CN115961141A - Eutectic solvent and preparation method and application thereof - Google Patents
Eutectic solvent and preparation method and application thereof Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及湿法冶金和二次资源综合回收技术领域，特别涉及一种低共熔溶剂及其制备方法和应用。The invention relates to the technical field of hydrometallurgy and comprehensive recovery of secondary resources, in particular to a deep eutectic solvent and its preparation method and application.
背景技术Background technique
近年来，特别是“双碳”目标提出以来，基于能源可持续发展及安全的迫切需求，新能源汽车、电子产品等产业的迅猛发展，我国锂离子电池的需求量也显著提升。然而，锂离子电池的使用寿命为3～6年，据预测，2023年我国将会产生283亿只废旧锂离子电池，废旧锂离子电池带来的环境污染和资源浪费问题日益严重。In recent years, especially since the "dual carbon" goal was put forward, based on the urgent need for sustainable energy development and safety, and the rapid development of new energy vehicles, electronic products and other industries, the demand for lithium-ion batteries in my country has also increased significantly. However, the service life of lithium-ion batteries is 3 to 6 years. It is predicted that 28.3 billion waste lithium-ion batteries will be produced in my country in 2023. Environmental pollution and resource waste caused by waste lithium-ion batteries are becoming increasingly serious.
目前，对于废旧锂离子电池的研究受到广泛的关注。国内外学者已开展了锂电池正极金属材料回收方法的研究，主要有火法、湿法、生物法等。火法工艺存在着操作温度高、成本高、以及产生有害废气等缺点，目前主要在欧美等发达国家应用。湿法工艺是我国处理废旧锂电池的主流工艺，主要采用强酸强碱等浸出剂提取正极材料中的有价组分，虽然回收成本、回收金属纯度以及回收率能得到有效解决，但是仍存在使用强酸强碱造成设备损坏率高、酸碱废酸污染等问题。At present, the research on spent lithium-ion batteries has received extensive attention. Scholars at home and abroad have carried out research on the recovery methods of lithium battery cathode metal materials, mainly including fire method, wet method, biological method and so on. The pyrotechnic process has disadvantages such as high operating temperature, high cost, and harmful waste gas, and is currently mainly used in developed countries such as Europe and the United States. The wet process is the mainstream process for treating waste lithium batteries in my country. It mainly uses leaching agents such as strong acid and strong alkali to extract valuable components in positive electrode materials. Although the recovery cost, recovery metal purity and recovery rate can be effectively solved, there are still problems Strong acid and strong alkali cause problems such as high equipment damage rate, acid-base waste acid pollution and so on.
低共熔溶剂是指由一定化学计量比的氢键受体和氢键给体组合而成的两组分或三组分低共熔混合物，具有溶解性优良、制备简单、不易挥发等优点，目前已被研究应用于电催化、金属去腐蚀、有机合成、材料制备等诸多领域。Deep eutectic solvent refers to a two-component or three-component deep eutectic mixture composed of a certain stoichiometric ratio of hydrogen bond acceptors and hydrogen bond donors. It has the advantages of excellent solubility, simple preparation, and low volatility. At present, it has been studied and applied in many fields such as electrocatalysis, metal corrosion removal, organic synthesis, and material preparation.
