CN114950005A - Recovery system and recovery method for ternary positive electrode precursor production regeneration waste liquid - Google Patents

Recovery system and recovery method for ternary positive electrode precursor production regeneration waste liquid Download PDF

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Publication number
CN114950005A
CN114950005A CN202210759035.8A CN202210759035A CN114950005A CN 114950005 A CN114950005 A CN 114950005A CN 202210759035 A CN202210759035 A CN 202210759035A CN 114950005 A CN114950005 A CN 114950005A
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China
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tank
precipitation
outlet
waste liquid
liquid
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Pending
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CN202210759035.8A
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Inventor
许开华
刘郁
周毅
任云强
吴雨晴
周林
陈先雄
余尚清
邓凯
孙越
董柯静
薛飞
胡丰献
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Green Aike Jingmen New Energy Materials Co ltd
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Green Aike Jingmen New Energy Materials Co ltd
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Priority to CN202210759035.8A priority Critical patent/CN114950005A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B01D36/04—Combinations of filters with settling tanks
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 relates to the technical field of ternary materials of lithium batteries, in particular to a system and a method for recovering a ternary positive electrode precursor production regeneration waste liquid. The method comprises the steps of feeding, primary solid-liquid separation, slurrying and solid-liquid separation. According to the invention, the regenerated waste liquid treated by the high-efficiency thickener is subjected to preliminary precipitation separation and then solid-liquid separation, so that the time for solid-liquid separation can be greatly saved, the energy consumption is low, and the production efficiency is high; the solid content of the slurry obtained by preliminary solid-liquid separation is detected, and different recovery strategies are adopted according to different solid contents, so that the recovery rate can be greatly improved, and the production cost is reduced.

Description

Recovery system and recovery method for ternary positive electrode precursor production regeneration waste liquid
Technical Field
The invention relates to the technical field of ternary materials of lithium batteries, in particular to a system and a method for recovering a ternary positive electrode precursor production regeneration waste liquid.
Background
At present, a nickel-cobalt hydroxide precursor material is mainly obtained by a coprecipitation method, and the main production flow is as follows: preparing binary solution of nickel sulfate and cobalt sulfate; adding the binary solution, liquid caustic soda and ammonia water into a reaction kettle for coprecipitation reaction; thirdly, washing and filter pressing the reaction slurry; dehydrating and drying; and fifthly, screening and packaging. In the second step reaction process, a concentration filtering device (high-efficiency concentrator) is usually used for concentrating and filtering the reaction liquid, part of grains with the grain diameter larger than that of the filter screen and part of small grains agglomerated to form larger grains (possibly containing other foreign matters) which are adhered to the filter screen to block the filter holes, so that the grains are cleaned by high-pressure backwashing water at regular time, meanwhile, materials attached to the inner wall of the device are also taken out, and finally, the materials are discharged, namely, the regeneration liquid waste.
Because the concentration of nickel and cobalt in the regenerated liquid waste is low and the components and the granularity are not uniform, the prior precursor material production process does not generally carry out recovery treatment on the waste, but directly discharges the waste into a waste water treatment system, thereby reducing the utilization rate and the recovery rate of raw materials; or directly enters the raw material preparation system again through filter pressing and acid dissolution, and the method directly performs filter pressing when the waste is at low concentration, so that the treatment time is greatly increased, the energy consumption is increased, and the treatment efficiency is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a system and a method for recovering a ternary cathode precursor production regeneration waste liquid, which specifically comprise the following contents:
a ternary positive precursor production regeneration waste liquid recovery system comprises a high-efficiency thickener, a precipitation recovery tank, a clear liquid tank, a precision filter, a regeneration binary liquid tank, a pressure filter and an acid dissolution tank, wherein the high-efficiency thickener is provided with a feed inlet and a discharge outlet respectively; a stirring device is arranged in the precipitation recovery tank, a discharge port of the precipitation recovery tank comprises a supernatant outlet and a slurry outlet, the supernatant outlet is connected with the clear solution tank, the slurry outlet is respectively connected with feed inlets of the precision filter and the filter press through a first pipeline and a second pipeline, a first valve is arranged on the first pipeline, and a second valve is arranged on the second pipeline; the discharge hole of the precision filter comprises a filtrate outlet and a filter residue outlet; the discharge hole of the filter press comprises a filtrate outlet and a filter residue outlet, and the filter residue outlet of the filter press is connected with the acid dissolving tank; and a discharge port of the acid dissolving tank and a filtrate outlet of the precision filter are respectively connected with a feed port of the regeneration binary liquid tank through pipelines, and a fifth valve is arranged on a pipeline between the acid dissolving tank and the regeneration binary liquid tank.
