Method for recycling lead paste in spent lead-acid battery

Patent metadata

Field	Value
Publication number	US-11196107-B2
Application number	US-201916446000-A
Country	US
Kind code	B2
Filing date	Jun 19, 2019
Priority date	Sep 13, 2017
Publication date	Dec 7, 2021
Grant date	Dec 7, 2021

Abstract

The disclosure discloses a method for recycling lead paste in a spent lead-acid battery, comprising: (1) pretreating lead paste in a spent lead-acid battery as a raw material under vacuum; mixing the pretreated lead paste with a chlorination reagent to obtain reactants; and heating the reactants under vacuum to carry out a chlorination volatilization reaction, so that lead element in the pretreated lead paste is combined with chlorine element in the chlorination reagent to form lead chloride, which is then volatilized, and after the reaction is completed, chlorination residue and a crude lead chloride product are obtained by condensation and crystallization after volatilization; (2) purifying the crude lead chloride product obtained in the step (1) under vacuum to obtain a refined lead chloride product. The disclosure improves the overall process flow of the recycling method as well as parameter conditions of the respective steps thereof, and can effectively solve the problem of serious pollution in lead paste recycling in the prior art.

First claim

What is claimed is:

1. A method for recycling lead paste in a spent lead-acid battery, comprising:
pretreating lead paste in a spent lead-acid battery as a raw material under vacuum to convert lead dioxide in the lead paste into lead oxide; mixing the pretreated lead paste with a chlorination reagent to obtain reactants, the chlorination reagent being used to provide a chlorine element; and heating the reactants under vacuum to carry out a chlorination volatilization reaction, so that a lead element in the pretreated lead paste is combined with the chlorine element in the chlorination reagent to form lead chloride, which is then volatilized, and after the reaction is completed, chlorination residue and a crude lead chloride product are obtained by condensation and crystallization after volatilization; and
purifying the crude lead chloride product under vacuum to separate other chloride impurities therein, thereby obtaining a refined lead chloride product.

2. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , further comprising:
dissolving the chlorination residue with water, performing filtration to obtain a filtrate, and evaporating the filtrate to obtain a precipitate.

3. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein the chlorination reagent is a mixture of calcium chloride and silica; and
a temperature of the chlorination volatilization reaction and a ratio of the calcium chloride to the silica are optimized such that a residual amount of lead in the chlorination residue is minimized.

4. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein the chlorination volatilization reaction is carried out by heating at a vacuum pressure of 0.1 to 10 5 Pa and a temperature of 400 to 650° C.;
the chlorination reagent is a mixture of calcium chloride and silica, wherein a molar ratio of the calcium chloride to the lead element in the pretreated lead paste is 12:1 to 30:1, and a molar ratio of the silica to the lead element in the pretreated lead paste is 12:1 to 60:1; and
a percentage of lead element contained in the crude lead chloride product relative to lead element contained in the reactants is at least 68.5%.

5. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein the step of purifying the crude lead chloride product is carried out by heating at a vacuum pressure of 0.1 to 1 Pa and a temperature of 200 to 400° C.

6. The method for recycling lead paste in a spent lead-acid battery according to claim 2 , wherein the step of evaporating the filtrate is carried out at a temperature of 100 to 120° C.

7. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein the lead paste has a lead content of 70 to 75 wt %.

8. The method for recycling lead paste in a spent lead-acid battery according to claim 2 , further comprising constituting the chlorination reagent from the precipitate.

9. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein a residual amount of lead in the chlorination residue is less than 0.05 mg/L.

10. The method for recycling lead paste in a spent lead-acid battery according to claim 1 , wherein lead chloride in the refined lead chloride product has a purity of 99.8 wt % or more.

Assignees

• Univ Huazhong Science Tech

Inventors

• Yang Jiakuan
• Liu Kang
• Liang Sha
• Chen Ye
• Xiao Keke
• Wang Junxiong
• Yu Wenhao
• Li Mingyang
• Hou Huijie
• Hu Jingping
• Liu Bingchuan

Classifications

• Y02E60/10

  Energy storage using batteries · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• Y02P10/20

  Recycling · CPC title

• C01G21/16 Primary

  Halides · CPC title

• Y02W30/84

  Recycling of batteries or fuel cells · CPC title