A novel approach to recover lead oxide from spent lead acid batteries by desulfurization and crystallization in sodium hydroxide solution after sulfation

Huang, Kui; Liu, Hengyi; Dong, Haili; Lin, Mi; Ruan, Jujun

doi:10.1016/j.resconrec.2020.105385

Cited by 37 publications

(13 citation statements)

References 22 publications

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“…Reaction ( 5) represents the conversion of lead sulfate to lead oxalate. The conversion of lead oxide sulfate (lanarkite) to lead oxalate is outlined by Reaction (6). As lead pastes also contain lead monoxide and lead dioxide, Reactions (7) and ( 8) illustrate the possible reactions for lead monoxide and lead dioxide in the presence of oxalate.…”

Section: Desulphurization In Oxalate-bearing Mediamentioning

confidence: 99%

“…Alkaline solutions, such as NaOH, have been suggested to be agents for desulphurization [6], and exhibit a higher desulphurization rate and efficiency than that using carbonate media, such as Na 2 CO 3 [38]. In alkaline solutions, lead sulfate is desulphurized, as the hydroxyl ion displaces the sulfate ion, PbSO 4 (cr) + 2OH − PbO(cr) + H 2 O(l) + SO 4 2− (13) Figure 8 shows the stability fields of lead monoxide and lead sulfate in the space of activity of sulfate in logarithmic units versus activity of the hydroxyl ion in logarithmic units (i.e., log a SO 2− 4 versus log a OH − ).…”

Section: Desulphurization In Alkaline Solutionsmentioning

confidence: 99%

Section: Desulphurization In Alkaline Solutionsmentioning

confidence: 99%

“…Lanarkite was also observed by other researchers [4]. The chemical components include lead sulfates (PbSO 4 and PbO•PbSO 4 ) (57.21 to 60.57 wt.%), lead dioxide (PbO 2 ) (5.66 to 26.70 wt.%), lead monoxide (PbO) (13.08 to 29.53 wt.%), and metallic lead (Pb) (1.24 to 4.5 wt.%) [5,6]. In spent lead-acid batteries, lead sulfates are primarily produced via the following reactions, Pb + SO 4…”

Section: Introductionmentioning

confidence: 99%

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Recycling of Lead Pastes from Spent Lead–Acid Batteries: Thermodynamic Constraints for Desulphurization

Xiong

2022

Recycling

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Lead–acid batteries are important to modern society because of their wide usage and low cost. The primary source for production of new lead–acid batteries is from recycling spent lead–acid batteries. In spent lead–acid batteries, lead is primarily present as lead pastes. In lead pastes, the dominant component is lead sulfate (PbSO4, mineral name anglesite) and lead oxide sulfate (PbO•PbSO4, mineral name lanarkite), which accounts for more than 60% of lead pastes. In the recycling process for lead–acid batteries, the desulphurization of lead sulfate is the key part to the overall process. In this work, the thermodynamic constraints for desulphurization via the hydrometallurgical route for recycling lead pastes are presented. The thermodynamic constraints are established according to the thermodynamic model that is applicable and important to recycling of lead pastes via hydrometallurgical routes in high ionic strength solutions that are expected to be in industrial processes. The thermodynamic database is based on the Pitzer equations for calculations of activity coefficients of aqueous species. The desulphurization of lead sulfates represented by PbSO4 can be achieved through the following routes. (1) conversion to lead oxalate in oxalate-bearing solutions; (2) conversion to lead monoxide in alkaline solutions; and (3) conversion to lead carbonate in carbonate solutions. Among the above three routes, the conversion to lead oxalate is environmentally friendly and has a strong thermodynamic driving force. Oxalate-bearing solutions such as oxalic acid and potassium oxalate solutions will provide high activities of oxalate that are many orders of magnitude higher than those required for conversion of anglesite or lanarkite to lead oxalate, in accordance with the thermodynamic model established for the oxalate system. An additional advantage of the oxalate conversion route is that no additional reductant is needed to reduce lead dioxide to lead oxide or lead sulfate, as there is a strong thermodynamic force to convert lead dioxide directly to lead oxalate. As lanarkite is an important sulfate-bearing phase in lead pastes, this study evaluates the solubility constant for lanarkite regarding the following reaction, based on the solubility data, PbO•PbSO4 + 2H+ ⇌ 2Pb2+ + SO42− + H2O(l).

