WO2018113477A1 - Method for recovering cobalt and lithium from positive electrode material of spent lithium cobalt oxide battery - Google Patents

Method for recovering cobalt and lithium from positive electrode material of spent lithium cobalt oxide battery Download PDF

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WO2018113477A1
WO2018113477A1 PCT/CN2017/113056 CN2017113056W WO2018113477A1 WO 2018113477 A1 WO2018113477 A1 WO 2018113477A1 CN 2017113056 W CN2017113056 W CN 2017113056W WO 2018113477 A1 WO2018113477 A1 WO 2018113477A1
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lithium
cobalt
spent
cathode material
recovering
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PCT/CN2017/113056
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French (fr)
Chinese (zh)
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郭永兴
祝宏帅
王迎春
曾小毛
欧阳红勇
刘金练
樊磊
刘志成
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江西合纵锂业科技有限公司
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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

Definitions

  • the invention relates to a method for recovering cobalt and lithium in a cathode material of a lithium cobalt oxide battery, which belongs to the field of waste recycling.
  • lithium ion secondary batteries As a "green energy source" has a certain life span, and is generally about three years. It can be predicted that lithium ion secondary batteries will become a non-negligible part of future solid waste. How to properly handle them will be a big problem for people.
  • the prior art mostly involves the extraction of cobalt and lithium by adding a reducing agent (such as hydrogen peroxide or Na 2 SO 3 ) to the acidic system.
  • a reducing agent such as hydrogen peroxide or Na 2 SO 3
  • SONY and other companies have proposed a solution for recovering cobalt compounds from used lithium ion secondary batteries.
  • some researchers have also carried out related research: Zhang et al. used extraction and precipitation to recover lithium carbonate and cobalt oxalate; Lee et al. proposed a solution for recovering LiCoO 2 .
  • Contestabile also comprehensively recovered the stainless steel casing of the waste lithium ion secondary battery and the collectors such as aluminum and copper.
  • no company has proposed its own waste lithium ion secondary battery recycling program. The purpose of these recycling programs is mainly to recover cobalt compounds or cobalt metal.
  • the present invention provides a cobalt recovery from the cathode material of the lithium cobalt oxide battery.
  • a method of lithium in which sodium hydrogen sulfate is mixed with a cathode material of a spent lithium cobaltate battery, the mixture is calcined at a high temperature, and then water is leached, and a sulfate solution containing a cobalt element and a lithium element is obtained by filtration.
  • the method has simple preparation process and strong controllability, and is very suitable for recycling cobalt and lithium elements of lithium cobaltate batteries.
  • a method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery which comprises mixing sodium hydrogen sulfate with a cathode material of a spent lithium cobaltate battery, and calcining the mixture at a high temperature, leaching with water, and filtering to obtain a cobalt element and a lithium element. Sulfate solution.
  • the method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery described above which specifically includes The following steps:
  • the leaching temperature is 20 ° C ⁇ 90 ° C, the leaching time is 4 ⁇ 6 h;
  • the filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
  • the mass ratio of water to the binder in the step 3) is 40 to 80:1.
  • the method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery according to the present invention is mixed and calcined with NaHSO 4 and the cathode material of the spent lithium cobaltate battery, and then leached with water; it can obtain a higher concentration of cobalt and lithium leachate.
  • the leaching rate of cobalt is 95% or more, and the leaching rate of lithium is 93% or more.
  • Embodiment 1 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
  • the sodium hydrogen sulphate and the spent lithium cobaltate battery cathode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 200 ° C for 40 min.
  • the baked material was taken out and then leached with water, and the leaching temperature was 90 ° C.
  • the filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
  • the leaching rate of the detected cobalt was 97.50%, and the leaching rate of lithium was 96.82%.
  • Embodiment 2 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
  • the sodium hydrogen sulphate and the lithium cobalt oxide battery positive electrode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 600 ° C for 20 min.
  • the baked material was taken out and then leached with water, and the leaching temperature was 20 ° C.
  • the filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
  • the leaching rate of the detected cobalt was 98.35%, and the leaching rate of lithium was 97.76%.
  • Embodiment 3 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
  • the sodium hydrogen sulphate and the lithium cobalt oxide battery positive electrode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 400 ° C for 30 min.
  • the baked material was taken out and then leached with water, and the leaching temperature was 60 ° C.
  • the filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
  • the leaching rate of the detected cobalt was 98.12%, and the leaching rate of lithium was 97.98%.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Secondary Cells (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

Provided is a method for recovering cobalt and lithium from a positive electrode material of a spent lithium cobalt oxide battery. Sodium hydrogen sulphate is mixed with the positive electrode material of the spent lithium cobalt oxide battery, the mixture is subjected to high temperature calcination, and then water is added for leaching, and a sulphate solution comprising cobalt and lithium elements is obtained by filtration.