The device comprises a sedimentation recovery tank, a liquid inlet, a liquid outlet and a liquid outlet.
Specifically, a fourth valve is arranged on a pipeline between the overflow groove and the precipitation recovery groove.
Specifically, a sight glass is arranged on the side wall of the precipitation recovery tank.
The method for recycling the ternary anode precursor production regeneration waste liquid by adopting the ternary anode precursor production regeneration waste liquid recycling system disclosed by the invention comprises the following steps of:
(1) feeding: opening a third valve, discharging the regenerated waste liquid treated by the high-efficiency concentrator into a precipitation recovery tank, and closing the third valve when the volume of the regenerated waste liquid in the precipitation recovery tank reaches 3/5-4/5 of the volume of the tank body;
(2) primary solid-liquid separation: standing the regenerated waste liquid in a precipitation recovery tank for 2-4h, discharging supernatant in the precipitation recovery tank into a clear solution tank after standing is finished, and leaving a small amount of supernatant in the precipitation recovery tank;
(3) slurrying: opening a stirring device in the precipitation recovery tank, uniformly mixing the precipitate in the precipitation recovery tank with a small amount of supernatant to obtain precipitation slurry, and testing the solid content in the precipitation slurry;
(4) solid-liquid separation: when the solid content of the precipitated slurry in the step (3) is smaller than a set value, opening a first valve, conveying the precipitated slurry into a precision filter for solid-liquid separation, conveying filtrate into a regeneration binary liquid tank, and periodically cleaning filter residues and putting the filter residues into a solid waste treatment system; and (4) when the solid content of the precipitated slurry in the step (3) is larger than or equal to a set value, opening the second valve, conveying the precipitated slurry into a filter press for solid-liquid separation, conveying a filter cake into an acid dissolution tank for acid dissolution, opening the fifth valve after the acid dissolution is finished, conveying an acid solution into a regeneration binary liquid tank, and discharging the filtrate of the filter press into a T-membrane wastewater treatment system.
Specifically, the solid content set value of the precipitation slurry in the step (3) is 260 g/L.
The invention has the beneficial effects that:
(1) in the method for recycling the regenerated waste liquid by adopting the device disclosed by the invention, the regenerated waste liquid treated by the high-efficiency thickener is subjected to preliminary precipitation separation and then solid-liquid separation, so that the time for solid-liquid separation can be greatly saved, the energy consumption is low, and the production efficiency is high;
(2) in the method for recycling the regeneration waste liquid by adopting the device disclosed by the invention, the solid content of the slurry obtained by primary solid-liquid separation is detected, and when the solid content is lower than 260g/L, useful components in the waste mainly exist in a liquid form, so that filtrate is recycled; when the solid content is more than or equal to 260g/L, the useful components in the waste materials mainly exist in a solid particle form, so that filter cakes are recovered, different recovery schemes are used according to different solid contents of the regenerated waste liquid, the recovery utilization rate can be greatly improved, and the production cost is reduced;
(3) the device disclosed by the invention is simple in structure, low in manufacturing cost and convenient to use.
Drawings
FIG. 1 is a schematic diagram of an apparatus for the disclosed method.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. The embodiments shown below do not limit the inventive content described in the claims. The entire contents of the configurations shown in the following embodiments are not limited to those required as solutions of the inventions described in the claims.
