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Method for achieving filter liquor circulation, recovering waste lead plaster through wet process and preparing high-purity red lead

A technology of waste lead paste and filtrate, which is applied in the field of preparing high-purity red lead, can solve the problems of large dosage of leaching reagents and high content of impurity elements, and achieve the effects of enhanced complexation, efficient leaching, and efficient separation

Active Publication Date: 2019-06-11
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention provides a method for preparing high-purity red lead from waste lead paste by wet recovery, and solves the technical problems of high content of impurity elements and large dosage of leaching reagents in the process of wet recovery of waste lead paste in the prior art

Method used

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  • Method for achieving filter liquor circulation, recovering waste lead plaster through wet process and preparing high-purity red lead
  • Method for achieving filter liquor circulation, recovering waste lead plaster through wet process and preparing high-purity red lead
  • Method for achieving filter liquor circulation, recovering waste lead plaster through wet process and preparing high-purity red lead

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Embodiment 1

[0057] figure 1 A process flow chart for the preparation of high-purity red lead based on wet recovery of waste lead paste based on filtrate circulation provided by the present invention. Waste lead paste (SLP) raw material is 9g, the dosage of ammonium acetate in the wet leaching process is 64mmol / g SLP, the dosage of acetic acid is 3mmol / g SLP, the dosage of hydrogen peroxide is 3mmol / gSLP, and the solid-liquid ratio is controlled at 90g / L, the pH was adjusted to 7.6. After leaching for 2 hours, separate by filtration to obtain leachate and residue. The concentration of lead ions in the leaching solution is 0.30mol / L, the concentration of the ammonium carbonate reagent added is 2mol / L, the volume of the ammonium carbonate added is 15mL, the pH is adjusted to 8.6 with ammonia water, the cation of the reagent for adjusting the pH is the same as that in the organic acid The cations are kept consistent to avoid introducing other impurity elements. In this embodiment, the cati...

Embodiment 2

[0059] The waste lead paste raw material is 9g, the dosage of ammonium acetate in the wet leaching process is 70mmol / g SLP, the dosage of acetic acid is 6mmol / g SLP, the dosage of hydrogen peroxide is 2mmol / g SLP, and the solid-liquid ratio is controlled at 100g / L , the pH was adjusted to 7.0. After leaching for 1 hour, filter and separate to obtain leachate and residue. The lead ion concentration in the leaching solution is 0.35mol / L, the concentration of the ammonium carbonate reagent added is 4mol / L, the volume of the ammonium carbonate added is 8mL, the pH is adjusted to 8.0 with ammonia water, and the reaction is 0.5h, and the solid-liquid mixture after the reaction is Seal it and place it in an environment of 80°C for aging for 6 hours to improve the filtration performance of lead carbonate. Subsequently, the lead carbonate product and filtrate were obtained by filtration. The sulfate ion concentration in the filtrate is 0.16mol / L, and 4.55g barium acetate is added in ...

Embodiment 3

[0061] The raw material of waste lead paste is 9g. During the wet leaching process, the dosage of ammonium acetate is 50mmol / g SLP, the dosage of acetic acid is 1mmol / g SLP, the dosage of hydrogen peroxide is 8mmol / g SLP, and the solid-liquid ratio is controlled at 60g / L , the pH was adjusted to 8.0. After leaching for 6 hours, filter and separate to obtain leachate and residue. The concentration of lead ions in the leach solution is 0.20mol / L, the concentration of ammonium carbonate reagent added is 2mol / L, the volume of ammonium carbonate added is 14mL, the pH is adjusted to 8.5 with ammonia water, the reaction is 2h, and the solid-liquid mixture after the reaction is sealed. , aged at 40°C for 24 hours to improve the filtration performance of lead carbonate. Subsequently, the lead carbonate product and filtrate were obtained by filtration. The sulfate ion concentration in the filtrate is 0.16mol / L, and 4.55g barium acetate is added in the filtrate. After standing still f...

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Abstract

The invention discloses a method for achieving filter liquor circulation, recovering waste lead plaster through a wet process and preparing high-purity red lead and relates to the technical field of waste lead-acid cell lead plaster wet process recovery and red lead preparation. The method comprises the following steps that 1, organic acid salt, organic acid and reducer mixed liquor are utilized for leaching out the waste lead plaster, and after solid and liquid are separated, lixivium is obtained; 2, a carbonate solution is added to the lixivium, the reaction pH is regulated, and solid and liquid separating is carried out to obtain lead carbonate sediment and filter liquor; and 3, lead carbonate is roasted in the aerobic atmosphere, and the high-purity red lead with low impurity content is prepared. The prepared red lead product is high in purity and low in impurity content, the content of main impurities Ba and Fe is smaller than 10 mg / kg, the content of Cu, Zn and Al impurity elements is smaller than 1 mg / kg, the filter liquor can achieve closed circulation of organic acid radical ligand in a leaching system, and the use efficiency of a leaching agent is improved remarkably.

Description

technical field [0001] The invention relates to the technical field of wet recovery of lead paste from waste lead-acid batteries and preparation of red lead, more specifically, a method for preparing high-purity red lead by wet recovery of waste lead paste with filtrate circulation. Background technique [0002] Red lead is an important industrial raw material used in pigments, battery manufacturing, lead glass and anti-rust primers. In the field of lead-acid batteries, red lead is an important positive electrode additive. It is often added to the positive electrode active material in an amount of 5-30wt% to improve the formation efficiency of the battery and increase the initial capacity of the battery. It is widely used. [0003] At present, the raw materials for preparing red lead mainly include lead ingot, lead oxide and positive electrode active material of lead-acid battery. Using lead ingots and lead oxide as raw materials, high-purity red lead products can be prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B13/00
CPCY02P10/20
Inventor 杨家宽李名扬梁莎喻文昊王俊雄肖可可胡雨辰胡敬平侯慧杰刘冰川杨自荣
Owner HUAZHONG UNIV OF SCI & TECH
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