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A selective recovery of zinc and manganese from the spent primary battery black mass as zinc hydroxide and manganese carbonate

  • Cornelius Satria Yudha EMAIL logo , Naufal Atha Winard , Anggraini Putri Sulistyowati , Meidiana Arinawati and Enni Apriliyani
Published/Copyright: September 25, 2025
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Open Engineering
From the journal Open Engineering Volume 15 Issue 1

Abstract

The major challenge in zinc–carbon battery recycling lies in achieving selective separation of zinc and manganese while producing high-purity materials suitable for advanced applications. This study aims to develop a selective hydrometallurgical approach for recovering high-purity zinc and manganese from spent primary zinc–carbon battery black mass (BM), addressing environmental concerns from improper battery disposal. A three-stage sequential leaching process was employed, consisting of water leaching for impurity removal, alkaline leaching for selective zinc extraction as zincate ions, and glucose-assisted reductive acid leaching for manganese recovery. The BM composition was characterized using scanning electron microscope (SEM)–energy-dispersive X-ray (EDX) analysis, while recovered products were precipitated as Zn(OH)2 and MnCO3 and characterized using X-Ray diffraction (XRD), Fourier transform-infra red (FTIR), SEM–EDX, and elemental mapping techniques. SEM–EDX analysis revealed that BM contains high concentrations of Zn, Mn, C, Na, and K. The sequential leaching achieved excellent metal recovery with 98.2% zinc extraction efficiency and 91.2% manganese recovery, demonstrating high selectivity with minimal cross-contamination. XRD analysis confirmed the formation of crystalline ZnO/Zn3(OH)4(NO3)2 and pure rhodochrosite MnCO3. SEM analysis revealed spherical morphologies for both products, with high purity confirmed by FTIR and EDX mapping. This work presents the first comprehensive study combining glucose-assisted reductive leaching with alkaline selective extraction for simultaneous zinc and manganese recovery from Zn–C batteries, achieving superior separation efficiency compared to conventional single-stage approaches. The as-obtained high-purity products show promising potential for advanced applications in catalysts, Li-ion batteries, and supercapacitors.

Keywords: batteries; hydrometallurgy; leaching; morphology; recovery

1 Introduction

The primary battery is a commercial product that is commonly found in households or offices. It stores chemical energy, which is then converted to electrical energy. This type of battery is non-rechargeable, which allows it to be used once in a cycle, resulting in numerous “dead” cells at the end of its use. The heavy metal content of the spent batteries makes them classified as hazardous waste; thus, the safe disposal of this waste becomes a challenge. Nowadays, alkaline and zinc–carbon batteries are the primary battery market that is commonly found in powering portable devices. These batteries have similarities in structure, such as metallic zinc anode, electrochemical manganese dioxide–carbon cathode, concentrated electrolyte(s), i.e., NaOH/KOH, and metal alloy as the case. The rising demand for these types of batteries results in increasing waste count and increasing demand in metal production. On the other hand, the metal in nature is very limited, and the cost of battery waste landfills becomes concerning. Thus, efficient and safe processing of the spent primary battery is one of the solutions to these problems [1–4].

In the early twentieth century, countries in Europe used pyrometallurgical processing to handle electronic waste. Up until recently, Hydrometallurgical processing has been considered a superior technique compared to the pyrometallurgical approach in metal waste processing due to the recent development in technology. This technique becomes more mature in efficiently converting waste into new products with high purity and less energy consumption. Spent primary batteries have been recycled using the hydrometallurgy method, specifically the leaching process. Acid and base can be used to leach dangerous yet valuable metals from the spent primary batteries with a high recovery rate. However, to improve the sustainability of the process, the final leaching product should be converted into products with high economic value [5].

Usually, the metal recovery from primary battery black mass (BM) is conducted via single-step leaching, single-step reduction leaching, and selective leaching. Single-step leaching, both with and without a reduction step, requires a follow-up separation process of Mn and Zn, which often requires a large amount of solvent or a strict crystallization protocol, which reduces the economic attractiveness due to the increasing operating cost [6]. A selective alkaline leaching and complex leaching are considered simple and in recovering Zn selectively, leaving manganese oxide as residue, which can be leached via reductive leaching. Though studies on metal recovery has been extensively investigated, the product derivation is an interesting topic to be developed [7,8].