Description

一种从失效钴酸锂电池正极材料中回收钴和锂的方法Method for recovering cobalt and lithium from cathode material of spent lithium cobaltate battery 技术领域Technical field
本发明涉及一种失效钴酸锂电池正极材料中回收钴和锂的方法，属于废弃物回收利用领域。The invention relates to a method for recovering cobalt and lithium in a cathode material of a lithium cobalt oxide battery, which belongs to the field of waste recycling.
背景技术Background technique
随着人口不断增加，资源不断枯竭，人们对化学能源提出了更高的要求，即高质量、长寿命、低污染，而高科技、高附加值的锂离子二次电池是其中一大亮点，引起了许多大公司竞相加入到该产品的研究开发行列中。作为“绿色能源”的锂离子二次电池有一定的寿命，一般为3年左右。可以预测，锂离子二次电池将成为未来固体废物中不可忽视的部分。如何妥善处理它们，将是人们面临的一大问题。With the continuous increase of population and the exhaustion of resources, people have put forward higher requirements for chemical energy, namely high quality, long life and low pollution. High-tech, high value-added lithium ion secondary batteries are one of the highlights. It has caused many large companies to compete in the research and development of this product. A lithium ion secondary battery as a "green energy source" has a certain life span, and is generally about three years. It can be predicted that lithium ion secondary batteries will become a non-negligible part of future solid waste. How to properly handle them will be a big problem for people.
关于从失效钴酸锂电池正极材料中回收钴、锂的方法，现有技术多为在酸性体系中加入还原剂(如双氧水、Na2SO3)浸出钴、锂。在国外，SONY等公司已提出了从废旧锂离子二次电池中回收钴化合物的方案。此外，一些研究者也进行了相关的研究：Zhang等采用萃取、沉淀的方法回收了碳酸锂和草酸钴；而Lee等提出了回收LiCoO2的方案。其中，Contestabile等还综合回收了废旧锂离子二次电池的不锈钢外壳及铝、铜等集流极。在国内尚未有公司提出自己的废旧锂离子二次电池回收方案，这些回收方案的目的主 要是回收钴化合物或钴金属单质。Regarding the method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery, the prior art mostly involves the extraction of cobalt and lithium by adding a reducing agent (such as hydrogen peroxide or Na 2 SO 3 ) to the acidic system. In foreign countries, SONY and other companies have proposed a solution for recovering cobalt compounds from used lithium ion secondary batteries. In addition, some researchers have also carried out related research: Zhang et al. used extraction and precipitation to recover lithium carbonate and cobalt oxalate; Lee et al. proposed a solution for recovering LiCoO 2 . Among them, Contestabile also comprehensively recovered the stainless steel casing of the waste lithium ion secondary battery and the collectors such as aluminum and copper. In China, no company has proposed its own waste lithium ion secondary battery recycling program. The purpose of these recycling programs is mainly to recover cobalt compounds or cobalt metal.
《废旧锂离子电池正极材料钴酸锂的回收》中采用不同的回收方案对废旧锂离子二次电池进行了回收研究：采用碳酸丙烯酯(PC)回收电解质；采用N-甲基吡咯烷酮(NMP)在70℃剥离活性物质；通过热处理方法除去碳粉；采用盐酸溶解钴，以Co(OH)2形式回收，再重新合成钴酸锂。该方法中钴的回收率大于99％，但该处理工艺过程复杂，且回收成本较高。Recycling of used lithium ion secondary batteries using different recycling schemes in the recycling of lithium lithium ion battery cathode material lithium cobalt oxide: using propylene carbonate (PC) to recover electrolytes; using N-methylpyrrolidone (NMP) The active material was peeled off at 70 ° C; the carbon powder was removed by a heat treatment method; cobalt was dissolved in hydrochloric acid, recovered as Co(OH) 2 , and lithium cobaltate was re-synthesized. The recovery rate of cobalt in the method is more than 99%, but the treatment process is complicated and the recovery cost is high.
发明内容Summary of the invention
为了克服现有技术中从失效钴酸锂电池正极材料中回收钴和锂过程中回收成本较高，且处理步骤复杂的技术不足，本发明提供一种从失效钴酸锂电池正极材料中回收钴和锂的方法，该方法中将硫酸氢钠与失效钴酸锂电池正极材料混合，将混合料高温焙烧后加水浸出，过滤得到包含钴元素和锂元素的硫酸盐溶液。该方法制备工艺简单，过程可控性强，非常适合钴酸锂电池钴和锂元素的回收利用。In order to overcome the prior art that the recovery cost is high in the process of recovering cobalt and lithium from the cathode material of the lithium cobalt oxide battery, and the processing steps are complicated, the present invention provides a cobalt recovery from the cathode material of the lithium cobalt oxide battery. And a method of lithium, in which sodium hydrogen sulfate is mixed with a cathode material of a spent lithium cobaltate battery, the mixture is calcined at a high temperature, and then water is leached, and a sulfate solution containing a cobalt element and a lithium element is obtained by filtration. The method has simple preparation process and strong controllability, and is very suitable for recycling cobalt and lithium elements of lithium cobaltate batteries.
本发明通过下述技术方案实现上述技术目的：The present invention achieves the above technical objectives by the following technical solutions:
一种从失效钴酸锂电池正极材料中回收钴和锂的方法，其将硫酸氢钠与失效钴酸锂电池正极材料混合，将混合料高温焙烧后加水浸出，过滤得到包含钴元素和锂元素的硫酸盐溶液。A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery, which comprises mixing sodium hydrogen sulfate with a cathode material of a spent lithium cobaltate battery, and calcining the mixture at a high temperature, leaching with water, and filtering to obtain a cobalt element and a lithium element. Sulfate solution.
上述所述从失效钴酸锂电池正极材料中回收钴和锂的方法，其具体包括 下述步骤：The method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery described above, which specifically includes The following steps:
(1)将硫酸氢钠与失效钴酸锂电池正极材料混合均匀得到混合料，控制钴元素与硫元素的摩尔比为1：3；(1) mixing sodium hydrogen sulfate with the lithium cobalt oxide battery cathode material to obtain a mixture, controlling the molar ratio of cobalt to sulfur is 1:3;
(2)将混合料置于200℃～600℃条件下焙烧5min～40min得焙料；(2) baking the mixture at 200 ° C ~ 600 ° C for 5 min ~ 40 min to obtain the baking;
(3)取出焙料后加水浸出，浸出温度为20℃～90℃，浸出时间为4～6h；(3) After taking out the baking material, adding water to leaching, the leaching temperature is 20 ° C ~ 90 ° C, the leaching time is 4 ~ 6 h;
(4)过滤液固分离，滤液即为包含钴元素和锂元素的硫酸盐溶液。(4) The filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
上述从失效钴酸锂电池正极材料中回收钴和锂的方法中，所述的步骤3)中水与焙料的质量比为40～80：1。In the above method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery, the mass ratio of water to the binder in the step 3) is 40 to 80:1.
该方法的原理是：The principle of this method is:
4LiCoO2+12NaHSO4＝＝2Li2SO4+6Na2SO4+4CoSO4+6H2O+O2 4LiCoO 2 +12NaHSO 4 ==2Li 2 SO 4 +6Na 2 SO 4 +4CoSO 4 +6H 2 O+O 2
本发明相对于现有技术具有如下技术优势：The present invention has the following technical advantages over the prior art:
本发明所述的从失效钴酸锂电池正极材料中回收钴和锂的方法使用NaHSO4与失效钴酸锂电池正极材料混合焙烧后，加水浸出；其可以得到较高浓度的钴、锂浸出液，钴的浸出率在95％以上、锂的浸出率为93％以上。The method for recovering cobalt and lithium from the cathode material of the spent lithium cobaltate battery according to the present invention is mixed and calcined with NaHSO 4 and the cathode material of the spent lithium cobaltate battery, and then leached with water; it can obtain a higher concentration of cobalt and lithium leachate. The leaching rate of cobalt is 95% or more, and the leaching rate of lithium is 93% or more.
具体实施方式detailed description
以下通过具体实施例进一步说明本发明的技术内容，但所述领域的技术人员应能知晓，所述实施例并不以任何方式限定本发明专利的保护范围。本 领域技术人员在此基础上作出的修饰或等同替代，均应包括在本专利保护范围之内。The technical content of the present invention is further illustrated by the following specific examples, but those skilled in the art should understand that the embodiments do not limit the scope of protection of the present invention in any way. Ben Modifications or equivalent substitutions made by those skilled in the art should be included in the scope of this patent.
实施例1一种从失效钴酸锂电池正极材料中回收钴和锂的方法Embodiment 1 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
将硫酸氢钠与失效钴酸锂电池正极材料以钴硫摩尔比为1：3混合后，于200℃焙烧40min，取出焙料后加水浸出，浸出温度为90℃。过滤液固分离，滤液即为包含钴元素和锂元素的硫酸盐溶液。经检测钴的浸出率为97.50％、锂的浸出率为96.82％。The sodium hydrogen sulphate and the spent lithium cobaltate battery cathode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 200 ° C for 40 min. The baked material was taken out and then leached with water, and the leaching temperature was 90 ° C. The filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element. The leaching rate of the detected cobalt was 97.50%, and the leaching rate of lithium was 96.82%.
实施例2一种从失效钴酸锂电池正极材料中回收钴和锂的方法Embodiment 2 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
将硫酸氢钠与失效钴酸锂电池正极材料以钴硫摩尔比为1：3混合后，于600℃焙烧20min，取出焙料后加水浸出，浸出温度为20℃。过滤液固分离，滤液即为包含钴元素和锂元素的硫酸盐溶液。经检测钴的浸出率为98.35％、锂的浸出率为97.76％。The sodium hydrogen sulphate and the lithium cobalt oxide battery positive electrode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 600 ° C for 20 min. The baked material was taken out and then leached with water, and the leaching temperature was 20 ° C. The filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element. The leaching rate of the detected cobalt was 98.35%, and the leaching rate of lithium was 97.76%.
实施例3一种从失效钴酸锂电池正极材料中回收钴和锂的方法Embodiment 3 A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery
将硫酸氢钠与失效钴酸锂电池正极材料以钴硫摩尔比为1：3混合后，于400℃焙烧30min，取出焙料后加水浸出，浸出温度为60℃。过滤液固分离，滤液即为包含钴元素和锂元素的硫酸盐溶液。经检测钴的浸出率为98.12％、锂的浸出率为97.98％。 The sodium hydrogen sulphate and the lithium cobalt oxide battery positive electrode material were mixed at a molar ratio of cobalt to sulfur of 1:3, and then calcined at 400 ° C for 30 min. The baked material was taken out and then leached with water, and the leaching temperature was 60 ° C. The filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element. The leaching rate of the detected cobalt was 98.12%, and the leaching rate of lithium was 97.98%.

