废锂离子电池放电路径与评价研究

doi:10.11949/0438-1157.20230759

化工学报 ›› 2023, Vol. 74 ›› Issue (9): 3903-3911.DOI: 10.11949/0438-1157.20230759

废锂离子电池放电路径与评价研究

康飞¹^,²^,³(), 吕伟光²^,³, 巨锋⁴, 孙峙¹^,²^,³()

^1.中国科学院大学化学工程学院，北京 100049
^2.中国科学院过程工程研究所，北京 100190
^3.中国科学院化学化工科学数据中心，北京 100190
^4.河南巨山新能源科技有限公司，河南安阳 456463

收稿日期:2023-07-21 修回日期:2023-09-02 出版日期:2023-09-25 发布日期:2023-11-20
通讯作者: 孙峙
作者简介:康飞（1988—），男，博士研究生，助理研究员，kangfei0604@126.com
基金资助:
国家重点研发计划项目(2020YFC1909004);中国科学院化学化工科学数据中心能力建设项目(WX145XQ07-12);国家自然科学基金项目(51934006);浙江省科技计划项目(2022C03074)

Research on discharge path and evaluation of spent lithium-ion batteries

Fei KANG¹^,²^,³(), Weiguang LYU²^,³, Feng JU⁴, Zhi SUN¹^,²^,³()

^1.School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
^2.Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
^3.Chemistry & Chemical Engineering Data Center, Chinese Academy of Sciences, Beijing 100190, China
^4.Henan Jushan New Energy Technology Co. , Ltd. , Anyang 456463, Henan, China

Received:2023-07-21 Revised:2023-09-02 Online:2023-09-25 Published:2023-11-20
Contact: Zhi SUN

摘要/Abstract

摘要：

随着新能源汽车迅猛发展，废锂离子电池资源化回收受到广泛关注，放电是废锂离子电池循环利用过程的重要环节。当前主要采用氯化钠溶液浸泡放电，导致大量含重金属、高有机物废液排放，处理成本高，且存在严重的环境与安全隐患。系统研究了溶液处理过程不同放电介质对放电时间、气体产生、电解液泄漏、金属溶出等的影响，探明了气液固三相组成变化规律，并对锂离子电池的电量释放路径机制进行了探索，明确了放电过程资源环境安全评价与控制方法，进一步构建了本征安全的高效放电技术。发现以电解水为主伴随极少量电解液溶出的硫酸钠溶液最优，以电量释放路径为引导从源头上解决了溶液放电过程大量电解液泄漏以及重金属溶出等问题，为实现废锂离子电池高效循环利用提供了有效支撑。

关键词: 废锂离子电池, 放电路径, 电解, 腐蚀, 过程控制, 评价

Abstract:

With the rapid development of new energy vehicles, the recycling of spent lithium-ion batteries has received widespread attention. Discharge is an important step in the recycling process of spent lithium-ion batteries. At present, sodium chloride solution is mainly used to achieve discharge, which leads to the discharge of a large amount of waste liquid containing heavy metals and high organic matter, and will produce hydrogen, methane, etc., which has high treatment cost and serious environmental and safety risks. This study systematically studied the effects of different discharge media during solution treatment on discharge time, gas generation, electrolyte leakage, metal dissolution, etc., analyzed the change law of gas-liquid-solid three-phase composition, explored the discharge path mechanism of lithium-ion batteries, and clarified the evaluation and control methods of discharge process resources, environment, and safety. An intrinsically safe and efficient discharge technique is further constructed. It is found that the decrease of residual voltage of lithium-ion battery during chemical discharge is mainly caused by three paths: electrolytic water, electrolyte leakage and battery short circuit heat release. The positive and negative electrodes of lithium-ion batteries produce oxygen and hydrogen respectively during the early water electrolysis process, and then the competitive reaction of electrochemical corrosion or external short circuit of metal deposition occurs, and the metal dissolution and electrolyte leakage process occur successively. Through the evaluation of different discharge media, it is found that a sodium sulfate solution based on electrolyzed water with a very small amount of electrolyte dissolved out is optimal. Using the electricity release path as a guide, it solved the problems of large amounts of electrolyte leakage and heavy metal dissolution during the solution discharge process from the source. It provides effective support for the efficient recycling of spent lithium-ion batteries.