申请号CN202210458210.X的专利，公布了一种由氢键受体(甜菜碱、硫代甜菜碱和盐酸甜菜碱中的至少一种)和氢键供体(乙醇、乙二醇和聚乙二醇中的至少一种；柠檬酸、甲酸、对甲苯磺酸、草酸、丙二酸和戊二酸中的至少一种)制备的低共熔溶剂，其中硫代甜菜碱与乙二醇、硫代甜菜碱与聚乙二醇、硫代甜菜碱与柠檬酸组合制备的低共熔溶剂对废旧锂电池三元正极材料中有价金属具有较优的浸出效果。申请号CN202111111233.5的专利，公布了一种由氢键受体(氯化胆碱)和氢键供体(对甲苯磺酸、十二烷基苯磺酸、甲磺酸、氨基磺酸中的至少一种)制备的低共熔溶剂，该低共熔溶剂对废旧锂电池三元正极材料中有价金属具有较优的浸出效果。但开发新型低共熔溶剂实现废旧锂电池三元正极材料中有价金属绿色高效回收，对锂电池行业可持续发展仍具有重要意义。The patent of application number CN202210458210.X discloses a hydrogen bond acceptor (at least one of betaine, thiobetaine and betaine hydrochloride) and a hydrogen bond donor (ethanol, ethylene glycol and polyethylene glycol) at least one of citric acid, formic acid, p-toluenesulfonic acid, oxalic acid, malonic acid and glutaric acid) prepared deep eutectic solvent, wherein thiobetaine and ethylene glycol, thio The deep eutectic solvent prepared by the combination of betaine and polyethylene glycol, thiobetaine and citric acid has a better leaching effect on the valuable metals in the ternary cathode materials of spent lithium batteries. Patent application number CN202111111233.5 discloses a hydrogen bond acceptor (choline chloride) and a hydrogen bond donor (p-toluenesulfonic acid, dodecylbenzenesulfonic acid, methanesulfonic acid, sulfamic acid) At least one of) prepared deep eutectic solvent, the deep eutectic solvent has a better leaching effect on valuable metals in waste lithium battery ternary positive electrode materials. However, the development of new deep eutectic solvents to realize the green and efficient recovery of valuable metals in the ternary cathode materials of waste lithium batteries is still of great significance to the sustainable development of the lithium battery industry.
发明内容Contents of the invention
本发明的目的在于提供一种低共熔溶剂及其制备方法和应用。通过以盐酸胍、乙二醇和有机酸配置的低共熔溶剂体系，高效地浸出废旧锂电池三元正极材料中的锂、钴、镍、锰。The object of the present invention is to provide a kind of deep eutectic solvent and its preparation method and application. Lithium, cobalt, nickel and manganese in waste lithium battery ternary cathode materials are efficiently leached through a deep eutectic solvent system configured with guanidine hydrochloride, ethylene glycol and organic acids.
为实现上述目的，本发明提供了如下技术方案：To achieve the above object, the present invention provides the following technical solutions:
本发明技术方案之一：提供一种低共熔溶剂，由盐酸胍、乙二醇和有机酸组成；所述有机酸为乙醇酸、苹果酸或乳酸中至少一种。One of the technical solutions of the present invention: a deep eutectic solvent is provided, which is composed of guanidine hydrochloride, ethylene glycol and an organic acid; the organic acid is at least one of glycolic acid, malic acid or lactic acid.
优选地，所述盐酸胍、乙二醇和有机酸的摩尔比为1:(1～2):(1～3)。Preferably, the molar ratio of the guanidine hydrochloride, ethylene glycol and organic acid is 1:(1-2):(1-3).
本发明技术方案之二：提供一种上述低共熔溶剂的制备方法，包括以下步骤：将盐酸胍、乙二醇和有机酸混合，搅拌后制得所述低共熔溶剂。The second technical solution of the present invention provides a method for preparing the above-mentioned deep eutectic solvent, comprising the following steps: mixing guanidine hydrochloride, ethylene glycol and an organic acid, and stirring to prepare the deep eutectic solvent.
优选地，所述搅拌的温度为80～90℃，时间为1～2h。Preferably, the stirring temperature is 80-90° C., and the stirring time is 1-2 hours.
本发明技术方案之三：提供一种上述低共熔溶剂在回收废旧锂电池三元正极材料中锂、钴、镍、锰的应用。The third technical solution of the present invention is to provide an application of the above-mentioned deep eutectic solvent in the recycling of lithium, cobalt, nickel and manganese in the ternary positive electrode materials of waste lithium batteries.