Extensive research has been performed to design products derived from alkaline and zinc carbon batteries, focusing on the repurposing of the key components in the batteries, such as zinc, manganese, and carbon. Semiconductors for photocatalysis [9], fertilizers [10], Li-ion batteries [11,12], carbon capture materials [13], pigments, and catalysts [14] have been successfully derived from primary batteries, which increased the economic potential of the overall process. The recovery of valuable metals was performed using hydrometallurgical leaching, followed by a further purification step. Mineral acids, i.e., H2SO4 and HNO3, are a good choice for a rapid recovery of Zn and Mn. However, the purification process often becomes a challenge due to the solubility properties of the elements. In the leachate, Zn is often separated using several techniques, such as electrowinning, selective precipitation, and solvent recovery [15]. On the other hand, the wide variety of products demands a process that is simple, safe, economical, and flexible. Since zinc is an amphoteric species, selective leaching followed by a subsequent precipitation route can result in high-purity zinc and manganese-based products [16].

In this research, the BM from the spent zinc–carbon batteries was processed in three sequential leaching steps to recover zinc (Zn) and manganese (Mn) precipitates. Water leaching of BM can remove the soluble potassium electrolyte; caustic leaching was employed to recover Zn, and reductive acidic leaching was used to recover Mn. The Zn and Mn precipitates were formed via chemical precipitation in the form of Zn(OH)2 and MnCO3, respectively. The novelty of this study lies in the comprehensive characterization-focused approach that combines glucose-assisted reductive leaching with systematic product quality assessment, achieving superior recovery efficiencies while demonstrating the transformation of recovered materials into application-ready derivatives (NCM and ZnO) through X-Ray diffraction (XRD) confirmation. The aim of the study is to analyze the quality of these products using XRD, scanning electron microscope (SEM), and Fourier transform-infra red (FTIR) to ensure that these products have the potential to be used as various precursors for the preparation of advanced materials, distinguishing this work from previous studies by emphasizing material characterization and application potential rather than solely focusing on process optimization.

2 Experimental methods

2.1 Selective leaching of Zn and Mn

The spent primary batteries were collected in the campus area of Universitas Sebelas Maret as a Green Campus Program. Primary batteries from several brands were dismantled and compiled as one. The BM was collected by manually separating the case and graphite rod electrode. The BM was washed using distilled water (DW), filtered, and then dried until a dry BM was obtained. A total of 50 g of dried BM was reacted with 1,000 mL 2 M NaOH solution in a 2,000 mL borosilicate vessel at a temperature of 80°C for 2 h. The solution was cooled to near room temperature, filtered using filter paper, and the residue was washed until the initial volume was reached. The filtrate was labeled as sodium zincate (Na2Zn(OH)4) solution and was stored in a glass bottle. Meanwhile, the residue was dried in an oven at 80°C for a night. About 10 g of residue was reacted with 200 mL of a 1 M H2SO4 solution in a 500 mL beaker at a temperature of 60–80°C. A 10 g of glucose (C6H12O6) was added to the beaker as a reductant. The reaction was maintained at 80°C for 2 h before the solution was cooled to near room temperature. The solution was then filtered, and the residue was washed with filter paper until the initial volume was reached. The filtrate was stored and labeled as MnSO4. The final residue was dried in an oven at 80°C.

The experimental parameters employed in this study were selected based on a comprehensive literature review of the hydrometallurgical processing of spent battery materials. The solid-to-liquid ratio of 0.05 g/mL was chosen to ensure adequate mass transfer while maintaining economic reagent consumption. The alkaline leaching temperature of 80°C was selected based on literature data demonstrating optimal zinc extraction efficiency with minimal manganese co-dissolution. The 2 M NaOH concentration and 2 h reaction time provide a balance between extraction kinetics and selectivity. For the reductive acid leaching stage, the 60–80°C temperature range and glucose addition facilitate controlled reduction of Mn(iv) oxides to extractable Mn(ii) species while minimizing zinc redissolution [7].

