Method for preparing high-purity PbO by cycle wet method

A cyclic, high-purity technology, applied in the field of recycling and regenerating lead from waste lead-acid batteries and lead-containing materials, can solve the problems of difficult process control, raw material consumption, long cycle, etc., and achieve high product purity and fewer process steps. , the effect of simple operation

Inactive Publication Date: 2016-08-24
NO 63971 TROOPS PLA
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Problems solved by technology

[0005] Aiming at the problems of difficult process control, many steps, long cycle and raw material consumption in the existing chemical wet lead regeneration technology, the present invention proposes and designs the approach of lead solution-liquid phase lead desulfurization-lye washing-low temperature sintering A new process for the production of high-purity ultrafine PbO powder, which can be directly used in the preparation of lead-acid battery electrodes

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  • Method for preparing high-purity PbO by cycle wet method

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Embodiment 1

[0017] (1) Use mechanical dismantling to separate and sort waste lead-acid batteries to obtain lead paste, grids, waste sulfuric acid, separators and shells. The separated positive / negative lead paste is crushed and screened with a 100-mesh stainless steel screen, and the larger lead paste particles are continuously transferred to the pulverizer for crushing until all the lead paste can pass through the screen. The crushed and sieved positive / negative lead paste is fully mixed in solid phase.

[0018] (2) Take 1kg of lead paste powder mixture, slowly heat up to 280°C under normal pressure, and keep it for 3 hours so that the lead dioxide and lead in it undergo redox reaction under heating conditions and convert into lead oxide to generate lead oxide and sulfuric acid Lead-based solid mixture; then add 3mL of 80% hydrazine hydrate solution and react at 20°C for 10 minutes to make the unreacted PbO 2 The solid compound is completely converted to PbO.

[0019] (3) The PbO obtai...

Embodiment 2

[0023] (1) Use mechanical dismantling to separate and sort waste lead-acid batteries to obtain lead paste, grids, waste sulfuric acid, separators and shells. The separated positive / negative lead paste is crushed and screened with a 100-mesh stainless steel screen, and the larger lead paste particles are continuously transferred to the pulverizer for crushing until all the lead paste can pass through the screen. The crushed and sieved positive / negative lead paste is fully mixed in solid phase.

[0024] (2) Take 2kg of lead plaster powder mixture, slowly heat up to 320°C under normal pressure, and keep it for 4 hours so that the lead dioxide and lead in it undergo oxidation-reduction reaction under heating conditions and convert into lead oxide to generate lead oxide and sulfuric acid Lead-based solid mixture; then add 6mL of 80% hydrazine hydrate solution and react at 25°C for 20 minutes to make the unreacted PbO 2 The solid compound is completely converted to PbO.

[0025](3...

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Abstract

The invention relates to a method for preparing high-purity PbO by a cycle wet method, and provides a method for recycling a waste lead-acid battery to directly produce high-purity PbO and recycling a chemical raw material. The preparation method for the high-purity PbO comprises the following steps of smashing a waste battery, separating positive / negative lead paste, and allowing lead in the lead paste to be completely converted to a lead raw material composed of PbO and PbSO4 through oxidation and reduction reaction of the positive / negative lead pate; immersing the lead raw material with a mixed solution of an organic acid and an organic acid salt to remove impurity, and carrying out lead deposition and desulfuration on the solution, generating a byproduct sodium sulfate to obtain a lead precipitate; purifying the lead precipitate with an alkaline solution by dissolving the precipitation process to obtain high-purity lead hydroxide; and carrying out low-temperature sintering on the lead hydroxide to obtain a high-purity PbO product, wherein an organic acid salt mother liquid can be used for next circulation. By the method, the defects of long process period of a PbO synthesis process, high energy consumption and a large amount of chemical raw materials required to be consumed are overcome, the cost is reduced, and the method is a new technology which has the advantages of high technological additional value, energy saving and environment friendliness, and is suitable for industrial production at a large scale.

Description

technical field [0001] The invention relates to a method for preparing high-purity PbO by a circulating wet method, and belongs to the technical field of recovering and regenerating lead from waste lead-acid batteries and lead-containing materials. Background technique [0002] Modern European, American and Chinese large enterprises have been using the traditional pyrometallurgical lead smelting process or sodium carbonate pre-desulfurization process, and then the crude lead smelted by pyrometallurgy is then converted into refined lead by electrolysis. Since pyro-smelting requires a high temperature of over 1200 degrees, a large amount of lead vapor and lead dust are generated during the high-temperature smelting process, which easily causes secondary lead pollution, and the mother liquor of the most commonly used carbonate desulfurization method is difficult to recycle. Lead refining has been using the Betts fluosilicic acid refining method in 1902, which consumes a lot of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54C22B7/00C22B13/00
CPCY02P10/20Y02W30/84
Inventor 文越华程杰何柯蔡丽莉尹元曹高萍杨裕生
Owner NO 63971 TROOPS PLA
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