Hydrothermal deep conversion desulfurization method for waste lead plaster of lead-acid storage battery

A technology of waste lead-acid batteries and waste lead paste, which is applied in the direction of improving process efficiency, can solve the problems of affecting the application effect, low reduction efficiency, difficult reagent reaction, etc., and achieves low production cost, low labor intensity and simple operation. Effect

Active Publication Date: 2016-09-21
CENT SOUTH UNIV
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Problems solved by technology

The purpose of the desulfurization process of waste lead paste conversion is to remove PbSO from waste lead paste 4 sulfate radical and convert it into lead carbonate or lead hydroxide. The conversion agent used in the desulfurization conversion process mainly includes Na 2 CO 3 、K 2 CO 3 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 , NaOH and KOH, etc. Usually, the removal rate of sulfate radicals in actual operation is only 85-95%. The incomplete desulfurization and low reduction efficiency seriously affect the application effect of this method. The researchers proposed to use supergravity, ball milling and ultrasonic methods Intensified conversion desulfurization process (Pan Junqing et al. Development status of lead-acid battery recycling technology [J]. Journal of Beijing University of Chemical Technology, 2014, 41(3): 1-14.), but still can not achieve the desired effect, the main reason It may be the non-conductive lead sulfate crystals precipitated on the grid of the waste lead-acid battery during the discharge process, which is difficult to react with the reagent in the conventional conversion desulfurization process

Method used

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  • Hydrothermal deep conversion desulfurization method for waste lead plaster of lead-acid storage battery

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Embodiment 1

[0020]The main components of waste lead paste in the dismantling products of waste lead-acid batteries are (%) by weight percentage: Pb73.80%, S5.25% and Sb0.15%, and sodium carbonate is an analytical reagent. Add 2000g of waste lead plaster and 356g of sodium carbonate to 4000ml of water at the same time for slurrying, then add the mixed slurry into a stainless steel high-pressure reactor, keep the stirring speed at 120r / min, control the partial pressure of nitrogen to 0.3MPa and ventilate for 2min, then raise the temperature To 160°C, control the partial pressure of nitrogen to 0.8MPa to react for 3 hours. When the reaction is completed, cool down and lower the temperature to 65°C, vacuum filtration is used to achieve liquid-solid separation, the sulfur content in the desulfurization conversion residue is reduced to 0.02%, and the desulfurization rate reaches 99.40%.

Embodiment 2

[0022] The main components of waste lead paste in the dismantling products of waste lead-acid batteries are (%): Pb73.80%, S5.25% and Sb0.15%, and sodium hydroxide is an analytical reagent. Add 2000g of waste lead plaster and 268g of sodium hydroxide to 4000ml of water at the same time for slurrying, then add the mixed slurry into a stainless steel high-pressure reactor, keep the stirring speed at 120r / min, control the partial pressure of nitrogen to 0.3MPa and ventilate for 2min, then increase Temperature to 180°C, control nitrogen partial pressure 0.8MPa to react for 3 hours, after the reaction is completed, cool down and lower the temperature to 70°C, use vacuum filtration to achieve liquid-solid separation, the sulfur content in the desulfurization conversion slag is reduced to 0.01%, and the desulfurization rate reaches 99.38% .

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Abstract

The invention discloses a hydrothermal deep conversion desulfurization method for waste lead plaster of a lead-acid storage battery. The method includes the steps that the waste lead plaster and aqueous alkali are mixed and then added into a high pressure reactor, and reacting is carried out under the required temperature and nitrogen partial pressure, so that lead sulfate is completely reacted with alkali to remove sulfate radicals; and solid-liquid separation is conducted after the requirement for reaction time is met, sodium sulfate is recovered from desulfuration conversion liquid, and lead is further extracted from desulfuration conversion slug. By the adoption of the hydrothermal mode, the alkaline conversion desulfuration process of the waste lead plaster is strengthened, the sulfate radicals in the waste lead plaster can be removed completely, the consumption of alkaline only accounts for 1.0-1.05 times of the theoretical dose, the desulfurization degree is above 99.0%, and therefore advantage conditions are created for subsequent extraction of lead from the conversion slag.

Description

technical field [0001] The invention relates to a hydrometallurgical process in the field of nonferrous metallurgy, in particular to a hydrometallurgical method for hydrothermal deep conversion desulfurization of waste lead-acid storage battery lead paste. Background technique [0002] Lead is a silvery-white heavy non-ferrous metal. Based on its special physical and chemical properties, it is mainly used to make alloys. Among them, lead-acid batteries are the main consumption area, accounting for more than 80.0% of the world's total lead consumption. Although the weight-to-energy ratio of lead-acid batteries is lower than that of MH-Ni batteries and Li-ion batteries, they are widely used in various fields of the national economy due to their high cost performance, mature technology and good safety performance. More than 70.0% of the secondary battery market share. In recent years, the rapid development of my country's automobile industry has stimulated the rapid developmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B13/00
CPCC22B7/006C22B13/045Y02P10/20
Inventor 刘伟锋邓循博傅新欣朱鹏春饶帅杨天足张杜超陈霖
Owner CENT SOUTH UNIV
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