CN108281726B - Method for extracting lithium hydroxide from lithium phosphate-containing waste residues - Google Patents

Method for extracting lithium hydroxide from lithium phosphate-containing waste residues Download PDF

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Publication number
CN108281726B
CN108281726B CN201711208921.7A CN201711208921A CN108281726B CN 108281726 B CN108281726 B CN 108281726B CN 201711208921 A CN201711208921 A CN 201711208921A CN 108281726 B CN108281726 B CN 108281726B
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lithium
hydroxide
lithium phosphate
containing waste
leaching
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CN108281726A (en
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陈亚
甘辉
曹利涛
关杰豪
陈白珍
石西昌
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Central South University
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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
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues; belongs to the technical field of lithium ion battery material and resource recycling. The invention aims to provide a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which is characterized in that the lithium phosphate-containing waste residues and more than one alkaline earth metal oxide or hydroxide are mixed, heated, strongly ground and leached, leachate is purified to remove residual alkaline earth metal ions, and then evaporated and crystallized to prepare lithium hydroxide monohydrate, so that the aim of efficiently utilizing the lithium phosphate-containing waste residues in an added value manner is fulfilled. The method has the advantages of reasonable process design, high resource utilization rate and high purity of the obtained product, and is convenient for large-scale industrial application.

Description

Method for extracting lithium hydroxide from lithium phosphate-containing waste residues
Technical Field
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues; belongs to the technical field of lithium ion battery material and resource recycling.
Technical Field
The lithium ion battery has the advantages of high specific energy, long cycle life, no memory effect and the like, so that the lithium ion battery is widely applied to the mobile electronic communication market and becomes one of the preferred power batteries of the pure electric vehicle at present. With the rapid development of the lithium ion battery industry, the demand for relevant battery materials continues to increase. In the preparation of electrode materials for lithium ion batteries, either early LiCoO2Is also LiMn developed gradually in the later period2O4、LiFePO4Or ternary materials and the like, without exception, high-purity lithium salt is required to be used as a raw material, and lithium carbonate or lithium hydroxide is mainly used. Because of the influence of reaction activity and the like, lithium phosphate is rarely directly used for producing the lithium ion battery anode material. In addition, high-purity lithium salt is also needed as a raw material when preparing lithium ion battery electrolyte, lithium metatitanate and other cathode materials. In order to meet the demand of the vigorous development of the lithium ion battery industry, a great deal of research work is carried out at home and abroad around the technology of extracting lithium carbonate or lithium hydroxide from spodumene, lepidolite and salt lake brine, and industrial production is carried out. In these processes, before the wastewater produced after lithium precipitation is discharged, soluble phosphate is usually added to remove heavy metals, alkaline earth metals and lithium in the water to form a large scaleMeasuring the waste residue containing lithium phosphate. In addition, in order to achieve the purpose of resource recycling, at present, much attention is paid to a process technology for recovering valuable metals from waste lithium ion batteries at home and abroad, but a great deal of research and production technical work mainly focuses on recovering metals such as Co, Ni and the like in the waste lithium ion batteries, and few technical researches on efficient lithium recovery are reported. Particularly, when the waste batteries are disassembled and cleaned, a large amount of waste electrolyte enters cleaning water to be hydrolyzed, so that waste residues containing a large amount of transition metal phosphate, lithium phosphate, a conductive agent and the like are generated, and an effective value-added recovery treatment technology is lacked.
Disclosure of Invention
The invention aims to provide a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which is characterized in that the lithium phosphate-containing waste residues and more than one alkaline earth metal oxide or hydroxide are mixed, heated, strongly ground and leached, leachate is purified to remove residual alkaline earth metal ions, and then evaporated and crystallized to prepare lithium hydroxide monohydrate, so that the aim of efficiently utilizing the lithium phosphate-containing waste residues in an added value manner is fulfilled.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the following steps:
step one
Mixing the waste residue containing lithium phosphate with alkaline earth metal oxide and/or hydroxide powder, adding water to prepare slurry, heating, grinding and leaching, cooling after complete reaction, filtering, washing a filter cake with clear water, and mixing the solution obtained by washing with the filtrate to obtain leachate;
step two
