiment of the invention, so that the reaction is more complete, and the fluoride removal effect is more excellent.
The embodiments described above are some, not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (9)

1. A method for harmlessly treating the pyrolysis tail gas of an old retired lithium battery is characterized in that an electrode material in the retired lithium battery material is pyrolyzed to obtain a mixture at least containing positive active powder and pyrolysis oil gas, the pyrolysis oil gas is condensed and refluxed to recover pyrolysis oil, the tail gas after condensation and reflux is treated by alkali liquor to intercept fluoride in the tail gas, the cobalt/manganese-based catalyst is prepared by using the positive active powder, and the tail gas after alkali liquor treatment is subjected to catalytic degradation treatment by the cobalt/manganese-based catalyst.
2. The method for harmlessly treating the pyrolysis tail gas of the ex-service used lithium battery as claimed in claim 1, wherein the electrode material comprises an ex-service positive electrode material or a mixture of an ex-service positive electrode material and an ex-service negative electrode material.
3. The method for harmlessly treating the pyrolysis tail gas of the obsolete lithium battery as claimed in claim 2, wherein the obsolete positive electrode material comprises any one or a combination of at least two of lithium cobaltate, lithium nickel cobalt manganese oxide, lithium manganese oxide and lithium iron phosphate; the ex-service cathode material comprises any one of a graphite cathode, a silicon cathode and a silicon-carbon cathode or the combination of at least two of the graphite cathode, the silicon cathode and the silicon-carbon cathode.
4. The method for harmlessly treating the pyrolysis tail gas of the retired old lithium battery as claimed in claim 1, wherein the binder contained in the electrode material comprises any one or a combination of at least two of styrene-butadiene rubber, carboxymethyl cellulose, polyacrylic acid and polyacrylonitrile.
5. The method for harmlessly treating the pyrolysis tail gas of the retired old lithium battery as claimed in claim 1, wherein the exhaust temperature of the tail gas after the pyrolysis oil is recovered by condensing and refluxing is lower than 100 ℃.
6. The method for harmlessly treating the pyrolysis tail gas of the retired old lithium battery as claimed in claim 1, wherein the alkali solution comprises one or more of a potassium hydroxide solution, a sodium hydroxide solution and a calcium hydroxide solution.
7. The method for harmlessly treating the pyrolysis tail gas of the retired old lithium battery as claimed in claim 1, wherein the cobalt/manganese-based catalyst is prepared by the following specific steps: mixing the positive active powder and sulfide according to the mass ratio of 0.25-4:1, roasting at 800 ℃ after mixing, carrying out water leaching treatment on a roasted product at normal temperature according to the solid-to-liquid ratio of 20-200g/L, and filtering and separating leached slurry to obtain a solid, wherein the solid is a cobalt/manganese-based catalyst.
8. The method as claimed in claim 7, wherein the sulfide includes any one or a combination of at least two of sulfuric acid, sulfate and pyrosulfate.
9. The method for harmlessly treating the pyrolysis tail gas of the retired old lithium battery according to claim 1, wherein the catalytic degradation treatment comprises the following specific processes: and introducing the tail gas treated by the alkali liquor into a fixed bed catalytic oxidation reactor with the filling amount of 50-100mg of cobalt/manganese-based catalyst at the flow rate of 50-100 ml/min.
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CN114024051A (en) * 2021-10-28 2022-02-08 中国科学院广州能源研究所 Method for treating electrolyte of waste lithium battery through pyrolysis
CN114534435B (en) * 2022-04-25 2022-07-19 广州天赐高新材料股份有限公司 Method and device for treating tail gas recovered from waste lithium ion batteries and recovering batteries
CN114832845B (en) * 2022-05-23 2024-05-10 濮阳天地人环保科技股份有限公司 Composite catalyst prepared by utilizing recycled lithium battery material and preparation method thereof

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