2.2 Precipitation of Zn and Mn

The Na2Zn(OH)4 was transferred into a beaker with vigorous stirring and heating at 60°C. A 2 M HNO3 solution was transferred slowly into the beaker to obtain a pH level of 8. After the desired pH was reached, a precipitate was formed, as indicated by a cloudy solution. The mixing was continued for 60 min. The precipitate was filtered and washed several times using DW. The formed cake was dried in an oven at 80°C for a day. The dried Zn precipitate was labeled as Zn(OH)2. Separately but similarly, MnSO4 was also transferred to a beaker with vigorous stirring and heating at 60°C. A 2 M Na2CO3 solution was added to the beaker to obtain a pH level of 8. A white precipitate was formed, and the stirring continued for 2 h. The precipitate was filtered and washed several times. The cake was dried in an oven at 80°C for a day. The dried Mn precipitate was labeled as MnCO3. The dried samples of Zn(OH)2 and MnCO3 were ground and sieved through a 200-mesh screen. The overall process can be seen in Figure 1.

Figure 1 Flow process of Zn(OH)2 and MnCO3 production from spent primary batteries.
Figure 1

Flow process of Zn(OH)2 and MnCO3 production from spent primary batteries.

2.3 Material characterization

Structural analysis was performed using an X-ray diffractometer by Bruker-D2 Phaser (Bruker, Germany). The functional groups of the prepared powders were analyzed using infrared spectroscopy (FTIR; IR-Spirit, Shimadzu, Japan) at a wavenumber range of 4,000–400 cm−1. The morphological features and chemical composition of the products were examined using a SEM and energy-dispersive X-ray (EDX) by JEOL, Japan. Sample EDX mappings were analyzed to ensure the chemical quality of the as-prepared product. The concentrations of zinc and manganese in the water, alkaline, acid leaching solutions, and recovered solid products were determined using atomic absorption spectroscopy (AAS) with a Shimadzu AA-700 spectrometer. The instrument was operated under flame atomization conditions using an acetylene-air flame, with wavelengths set at 213.9 nm for zinc and 279.5 nm for manganese determination. Calibration standards were prepared from 1,000 mg/L stock solutions to establish linear calibration curves ranging from 0.1 to 5.0 mg/L for both elements.

For liquid samples, the alkaline leaching solution was appropriately diluted with deionized water to bring metal concentrations within the calibration range. Solid samples, including the precipitated Zn(OH)2 and MnCO3 products, were subjected to acid digestion prior to AAS analysis. Approximately 0.1 g of each solid sample was dissolved in 10 mL of concentrated nitric acid (65%) under gentle heating at 80°C for 2 h to ensure complete dissolution. The digested solutions were then cooled, filtered through 0.45 μm membrane filters, and diluted to 100 mL with deionized water. All measurements were performed in triplicate, and the results were expressed as mean values with standard deviations.

3 Results and discussion

3.1 Leaching performance

The leaching efficiency results in Figure 2 demonstrate the effectiveness of the sequential three-stage leaching approach for comprehensive metal recovery from zinc–carbon battery BM. The initial water-leaching step achieved minimal extraction with only 7.8% zinc and 0.8% manganese recovery, serving primarily to remove water-soluble impurities and salts while leaving the majority of metals intact in the solid matrix. The subsequent alkaline leaching stage showed dramatically improved performance with 88.1% zinc extraction while maintaining excellent selectivity with only 1.1% manganese dissolution, confirming the preferential dissolution of zinc as zincate ions [Zn(OH)4]2− under high pH conditions while manganese oxides remained largely unaffected. The final reductive acid leaching using glucose as a reducing agent achieved 91.2% manganese extraction with minimal additional zinc dissolution (2.3%), where glucose effectively reduced Mn(iv) oxides to soluble Mn(ii) species under acidic conditions.

Figure 2 Mn and Zn leaching performance.
Figure 2

Mn and Zn leaching performance.

The cumulative leaching efficiency of 98.2% for zinc and 91.2% for manganese validates the synergistic effect of the sequential approach, where each stage targets specific metal species based on their distinct chemical behaviors. The water leaching pre-treatment removes interfering ions that could complicate subsequent extraction steps, while the alkaline stage exploits zinc’s amphoteric nature for selective dissolution, leaving manganese-rich residues for the final reductive treatment. The use of glucose in the acid leaching stage is particularly effective as it provides controlled reduction conditions that convert insoluble MnO2 to extractable Mn2+ ions without excessive zinc co-dissolution. The minimal cross-contamination observed throughout the process (1.1% Mn in alkaline leachate and 2.3% Zn in acid leachate) demonstrates the high selectivity achieved, enabling the production of separate metal-rich solutions suitable for recovering high-purity zinc hydroxide and manganese carbonate products from battery waste materials [7,8,17].