Key words: spent lithium-ion battery, discharge path, electrolysis, corrosion, process control, evaluate

中图分类号:

TQ 152

康飞, 吕伟光, 巨锋, 孙峙. 废锂离子电池放电路径与评价研究[J]. 化工学报, 2023, 74(9): 3903-3911.

Fei KANG, Weiguang LYU, Feng JU, Zhi SUN. Research on discharge path and evaluation of spent lithium-ion batteries[J]. CIESC Journal, 2023, 74(9): 3903-3911.

图/表 12

图1 锂电池放电过程示意图

Fig.1 Schematic diagram of the discharge process of lithium-ion battery

表1 18650圆柱锂电池主要成分

Table 1 Main components of 18650 cylindrical lithium-ion battery

碳钢外壳	正极材料	铝箔	负极材料	铜箔	其他
20.56%	35.90%	4.32%	17.83%	7.18%	14.21%

表2 正极可能发生的竞争性氧化反应及其理论电位

Table 2 Competitive oxidation reaction and theoretical potential of positive electrode

正极半反应	E⁰/V	编号
Fe(s) $⇌$ Fe²⁺(aq)+2e^–	0.45	(7)
Fe²⁺(aq) $⇌$ Fe³⁺(aq)+e^–	-0.77	(8)
Al(s) $⇌$ Al³⁺(aq)+3e^–	1.66	(9)
Cu(s) $⇌$ Cu²⁺(aq)+2e^–	-0.34	(10)
Ni(s) $⇌$ Ni²⁺(aq)+2e^–	0.26	(11)
Mn(s) $⇌$ Mn²⁺(aq)+2e^–	1.19	(12)
Mn²⁺(aq) $⇌$ Mn³⁺(aq)+e^-	-1.54	(13)
Mn²⁺(aq)+2H₂O(l) $⇌$ MnO₂(s)+4H⁺(aq)+2e^–	-1.22	(14)
2Mn²⁺(aq)+3H₂O(l) $⇌$ Mn₂O₃(s)+6H⁺(aq)+e^-	-1.49	(15)
Mn²⁺(aq)+4H₂O(l) $⇌$ MnO₄^-(aq)+8H⁺(aq)+5e^–	-1.51	(16)
2NH $4 +$ (aq) $⇌$ N₂H $5 +$ (aq)+3H⁺(aq)+2e^–	-1.28	(17)
2Cl^-(aq) $⇌$ Cl₂(g)+2e^-	-1.36	(18)
2CO $3 2 -$ (aq) $⇌$ 2CO₂(g)+O₂(g)+2e^–	-1.90~-1.95	(19)
4HCO $3 2 -$ (aq) $⇌$ 2H₂O(l)+4CO₂(g)+O₂(g)+4e^–	-1.45~-1.50	(20)

表2 正极可能发生的竞争性氧化反应及其理论电位

Table 2 Competitive oxidation reaction and theoretical potential of positive electrode

正极半反应	E⁰/V	编号
Fe(s) $⇌$ Fe²⁺(aq)+2e^–	0.45	(7)
Fe²⁺(aq) $⇌$ Fe³⁺(aq)+e^–	-0.77	(8)
Al(s) $⇌$ Al³⁺(aq)+3e^–	1.66	(9)
Cu(s) $⇌$ Cu²⁺(aq)+2e^–	-0.34	(10)
Ni(s) $⇌$ Ni²⁺(aq)+2e^–	0.26	(11)
Mn(s) $⇌$ Mn²⁺(aq)+2e^–	1.19	(12)
Mn²⁺(aq) $⇌$ Mn³⁺(aq)+e^-	-1.54	(13)
Mn²⁺(aq)+2H₂O(l) $⇌$ MnO₂(s)+4H⁺(aq)+2e^–	-1.22	(14)
2Mn²⁺(aq)+3H₂O(l) $⇌$ Mn₂O₃(s)+6H⁺(aq)+e^-	-1.49	(15)
Mn²⁺(aq)+4H₂O(l) $⇌$ MnO₄^-(aq)+8H⁺(aq)+5e^–	-1.51	(16)
2NH $4 +$ (aq) $⇌$ N₂H $5 +$ (aq)+3H⁺(aq)+2e^–	-1.28	(17)
2Cl^-(aq) $⇌$ Cl₂(g)+2e^-	-1.36	(18)
2CO $3 2 -$ (aq) $⇌$ 2CO₂(g)+O₂(g)+2e^–	-1.90~-1.95	(19)
4HCO $3 2 -$ (aq) $⇌$ 2H₂O(l)+4CO₂(g)+O₂(g)+4e^–	-1.45~-1.50	(20)

