CN112827337A - Fluorine removal device, waste lithium battery treatment system, treatment method and application thereof - Google Patents
Fluorine removal device, waste lithium battery treatment system, treatment method and application thereof Download PDFInfo
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- CN112827337A CN112827337A CN202110019144.1A CN202110019144A CN112827337A CN 112827337 A CN112827337 A CN 112827337A CN 202110019144 A CN202110019144 A CN 202110019144A CN 112827337 A CN112827337 A CN 112827337A
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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
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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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
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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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
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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
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/804—UV light
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
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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 invention discloses a fluorine removal device, a waste lithium battery treatment system, a treatment method and application thereof. The fluorine removal device is a hollow cylindrical body, the upper end of the hollow cylindrical body is provided with a fluorine-containing liquid inlet, the lower end of the hollow cylindrical body is provided with a slag hole and a liquid outlet, at least one layer of partition plate is arranged in a cavity of the hollow cylindrical body, a fluorine adsorbent is arranged on the partition plate, and a fluorine adsorbent replacing hole is arranged at the position of the partition plate on the side wall of the hollow cylindrical body. The fluorine removal device provided by the invention can realize effective removal of fluorine, is simple and convenient to operate, can directly replace the fluorine adsorbent, saves cost on the premise of ensuring higher fluorine removal efficiency, can fully volatilize and effectively collect electrolyte and solvent in the electrolyte by using the waste lithium battery treatment system and method, avoids leakage, and has the total collection rate of the electrolyte of more than 99 percent and the total treatment rate of more than 98 percent.
Description
Technical Field
The invention relates to the field of solid waste treatment, in particular to a fluorine removal device, a waste lithium battery treatment system containing the fluorine removal device, a treatment method and application thereof.
Background
In recent years, the scrapped lithium ion batteries comprise scrapped consumer (3C) batteries and scrapped power lithium batteries of new energy automobiles, and particularly, the scrapped power lithium batteries are high in growth speed and large in scrapped amount. The harm factors of the lithium ion battery to the environment mainly comprise heavy metals and electrolyte. Wherein, the heavy metal is valuable metal, exists in the solid electrode sheet material and is easy to recover.
The electrolyte special for the lithium ion battery mainly comprises three parts, namely lithium salt, a solvent and an additive. Wherein, the lithium salt accounts for 7 to 17 percent of the weight of the electrolyte, the solvent accounts for 75 to 90 percent of the weight of the electrolyte, and the additive accounts for 0.5 to 10 percent of the weight of the electrolyte. The solvent is a carbonate mixed solution comprising chain carbonate and cyclic carbonate, a small part of functional electrolyte may also contain carboxylate, and the ester solution is generally a combustible liquid with a low boiling point and has low toxicity. The lithium salt that is mainly used at present is lithium hexafluorophosphate (LiPF6), which is the most difficult part of the spent electrolyte. Lithium hexafluorophosphate itself is unstable and is easily decomposed at an excessively high temperature or when it meets water. Lithium hexafluorophosphate is decomposed to easily generate hydrofluoric acid (HF), which is toxic and highly corrosive, resulting in the risk of leakage of the waste electrolyte during long-term storage. It also causes serious harm to the environment if it is directly discharged.
At present, the recovery process of the waste lithium ion battery mainly comprises mechanical coarse crushing, cracking and fine crushing and sorting. In the crushing process, the electrolyte can leak and volatilize into the air, and if the electrolyte is not effectively collected and treated, the electrolyte can cause serious pollution to the environment.
The technical reports about the treatment process of the discarded lithium battery electrolyte are less, and the collection and treatment effects of the waste are not ideal. The main treatment method comprises the steps of collecting volatilized electrolyte under negative pressure in the treatment process, spraying and adsorbing fluorine-containing components by alkali liquor, degrading organic components by photocatalysis, and finally discharging. However, in the treatment process, the electrolyte can be brought into each link in the treatment process, the sealing performance of the joint of each link of the equipment is difficult to ensure, and the problems of leakage and disorganized diffusion are easy to occur. Moreover, the fluorine content in the wastewater sprayed by the alkali liquor is high, and the wastewater needs to be replaced frequently in the follow-up process, so that the generated wastewater has high content and the fluorine is not completely adsorbed.