回收方法包括以下步骤：The recycling method includes the following steps:
将所述低共熔溶剂与所述三元锂电池正极材料混合，浸出，固液分离，得到含锂、钴、镍、锰的溶液。The deep eutectic solvent is mixed with the positive electrode material of the ternary lithium battery, leached, and solid-liquid separated to obtain a solution containing lithium, cobalt, nickel, and manganese.
优选地，所述废旧锂电池三元正极材料与所述低共熔溶剂的质量体积比为1g:(40～100)mL。Preferably, the mass volume ratio of the waste lithium battery ternary positive electrode material to the deep eutectic solvent is 1g:(40-100)mL.
优选地，所述浸出的温度为90～120℃，时间为2～6h。Preferably, the temperature of the leaching is 90-120° C., and the time is 2-6 hours.
本发明的有益技术效果如下：Beneficial technical effect of the present invention is as follows:
本发明利用盐酸胍、乙二醇和有机酸配置的低共熔溶剂体系，具有粘度低(粘度高不利于锂电池正极材料在低共熔溶剂中的分散和溶解，导致浸出时间长，浸出率偏低)、成本低等优点。利用该体系浸出三元锂电池正极材料中的锂、钴、镍、锰，具有浸出温度低、浸出时间短，锂、钴、镍、锰浸出效率高的优势。The present invention utilizes the deep eutectic solvent system configured by guanidine hydrochloride, ethylene glycol and organic acid to have low viscosity (high viscosity is not conducive to the dispersion and dissolution of lithium battery cathode materials in the deep eutectic solvent, resulting in long leaching time and partial leaching rate. low), low cost and other advantages. Using this system to leach lithium, cobalt, nickel, and manganese in the positive electrode material of the ternary lithium battery has the advantages of low leaching temperature, short leaching time, and high leaching efficiency of lithium, cobalt, nickel, and manganese.
附图说明Description of drawings
图1为本发明利用低共熔溶剂回收废旧锂电池三元正极材料锂、钴、镍、锰的工艺流程示意图；Fig. 1 is the schematic diagram of the technological process of utilizing the deep eutectic solvent to reclaim the ternary positive electrode material lithium, cobalt, nickel and manganese of the waste lithium battery in the present invention;
图2为浸出时间对实施例1制备的低共熔溶剂浸出锂、钴、镍、锰的影响；Fig. 2 is the impact of leaching time on the deep eutectic solvent leaching lithium, cobalt, nickel, manganese prepared by embodiment 1;
图3为浸出温度对实施例1制备的低共熔溶剂浸出锂、钴、镍、锰的影响；Fig. 3 is the influence of leaching temperature on the deep eutectic solvent leaching lithium, cobalt, nickel, manganese prepared in embodiment 1;
图4为浸出液固比对实施例1制备的低共熔溶剂浸出锂、钴、镍、锰的影响。Figure 4 is the effect of the leaching liquid-solid ratio on the leaching of lithium, cobalt, nickel and manganese by the deep eutectic solvent prepared in Example 1.
具体实施方式Detailed ways
现详细说明本发明的多种示例性实施方式，该详细说明不应认为是对本发明的限制，而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。应理解本发明中所述的术语仅仅是为描述特别的实施方式，并非用于限制本发明。Various exemplary embodiments of the present invention will now be described in detail. The detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features and embodiments of the present invention. It should be understood that the terminology described in the present invention is only used to describe specific embodiments, and is not used to limit the present invention.
另外，对于本发明中的数值范围，应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值，以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。In addition, regarding the numerical ranges in the present invention, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Any stated value or intervening value in a stated range, and each smaller range between any other stated value or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded from the range.
除非另有说明，否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料，但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only the preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等，均为开放性的用语，即意指包含但不限于。As used herein, "comprising", "comprising", "having", "comprising" and so on are all open terms, meaning including but not limited to.