3.2 Spent primary batteries characterization

The dismantled spent primary batteries were characterized before being processed in the next step. SEM–EDX was used to evaluate the composition and the topological feature of the BM. Figure 2 shows the SEM image of the BM and the EDX mapping. Meanwhile, the quantitative analysis is listed in Table 1.

Table 1

Spent primary battery BM quantitative analysis using EDX and AAS

Element EDX AAS
Mass composition (%) Atomic composition (%) Mass composition (%)
Zn 32.63 ± 2.90 17.04 ± 1.52 29.2 ± 1.8
Mn 26.61 ± 1.38 16.54 ± 0.86 22.5 ± 2.2
K 16.59 ± 0.60 15.98 ± 0.58 5 ± 1.8
Cl 1.32 ± 0.91 1.66 ± 0.26 —
O 22.86 ± 0.91 48.78 ± 1.94 —

Based on Figure 3 and Table 1, the main elements contained in the BM are Zn, Mn, C, K, and Cl. These materials were formed due to the exhausted chemical reaction during the utilization of the primary battery. The presence of K and Cl indicated that the spent battery used in this research used a conventional alkaline battery and Zn–carbon battery, which often use KOH and chloride-based salt (ZnCl2, NH4Cl) as the electrolyte, respectively. The reaction in exhausted primary batteries can be seen in the following equations [18]:

Figure 3 SEM image (a) and EDX mapping of BM on Zn (b), Mn (c), K (d), and C (e).
Figure 3

SEM image (a) and EDX mapping of BM on Zn (b), Mn (c), K (d), and C (e).

Reaction in alkaline batteries

(1) Zn (s) + 2MnO 2(s) → ZnO (s) + Mn 2 O 3 ( s ) .

Reaction in zinc–carbon batteries

(2) Zn (s) + 2MnO 2(s) + ZnCl 2(aq) + 2H 2 O (l) → 2MnO ( OH ) (s) + 2Zn ( OH ) Cl (aq) ,

(3) Zn (s) + 2MnO 2(s) + H 2 O (l) → Mn 2 O 3(s) + Zn ( OH ) 2(s) .

(4) ZnO (s) + H 2 O (l) + 2NaOH (aq) → Na 2 Zn ( OH ) 4(aq) ,

(5) Zn ( OH ) 2 + 2NaOH (aq) → Na 2 Zn ( OH ) 4(aq) ,

(6) Zn + 2H 2 O (l) + 2NaOH (aq) → Na 2 Zn ( OH ) 4(aq) + H 2(g) ,

(7) Na 2 Zn ( OH ) 4(aq) + 2HNO 3(aq) → Zn ( OH ) 2(s) + 2NaNO 3(aq) + 2H 2 O (l) ,

(8) 2Na 2 Zn ( OH ) 4(aq) + 2HNO 3(aq) → Zn 2 ( OH ) 2 ( NO 3 ) 2 + 2H 2 O (l) + 2NaNO 3(aq) .

Based on these reactions, the products that can be processed are either metal oxides (Mn2O3, ZnO) or metal hydroxides (Zn(OH)2). Potassium and chloride ions are expected to be leached during neutral leaching due to their high solubility.

3.3 Zn(OH)2 characterization

The Zn recovery was employed during the second step of the leaching process. It is expected that the Zn-based compounds are leached in a NaOH solution according to Equations (4)–(6). The soluble zincate ions were then precipitated using HNO3 to form a precipitate. The morphology and elemental mapping of the as-prepared precipitate are shown in Figure 4. The Zn(OH)2 secondary particle has a spherical shape (Figure 4a), containing Zn and O based on the elemental mapping. This particle consists of smaller primary particles with a narrow particle distribution that can be seen in Figure 4e and an average particle diameter of 0.146 µm. The small particle size can be advantageous for the formation of nanosized particles [19].

Figure 4 SEM image (a), EDX mapping of Zn(OH)2 on Zn (b), O (c), EDX spectra (d), and particle size histogram (e).
Figure 4

SEM image (a), EDX mapping of Zn(OH)2 on Zn (b), O (c), EDX spectra (d), and particle size histogram (e).