Referring to the attached drawing 1, the system for recovering the regeneration waste liquid in the production of the ternary anode precursor comprises a high-efficiency thickener 1, a precipitation recovery tank 2, a clear liquid tank 3, a precision filter 4, a regeneration binary liquid tank 5, a filter press 6 and an acid dissolution tank 7, wherein the high-efficiency thickener 1 is provided with a feed inlet and a discharge outlet respectively, the discharge outlet of the high-efficiency thickener 1 is connected with the feed inlet of the precipitation recovery tank 2 through a pipeline, and a third valve 8 is arranged on the pipeline between the high-efficiency thickener 1 and the precipitation recovery tank 2; a stirring device is arranged in the precipitation recovery tank 2, a discharge hole of the precipitation recovery tank 2 comprises a supernatant outlet and a slurry outlet, the supernatant outlet is connected with the clear solution tank 3, the slurry outlet is respectively connected with feed holes of the precision filter 4 and the filter press 6 through a first pipeline 9 and a second pipeline 10, a first valve 11 is arranged on the first pipeline 9, and a second valve 12 is arranged on the second pipeline 10; the discharge hole of the precision filter 4 comprises a filtrate outlet and a filter residue outlet; the discharge hole of the filter press 6 comprises a filtrate outlet and a filter residue outlet, and the filter residue outlet of the filter press 6 is connected with the acid dissolving tank 7; the discharge hole of the acid dissolving tank 7 and the filtrate outlet of the precision filter 4 are respectively connected with the feed hole of the regeneration binary liquid tank 5 through pipelines, and a fifth valve 13 is arranged on the pipeline between the acid dissolving tank 7 and the regeneration binary liquid tank 5.
In an embodiment of the present invention, the apparatus further comprises an overflow tank 14, wherein the overflow tank 14 is provided with a feed inlet and a discharge outlet, the feed inlet of the overflow tank 14 is connected with the supernatant outlet of the precipitation recovery tank 2 through a pipeline, and the discharge outlet of the overflow tank 14 is connected with the feed inlet of the clear solution tank 3.
In one embodiment of the invention, a fourth valve 15 is provided in the conduit between the overflow launder 14 and the precipitation recovery tank 2.
In one embodiment of the invention, a viewing mirror is arranged on the side wall of the precipitation recovery tank 2, and can be used for observing the precipitation condition in the precipitation recovery tank 2.
The method for recovering the ternary anode precursor production regeneration waste liquid by adopting the ternary anode precursor production regeneration waste liquid recovery system disclosed by the invention comprises the following steps of:
(1) feeding: opening a third valve 8, discharging the regenerated waste liquid treated by the high-efficiency concentrator 1 into the precipitation recovery tank 2, and closing the third valve 8 when the volume of the regenerated waste liquid in the precipitation recovery tank 2 reaches 3/5-4/5 of the volume of the tank body, wherein the third valve 8 can specifically reach 3/5, 7/10 or 4/5 of the volume of the precipitation recovery tank 2, and is preferably 4/5;
(2) primary solid-liquid separation: standing the regenerated waste liquid in a precipitation recovery tank 2 for 2-4h, discharging the supernatant in the precipitation recovery tank 2 into a clear solution tank 3 after the standing is finished, leaving a small amount of supernatant in the precipitation recovery tank 2, wherein the specific standing time can be determined according to the specific situation of precipitation, the precipitation situation in the precipitation recovery tank 2 can be seen in a sight glass of the precipitation recovery tank 2, and the precipitation time can be 2h, 3h, 4h, 3.5h and the like;
(3) slurrying: opening a stirring device in the precipitation recovery tank 2, uniformly mixing the precipitate in the precipitation recovery tank 2 with a small amount of supernatant to obtain precipitation slurry, and testing the solid content in the precipitation slurry;
(4) solid-liquid separation: when the solid content of the precipitated slurry in the step (3) is smaller than a set value, opening a first valve 11, conveying the precipitated slurry into a precision filter 4 for solid-liquid separation, conveying filtrate into a regeneration binary liquid tank 5, and periodically cleaning filter residues and putting the filter residues into a solid waste treatment system; and (4) when the solid content of the precipitated slurry in the step (3) is larger than or equal to a set value, opening the second valve 12, conveying the precipitated slurry into the filter press 6 for solid-liquid separation, conveying the filter cake into the acid dissolution tank 7 for acid dissolution, opening the fifth valve 13 after the acid dissolution is finished, conveying the acid solution into the regeneration binary liquid tank 5, and discharging the filtrate of the filter press 6 into the T-membrane wastewater treatment system.