CN111498878A discloses a resource utilization method of waste lithium hexafluorophosphate. The method comprises the following steps of disassembling a battery, adding an alkali solution, dissolving a solvent in an electrolyte into water, adding dimethylbenzene, performing 3-4-stage countercurrent extraction to obtain an organic phase and a water phase, distilling the organic phase to obtain DME, introducing carbon dioxide into the residual solution, adjusting the pH value to convert meta-aluminate into aluminum hydroxide precipitate, adding sulfuric acid into a filtrate to adjust the pH value of the solution, and adding ferrous sulfate and hydrogen peroxide to obtain iron phosphate filter residue and fluorine-containing filtrate; and adding sulfuric acid into filter residues for dissolving, then mixing a lithium-fluorine-containing solution with a fluoride ion solution, then adding magnesium sulfate, reacting to obtain magnesium fluoride precipitate, raising the pH value of the residual lithium solution to be alkaline, and adding sodium carbonate to obtain crude lithium carbonate. The invention can realize the comprehensive recovery of fluorine, phosphorus and lithium in the lithium hexafluorophosphate and can realize the recycling of DME organic solvent.
CN110783658A discloses a retired power ternary lithium battery recycling demonstration process method. The technical scheme includes that the retired lithium ion battery is discharged, physical dismantling is carried out in a sealed inert atmosphere container after drying, the dismantled lithium battery is transferred to a negative pressure reaction kettle, electrolyte volatilizes through heating, an external condensing device recovers an organic solvent with a low boiling point, the volatilized battery waste is transferred to a cleaning kettle, the battery waste is cleaned by water, waste gas generated is sprayed through alkali liquor and is discharged after being adsorbed by activated carbon, then mixed liquid in the kettle is settled and separated, sewage is treated and discharged, battery residues are dried and then are crushed and sorted, and aluminum plastic films, steel shells, diaphragms, copper powder, aluminum powder and electrode materials are recycled in a classified mode. And acid leaching and impurity removal are carried out on the electrode material, and a coprecipitation method is carried out to obtain the nickel cobalt lithium manganate precursor.
CN111816947A discloses a harmless removal process, a removal device and a use method of waste lithium battery electrolyte. The technical scheme includes that the device comprises a shredder, a feeding device is connected to a feeding port of the shredder, a vacuum heating/hydrolysis liquid removing device is installed at an outlet of the shredder, a gas filter is connected to the top end of the shredder, the vacuum heating/hydrolysis liquid removing device is connected to the gas filter, an outlet end of the gas filter is connected with a gas condenser, the gas condenser is connected with an alkali liquor spraying device, a vacuum pump is installed on a pipeline between the gas condenser and the alkali liquor spraying device, and an air outlet port of the alkali liquor spraying device is connected with an active carbon adsorption device; a spray liquid condenser is arranged on the alkali liquor spray device; liquefying and removing lithium hexafluorophosphate, organic carbonate electrolyte and decomposed harmful gas in the large pole piece obtained by shredding by a gas condenser, cleaning and absorbing by alkali liquor, and purifying the discharged air; and the waste gas release in the waste lithium battery recovery process is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a fluorine removal device, a waste lithium battery treatment system containing the fluorine removal device, a treatment method and application thereof, solves the problems of low collection rate and treatment efficiency of electrolyte waste gas generated in the process of crushing and recycling waste lithium batteries, and can effectively remove fluorine contained in the waste lithium batteries.
The invention provides a fluorine removal device, which is a hollow cylindrical body, wherein the upper end of the hollow cylindrical body is provided with a fluorine-containing liquid inlet, the lower end of the hollow cylindrical body is provided with a slag hole and a liquid outlet, at least one layer of partition plate is arranged in a cavity of the hollow cylindrical body, a fluorine adsorbent is arranged on the partition plate, and a fluorine adsorbent replacing hole is arranged at the position of the partition plate on the side wall of the hollow cylindrical body.
In the fluorine removal device provided by the invention, fluorine in the fluorine-containing liquid sent from the fluorine-containing liquid inlet is absorbed by the fluorine adsorbent on the partition plate, so that the fluorine in the fluorine-containing liquid can be removed in a form of precipitation, and the fluorine adsorbent on the partition plate can be directly replaced through the fluorine adsorbent replacement port, so that the operation is simple and convenient, and the fluorine removal efficiency is high.
According to some embodiments of the fluorine removal device of the present invention, the fluorine adsorbent is selected from at least one of a calcium-containing compound, a magnesium-containing compound, and a barium-containing compound. Preferably, the fluorine adsorbent is selected from at least one of calcium-containing basic oxide or hydroxide, magnesium-containing basic oxide or hydroxide, barium-containing basic oxide or hydroxide.
According to a specific embodiment of the fluorine removal device of the present invention, the fluorine adsorbent is at least one selected from the group consisting of calcium oxide, calcium hydroxide and calcium carbonate.
According to some embodiments of the fluorine removal device of the present invention, the fluorine adsorbent has a particle size of 1 to 10 mm.
In different embodiments of the invention, the fluorine adsorbent is contained in the alkali-resistant cloth bag, so that the fluorine adsorbent can be effectively prevented from being mixed into liquid after being pulverized, and the fluorine adsorbent is convenient to replace. Preferably, the alkali-resistant cloth bag is made of terylene, polypropylene and the like.