Adding soluble carbonate and/or introducing carbon dioxide into the leachate obtained in the step one, stirring and reacting completely, and filtering to obtain a purified solution;
step three
And (5) evaporating and crystallizing the solution obtained in the step two, and filtering to obtain the lithium hydroxide monohydrate.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the step one, wherein alkaline earth metal oxide and/or hydroxide powder is selected from at least one of calcium oxide, barium oxide, strontium oxide, calcium hydroxide, barium hydroxide and strontium hydroxide, and the dosage of the alkaline earth metal oxide and/or hydroxide powder is 100-120% of the theoretical dosage, preferably 105-110%. The theoretical dosage is the dosage required for completely generating precipitates from all phosphate radicals, monohydrogen phosphate radicals and dihydrogen phosphate radicals in the lithium phosphate waste residues. In a further preferred embodiment, the alkaline earth metal oxide and/or hydroxide powder is barium hydroxide.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the following steps that in the first step, the adding amount of water is 1: 5-50, preferably 1: 7-15.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the following steps that in the first step, grinding can be realized by adopting a powerful stirring paddle or adding grinding balls through ball milling, wherein the grinding speed is 200-800 revolutions per minute, and preferably 300-500 revolutions per minute; in order to improve the production efficiency, the grinding is preferably carried out by ball milling, and the volume ratio of the grinding balls to the slurry is 1: 1 to 5.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the step one of controlling the temperature of slurry to be 60-150 ℃ and preferably 60-90 ℃ during heating, grinding and leaching.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the step one, wherein the time for heating, grinding and leaching is 0.5-5 hours, and preferably 1-2.5 hours. Or the continuous carbon dioxide introduction time is 0.5-2 hours.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which comprises the step one, wherein the solid-liquid ratio of water to rate cake is 1: 2-5 when a filter cake is washed, and the washing times are 1-5.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, wherein soluble carbonate used in the second step is more than one of sodium carbonate, potassium carbonate and ammonium carbonate, the using amount of the soluble carbonate is determined according to the amount of alkaline earth metal ions in the solution, and the preferable using amount is 100-120% of the theoretical using amount calculated according to the amount of the alkaline earth metal ions in the solution.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, wherein the stirring reaction time after adding carbonate in the second step is 0.5-2 hours.
The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste residues, which can ensure that the recovery rate of lithium in the waste residues can reach more than 80%.
Principles and advantages
According to the invention, alkaline earth metal oxide and lithium phosphate waste residue are mixed and then heated, ground and leached, so that on one hand, the mass transfer speed of reactants in a solution is increased by grinding and stirring, and the overall reaction rate is improved, on the other hand, the solid alkaline earth metal phosphate product generated by the reaction of alkaline earth metal ions and lithium phosphate in the leaching process can be timely stripped from the surface of lithium phosphate particles by grinding, so that the lithium phosphate particles can be fully contacted with an external alkaline solution in the whole reaction process to generate the leaching reaction, and the leaching rate of lithium in the alkaline solution is improved. And finally, purifying the leachate to remove impurities such as unreacted alkaline earth metal ions and the like, and then evaporating and crystallizing to directly extract the lithium hydroxide monohydrate, thereby realizing high-efficiency value-added utilization of the lithium phosphate-containing waste residues.
Compared with the prior preparation process, the technical thought and the process principle of the invention have obvious characteristics and technical advantages, which are specifically shown in the following steps:
(1) the invention provides a method for grinding and leaching lithium phosphate-containing waste residues in an alkaline-earth metal alkali environment to extract lithium hydroxide, which ensures that phosphate radicals are solidified in the residues and do not enter a leaching solution in the leaching process, lithium phosphate can be fully reacted, the leaching rate of lithium is improved, the process flow is short, and the problems of waste gas emission and the like are avoided;
(2) according to the invention, alkaline earth metal oxide or hydroxide is mixed with the lithium phosphate waste residue and then leached, so that elements such as transition metal in the waste residue cannot enter the leachate, the burden of a subsequent leachate purification process is reduced, and the content of the transition metal oxide in the obtained lithium hydroxide monohydrate is ensured to be at an extremely low level;
(3) the invention converts the lithium phosphate in the waste residue containing lithium phosphate into a bulk raw material of lithium hydroxide widely used in the lithium ion battery industry, and can achieve the purpose of value-added utilization of the waste residue containing lithium phosphate.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.