表3 负极可能发生的竞争性还原反应及其理论电位

Table 3 Competitive reduction reaction and theoretical potential of negative electrode

负极半反应	E⁰/V	编号
Na⁺(aq)+e^- $⇌$ Na(s)	-2.71	(21)
K⁺(aq)+e^- $⇌$ K(s)	-2.93	(22)
2NH $4 +$ (aq)+2e^-=H₂(g)+2NH₃(g)	≥-0.83	(23)
Fe³⁺(aq)+e^- $⇌$ Fe²⁺(aq)	0.77	(24)
Fe²⁺(aq)+2e^- $⇌$ Fe(s)	-0.45	(25)
Cu²⁺(aq)+2e^- $⇌$ Cu(s)	0.34	(26)
Mn²⁺(aq)+2e^- $⇌$ Mn(s)	-1.19	(27)
Ni²⁺(aq)+2e^- $⇌$ Ni(s)	-0.26	(28)
SO $4 2 -$ (aq)+4H⁺(aq)+2e^- $⇌$ H₂SO₃(aq)+H₂O(aq)	0.17	(29)
SO $4 2 -$ (aq)+H₂O(l)+2e^- $⇌$ SO $3 2 -$ (aq)+2OH^-(aq)	-0.93	(30)

表3 负极可能发生的竞争性还原反应及其理论电位

Table 3 Competitive reduction reaction and theoretical potential of negative electrode

负极半反应	E⁰/V	编号
Na⁺(aq)+e^- $⇌$ Na(s)	-2.71	(21)
K⁺(aq)+e^- $⇌$ K(s)	-2.93	(22)
2NH $4 +$ (aq)+2e^-=H₂(g)+2NH₃(g)	≥-0.83	(23)
Fe³⁺(aq)+e^- $⇌$ Fe²⁺(aq)	0.77	(24)
Fe²⁺(aq)+2e^- $⇌$ Fe(s)	-0.45	(25)
Cu²⁺(aq)+2e^- $⇌$ Cu(s)	0.34	(26)
Mn²⁺(aq)+2e^- $⇌$ Mn(s)	-1.19	(27)
Ni²⁺(aq)+2e^- $⇌$ Ni(s)	-0.26	(28)
SO $4 2 -$ (aq)+4H⁺(aq)+2e^- $⇌$ H₂SO₃(aq)+H₂O(aq)	0.17	(29)
SO $4 2 -$ (aq)+H₂O(l)+2e^- $⇌$ SO $3 2 -$ (aq)+2OH^-(aq)	-0.93	(30)

图2 不同溶液放电效率与参数变化

Fig.2 Discharge efficiency and parameter variation of different solutions

表4 不同放电溶液初始pH和电导率

Table 4 Initial pH and conductivity of different discharge solutions

放电溶液	初始pH	初始电导率/ (mS/cm)	放电溶液	初始pH	初始电导率/(mS/cm)
自来水	8.00	0.47	氯化铁	1.40	41.33
纯水	8.40	0.07	氯化铜	3.25	51.57
碳酸钠	11.32	48.73	氯化锰	5.22	39.03
碳酸钾	11.92	61.23	硫酸钠	5.73	45.43
碳酸氢钠	8.36	34.50	硫酸钾	6.43	50.73
碳酸铵	9.43	54.20	硫酸亚铁	3.53	22.43
氯化钠	6.57	74.23	硫酸铜	3.65	21.17
氯化钾	5.66	76.63	硫酸锰	3.87	20.57

