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Method for preparing graphene by taking graphite electrodes of waste lithium batteries as raw materials and recycling lithium

A technology for waste lithium batteries and graphite electrodes, which is applied in battery recycling, recycling by waste collectors, recycling technology, etc., can solve the problems of poor controllability, cumbersome process, and large amount of waste liquid, and achieve precise control and high efficiency. Value-added recovery technology and high production efficiency

Active Publication Date: 2018-11-06
高彪峰
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  • Abstract
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  • Application Information

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Problems solved by technology

With the vigorous promotion of global electric vehicles, a large number of lithium batteries will face the problem of being scrapped in the future. Although waste lithium batteries contain a lot of reusable resources, the recovery rate of waste batteries in my country is less than 2% (China Automotive Technology Research Center) , and mainly focus on the recovery of heavy metals from lithium battery electrode materials (CN101847763 A is a comprehensive recovery method for waste lithium iron phosphate batteries, CN 107069133 A is a method for recovering lithium in lithium battery negative electrode materials, CN 105355999 A is a kind of waste lithium batteries new recycling method)
[0004] At present, there are fewer reports on the preparation of graphene with graphite electrodes for waste lithium batteries. Among them, CN103508446A utilizes a method for preparing graphene by using graphite electrodes for waste lithium batteries to use ultrasonic stripping. The stripping efficiency of graphene is low, and the controllability is poor, and CN 102868006A A method for preparing graphene from waste lithium batteries is one or more of mechanical stripping, stripping agent stripping, and electrolytic stripping. Although the stripping efficiency is improved, more emphasis is placed on mechanical stripping
[0005] In the recycling process of graphite electrodes, the recycling of high value-added products graphene and lithium is rarely considered at the same time. CN105355996A is a method for separating lithium and graphite from waste lithium battery anode materials and recycling them, realizing lithium and graphite resources. However, in this method, lithium metal is leached, graphene is redox, the controllability of the method is poor, the process is cumbersome, and the amount of waste liquid is large.
The above problems limit the large-scale recycling and recycling of lithium batteries

Method used

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  • Method for preparing graphene by taking graphite electrodes of waste lithium batteries as raw materials and recycling lithium

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Embodiment 1: reactor structure

[0029] Such as figure 1 As shown, the reactor includes a central bottom plate 1, and an outer bottom plate 2 that rotates relative to the central bottom plate 1 is arranged on the outer side of the central bottom plate 1. A conductive column 3 protruding vertically upwards is arranged in the center of the upper surface of the central bottom plate 1. The outer periphery of the upper surface of the outer bottom plate 2 is provided with There is an outer baffle plate 4 that is fixed with the outer bottom plate and protrudes vertically upwards, and a semi-permeable membrane 9 that is fixed with the central bottom plate and protrudes vertically upwards is arranged on the outer periphery of the upper surface of the central bottom plate 1. The accommodating space enclosed by the semi-permeable membrane 9 and the central bottom plate 1 constitutes the cathode area 7, and the accommodating space enclosed by the semi-permeable membrane 9, the out...

Embodiment 2

[0034] Example 2: A method for preparing graphene and reclaiming lithium using graphite electrodes for waste lithium batteries as raw material

[0035] Raw materials: select waste lithium batteries, break the shell, and put the graphite negative electrode in N 2 Dry at 90° C. for 2 hours under atmosphere to remove the electrolyte, then add it into deionized water, stir, filter, and dry to obtain graphite electrode material.

[0036]Crush the graphite electrode material to a particle size of ≤10 μm, then add 2 g of the crushed graphite electrode into the anode area of ​​the reactor containing 1 mol / L lithium sulfate solution (5°C), the solid-to-liquid ratio of the graphite electrode to the solution in the reactor is 1 : 30 (g / ml), the anode area rotates counterclockwise under the condition of a centrifugal speed of 200 rpm, and a constant voltage direct current of 1.7V is introduced at the same time, and the electrification time is 30min, and then CO is introduced into the cath...

Embodiment 3

[0037] Example 3: A method for preparing graphene and reclaiming lithium using graphite electrodes for waste lithium batteries as raw material

[0038] Raw materials: select waste lithium-ion batteries, break the shell, and put the graphite negative electrode in N 2 Dry at 90°C for 4 hours under atmosphere to remove the electrolyte, then add it into a mixture of deionized water and ethanol (volume ratio 1:1) and stir, filter and dry to obtain graphite electrode material.

[0039] The graphite electrode material is crushed to a particle size ≤ 8 μm, and then 10 g of the crushed graphite electrode is added to the anode area of ​​the reactor containing a 3mol / L lithium chloride solution (20°C). The solid-to-liquid ratio of the graphite electrode to the solution in the reactor is 1:70 (g / ml), the anode area rotates clockwise under the condition of centrifugal speed of 300 rpm, and at the same time, 1.5V constant voltage direct current is applied for 30 minutes, the ultrasonic powe...

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Abstract

The invention discloses a method for preparing graphene by taking graphite electrodes of waste lithium batteries as raw materials and recycling lithium. The method comprises the following steps: crushing the graphite electrodes of the waste lithium batteries, adding the crushed graphite electrodes into a reactor with a solution, mixing through external force and energizing to obtain graphene and lithium-containing materials. Through combination of factors such as electric potential and the solution shearing force, the preparation efficiency is higher; the size of the graphene and the existingform of the lithium ions can be effectively controlled; meanwhile, the doping of metal ion impurities such as lithium can be avoided; dual recovery of graphene and lithium can be achieved. Through themethod, the problems that a large number of waste lithium batteries are stored and the recovery pressure is high are effectively solved; the prepared graphene can be applied to the field of efficientheat dissipation, supercapacitors, metal-air batteries, catalyst carriers and conductive agents and the like; the metal lithium can be recycled; a sustainable path can be provided for recycling the lithium batteries; the method is a simple, efficient and high value-added lithium battery recycling technology as well as a low-cost and short-process graphene preparation technology.

Description

technical field [0001] The invention relates to a method for preparing graphene and recovering lithium by using graphite electrodes for waste lithium batteries as raw materials, and belongs to the field of recycling new carbon materials and lithium batteries. Background technique [0002] Lithium batteries have the advantages of high voltage, large specific capacity, good cycle performance, and no memory effect, and are widely used in 3C, electric vehicles, aerospace and other fields. With the vigorous promotion of global electric vehicles, a large number of lithium batteries will face the problem of being scrapped in the future. Although waste lithium batteries contain a lot of reusable resources, the recovery rate of waste batteries in my country is less than 2% (China Automotive Technology Research Center) , and mainly focus on the recovery of heavy metals from lithium battery electrode materials (CN101847763 A is a comprehensive recovery method for waste lithium iron phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54
CPCH01M10/54Y02W30/84
Inventor 高彪峰谷保祥刘碧波陈晓阳陈锋张继伟刘帅霞邓天天周亚倩
Owner 高彪峰
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