The specific embodiment of the invention is as follows:
example one
Weighing 50g of lithium phosphate waste residue, grinding the lithium phosphate waste residue to minus 80 meshes, mixing the lithium phosphate waste residue with barium oxide powder with the stoichiometric ratio of 100%, and mixing the lithium phosphate waste residue with the barium oxide powder according to the solid-to-liquid ratio of 1: 5, adding water to prepare slurry, putting the slurry into a ball-milling reaction kettle, and grinding and leaching at the temperature of 60 ℃, wherein the volume ratio of grinding balls to the slurry is 1: 3, the grinding speed is 200 rpm, and the leaching time is 0.5 hour. And filtering the slurry after leaching is finished, and mixing the slurry according to a solid-liquid ratio of 1:2 adding water to wash the filter cake of the leaching residue once, mixing the collected washing liquid with the filtrate, adding 5 ml of 300 g/L sodium carbonate solution, stirring and reacting for 0.5 hour, and filtering to obtain the purified liquid. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 84.6% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.07%.
Example two
The operation process is the same as that of the first embodiment, except that calcium oxide replaces barium oxide, the dosage is 120% of the stoichiometric ratio, and the solid-to-liquid ratio of the leaching slurry is 1: 50, the leaching temperature is 150 ℃, the grinding speed is 800 rpm, the leaching time is 5 hours, and the solid-to-liquid ratio of leaching residue filter cake washing is 1: 5, the number of washing times was 5, and the purification reaction time was 2 hours. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 87.1% by atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.01%.
EXAMPLE III
The operation process is the same as that of the first embodiment, only barium hydroxide replaces barium oxide, the dosage is 110% of the stoichiometric ratio, and the solid-to-liquid ratio of the leaching slurry is 1:7, leaching temperature is 90 ℃, grinding speed is 300 rpm, leaching time is 1.5 hours, and the solid-to-liquid ratio of leaching residue filter cake washing is 1: 3, the washing times are 3 times, and the purification reaction time is 1 hour. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 92.1% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.22%.
Example four
The operation process is the same as that of the first embodiment, only barium hydroxide replaces barium oxide, and the solid-to-liquid ratio of the leaching slurry is 1:7, the leaching temperature is 90 ℃, the grinding speed is 300 rpm, a powerful stirring paddle is adopted for grinding, the leaching time is 2 hours, and the solid-to-liquid ratio of leaching residue filter cake washing is 1: 3, the washing times are 3 times, and the purification reaction time is 1 hour. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 85.7% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.14%.
EXAMPLE five
The operation process is the same as that of the first example, except that calcium hydroxide replaces barium oxide, the dosage is 110% of the stoichiometric ratio, and the solid-to-liquid ratio of the leaching slurry is 1: 15, leaching temperature is 80 ℃, grinding speed is 500 rpm, leaching time is 3 hours, and the solid-to-liquid ratio of leaching residue filter cake washing is 1:2, the number of washing times was 3, and the purification reaction time was 1 hour. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 85.4% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.09%.
EXAMPLE six
The operation process is the same as that of the first example, only barium hydroxide replaces barium oxide, the dosage is 105% of the stoichiometric ratio, and the solid-to-liquid ratio of the leaching slurry is 1: 9, the leaching temperature is 90 ℃, the grinding speed is 500 rpm, the leaching time is 2 hours, and the solid-to-liquid ratio of the leached residue filter cake washing is 1: 3, the washing times are 3 times, and the purification reaction time is 1 hour. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 90.8% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.23%.
Comparative example 1
The operation process is the same as that of the first embodiment, only a common stirrer is adopted for stirring and leaching, the stirring speed is 150 rpm, the leaching time is 2 hours, and the solid-to-liquid ratio of the leached residue filter cake washing is 1: 3, the washing times are 3 times, and the purification reaction time is 1 hour. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 34.7% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 70.01%.
Comparative example 2
The operation process is the same as that of the first embodiment, only a common stirrer is adopted for stirring and leaching, the stirring speed is 150 rpm, the leaching time is 2 hours, and the solid-to-liquid ratio of the leached residue filter cake washing is 1: and 20, washing for 3 times, mixing the collected washing liquid with the filtrate, adding 10 ml of 300 g/L sodium carbonate solution, stirring and reacting for 1 hour, and filtering to obtain a purified liquid. Evaporating the obtained purified liquid at 80 ℃, cooling, crystallizing and filtering, and drying a crystal filter cake obtained by filtering at 120 ℃ to obtain the lithium hydroxide monohydrate. The leaching rate of lithium was calculated to be 43.9% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 90.01%.

