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Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon residues

A lithium-ion battery and combined treatment technology, applied in water/sewage treatment, water/sludge/sewage treatment, chemical instruments and methods, etc., can solve the problem of low purity of negative electrode materials, poor control of the ratio, and lithium-ion battery production. Difficulties and other problems, to achieve the effect of creating industrial value, reducing processing costs, and realizing utilization

Active Publication Date: 2021-01-26
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It should be pointed out that the purity of the negative electrode material obtained by this method is not high, and the ratio between the active material, conductive agent and thickener is not well controlled, which makes the production of lithium-ion batteries difficult.

Method used

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  • Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon residues
  • Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon residues
  • Combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Weigh 20 g of the crushed and screened waste lithium-ion battery carbon slag and put it into a planetary ball mill for activation for 7 hours with a ball-to-material ratio of 12:1 and a rotational speed of 300 r / min.

[0041]The activated material is placed in a hydrothermal kettle with fluosilicic acid wastewater (H 2 SiF 6 39.83 wt %, HF 2.16 wt %, HCl 0.22 wt %, H 2 O is 57.7wt%, etc.) for the reaction, wherein the liquid-solid mass ratio is 8:1, and the temperature is 200°C for 10h. The filtrate obtained after liquid-solid separation (H 2 SiF 6 41.20%wt, HF 1.56%wt, HCl 0.21%wt, H 2 O is 56.8%wt, etc.) to make white carbon black, and the material powder obtained by solid-liquid separation is washed with water and dried.

[0042] Specifically, the filtrate can be placed in a stirring reactor, pre-heated in a constant temperature water bath to 95°C, then add aluminum hydroxide according to 0.9 times the theoretical amount, stir and react for 45 minutes at a deter...

Embodiment 2

[0046] Weigh 100 g of the crushed and screened waste lithium-ion battery carbon slag and put it into a planetary ball mill for activation for 3 hours with a ball-to-material ratio of 20:1 and a rotational speed of 200 r / min.

[0047] The activated material is placed in a hydrothermal kettle with fluosilicic acid wastewater (H 2 SiF 6 32.17wt%, HF 1.75wt%, HCl 0.18wt%, H 2 O is 65.82wt%, etc.) for the reaction, wherein the liquid-solid ratio is 12:1, and the temperature is 180°C for 8 hours. The filtrate obtained after liquid-solid separation (H 2 SiF 6 33.17%wt, HF 1.36%wt, HCl 0.18%wt, H 2 O is 65.29%wt, etc.) to make white carbon black, and the material powder obtained by solid-liquid separation is washed with water and dried. Specifically, the filtrate can be placed in a stirring reactor, pre-heated in a constant temperature water bath to 85°C, then add aluminum hydroxide according to 1.1 times the theoretical amount, stir and react for 30 minutes at a determined react...

Embodiment 3

[0051] Weigh 70 g of the crushed and screened waste lithium-ion battery carbon slag and put it into a planetary ball mill for activation for 10 h with a ball-to-material ratio of 6:1 and a rotational speed of 400 r / min.

[0052] The activated material is placed in a hydrothermal kettle with fluosilicic acid wastewater (H 2 SiF 6 23.79%wt, HF 1.29%wt, HCl 0.13%wt, H 2 O is 74.75%wt, etc.) for the reaction, wherein the liquid-solid ratio is 16:1, and the temperature is 220°C for 12h. The filtrate obtained after liquid-solid separation (H 2 SiF 6 24.61%wt, HF 1.00%wt, HCl 0.13%wt, H 2 O is 74.37%wt, etc.) to make white carbon black, and the material powder obtained by solid-liquid separation is washed with water and dried. Specifically, the filtrate can be placed in a stirring reactor, pre-heated in a constant temperature water bath to 100°C, then add aluminum hydroxide according to 0.7 times the theoretical amount, stir and react for 50 minutes at a determined reaction temp...

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Abstract

The invention relates to a fluosilicic acid wastewater and waste lithium ion battery carbon slag combined treatment method, which comprises the following steps: crushing and screening to-be-treated waste lithium ion battery carbon residues to obtain carbon residue powder; carrying out mechanical activation on the obtained carbon residue powder under the condition of 100-500 r / min to obtain an activated material; mixing the obtained activated material with fluosilicic acid wastewater according to a mass ratio of 1:4-16, reacting in a reaction kettle at 100-220 DEG C for 6-12 h, cooling, and carrying out solid-liquid separation to obtain a solid phase substance and a leachate; and finally, carrying out normal-pressure acid leaching on the solid-phase substance obtained in the step S3 for 2-6hours at a temperature of 30-90 DEG C, carrying out solid-liquid separation, and sequentially washing and drying to obtain the graphite powder with the purity not lower than 99.9 wt%. According to the method, the waste battery carbon residues from which valuable metals are extracted can be converted into high-purity graphite powder, impurities silicon in the carbon residues are enriched and impurities in the ink are activated by circulating fluosilicic acid wastewater, and the method is suitable for innocent treatment of fluosilicic acid and industrial cleaning treatment and high-valued utilization of waste lithium ion battery negative electrode materials.

Description

technical field [0001] The invention relates to a combined treatment method of fluosilicic acid wastewater and waste lithium ion battery carbon slag. Background technique [0002] Chemical power sources are more and more widely used in industrial production and daily life, and play a leading role in electronic products such as mobile phones and notebook computers. At present, they are also attracting attention in the field of new energy vehicles, especially the new Energy-powered vehicles and hybrid vehicles have adopted lithium-ion batteries as the main power source, and the advantages of good electrical conductivity and large specific surface area make graphite an important active material and additive in this field. During the service cycle of lithium-ion batteries, it is inevitable to produce a large number of waste materials, defective products, and retired products. The emergence of these wastes has brought a series of new problems such as resource waste and environmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205C01B32/215C02F1/00C02F101/14
CPCC01B32/205C01B32/215C02F1/00C02F2101/14
Inventor 仲奇凡肖劲叶圣超刘晋麟姚桢唐雷诸向东
Owner CENT SOUTH UNIV