According to some embodiments of the fluorine removal device of the present invention, the separator is provided with 1 to 3 layers. Preferably, in the fluorine removal device of the present invention, the partition plate is provided with two layers. In different embodiments of the invention, different layers of partition boards can be selected and arranged according to different working condition requirements, and each layer of partition board is provided with the fluorine adsorbent.
According to some embodiments of the fluorine removal device of the present invention, a sprayer is provided at the fluorine-containing liquid inlet for spraying the fluorine-containing liquid into the fluorine removal device.
The invention provides a waste lithium battery treatment system in a second aspect, which comprises a heating unit, a spraying adsorption unit and a catalytic degradation unit;
the heating unit comprises a hot air heating device, a conveying device and a negative pressure collecting device, the hot air heating device is used for heating the waste lithium battery crushed materials on the conveying device in a hot air mode, the negative pressure collecting device is used for sealing the conveying device in a negative pressure mode, the negative pressure collecting device is provided with a waste gas inlet and a waste gas outlet, and the waste gas inlet is located above the conveying device and used for collecting waste gas generated after the waste lithium battery crushed materials are heated in the hot air mode;
the spraying and adsorbing unit comprises a spraying device, a circulating pump and the defluorination device, wherein the spraying device is provided with an air inlet, a spraying liquid spraying device and a fluorine-containing liquid outlet, the air inlet is connected with a waste gas outlet of the negative pressure collecting device, and the fluorine-containing liquid outlet is connected with a fluorine-containing liquid inlet of the defluorination device through the circulating pump;
the catalytic degradation unit comprises a photocatalytic degradation device, the photocatalytic degradation device is provided with a waste gas inlet after defluorination and a waste gas outlet after degradation, and the waste gas inlet after defluorination is connected with a liquid outlet of the defluorination device.
Among the broken material of useless lithium cell, the electrolyte that partial boiling point is higher and mix with between positive and negative pole piece and diaphragm is more intractable, carry out high temperature heating to it through hot-blast heating device and make it fully volatilize, and make the gas that volatilizees the production get into the negative pressure collection device and realize effective collection under the negative pressure sealing strip spare, prevent to reveal, then send into the waste gas that volatilizees the production and spray it with alkali lye in the spray set, alkali lye and waste gas fully contact, realize the absorption of fluorinion in the waste gas, make the waste gas in contain the absorption of fluorinion, make the waste gasSome HF and PF6When all fluorine-containing gas enters the alkali liquor, the fluorine-containing gas reacts with the alkali liquor to form fluorine-containing ions (F)-) And the solution is used for realizing the precipitation adsorption and desorption of fluorine in the fluorine-containing device, and the generated waste gas after fluorine removal is further purified by the photocatalytic degradation device.
According to some embodiments of the waste lithium battery treatment system of the present invention, the gas inlet of the spraying device and the liquid outlet of the fluorine removal device are connected via the circulation pump. Through this embodiment for realize the circulation via the circulating pump between fluorine removal device and the spray set, fluorine-containing liquid gets into fluorine removal device by spray set and carries out the desorption of fluorine, and the low fluorine liquid that produces after fluorine removal device removes fluorine returns to spray set again and carries out further contact absorption to fluorine, realizes circulation continuous operation.
According to some embodiments of the waste lithium battery treatment system of the present invention, the system further comprises a crushing unit comprising a crushing device having a feed inlet through which the waste lithium battery raw material is fed into the crushing device and through which the waste lithium battery raw material is fed onto the conveyor. The crushing device can crush waste lithium battery raw materials, so that the electrolyte in the waste lithium battery raw materials is partially released.
According to some embodiments of the waste lithium battery treatment system, the system further comprises a dust removal unit, the dust removal unit comprises a dust removal device and a fan, the dust removal device is provided with a dust-containing waste gas inlet and a dust-removing waste gas outlet, the dust-containing waste gas inlet is connected with the waste gas outlet of the negative pressure collection device, and the dust-removing waste gas outlet is connected with the air inlet of the spray device through the fan. The dust removal device can intercept and collect dust particles generated in the crushing process, and the dust removal device is preferably a pulse cloth bag.
According to some embodiments of the waste lithium battery treatment system of the present invention, the system further comprises an activated carbon adsorption unit comprising an activated carbon adsorption device having a degraded exhaust gas inlet connected to a degraded exhaust gas outlet of the photocatalytic degradation device. The activated carbon adsorption device can further treat the degraded waste gas generated after photocatalytic degradation, so that trace organic waste gas which is not degraded and is contained in the degraded waste gas can be adsorbed and removed in the activated carbon adsorption device, and the waste gas is ensured to be discharged up to the standard.
