Method for recovering lead-containing raw material by using wet process

A raw material, wet process technology, applied in the field of waste lead-acid battery recycling and regeneration, can solve the problems of large consumption of desulfurizer, generation of alkali mist, inclusion of impurities, etc., to achieve high-efficiency recovery methods and eliminate environmental pollution.

Active Publication Date: 2014-01-22
北京中金瑞丰环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] 1) Acidic electrolysis produces toxic gases that pollute the environment
[0011] 2) The reduction of solid-phase electrolytic lead paste is not complete and contains a large amount of impurities, which is not suitable for industrialization
[0012] 3) The operating cost of alkaline electrolysis is relatively high, and alkali mist is generated during the electrolysis process
[0013] 4) Acidic and alkaline electrolysis need to consume a large amount of desulfurizers (sodium carbonate, ammonium carbonate, sodium hydroxide), resulting in increased costs

Method used

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  • Method for recovering lead-containing raw material by using wet process
  • Method for recovering lead-containing raw material by using wet process
  • Method for recovering lead-containing raw material by using wet process

Examples

Experimental program
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Effect test

Embodiment 1

[0069] Take a commercially available waste valve-regulated sealed lead-acid battery with a specification of 12V, 7Ah and a weight of 2 kg. The treatment process is as follows:

[0070] 1) Break it up and separate the lead plaster, grid, waste sulfuric acid and waste plastic.

[0071]2) Put 1 kg of lead paste into 10L reactor 1, which contains excess iron powder, 0.01mol / L iron sulfate, 1mol / L sodium sulfate, 0.9mol / L diethylenetriamine , adding sodium carbonate-sodium bicarbonate buffer solution to maintain the pH value of the solution between 10.0±0.2 during the reaction. Stir at a constant temperature of 50°C for 1 hour until the reddish-brown lead dioxide reacts completely.

[0072] 3) Filter and separate the solution in the process of 2) to obtain filtrate A and filter residue.

[0073] 4) Transfer the filtrate A into the 10L reactor 2, stir at a constant temperature of 75°C, add sulfuric acid to adjust the pH of the solution to 5.0, and precipitate the lead salt in the ...

Embodiment 2

[0085] Take a 12V, 100Ah waste lead-acid battery for backup power supply, weighing 30 kg, and the specific treatment process is as follows:

[0086] 1) Crush it and sort out the lead paste for later use.

[0087] 2) Configure 50L solution, which contains 0.5mol / L sodium sulfate, 0.001mol / L cobalt chloride, 1.5mol / L phenylalanine, and use sodium hydroxide solution to maintain the pH value of the solution during the reaction process between 7.0±0.2 , and then add 10 kg of lead paste obtained in the process of 1) and excess lead powder to the solution, and stir for 1.5 hours at a constant temperature of 65°C until the reddish-brown lead dioxide reacts completely.

[0088] 3) Filter the solution obtained in 2) and separate 50L of filtrate A and filter residue.

[0089] 4) Put 50L of filtrate A at a constant temperature of 80°C, add perchloric acid to adjust the pH value to below 4.5, so that all lead salts are precipitated in the form of lead sulfate.

[0090] 5) Filter the reac...

Embodiment 3

[0099] 1) Break a 60kg, 12V, 200Ah lead-acid battery and separate the lead paste.

[0100] 2) Add 40L of a solution containing 0.7mol / L ammonium sulfate, 0.05mol / L manganese nitrate, and 0.8mol / L histidine to reactor 1, and use 10% potassium hydroxide solution to maintain the pH of the solution during the reaction process. Between 8.5-9.5, add 2 kg of lead paste obtained in process 1). Stir for 0.75 hours under the condition of a constant temperature of 70°C, and feed in an appropriate amount of sulfur dioxide gas, so that the lead dioxide is completely reduced and dissolved by the lead powder and sulfur dioxide in the lead paste.

[0101] 3) Filter the solution after the reaction in process 2) to obtain filtrate A and filter residue.

[0102] 4) Filtrate A is kept at a constant temperature of 60°C, and hydrogen chloride gas is passed through to adjust the pH value of filtrate A to gradually decrease to completely precipitate lead sulfate.

[0103] 5) Filter the solution aft...

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Abstract

The invention discloses a method for recovering a lead-containing raw material by using a wet process. The method comprises the steps: (1) leaching the lead-containing raw material by using a solution, adding a reducing agent to reduce lead dioxide or lead orthoplumbate in the lead-containing raw material into a soluble lead salt, after a lead compound is completely dissolved, filtering the solution, and separating to obtain a filtrate A and an insoluble substance, wherein the solution contains sulfate, a complexing agent and a catalyst; (2) adjusting the pH value of the filtrate A, separating to obtain lead sulfate and a filtrate B, and returning the filtrate B to the step (1) after sulfate radicals are replenished and the pH value is adjusted; (3) directly using lead sulfate as battery materials or commodities, subjecting a sulfate-containing alkaline solution and lead sulfate to reaction, and separating to obtain basic lead sulfates and a filtrate C, wherein the basic lead sulfates include tribasic lead sulfate and tetrabasic lead sulfate. The method can be used for purifying the lead-containing raw material to form lead sulfate and basic lead sulfates directly used for producing lead-acid batteries, thereby being an environment-friendly wet-process recovery method.

Description

technical field [0001] The invention belongs to the technical field of recovery and regeneration of waste lead-acid batteries, and relates to a method for preparing high-purity lead sulfate or basic lead sulfate by chemically using lead paste or lead-containing raw materials in waste lead-acid batteries. Background technique [0002] Since its birth, lead-acid batteries have occupied an important position in the secondary battery market, especially in automotive batteries, with its low price and reliable stability. According to statistics from relevant industry associations, the consumption of refined lead in China exceeded 4 million tons in 2011, of which the consumption of lead-acid batteries accounted for about 70%. Lead-acid batteries contain a large amount of toxic lead and its compounds. At present, the pyro-method recovery technology that has been industrialized produces lead vapor in the process of lead smelting and reduction, which causes serious pollution to the en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B3/44C22B13/00
CPCY02P10/20
Inventor 张超
Owner 北京中金瑞丰环保科技有限公司
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