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Section: Desulphurization In Oxalate-bearing Mediamentioning

confidence: 99%

Section: Desulphurization In Alkaline Solutionsmentioning

confidence: 99%

Section: Desulphurization In Alkaline Solutionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Recycling of Lead Pastes from Spent Lead–Acid Batteries: Thermodynamic Constraints for Desulphurization

Xiong

2022

Recycling

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“…In previous studies, researchers have tried to convert SLP into lead products such as metallic lead, − organic lead compounds, , lead oxide, ,− lead chloride, , lead iodide, − and lead sulfide. − Yang et al used a combination of wet desulfurization and a roasting process to prepare lead oxide products . Liu et al reported on a vacuum chlorination process with calcium chloride as a reagent to successfully produce high-purity lead chloride products .…”

Section: Introductionmentioning

confidence: 99%

Batch Production of Lead Sulfate from Spent Lead–Acid Batteries via an Oxygen-Free Roasting Route: A Negative-Carbon Strategy

Liu

Wang

et al. 2023

ACS Sustainable Chem. Eng.

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Multicomponent lead compounds, including lead (Pb), lead oxide (PbO), lead dioxide (PbO 2 ), and lead sulfate (PbSO 4 ), in spent lead−acid batteries (LABs), if not properly disposed of and recycled, will cause serious pollution and damage to the ecological environment. Pyrometallurgical smelting performed above 1000 °C often incurs high energy consumption and lead pollution. In this study, a low-temperature (300 °C), oxygen-free roasting process was proposed. With potassium bisulfate (KHSO 4 ) as the roasting reagent, the uniform conversion of multicomponent lead compounds from spent lead paste (SLP) to PbSO 4 was successfully realized in one step. We observed that PbO 2 species were relatively chemically stable, during the oxygen-free roasting. However, the decomposition of PbO 2 into PbO can be achieved by heating to 300 °C, resulting in an effective conversion to PbSO 4 . The optimal conditions for PbSO 4 production were a heating temperature of 300 °C, an SLP/KHSO 4 mass ratio of 1:1, and a holding time of 10.0 min. Life cycle assessment results show that the recycling of 1.0 t spent LABs can reduce carbon emissions of 2.45 t CO 2 and smog of 0.13 t. Our research provides an emission-free, low-temperature, and negative-carbon strategy for facile and cost-effective recycling of spent LABs, as an alternative to traditional pyrometallurgical smelting.

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Efficient Desulfurizer Recycling during Spent Lead–Acid Batteries Paste Disposal by Zero‐Carbon Precursor Hypothermic Smelting

Li,

Zhu,

et al. 2024

Advanced Science

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Recycling of spent lead‐acid batteries (LABs) is extremely urgent in view of environmental protection and resources reuse. The current challenge is to reduce high consumption of chemical reagents. Herein, a closed‐loop spent LABs paste (SLBP) recovery strategy is demonstrated through Na2MoO4 consumption‐regeneration‐reuse. Experimental and DFT calculations verify that MoO42− competes Pb/Ca ions and weakens the metal‐oxygen bond of PbSO4/CaSO4.2H2O in SLBP, facilitating PbMoO4/CaMoO4 formation and 99.13 wt% of SO42− elimination. Pb of 99.97 wt% is obtained as zero‐carbon precursors (PbO2 and PbMoO4) by green leaching coupled with re‐crystallization. The regeneration of Na2MoO4 is realized at 600 ℃ using LABs polypropylene shells and NaOH as reagents. Compared with the traditional smelting technologies, the temperature is reduced from ＞1000 to 600 °C. The extraction of Na2MoO4 require only water, and satisfactory re‐used desulfurization efficiency (98.67 wt%) is achieved. For the residual Na2MoO4 after first SLBP desulfurization, the desulfurization efficiency remains above 97.36 wt% after adding fresh reagents for two running cycles. The new principle enables the reuse of 99.83 wt% of Na2MoO4 and the recycling of 95.27 wt% of Pb without generating wastewater and slags. The techno‐economic analysis indicates this strategy is efficient, economical, and environmentally‐friendly.

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A novel approach to recover lead oxide from spent lead acid batteries by desulfurization and crystallization in sodium hydroxide solution after sulfation

Cited by 37 publications

References 22 publications

Recycling of Lead Pastes from Spent Lead–Acid Batteries: Thermodynamic Constraints for Desulphurization

Recycling of Lead Pastes from Spent Lead–Acid Batteries: Thermodynamic Constraints for Desulphurization

Batch Production of Lead Sulfate from Spent Lead–Acid Batteries via an Oxygen-Free Roasting Route: A Negative-Carbon Strategy

Efficient Desulfurizer Recycling during Spent Lead–Acid Batteries Paste Disposal by Zero‐Carbon Precursor Hypothermic Smelting

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