A third aspect of the present invention provides a method for treating a waste lithium battery according to the above waste lithium battery treating system, the method comprising the steps of:
step A: starting the hot air heating device to heat the waste lithium battery crushed materials on the conveying device by hot air to generate waste gas, wherein the waste gas is collected in the negative pressure collecting device through the waste gas inlet;
and B: the waste gas is sent into the spraying device through a waste gas outlet of the negative pressure collecting device, the spraying liquid released by the spraying liquid spraying device adsorbs the waste gas, and the obtained fluorine-containing liquid is sent into the defluorination device through the fluorine-containing liquid inlet through the circulating pump for defluorination treatment to obtain fluorine-containing precipitate and defluorinated waste gas;
and C: and the defluorinated waste gas is sent into the photocatalytic degradation device through the defluorinated waste gas inlet to be subjected to photocatalytic degradation treatment, so that the degraded waste gas is obtained.
According to some embodiments of the treatment method of the present invention, in step a, the particle size of the waste crushed material of the lithium battery is 2-5cm, and too large or too small particle size is likely to cause incomplete volatilization of the electrolyte, resulting in a reduction in waste gas collection rate. In different embodiments of the invention, the crushing device is used for crushing waste lithium battery raw materials to obtain a waste lithium battery crushed material.
According to some embodiments of the treatment method of the present invention, the conditions of the hot air heating include: the heating temperature is 80-120 deg.C, and the heating time is 3-8 min. Under the hot air heating condition, part of electrolyte with higher boiling point and electrolyte mixed between the positive and negative pole pieces and the diaphragm in the waste lithium battery crushing material can be fully volatilized and released. The higher the heating temperature in the hot air heating process, the better, but the higher the temperature, the higher the energy consumption is increased, the dangerous operation process of the device is, and the electrolyte can be caused to fire. The longer the heating retention time is, the better, the waste gas in the electrolyte can be completely volatilized after the heating retention time is generally about 5 minutes.
According to some embodiments of the process according to the invention, the negative pressure in the negative pressure collecting device is 20-100 Pa. Under the condition, the volatile waste gas can be fully collected, so that the treatment efficiency is improved, wherein the collection rate can reach more than 99%, and the total treatment efficiency reaches more than 98%. In different embodiments of the present invention, the negative pressure seal of the negative pressure collecting device is specifically realized by: except the pan feeding mouth to breaker, all adopt sealed butt joint to discharge gate etc. and the pan feeding mouth installs plastics additional and hangs down the curtain, and conveyer, sorting facilities etc. of the broken material of useless lithium cell are all installed additional sealed protection casing, prevent that waste gas from leaking, install negative pressure collection pipeline additional to parts such as breaker, sorting facilities, further prevent inside gas outward diffusion.
According to some embodiments of the treatment method of the present invention, in the step B, the spray solution is a sodium hydroxide solution with a mass concentration of 2% to 10%.
According to the specific embodiment of the treatment method of the present invention, in the step B, the fluorine adsorbent provided in the fluorine removal device during the fluorine removal treatment is preferably CaO, Ca (OH)2And CaCO3The particle size of at least one of the particles is preferably 1-10mm, the fluorine adsorbent is contained in an alkali-resistant cloth bag and then placed on a partition board, the partition board is provided with an upper layer and a lower layer, and the alkali-resistant cloth bag is respectively tiled on the partition board. The fluorine-containing liquid is sprayed by a sprayer at the top end of the fluorine removal device and then sequentially contacts with the fluorine adsorbent on the partition plate, and calcium fluoride precipitate is formed by reaction, so that the fluorine is removed. The specific reaction process is as follows:
2F-+Ca2+＝＝CaF2↓；Ca(OH)2+2HF＝＝CaF2↓+2H2O
when the fluorine is adsorbed for a certain time, the effect of fluorine precipitation adsorption is poor or the circulation pump is out of work, the circulation pump is closed, the fluorine adsorbent replacing port is opened, and the fluorine adsorbent is replaced. The lost tap water and the sodium hydroxide solution are replenished in the spraying device, and the continuous use is realized.
According to some embodiments of the treatment method of the present invention, step B further comprises: and sending the waste gas after defluorination into the spraying device through the air inlet of the spraying device by the circulating pump.
In the invention, when the circulating pump conveys the fluorine-containing liquid into the fluorine removal device, the adsorption and precipitation speed cannot be reached due to too small flow, the accumulation of fluorine is caused, the energy consumption is increased due to too large flow, and the precipitation effect is not greatly influenced.