本发明利用低共熔溶剂回收废旧锂电池三元正极材料锂、钴、镍、锰的工艺流程示意图见图1。The present invention uses a deep eutectic solvent to recover the waste lithium battery ternary positive electrode material lithium, cobalt, nickel and manganese for a schematic diagram of the process flow shown in Figure 1.
实施例1Example 1
(1)低共熔溶剂的制备：将盐酸胍、乙二醇及乳酸按1:1:2的摩尔比混合，采用水浴加热的方式在70℃下混合搅拌1h，获得澄清透明溶液，即为低共熔溶剂(粘度为130mPa.s)。(1) Preparation of deep eutectic solvent: Mix guanidine hydrochloride, ethylene glycol and lactic acid at a molar ratio of 1:1:2, and heat them in a water bath at 70°C for 1 hour to obtain a clear and transparent solution, which is Deep eutectic solvent (viscosity 130mPa.s).
(2)废旧锂电池三元正极材料浸出：将废旧锂电池三元正极材料加入到步骤(1)制备成的低共熔溶剂中，所加的废旧锂电池三元正极材料与低共熔溶剂质量体积比为1g:50mL，在90℃恒温搅拌浸出3h。(2) Leaching of the waste lithium battery ternary positive electrode material: the waste lithium battery ternary positive electrode material is added to the deep eutectic solvent prepared in step (1), the added waste lithium battery ternary positive electrode material and the deep eutectic solvent The mass volume ratio is 1g:50mL, and it is stirred and leached at a constant temperature of 90°C for 3h.
(3)将步骤(2)所得浸出液体系离心，离心速率为4000rpm。(3) Centrifuge the leaching liquid system obtained in step (2), and the centrifugation speed is 4000rpm.
(4)对步骤(3)离心得到的溶液进行锂和锰含量检测，计算得到锂、钴、镍、锰的浸出率分别为92.6％、89.6％、89.7％、88.4％。(4) Lithium and manganese content detection is carried out to the solution obtained by step (3) centrifugation, and the calculated leaching rates of lithium, cobalt, nickel, and manganese are 92.6%, 89.6%, 89.7%, and 88.4%, respectively.
实施例2Example 2
(1)低共熔溶剂的制备：将盐酸胍、乙二醇及乙醇酸按1:1:2的摩尔比混合，采用水浴加热的方式在80℃下混合搅拌2h，获得澄清透明溶液，即为低共熔溶剂(粘度为112mPa.s)。(1) Preparation of deep eutectic solvent: Mix guanidine hydrochloride, ethylene glycol and glycolic acid at a molar ratio of 1:1:2, and heat them in a water bath at 80°C for 2 hours to obtain a clear and transparent solution, namely It is a deep eutectic solvent (viscosity of 112mPa.s).
(2)三元锂电池正极材料浸出：将废旧锂电池三元正极材料加入到步骤(1)制备成的低共熔溶剂中，所加的废旧锂电池三元正极材料与低共熔溶剂质量体积比为1g:60mL，在100℃恒温搅拌浸出4h。(2) Leaching of ternary lithium battery cathode material: Add waste lithium battery ternary cathode material to the deep eutectic solvent prepared in step (1), the added waste lithium battery ternary cathode material and deep eutectic solvent mass The volume ratio is 1g:60mL, and it is stirred and leached at a constant temperature of 100°C for 4h.
(3)将步骤(2)所得浸出液体系离心，离心速率为4000rpm。(3) Centrifuge the leaching liquid system obtained in step (2), and the centrifugation speed is 4000rpm.
(4)对步骤(3)离心得到的溶液进行锂、钴、镍、锰含量检测，计算得到锂、钴、镍、锰的浸出率分别为91.4％、85.2％、83.1％、79.6％。(4) Lithium, cobalt, nickel, and manganese are detected in the centrifuged solution obtained in step (3), and the calculated leaching rates of lithium, cobalt, nickel, and manganese are 91.4%, 85.2%, 83.1%, and 79.6%, respectively.