In one embodiment of the invention, the solids content set point of the precipitation slurry in step (3) is 260 g/L. Detecting the solid content of the slurry obtained by the preliminary solid-liquid separation, wherein when the solid content is lower than 260g/L, the useful components in the waste materials mainly exist in a liquid form, so that the filtrate is recovered; when the solid content is more than or equal to 260g/L, the useful components in the waste materials mainly exist in a solid particle form, so that filter cakes are recovered, different recovery schemes are used according to different solid contents of the regenerated waste liquid, the recovery utilization rate can be greatly improved, and the production cost is reduced.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (6)

1. The system for recovering the waste liquid generated in the production and regeneration of the ternary anode precursor is characterized by comprising a high-efficiency thickener, a precipitation recovery tank, a clear liquid tank, a precision filter, a regeneration binary liquid tank, a filter press and an acid dissolution tank, wherein the high-efficiency thickener is respectively provided with a feeding hole and a discharging hole; a stirring device is arranged in the precipitation recovery tank, a discharge port of the precipitation recovery tank comprises a supernatant outlet and a slurry outlet, the supernatant outlet is connected with the clear solution tank, the slurry outlet is respectively connected with feed ports of the precision filter and the filter press through a first pipeline and a second pipeline, a first valve is arranged on the first pipeline, and a second valve is arranged on the second pipeline; the discharge hole of the precision filter comprises a filtrate outlet and a filter residue outlet; the discharge hole of the filter press comprises a filtrate outlet and a filter residue outlet, and the filter residue outlet of the filter press is connected with the acid dissolving tank; and a discharge port of the acid dissolving tank and a filtrate outlet of the precision filter are respectively connected with a feed port of the regeneration binary liquid tank through pipelines, and a fifth valve is arranged on a pipeline between the acid dissolving tank and the regeneration binary liquid tank.
2. The system for recovering the waste liquid from the production regeneration of the ternary cathode precursor according to claim 1, further comprising an overflow tank, wherein the overflow tank is provided with a feed inlet and a discharge outlet, the feed inlet of the overflow tank is connected with the supernatant outlet of the precipitation recovery tank through a pipeline, and the discharge outlet of the overflow tank is connected with the feed inlet of the clear solution tank.
3. The system for recovering the ternary cathode precursor production regeneration waste liquid according to claim 2, wherein a fourth valve is arranged on a pipeline between the overflow tank and the precipitation recovery tank.
4. The system for recycling the ternary positive electrode precursor production regeneration waste liquid according to claim 1, wherein a viewing mirror is disposed on a side wall of the precipitation recycling tank.
5. A method for recovering a ternary cathode precursor production regeneration waste liquid by using the ternary cathode precursor production regeneration waste liquid recovery system of any one of claims 1 to 4, is characterized by comprising the following steps:
(1) feeding: opening a third valve, discharging the regenerated waste liquid treated by the high-efficiency concentrator into a precipitation recovery tank, and closing the third valve when the volume of the regenerated waste liquid in the precipitation recovery tank reaches 3/5-4/5 of the volume of the tank body;
(2) primary solid-liquid separation: standing the regenerated waste liquid in a precipitation recovery tank for 2-4h, discharging supernatant in the precipitation recovery tank into a clear solution tank after standing is finished, and leaving a small amount of supernatant in the precipitation recovery tank;
(3) pulping: opening a stirring device in the precipitation recovery tank, uniformly mixing the precipitate in the precipitation recovery tank with a small amount of supernatant to obtain precipitation slurry, and testing the solid content in the precipitation slurry;
(4) solid-liquid separation: when the solid content of the precipitation slurry in the step (3) is smaller than a set value, opening a first valve, conveying the precipitation slurry into a precision filter for solid-liquid separation, and conveying the filtrate into a regeneration binary liquid tank; and (4) when the solid content of the precipitated slurry in the step (3) is larger than or equal to the set value, opening the second valve, conveying the precipitated slurry to a filter press for solid-liquid separation, conveying a filter cake to an acid dissolution tank for acid dissolution, opening the fifth valve after the acid dissolution is finished, and conveying the acid solution to a regeneration binary liquid tank.
6. The method for recovering the ternary positive electrode precursor production regeneration waste liquid as claimed in claim 5, wherein the solid content set value of the precipitation slurry in the step (3) is 260 g/L.
CN202210759035.8A 2022-06-29 2022-06-29 Recovery system and recovery method for ternary positive electrode precursor production regeneration waste liquid Pending CN114950005A (en)

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