According to some embodiments of the treatment method of the present invention, the photocatalytic degradation treatment in step C is preferably ultraviolet photocatalytic degradation, and carbon dioxide and water are generated after the degradation, and the specific process is as follows:
according to some embodiments of the treatment method of the present invention, before step a, the method further comprises: and crushing the waste lithium battery raw material to obtain the waste lithium battery crushed material.
According to some embodiments of the treatment method of the present invention, before step B, the method further comprises: and the waste gas is sent into the dust removal device through a waste gas outlet of the negative pressure collection device, and is sent into the spraying device through a fan after dust removal treatment.
According to some embodiments of the treatment method of the present invention, after step C, the method further comprises: and sending the degraded waste gas into an activated carbon adsorption device for adsorption and purification.
The invention provides the application of the fluorine removal device, the waste lithium battery treatment system or the waste lithium battery treatment method in waste lithium battery treatment.
The invention has the beneficial effects that:
the fluorine removal device provided by the invention can realize effective removal of fluorine, is simple and convenient to operate, can directly replace the fluorine adsorbent, and saves the cost on the premise of ensuring higher fluorine removal efficiency.
According to the waste lithium battery treatment system and the waste lithium battery treatment method, the hot air heating and the negative pressure sealing collection are adopted, so that the electrolyte and the solvent in the electrolyte can be fully volatilized and effectively collected, the leakage is avoided, and the treatment efficiency is further improved, wherein the total collection rate of the electrolyte is more than 99%, and the total treatment rate is more than 98%.
In the waste lithium battery treatment system, the circulating pump is arranged between the spraying device and the defluorination device to realize the circulating spraying and defluorination treatment of the materials, and the low-fluorine alkaline solution generated after the defluorination treatment of the fluorine-containing liquid is carried out by the defluorination device is returned to the spraying device to be subjected to circulating treatment, so that the continuous recycling of the sprayed and adsorbed alkaline solution is realized, the fluorine-containing wastewater is not generated, and the environment is more friendly.
Drawings
Fig. 1 is a schematic structural diagram of a fluorine removal device provided in embodiment 1 of the present invention.
Fig. 2 is a schematic structural diagram of a waste lithium battery treatment system according to embodiment 1 of the present invention.
Fig. 3 is a schematic flow chart of a method for treating a waste lithium battery according to an embodiment of the present invention.
Description of reference numerals:
100. a feeding and conveying device;
200. a crushing device;
310. a hot air heating device 320, a conveying device 330 and a negative pressure collecting device;
410. a residue crushing device 420, a residue conveying device;
510. a dust removing device 520 and a fan;
610. the device comprises a spraying device, a 620, a circulating pump, a 630, a fluorine removal device, 631, a fluorine-containing liquid inlet, 632, a slag outlet, 633, a liquid outlet, 634, a fluorine adsorbent replacing port, 635 and a partition plate;
710. a drying device 720, a photocatalytic degradation device 730 and a draught fan;
800. and an exhaust gas discharge device.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given by way of example only, and is not intended to limit the scope of the invention.
The test method of the invention is as follows:
(1) the method for testing the waste gas collection rate comprises the following steps: with a volatile composition in the useless lithium cell electrolyte as the test index, when stable continuous production, collect the concentration and the amount of wind of being responsible for carrying out the sample test target composition to waste gas, calculate the collection volume of target composition, to limiting the space sample test target composition concentration around the equipment simultaneously, calculate the volume of revealing in this period of time. The collection rate is collection amount/(collection amount + leakage amount) × 100%.
(2) The method for testing the fluorine removal rate comprises the following steps: the total concentration of the collected waste gas is sampled and tested before entering the fluorine removal device, the concentration after treatment is sampled and tested at the liquid outlet after passing through the fluorine removal device, the removal rate is 100 percent of the concentration of the fluorine after treatment/the total concentration of the fluorine before treatment, and multiple sampling and averaging are needed.
(3) The method for testing the degradation rate of the organic solvent comprises the following steps: the total concentration of the collected waste gas is sampled and tested before ultraviolet light catalytic degradation, after the waste gas is subjected to ultraviolet light catalytic degradation, the concentration after treatment is sampled and tested at an outlet, the degradation rate is the concentration after degradation/the concentration before degradation is 100%, and multiple sampling is needed for averaging.
[ example 1 ]
As shown in fig. 1, the fluorine removal device provided in this embodiment is a hollow cylindrical body. The upper end of the fluorine removal device is provided with a fluorine-containing liquid inlet 631, and the fluorine-containing liquid inlet 631 is provided with a sprayer. The lower end is provided with a slag outlet 632 and a liquid outlet 633. Two layers of partition plates 635 are arranged in the cavity of the hollow cylindrical body and used for placing fluorine adsorbents, and the fluorine adsorbents are contained in alkali-resistant cloth bags. Also, a fluorine adsorbent replacing port 634 is provided on the side wall at the position of the partition 635.