实施例3Example 3
(1)低共熔溶剂的制备：将盐酸胍、乙二醇及乳酸按1:2:3的摩尔比混合，采用水浴加热的方式在80℃下混合搅拌1h，获得澄清透明溶液，即为低共熔溶剂(粘度为176mPa.s)。(1) Preparation of deep eutectic solvent: Mix guanidine hydrochloride, ethylene glycol and lactic acid in a molar ratio of 1:2:3, and heat them in a water bath at 80°C for 1 hour to obtain a clear and transparent solution, which is Deep eutectic solvent (viscosity of 176mPa.s).
(2)三元锂电池正极材料浸出：将废旧锂电池三元正极材料加入到步骤(1)制备成的低共熔溶剂中，所加的废旧锂电池三元正极材料与低共熔溶剂质量体积比为1g:60mL，在90℃恒温搅拌浸出4h。(2) Leaching of ternary lithium battery cathode material: Add waste lithium battery ternary cathode material to the deep eutectic solvent prepared in step (1), the added waste lithium battery ternary cathode material and deep eutectic solvent mass The volume ratio is 1g:60mL, and it is stirred and leached at a constant temperature of 90°C for 4h.
(3)将步骤(2)所得浸出液体系离心，离心速率为4000rpm。(3) Centrifuge the leaching liquid system obtained in step (2), and the centrifugation speed is 4000rpm.
(4)对步骤(3)离心得到的溶液进行锂、钴、镍、锰含量检测，计算得到锂、钴、镍、锰的浸出率分别为98.8％、92.8％、95.5％、91.3％。(4) detect the content of lithium, cobalt, nickel and manganese in the centrifuged solution obtained in step (3), and calculate the leaching rates of lithium, cobalt, nickel and manganese to be 98.8%, 92.8%, 95.5%, 91.3% respectively.
实施例4Example 4
(1)低共熔溶剂的制备：将盐酸胍、乙二醇及苹果酸按1:2:1的摩尔比混合，采用水浴加热的方式在90℃下混合搅拌2h，获得澄清透明溶液，即为低共熔溶剂(粘度为1862mPa.s)。(1) Preparation of deep eutectic solvent: Mix guanidine hydrochloride, ethylene glycol, and malic acid in a molar ratio of 1:2:1, and heat them in a water bath at 90°C for 2 hours to obtain a clear and transparent solution, namely It is a deep eutectic solvent (viscosity is 1862mPa.s).
(2)三元锂电池正极材料浸出：将废旧锂电池三元正极材料加入到步骤(1)制备成的低共熔溶剂中，所加的废旧锂电池三元正极材料与低共熔溶剂质量体积比为1g:100mL，在120℃恒温搅拌浸出6h。(2) Leaching of ternary lithium battery cathode material: Add waste lithium battery ternary cathode material to the deep eutectic solvent prepared in step (1), the added waste lithium battery ternary cathode material and deep eutectic solvent mass The volume ratio is 1g:100mL, and it is stirred and leached at a constant temperature of 120°C for 6h.
(3)将步骤(2)所得浸出液体系离心，离心速率为4000rpm。(3) Centrifuge the leaching liquid system obtained in step (2), and the centrifugation speed is 4000rpm.
(4)对步骤(3)离心得到的溶液进行锂、钴、镍、锰含量检测，计算得到锂、钴、镍、锰的浸出率分别为91.1％、82.3％、80.4％、79.6％。(4) Lithium, cobalt, nickel, manganese content detection is carried out to the solution that step (3) centrifugally obtains, and the leaching rate that calculates lithium, cobalt, nickel, manganese is respectively 91.1%, 82.3%, 80.4%, 79.6%.