Claims (3)

  1. 一种从失效钴酸锂电池正极材料中回收钴和锂的方法，其将硫酸氢钠与失效钴酸锂电池正极材料混合，将混合料高温焙烧后加水浸出，过滤得到包含钴元素和锂元素的硫酸盐溶液。A method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery, which comprises mixing sodium hydrogen sulfate with a cathode material of a spent lithium cobaltate battery, and calcining the mixture at a high temperature, leaching with water, and filtering to obtain a cobalt element and a lithium element. Sulfate solution.
  2. 根据权利要求1所述的从失效钴酸锂电池正极材料中回收钴和锂的方法，其特征在于，其具体包括下述步骤：The method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery according to claim 1, wherein the method comprises the following steps:
    (1)将硫酸氢钠与失效钴酸锂电池正极材料混合均匀得到混合料，控制钴元素与硫元素的摩尔比为1：3；(1) mixing sodium hydrogen sulfate with the lithium cobalt oxide battery cathode material to obtain a mixture, controlling the molar ratio of cobalt to sulfur is 1:3;
    (2)将混合料置于200℃～600℃条件下焙烧5min～40min得焙料；(2) baking the mixture at 200 ° C ~ 600 ° C for 5 min ~ 40 min to obtain the baking;
    (3)取出焙料后加水浸出，浸出温度为20℃～90℃，浸出时间为4～6h；(3) After taking out the baking material, adding water to leaching, the leaching temperature is 20 ° C ~ 90 ° C, the leaching time is 4 ~ 6 h;
    (4)过滤液固分离，滤液即为包含钴元素和锂元素的硫酸盐溶液。(4) The filtrate is solid-separated, and the filtrate is a sulfate solution containing a cobalt element and a lithium element.
  3. 根据权利要求1所述的从失效钴酸锂电池正极材料中回收钴和锂的方法，其特征在于，所述的步骤3)中水与焙料的质量比为40～80：1。 The method for recovering cobalt and lithium from a cathode material of a spent lithium cobaltate battery according to claim 1, wherein the mass ratio of water to the binder in the step 3) is 40 to 80:1.
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