As shown in fig. 2, the present embodiment further provides a waste lithium battery treatment system, which includes a feeding conveyer 100, a crushing device 200, a heating unit, a spraying adsorption unit, a residue treatment unit, and a catalytic degradation unit.
Wherein, material loading conveyer 100 is connected with breaker 200, and useless lithium cell raw materials send into breaker 200 via material loading conveyer 100 and carry out the breakage, obtains the broken material of useless lithium cell.
The heating unit includes a hot wind heating device 310, a transfer device 320, and a negative pressure collecting device 330. The crushing device 200 is connected with the conveying device 320, the hot air heating device 310 is used for heating the crushed waste lithium battery materials on the conveying device 320 in a hot air mode, and the negative pressure collecting device 330 is used for sealing the conveying device 320 in a negative pressure mode. The negative pressure collecting device 330 has a waste gas inlet and a waste gas outlet, and the waste gas inlet is located above the conveying device 320 and is used for collecting waste gas generated after the waste lithium battery crushed material is heated by hot air.
The waste lithium battery residue on the conveyor 320 is sent to a subsequent sorting device (not shown) through the residue crushing device 410 and the residue conveyor 420 in sequence.
The exhaust gas enters the dust removing device 510 through the negative pressure collecting device 330 for dust removing treatment, and then is sent to the spraying device 610 through the fan 520.
The spray adsorption unit includes a spray device 610, a circulation pump 620, and a fluorine removal device 630. The air inlet of the spraying device 610 is communicated with the fan 520, and the fluorine-containing liquid outlet of the spraying device 610 is connected with the fluorine-containing liquid inlet 631 of the fluorine removal device 630 through the circulating pump 620. The gas inlet of the spraying device 610 is also connected with the liquid outlet 633 of the fluorine removing device 630 via the circulating pump 620.
The catalytic degradation unit comprises a drying device 710, a photocatalytic degradation device 720 and a draught fan 730, wherein the drying device 710 is connected with a liquid outlet 633 of the fluorine removal device 630, and then the liquid is sent into the photocatalytic degradation device 720 for photocatalytic degradation. The degraded exhaust gas generated after the photocatalytic degradation is sent to an activated carbon adsorption device (not shown in the figure) through a draught fan 730 for further purification, and finally is discharged by the exhaust gas discharge device 800 after reaching the standard.
[ example 2 ]
As shown in fig. 3, a schematic flow chart of a waste lithium battery treatment method provided in this embodiment is based on the fluorine removal device and system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 3cm, and the micro negative pressure in the crushing process is controlled to be 55 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 95 ℃, the heating retention time is 5min, and the micro negative pressure of the negative pressure collecting device is controlled to be 40 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 3 times of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 6m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, wherein the fluorine adsorbent is Ca (OH)2Particle, the number of layers is 2. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 99%, the removal rate of fluorine in the electrolyte is more than or equal to 99%, and the degradation rate of the organic solvent is more than or equal to 99.5%.
[ example 3 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 3cm, and the micro negative pressure in the crushing process is controlled to be 50 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 85 ℃, the heating retention time is 3min, and the micro negative pressure of the negative pressure collecting device is controlled to be 30 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 8%. The flow of the circulating pump is 3 times of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 6m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, wherein the fluorine adsorbent is Ca (OH)2Particle, the number of layers is 2. After defluorination, part of waste gas is circularly sent into a spraying device for spraying, part of waste gas is subjected to photocatalytic degradation treatment, and the degraded waste gas is then activatedAnd (4) performing adsorption treatment on the charcoal, and discharging the final waste gas up to the standard.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 90%, the removal rate of fluorine in the electrolyte is more than or equal to 99%, and the degradation rate of the organic solvent is more than or equal to 99.5%.
[ example 4 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 3cm, and the micro negative pressure in the crushing process is controlled to be 55 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 95 ℃, the heating retention time is 5min, and the micro negative pressure of the negative pressure collecting device is controlled to be 40 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 1 time of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 2m3H is used as the reference value. And (3) delivering fluorine-containing liquid generated after the waste gas is sprayed into a fluorine-containing device for fluorine adsorption and precipitation treatment, wherein the fluorine adsorbent is CaO particles, and the number of layers is 2. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 99%, the removal rate of fluorine in the electrolyte is more than or equal to 91%, and the degradation rate of the organic solvent is more than or equal to 98%.
[ example 5 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 3cm, and the micro negative pressure in the crushing process is controlled to be 55 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 95 ℃, the heating retention time is 5min, and the micro negative pressure of the negative pressure collecting device is controlled to be 40 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 3 times of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3Circulation pumpThe flow rate is 6m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, and the fluorine adsorbent is CaCO3Particle, the number of layers is 2. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 99%, the removal rate of fluorine in the electrolyte is more than or equal to 82%, and the degradation rate of the organic solvent is more than or equal to 98%.