Claims (5)

1. A method for extracting lithium hydroxide from lithium phosphate-containing waste residues is characterized by comprising the following steps:
step one
Mixing the waste residue containing lithium phosphate with alkaline earth metal oxide and/or hydroxide powder, adding water to prepare slurry, heating, grinding and leaching, cooling after complete reaction, filtering, washing a filter cake with clear water, and mixing the solution obtained by washing with the filtrate to obtain leachate; when heating, grinding and leaching, controlling the temperature of the slurry to be 60-150 ℃; in the first step; the granularity of the lithium phosphate waste residue is-80 meshes; the alkaline earth metal oxide and/or hydroxide is selected from at least one of calcium oxide, barium oxide, strontium oxide, calcium hydroxide, barium hydroxide and strontium hydroxide; the dosage of the additive is 100-120% of the theoretical dosage;
in the first step, the grinding is realized by adopting a powerful stirring paddle or adding grinding balls through ball milling, and the grinding rotating speed is 200-800 r/min; in the first step, the time for heating, grinding and leaching is 0.5-5 hours;
step two
Adding soluble carbonate into the leachate obtained in the step one, stirring and reacting completely, and filtering to obtain a purified solution; the soluble carbonate used in the second step is more than one of sodium carbonate, potassium carbonate and ammonium carbonate, and the usage amount of the soluble carbonate is determined by 100-120% of the theoretical usage amount calculated by the alkaline earth metal ions in the solution;
step three
And (5) evaporating and crystallizing the solution obtained in the step two, and filtering to obtain the lithium hydroxide monohydrate.
2. The method for extracting lithium hydroxide from lithium phosphate-containing waste residue according to claim 1, wherein the method comprises the following steps: in the first step, the adding amount of water is 1: 5-50.
3. The method for extracting lithium hydroxide from lithium phosphate-containing waste residue according to claim 1, wherein the method comprises the following steps: and in the first step, the solid-liquid ratio of water to the filter cake is 1: 2-5 when the filter cake is washed, and the washing times are 1-5.
4. The method for extracting lithium hydroxide from lithium phosphate-containing waste residue according to claim 1, wherein the method comprises the following steps: and the stirring reaction time after the carbonate is added in the second step is 0.5-2 hours.
5. The method for extracting lithium hydroxide from lithium phosphate-containing waste residue according to claim 1, wherein the method comprises the following steps: the method can lead the recovery rate of lithium in the waste residue to reach more than 80 percent.
CN201711208921.7A 2017-11-27 2017-11-27 Method for extracting lithium hydroxide from lithium phosphate-containing waste residues Active CN108281726B (en)

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CN109264748B (en) * 2018-09-29 2021-04-20 广东邦普循环科技有限公司 Method for preparing lithium carbonate from crude lithium phosphate
TW202107764A (en) * 2019-07-26 2021-02-16 德商巴斯夫歐洲公司 Process for the recovery of lithium from waste lithium ion batteries
CN111172397B (en) * 2020-01-16 2021-07-20 赣州逸豪优美科实业有限公司 Method for carrying out continuous grinding and leaching by short-process double coupling
WO2021153816A1 (en) 2020-01-29 2021-08-05 전웅 Lithium extraction method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104220371A (en) * 2012-04-05 2014-12-17 Posco公司 Method for manufacturing lithium hydroxide and method using the lithium hydroxide for manufacturing lithium carbonate
CN106785166A (en) * 2016-12-12 2017-05-31 江西赣锋锂业股份有限公司 The method that lithium prepares battery-level lithium carbonate is reclaimed in a kind of old and useless battery from LiFePO 4

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104220371A (en) * 2012-04-05 2014-12-17 Posco公司 Method for manufacturing lithium hydroxide and method using the lithium hydroxide for manufacturing lithium carbonate
CN106785166A (en) * 2016-12-12 2017-05-31 江西赣锋锂业股份有限公司 The method that lithium prepares battery-level lithium carbonate is reclaimed in a kind of old and useless battery from LiFePO 4

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