Table 2 shows the quantitative analysis of the samples, which are dominant in Zn and O. It is expected that the majority of the sample is zinc hydroxide compound. Figure 5(a) and (b) shows the X-ray diffraction pattern and FTIR spectra of the zinc hydroxide sample. The XRD analysis reveals a heterogeneous phase assemblage consisting of zinc oxide (ZnO) and zinc hydroxide nitrate (Zn3(OH)4(NO3)2), indicating successful selective leaching as evidenced by the absence of manganese-containing phases in the precipitate. The zinc hydroxide formed due to neutralization of zincate ions [Zn(OH)4]2⁻ with HNO3, by competing equilibria, favors nitrate incorporation into the crystal structure, forming Zn3(OH)4(NO3)2, where NO 3 − NO3⁻ partially substitutes hydroxide ions in the lattice. The ZnO phase results from thermal dehydration of zinc hydroxide (Zn(OH)2 → ZnO + H2O) during the drying process [20,21]. The absence of detectable manganese phases (such as MnO2 or Mn2O3) in the XRD pattern confirms the effectiveness of the alkaline leaching process in selectively dissolving zinc while leaving manganese compounds in the solid residue, demonstrating successful separation of these two major components from zinc–carbon battery waste and validating the selectivity of the hydrometallurgical approach. The FTIR spectra show a consistent interesting result. Strong transmittance peaks at 3,577, 3,483, 1,640, 1,373 cm−1, and around 800 cm−1 show the presence of an intercalated zinc hydroxide compound. This intercalated zinc hydroxide is often called zinc-layered hydroxide. In this case, the zinc hydroxide intercalates the nitrate anion. However, based on the SEM–EDX result, it is predicted that the intercalation only occurred on the particle surface. Thus, we can conclude that the reaction during the precipitation using HNO3 can be seen in Equations (7) and (8) [22].

Table 2

EDX and AAS analysis of Zn(OH)2

Element EDX AAS
Mass composition (%) Atomic composition (%) Mass composition (%)
Zn 74.02 ± 3.41 41.08 ± 1.89 49.8 ± 1.3
O 25.98 ± 0.71 58.92 ± 1.61 —
Mn n.d. n.d. 0.4 ± 0.12
Figure 5 XRD spectra of Zn(OH)2 (a) and FTIR spectra of Zn(OH)2 (b) from spent primary battery.
Figure 5

XRD spectra of Zn(OH)2 (a) and FTIR spectra of Zn(OH)2 (b) from spent primary battery.

The caustic leaching results in a BM residue. The SEM image and EDX spectra of the residue can be seen in Figure 6. As we can see, the residue only contains Mn, O, and a small portion of residual Na. In comparison with Figure 3, the sample contains no Zn, which proves the efficient Zn recovery using such an approach. The evaluation of Zn recovery and kinetic study would be interesting to investigate, especially by employing various other base solutions [16].

Figure 6 SEM image (a), EDX mapping of Mn (b), O (c), Na (d), and EDX spectra of BM caustic leaching residue (e).
Figure 6

SEM image (a), EDX mapping of Mn (b), O (c), Na (d), and EDX spectra of BM caustic leaching residue (e).

3.4 MnCO3 characterization

The last leaching process was employed to recover the manganese oxide material. The leaching of manganese oxide is well discussed in a previous study by Sinha and Purcell [23]. When the battery is exhausted, MnO2 is largely reduced to Mn2O3. Mn2O3 can spontaneously react with dilute sulfuric acid, forming MnSO4 and a residue of insoluble MnO2, as expressed in the following equation:

(9) Mn 2 O 3(s) + H 2 SO 4(aq) → MnSO 4(aq) + MnO 2(s) + H 2 O (l) .

To further recover Mn from the unreacted MnO2, a reducing agent, glucose, is added. The reductive leaching reaction is expressed in the following equation:

(10) 12MnO 2(s) + 12H 2 SO 4(aq) + C 6 H 12 O 6(aq) → 12MnSO 4(aq) + 6CO 2(g) + 18H 2 O (l) .

The recovered MnSO4 solution was further processed via carbonate coprecipitation, forming MnCO3. The precipitation reaction can be seen in the following equation:

(11) MnSO 4(aq) + Na 2 CO 3(aq) → MnCO 3(s) + Na 2 SO 4(aq) .