实施例5Example 5
(1)低共熔溶剂的制备：将盐酸胍、乙二醇、乳酸、乙醇酸按1:2:1:1的摩尔比混合，采用水浴加热的方式在80℃下混合搅拌2h，获得澄清透明溶液，即为低共熔溶剂(粘度为92mPa.s)。(1) Preparation of deep eutectic solvent: Mix guanidine hydrochloride, ethylene glycol, lactic acid, and glycolic acid in a molar ratio of 1:2:1:1, and heat them in a water bath at 80°C for 2 hours to obtain clarification The transparent solution is a deep eutectic solvent (viscosity is 92mPa.s).
(2)三元锂电池正极材料浸出：将废旧锂电池三元正极材料加入到步骤(1)制备成的低共熔溶剂中，所加的废旧锂电池三元正极材料与低共熔溶剂质量体积比为1g:100mL，在110℃恒温搅拌浸出4h。(2) Leaching of ternary lithium battery cathode material: Add waste lithium battery ternary cathode material to the deep eutectic solvent prepared in step (1), the added waste lithium battery ternary cathode material and deep eutectic solvent mass The volume ratio is 1g:100mL, and it is stirred and leached at a constant temperature of 110°C for 4h.
(3)将步骤(2)所得浸出液体系离心，离心速率为4000rpm。(3) Centrifuge the leaching liquid system obtained in step (2), and the centrifugation speed is 4000rpm.
(4)对步骤(3)离心得到的溶液进行锂、钴、镍、锰含量检测，计算得到锂、钴、镍、锰的浸出率分别为99.2％、94.6％、94.8％、90.2％。(4) Lithium, cobalt, nickel, manganese content detection is carried out to the solution that step (3) centrifugally obtains, and the leaching rate that calculates lithium, cobalt, nickel, manganese is respectively 99.2%, 94.6%, 94.8%, 90.2%.
考查浸出时间、浸出温度及浸出液固比对本发明实施例1制备的低共熔溶剂浸出锂、钴、镍、锰的浸出率的影响；Investigate the influence of leaching time, leaching temperature and leaching liquid-solid ratio on the leaching rate of deep eutectic solvent leaching lithium, cobalt, nickel, manganese prepared by the embodiment of the present invention 1;
将废旧锂电池三元正极材料与低共熔溶剂按照质量体积比为1:20g/mL，并在90℃下恒温搅拌浸出时，考察浸出时间对锂、钴、镍、锰的浸出率的影响，结果见图2；When the waste lithium battery ternary positive electrode material and the deep eutectic solvent were leached at a mass volume ratio of 1:20g/mL, and stirred and leached at a constant temperature at 90°C, the effect of leaching time on the leaching rate of lithium, cobalt, nickel, and manganese was investigated. , the results are shown in Figure 2;
将废旧锂电池三元正极材料与低共熔溶剂按照质量体积比为1:20g/mL，恒温搅拌浸出2h，考察浸出温度对锂、钴、镍、锰的浸出率的影响，结果见图3；The waste lithium battery ternary positive electrode material and the deep eutectic solvent were leached at a mass volume ratio of 1:20g/mL, stirred and leached at a constant temperature for 2 hours, and the effect of leaching temperature on the leaching rate of lithium, cobalt, nickel, and manganese was investigated. The results are shown in Figure 3 ;
将废旧锂电池三元正极材料与低共熔溶剂按照一定质量体积比90℃下恒温搅拌浸出2h，考察浸出液固体积质量比对锂、钴、镍、锰的浸出率的影响，结果见图4。The waste lithium battery ternary positive electrode material and the deep eutectic solvent were leached at a constant temperature of 90°C for 2 hours according to a certain mass-volume ratio, and the influence of the volume-to-mass ratio of the leaching liquid to solid on the leaching rate of lithium, cobalt, nickel, and manganese was investigated. The results are shown in Figure 4 .
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。The above-mentioned embodiments are only to describe the preferred mode of the present invention, not to limit the scope of the present invention. Without departing from the design spirit of the present invention, those skilled in the art may make various Variations and improvements should fall within the scope of protection defined by the claims of the present invention.
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