Method for synthesizing zinc-doped ternary material precursor from waste lithium battery through recovery

A technology for waste lithium batteries and ternary materials, applied in the field of ternary material precursors, can solve the problem of inability to remove impurity metals, and achieve the effect of increasing added value and reducing process flow

Active Publication Date: 2018-06-01
TIANQI LITHIUM CORP
9 Cites 6 Cited by

AI-Extracted Technical Summary

Problems solved by technology

This method uses a high-temperature roasting method to recover the positive electrode material, which cannot remove impurity...
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Abstract

A waste lithium battery contains Zn, and after a ternary precursor is doped with Zn, interface stability of an electrode/electrolyte and the structural stability at high voltage can be improved, increase of charge transfer resistance during the cycle is inhibited, and Li<+> diffusion is facilitated. Therefore, the invention discloses a method for synthesizing a zinc-doped ternary material precursor from the waste lithium battery through recovery. The method comprises the following steps: removing doping elements except Zn from an acid leaching solution of a waste lithium battery cell crushingmaterial, adjusting the content of Ni, Co and Mn, synthesizing a doping material with a coprecipitation method, and performing precipitation, washing and drying to obtain the single zinc-doped ternarymaterial precursor. The single zinc-doped ternary material precursor is obtained while the ternary precursor is synthesized from the waste lithium battery through recovery; the method has the advantages of being simple in process flow, good in doping effect, cost-saving and capable of significantly improving electrochemical performance of the precursor and the like.

Application Domain

Waste accumulators reclaimingBattery recycling

Technology Topic

Structural stabilityCoprecipitation +8

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  • Method for synthesizing zinc-doped ternary material precursor from waste lithium battery through recovery
  • Method for synthesizing zinc-doped ternary material precursor from waste lithium battery through recovery
  • Method for synthesizing zinc-doped ternary material precursor from waste lithium battery through recovery

Examples

  • Experimental program(3)

Example Embodiment

[0042] Example 1
[0043] A method for recycling and synthesizing zinc-doped ternary material precursors from waste lithium batteries, comprising the following steps:
[0044] 1. The composition of the acid leaching solution of the cathode material of the waste lithium battery is shown in Table 1. Adjust the pH to 4 with 5% NaOH solution, add iron powder with 3 times of Cu content, stir at 150rpm for 0.5h, and then add 1.2% of the iron powder. The other doping elements can be removed after stirring and reacting at the same rate for 0.5-1 h.
[0045] Table 1 (unit: g/L)
[0046] Mn
[0047] 2. The composition of the acid leaching solution after removing other doping elements is shown in Table 2. Take 200mL of acid leaching solution after impurity removal, add 8.15g NiSO 4.6H 2 O and 5.58g MnSO 4.H 2 O, prepared into a solution with a molar ratio of Ni, Co, and Mn of 1:1:1.
[0048] Table 2 (unit: g/L)
[0049] Mn
[0050] 3. Adjust the acid leaching solution of Ni, Co, Mn molar ratio in step 2 at 40 ° C, under the condition of stirring speed 400rpm, with the complexing agent of concentration 0.5mol/L, the precipitating agent of 3mol/L under nitrogen atmosphere with The reaction was carried out at pH 10.9.
[0051] 4. The obtained precipitate is washed and dried at 100° C. to obtain a Zn-doped ternary precursor.
[0052] The undoped ternary material precursor and the Zn-doped ternary material precursor in this example were mixed with Li respectively. 2 CO 3 It was sintered into a positive electrode material, and the electrochemical properties were tested. The relevant data are shown in Table 3.
[0053] table 3
[0054]

Example Embodiment

[0055] Example 2
[0056] A method for recycling and synthesizing zinc-doped ternary material precursors from waste lithium batteries, comprising the following steps:
[0057] 1. The composition of the acid leaching solution of the cathode material of the waste lithium battery is shown in Table 4. Adjust the pH to 4 with 5% NaOH solution, add iron powder with 3 times of Cu content, stir at 150rpm for 0.5h, and then add 1.2% of the iron powder. The other doping elements can be removed after stirring and reacting at the same rate for 0.5 h.
[0058] Table 4 (unit: g/L)
[0059] Mn
[0060] 2. The composition of the acid leaching solution after removing other doping elements is shown in Table 5. Take 200mL of acid leaching solution after impurity removal, add 36.14g NiSO 4.6H 2 O and 11.58g MnSO 4.H 2 O, prepared into a solution with a molar ratio of Ni, Co, and Mn of 5:2:3.
[0061] Table 5 (unit: g/L)
[0062] Mn
[0063] 3. Adjust the acid leaching solution of Ni, Co, Mn molar ratio in step 2 at 50 ° C, under the condition of stirring speed 500rpm, with the complexing agent of concentration 0.6mol/L, the precipitating agent of 4mol/L under nitrogen atmosphere with The reaction was carried out at pH 11.0.
[0064] 4. The obtained precipitate is washed and dried at 100° C. to obtain a Zn-doped ternary precursor.
[0065] The undoped ternary material precursor and the Zn-doped ternary material precursor in this example were mixed with Li respectively. 2 CO 3 It was sintered into a cathode material, and the electrochemical properties were tested. The relevant data are shown in Table 6.
[0066] Table 6
[0067]

Example Embodiment

[0068] Example 3
[0069] A method for recycling and synthesizing zinc-doped ternary material precursors from waste lithium batteries, comprising the following steps:
[0070] 1. The composition of the acid leaching solution of the cathode material of the waste lithium battery is shown in Table 7. Adjust the pH to 5 with 5% NaOH solution, add iron powder with 4 times of Cu content, stir at 150rpm for 0.5h, and then add 1.4% of the iron powder. The other doping elements can be removed by stirring the reaction at the same rate.
[0071] Table 7 (unit: g/L)
[0072] Mn
[0073] 2. The composition of the acid leaching solution after removing other doping elements is shown in Table 8. Take 200mL of acid leaching solution after impurity removal, add 8.41g NiSO 4.6H 2 O, 6.08g MnSO 4.H 2 O and 0.1 g ZnSO 4 , prepared into a solution with a molar ratio of Ni, Co, and Mn of 1:1:1.
[0074] Table 8 (unit: g/L)
[0075]
[0076] 3. Adjust the acid leaching solution of Ni, Co, Mn molar ratio in step 2 at 60 ° C, under the condition of stirring speed 400rpm, with the complexing agent of concentration 0.6mol/L, the precipitating agent of 4mol/L under nitrogen atmosphere with The reaction was carried out at pH 11.1.
[0077] 4. The obtained precipitate is washed and dried at 100° C. to obtain a Zn-doped ternary precursor.
[0078] The undoped ternary material precursor and the Zn-doped ternary material precursor in this example were mixed with Li respectively. 2 CO 3 It was sintered into a positive electrode material, and the electrochemical properties were tested. The relevant data are shown in Table 9.
[0079] Table 9
[0080]
[0081] According to the test results of the above examples, the method of the present invention effectively removes other doping elements in the process of recycling waste lithium batteries, and obtains a single Zn-doped ternary material precursor, which is sintered into The positive electrode material significantly improves the electrochemical performance, increases the added value of recycled products, combines recycling and modified production, reduces the subsequent process flow, and saves costs.

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