Figure 6a–f displays the SEM and EDX spectra/mapping of MnCO3, exhibiting a near-perfect spherical particle with an even atomic distribution on the surface. The particle was highly uniform in both shape and size. The distribution histogram is displayed in Figure 7g. This confirms a narrow distribution of particles with submicron size. The average particle size is 0.659 µm. The formation of spherical manganese carbonate was also reported in other studies employing K2CO3 as the precipitation agent [24]. Overall, the utilization of glucose as a reducing agent improves the process’s eco-friendliness compared with other inorganic reducing agents such as SO2 gas, H2O2, and/or FeSO4 [23]. The element compositions of the MnCO3 based on EDX spectroscopy are listed in Table 3. Based on the atomic composition, Mn and O are dominant in the sample. Based on the AAS analysis, a small amount of Zn is detected due to the residual Zn leached using sulfuric acid. The Zn amount is less than 1%. Solvent extraction can be used to separate Zn and Mn; however, it is economically challenging.

Figure 7 (a) SEM image, (b) EDX mapping of MnCO3 on (c) Mn, (d) O, and (e) C, (f) EDX spectra, and (g) particle size histogram.
Figure 7

(a) SEM image, (b) EDX mapping of MnCO3 on (c) Mn, (d) O, and (e) C, (f) EDX spectra, and (g) particle size histogram.

Table 3

EDX and AAS analysis of MnCO3

Element EDX AAS
Mass composition (%) Atomic composition (%) Mass composition (%)
Mn 64.14 ± 2.11 33.6 ± 1.1 47.77 ± 2.1
C 3.19 ± 0.25 7.64 ± 0.65 —
O 32.67 ± 0.84 58.76 ± 1.5 —
Zn n.d. n.d. 0.78 ± 0.22

Figure 8 shows the XRD pattern and FTIR spectra of the MnCO3 sample. The XRD analysis of the recovered manganese carbonate product (Figure 8a) confirms the successful formation of pure rhodochrosite (MnCO3) phase with a well-defined crystalline structure. The diffraction pattern exhibits characteristic peaks at 2θ values of 31.2°, 36.0°, 38.1°, 42.1°, 45.2°, 48.2°, 51.4°, 56.2°, and 58.1°, corresponding to the (104), (006), (110), (113), (202), (024), (018), (116), (221), and (214) crystallographic planes of hexagonal MnCO3, respectively. The sharp, intense peaks with minimal background noise indicate high crystallinity and phase purity of the product, with no detectable impurity phases or residual zinc contamination. The prominence of the (104) reflection as the strongest peak is consistent with the preferred orientation typical of well-crystallized manganese carbonate formed under controlled precipitation conditions. This XRD confirmation validates the effectiveness of the reductive acid leaching followed by carbonate precipitation strategy, demonstrating that the sequential processing approach successfully separates and recovers manganese from the battery BM in a highly pure crystalline form suitable for potential reuse in battery manufacturing or other applications [25,26]. Meanwhile, the FTIR spectra (Figure 8b) confirm a sharp vibration mode of vC═O at the wavenumber range between 1,100 and 1,400, which can be assigned to a carbonate species. A slight and broad peak at wavenumbers ∼3,400 and 1,600 cm−1 indicates the presence of adsorbed H2O molecules as a result of the hydrophilic nature of carbonate.

Figure 8 XRD pattern of MnCO3 (a) and FTIR spectra of MnCO3 (b) from spent primary battery.
Figure 8

XRD pattern of MnCO3 (a) and FTIR spectra of MnCO3 (b) from spent primary battery.

3.5 Potential utilization of Zn(OH)2 and MnCO3

Based on the deep investigation of XRD, FTIR, and SEM–EDX results, both Zn(OH)2 and MnCO3 are promising products with good purity. These products can be used as precursors for many products. The submicron size of the samples can be used for the development of nanoparticles. The nanoparticle products can be used as catalysts, sensors, adsorbents, and energy storage applications [27]. Table 4 shows the products that can be derived from Zn(OH)2 and MnCO3.

Table 4

List of products derived from Zn(OH)2 and MnCO3

Precursors Products Method Ref.
Zn(OH)2 Photocatalyst ZnO Thermal degradation [28–30]
ZnO anode Thermal degradation [31–33]
Catalyst Thermal degradation [34–36]
Supercapacitor ZnO Degradation [37]
Hydrothermal
MnCO3 Li-ion cathode material (NCM) Solid state reaction, sol–gel [38–40]
Supercapacitor Thermal degradation [41,42]

Based on Table 4, the recovered Zn(OH)2 and MnCO3 were used to prepare ZnO material and LiNi0.33Mn0.33Co0.33O2 (NMC111) material. The ZnO was prepared through a simple sintering process as described in our previous study [43]. Meanwhile the NCM111 was prepared through oxalate coprecipitation [44]. The X-ray diffractogram of the materials can be seen in Figure 8.