[ example 6 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 3cm, and the micro negative pressure in the crushing process is controlled to be 15 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 95 ℃, the heating retention time is 5min, and the micro negative pressure of the negative pressure collecting device is controlled to be 10 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 3 times of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 6m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, wherein the fluorine adsorbent is Ca (OH)2Particle, the number of layers is 2. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 75%, the removal rate of fluorine in the electrolyte is more than or equal to 95%, and the degradation rate of the organic solvent is more than or equal to 91%.
[ example 7 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 10cm, and the micro negative pressure in the crushing process is controlled to be 55 Pa. To waste lithium batteryAnd heating the crushed aggregates by hot air to generate waste gas, wherein the heating temperature is 95 ℃, the heating retention time is 5min, and the micro negative pressure of the negative pressure collecting device is controlled to be 40 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 3 times of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 6m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, wherein the fluorine adsorbent is Ca (OH)2Particle, the number of layers is 2. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of the electrolyte waste gas in the waste lithium battery is more than or equal to 98%, the removal rate of fluorine in the electrolyte is more than or equal to 99%, and the degradation rate of the organic solvent is more than or equal to 99.5%.
[ example 8 ]
The method of the embodiment is carried out based on the fluorine removal device and the system shown in fig. 1 and fig. 2.
The waste lithium battery raw material is crushed to obtain a crushed waste lithium battery material with the particle size of 10cm, and the micro negative pressure in the crushing process is controlled to be 15 Pa. And (3) carrying out hot air heating on the waste lithium battery crushed material to generate waste gas, wherein the heating temperature is 80 ℃, the heating retention time is 1min, and the micro negative pressure of the negative pressure collecting device is controlled to be 15 Pa. And carrying out alkali liquor spraying treatment on the waste gas after dust removal, wherein the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. The flow of the circulating pump is 1 time of the volume of the alkali liquor, wherein the volume of the alkali liquor is 2m3The circulation pump flow is 2m3H is used as the reference value. The fluorine-containing liquid generated after the waste gas is sprayed is sent into a fluorine-containing device for fluorine adsorption and precipitation treatment, and the fluorine adsorbent is CaCO3Particles, the number of layers is 1. And after defluorination, part of the waste gas is circularly sent into a spraying device for spraying, part of the waste gas is subjected to photocatalytic degradation treatment, the degraded waste gas is subjected to activated carbon adsorption treatment, and the final waste gas reaches the standard and is discharged.
In the embodiment, the collection rate of electrolyte waste gas in the waste lithium battery is more than or equal to 75%, the removal rate of fluorine in the electrolyte is more than or equal to 86%, and the degradation rate of the organic solvent is more than or equal to 88%.
Through the embodiments 1-5, it can be seen that the system and the method of the invention can achieve better effects on the electrolyte waste gas collection rate, the fluorine removal rate and the organic solvent degradation rate in the waste lithium battery after the waste lithium battery is treated, and solve the problems of low waste gas collection rate and low treatment efficiency in the waste lithium battery recovery treatment process. As can be seen by comparing example 2, example 4 and example 5, the adsorption precipitation effect of the fluorine adsorbent is Ca (OH) from good to poor2、CaO、CaCO3. The methods provided in examples 6 to 8 are inferior to those of examples 2 to 5 in the overall technical effects of the electrolyte off-gas collection rate, the fluorine removal rate, and the organic solvent degradation rate in the waste lithium battery.
What has been described above is merely a preferred example of the present invention. It should be noted that other equivalent variations and modifications can be made by those skilled in the art based on the technical teaching provided by the present invention, and the protection scope of the present invention should be considered.
Claims (10)
1. The utility model provides a defluorination device, the device is the cavity cylindricality body, cavity cylindricality body upper end sets up fluorine-containing liquid import, and the lower extreme sets up slag notch and liquid outlet, set up at least one deck baffle in the cavity of cavity cylindricality body, set up fluorine adsorbent on the baffle, be in on the cavity cylindricality lateral wall baffle position department sets up fluorine adsorbent and changes the mouth.
2. The fluorine removal device of claim 1, wherein the fluorine adsorbent is selected from at least one of a calcium-containing compound, a magnesium-containing compound, and a barium-containing compound, preferably the fluorine adsorbent is selected from at least one of calcium oxide, calcium hydroxide, and calcium carbonate; and/or the particle size of the fluorine adsorbent is 1-10 mm.
3. The fluorine removal device according to claim 1 or 2, wherein the separator is provided with 1 to 3 layers; and/or a sprayer is arranged at the fluorine-containing liquid inlet.