图3 化学溶液放电路径

Fig.3 Discharge path of chemical solution

图4 四种放电溶液的GC-TCD气相色谱图

Fig.4 GC-TCD gas chromatograms of four discharge solutions

表5 不同放电溶液的气体成分与含量

Table 5 Gas composition and content of different discharge solutions

溶液	气体成分/%
溶液	氢气	二氧化碳	氧气	氮气	甲烷	一氧化碳	总计
纯水	60.75	0.82	6.62	24.59	0.55	0.02	99.97
自来水	71.22	1.83	2.23	18.95	0.54	0	99.87
碳酸钠	63.42	0	25.34	8.85	0	0	99.99
碳酸钾	65.54	0.02	26.29	6.42	0	0	100
碳酸氢钠	58.71	5.06	26.36	7.75	0.03	0	100
碳酸铵	71.64	0.52	11.54	12.84	0	0	100
氯化钠	64.99	0.13	3.07	24.86	0.25	0.01	100
氯化钾	78.90	0.08	1.34	15.28	0.28	0.01	100
氯化铁	80.50	0.67	1.47	12.68	1.17	0.02	99.92
氯化铜	79.42	1.42	0.39	13.51	1.50	0.03	99.91
氯化锰	76.62	1.18	1.62	15.54	0.68	0.04	99.86
硫酸钠	58.26	0.03	24.06	13.91	0	0	100
硫酸钾	55.70	0.04	21.18	18.17	0	0.02	100
硫酸亚铁	49.02	0.09	8.01	33.69	0.11	0.01	100
硫酸铜	36.10	0.65	9.71	41.55	0.72	0.06	99.98
硫酸锰	65.12	0.04	23.92	8.56	0.05	0.01	100

图5 三种不同放电溶液的沉淀物XRD谱图

Fig.5 XRD patterns of precipitates of three discharge solutions

表6 放电后固液两相金属总含量

Table 6 Total metal content in solid-liquid phase after discharge

溶液	金属含量/mg
溶液	Li	Co	Mn	Ni	Al	Fe	Cu	总和
纯水	3.43	0.09	1.81	11.16	21.39	684.07	1.39	723.34
自来水	2.22	0.22	2.67	7.51	79.51	926.80	0.24	1019.17
碳酸钠	0.15	0.00	0.00	0.00	42.64	0.88	0.40	44.07
碳酸钾	0.08	0.08	0.08	0.10	67.66	3.53	3.69	75.22
碳酸氢钠	0.15	0.16	0.00	8.40	0.24	4.24	7.76	20.95
碳酸铵	0.17	0.13	0.18	30.29	0.48	41.02	7.40	79.67
氯化钠	3.46	1.31	3.95	19.40	152.23	817.13	0.31	997.79
氯化钾	5.34	1.21	2.92	12.57	218.43	837.70	1.34	1079.51
氯化铁	6.10	0.39	17.69	42.65	330.05	—	2.06	398.94
氯化铜	4.18	0.36	8.32	40.51	288.05	2170.68	—	2512.10
氯化锰	3.25	0.74	—	18.66	173.76	1262.75	1.04	1460.20
硫酸钠	0.25	0.09	0.92	27.61	3.36	247.88	0.33	280.44
硫酸钾	1.19	0.05	4.87	17.44	179.58	1050.98	0.66	1254.77
硫酸亚铁	0.34	1.87	23.59	12.43	2.85	—	42.07	83.15
硫酸铜	0.08	0.56	83.79	32.08	50.97	2200.51	—	2367.99
硫酸锰	0.08	0.85	—	42.93	6.46	315.70	0.88	366.90

表7 不同溶液放电效果评价

Table 7 Evaluation of discharge effect of different solutions

溶液	评分
溶液	放电时间	金属总损失	总磷泄漏量	溶液TOC	溶液pH	气体危害等级	介质成本	总分
纯水	68	63	35	18	80	70	100	66.5
自来水	84	49	10	10	80	80	100	64.6
碳酸钠	10	97	99	83	80	90	67	70.0
碳酸钾	10	96	98	64	80	90	13	57.0
碳酸氢钠	10	98	99	97	90	80	77	73.6
碳酸铵	10	96	99	87	90	80	51	67.0
氯化钠	100	50	61	46	100	90	94	78.5
氯化钾	100	46	20	10	100	90	49	61.0
氯化铁	100	80	10	10	50	80	60	63.0
氯化铜	100	10	19	69	70	70	10	46.8
氯化锰	100	26	48	14	80	70	25	51.4
硫酸钠	98	85	99	100	100	90	94	94.3
硫酸钾	99	37	100	100	100	90	50	76.2
硫酸亚铁	100	86	100	100	60	90	94	92.8
硫酸铜	100	10	35	100	70	70	10	51.5
硫酸锰	89	81	98	100	70	90	42	78.2

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废锂离子电池放电路径与评价研究

Research on discharge path and evaluation of spent lithium-ion batteries

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