Based on Figure 9a, the X-ray diffraction pattern displays the successful synthesis of ZnO from Zn(OH)2 recovered from spent primary batteries. The diffractogram exhibits characteristic peaks indexed to (100), (002), (101), (102), (110), and (103) planes, which perfectly match the hexagonal wurtzite structure of ZnO (JCPDS #79-2205) [32,45,46]. The high-intensity, sharp diffraction peaks indicate excellent crystallinity, while the absence of additional peaks confirms phase purity and complete conversion from the Zn(OH)2 precursor. The dominant (101) reflection and well-defined peak positions demonstrate the formation of a well-ordered crystal structure. This result validates the effectiveness of the battery recycling process in producing high-quality ZnO crystals from waste materials. In Figure 9b, the X-ray diffraction pattern shows the successful synthesis of LiNi0.33Mn0.33Co1/3O2 (NMC111) cathode material from BM-derived MnCO3. The diffractogram exhibits characteristic peaks indexed to (003), (101), (006)/(102), (104), (105), (107), and (108)/(110) planes, corresponding to the α-NaFeO2 layered structure (JCPDS #49-0524). The sharp, intense (003) and (104) reflections indicate well-defined layered ordering, while the clear splitting of the (006)/(102) and (108)/(110) doublets suggest good hexagonal structure formation. The relatively high-intensity ratio of I(003)/I(104) suggests minimal cation mixing between lithium and transition metal layers, indicating successful structural development of the NMC cathode material. High background noise can be attributed to the high Co and Mn content, which in the future can be reduced by adding a filter during XRD analysis [47,48]. These preliminary studies provide interesting topics to be developed in future research.

Figure 9 X-ray diffraction pattern of (a) ZnO and (b) NMC111.
Figure 9

X-ray diffraction pattern of (a) ZnO and (b) NMC111.

4 Conclusion

This study successfully demonstrated a selective three-stage hydrometallurgical approach for recovering high-purity zinc and manganese from spent primary zinc–carbon battery BM. The sequential process comprising water leaching, alkaline leaching, and glucose-assisted reductive acid leaching achieved exceptional metal recovery efficiencies of 98.2% for zinc and 91.2% for manganese with minimal cross-contamination. XRD analysis confirmed the formation of crystalline products, with zinc recovered as a heterogeneous phase mixture containing ZnO and Zn3(OH)4(NO3)2, while manganese was obtained as pure rhodochrosite (MnCO3). The absence of manganese phases in the zinc product XRD pattern validated the selectivity of the alkaline leaching process. SEM characterization revealed submicron-sized spherical particles for both products, while FTIR analysis confirmed the successful formation of target compounds throughout the precipitation processes. The glucose-mediated reductive leaching represents a novel approach for manganese extraction, offering controlled reduction conditions that effectively convert insoluble Mn(iv) oxides to extractable Mn(ii) species. The recovered high-purity zinc and manganese products demonstrate significant potential as precursor materials for advanced applications in sustainable energy storage technologies, catalysts, and environmental remediation. This environmentally sustainable approach provides an effective solution for battery waste management while recovering valuable metals, offering strong potential for industrial scale-up implementation.

Funding information

This research is financially supported by Lembaga Penelitian dan Pengabdian Masyarakat (LPPM) Universitas Sebelas Maret through Research Group Grant (HGR) with contract number 194.2/UN27.22/PT.01.03/2024.

  1. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and consented to its submission to the journal, reviewed all the results and approved the final version of the manuscript. Cornelius Satria Yudha prepared the conceptualization, developed the methodology, and wrote the final manuscript. Naufal Atha Winard and Anggraini Putri performed the experiments and data curation. Meidiana Arinawati and Enni Apriliyani performed data analysis and project administration.

  2. Conflict of interest: Authors state no conflict of interest.

  3. Data availability statement: The data that support the findings of this study are available from the corresponding author upon reasonable request.

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Received: 2025-01-03
Revised: 2025-07-26
Accepted: 2025-08-22
Published Online: 2025-09-25

© 2025 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/eng-2025-0134
Keywords for this article
batteries; hydrometallurgy; leaching; morphology; recovery
Creative Commons
BY 4.0

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