4. A waste lithium battery treatment system is characterized by comprising a heating unit, a spraying adsorption unit and a catalytic degradation unit;
the heating unit comprises a hot air heating device, a conveying device and a negative pressure collecting device, the hot air heating device is used for heating the waste lithium battery crushed materials on the conveying device in a hot air mode, the negative pressure collecting device is used for sealing the conveying device in a negative pressure mode, the negative pressure collecting device is provided with a waste gas inlet and a waste gas outlet, and the waste gas inlet is located above the conveying device and used for collecting waste gas generated after the waste lithium battery crushed materials are heated in the hot air mode;
the spray adsorption unit comprises a spray device, a circulating pump and the defluorination device as claimed in any one of claims 1 to 3, wherein the spray device is provided with a gas inlet, a spray liquid spraying device and a fluorine-containing liquid outlet, the gas inlet is connected with the waste gas outlet of the negative pressure collection device, and the fluorine-containing liquid outlet is connected with the fluorine-containing liquid inlet of the defluorination device through the circulating pump;
the catalytic degradation unit comprises a photocatalytic degradation device, the photocatalytic degradation device is provided with a waste gas inlet after defluorination and a waste gas outlet after degradation, and the waste gas inlet after defluorination is connected with a liquid outlet of the defluorination device.
5. The used lithium battery treatment system as claimed in claim 4, wherein the gas inlet of the spray means and the liquid outlet of the fluorine removal means are connected via the circulation pump.
6. The waste lithium battery treatment system of claim 4 or 5, further comprising a crushing unit comprising a crushing device having a feed inlet through which the waste lithium battery raw material is fed into the crushing device and a discharge outlet through which the waste lithium battery raw material is fed onto the conveyor; and/or the presence of a gas in the gas,
the system also comprises a dust removal unit, wherein the dust removal unit comprises a dust removal device and a fan, the dust removal device is provided with a dust-containing waste gas inlet and a dust-removing waste gas outlet, the dust-containing waste gas inlet is connected with the waste gas outlet of the negative pressure collection device, and the dust-removing waste gas outlet is connected with the air inlet of the spray device through the fan; and/or the presence of a gas in the gas,
the system still includes the active carbon adsorption unit, the active carbon adsorption unit include active carbon adsorption device, active carbon adsorption device has degradation back waste gas entry, degradation back waste gas entry with photocatalytic degradation device's degradation back waste gas exit linkage.
7. A method for treating a waste lithium battery by the waste lithium battery treating system according to any one of claims 4 to 6, comprising the steps of:
step A: starting the hot air heating device to heat the waste lithium battery crushed materials on the conveying device by hot air to generate waste gas, wherein the waste gas is collected in the negative pressure collecting device through the waste gas inlet;
and B: the waste gas is sent into the spraying device through a waste gas outlet of the negative pressure collecting device, the spraying liquid released by the spraying liquid spraying device adsorbs the waste gas, and the obtained fluorine-containing liquid is sent into the defluorination device through the fluorine-containing liquid inlet through the circulating pump for defluorination treatment to obtain fluorine-containing precipitate and defluorinated waste gas;
and C: and the defluorinated waste gas is sent into the photocatalytic degradation device through the defluorinated waste gas inlet to be subjected to photocatalytic degradation treatment, so that the degraded waste gas is obtained.
8. The method for treating a waste lithium battery as claimed in claim 7, wherein in the step a, the crushed material of the waste lithium battery has a particle size of 2 to 5 cm; and/or the conditions for heating the hot air comprise: heating at 80-120 deg.C for 3-8 min; and/or the negative pressure value in the negative pressure collecting device is 20-100 Pa; and/or the presence of a gas in the gas,
in the step B, the spraying liquid is a sodium hydroxide solution with the mass concentration of 2-10%; and/or the presence of a gas in the gas,
the step B also comprises the following steps: and sending the waste gas after defluorination into the spraying device through the air inlet of the spraying device by the circulating pump.
9. The method for treating a waste lithium battery as claimed in claim 7 or 8, further comprising, before the step a: crushing a waste lithium battery raw material to obtain a crushed waste lithium battery material; and/or the presence of a gas in the gas,
before the step B, the method also comprises the following steps: the waste gas is sent into a dust removal device through a waste gas outlet of the negative pressure collection device, and is sent into the spraying device through a fan after dust removal treatment; and/or the presence of a gas in the gas,
after the step C, the method also comprises the following steps: and sending the degraded waste gas into an activated carbon adsorption device for adsorption and purification.
10. Use of the fluorine removal device of any one of claims 1 to 3, the waste lithium battery treatment system of any one of claims 4 to 6, or the waste lithium battery treatment method of any one of claims 7 to 9 in the treatment of waste lithium batteries.
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