Purification of Industrial Copper Electrolyte from Bismuth Impurity

This work focused on purifying copper electrolytes from a bismuth impurity on a laboratory scale. The electrolyte came from Polish copper electrorefineries with the content of main components, g/dm3: 49.6 Cu, 160 H2SO4. The electrolyte was enriched in bismuth by Bi2O3 addition. Purification of bismuth contamination was carried out using selected agents with adsorbing effects, such as barium hydroxide octahydrate, strontium carbonate, barium carbonate, barium and lead sulfates. The trials were performed until achieving the Bi level—below 0.1 g/dm3. During the experiments, it was noticed that electrolyte purification degree depends on initial Bi concentration in electrolyte, time and temperature, as well as on the type and amount of the bismuth-lowering agent. The most satisfactory results of Bi impurity removal were with additions of barium hydroxide octahydrate, strontium carbonate and barium carbonate to electrolyte at 60 °C for 1 h. These parameters revealed the highest electrolyte purification degree. Bismuth is not removed effectively from electrolytes by barium sulfate or lead sulfate addition. The efficiency of the purification process is much higher when the agents are added to the solution in the form of carbonates or hydroxides. Extending the electrolyte purification process time may cause dissolution of bismuth from the resulting precipitate and increase of bismuth concentration in electrolytes.

In-situ Confocal Laser Microscopy Study of Lead Sulfate Crystal Growth on Negative Electrode of Lead-acid Batteries

Confocal Laser Scanning Microscopy (CLSM) is a widely used technique mainly in fields of biology or multidisciplinary material sciences. Although CLSM has the ability to monitor also electrochemical processes like lead sulfate-crystal growth, nobody used CLSM for such application. We performed operando observation of the pasted active mass of negative electrode for lead-acid batteries during deep cycling. Electrode with pasted negative active mass was optimized for cycling in ECC-opto-std electrochemical cell by EL-CELL. Lead sulfate crystal growth and changes of electrode surface during cycling were observed using a laser scanning confocal microscope Olympus Lext OLS4100. We evaluate the surface changes and sulfate crystal growth. The cycling mode leads to fast gradual degradation of the negative electrode and massive growth of lead sulfate crystals. Confocal laser scanning microscopy was identified as a powerful technique for visualization of lead sulfate crystal promotion during battery cycling.

Simultaneous neutron powder diffraction and Raman spectroscopy – an approach of combining two complementary techniques

Diffraction techniques are well-established methods for crystal structure determination as well as phase identification and quantification. Raman spectroscopy can be a valuable complementary characterization technique, because in contrast to the former it yields also information on amorphous materials and it is a probe for short-range structural effects. The herein presented setup allows for simultaneous neutron diffraction and Raman spectroscopy, shown with a sample of lead sulfate under ambient conditions as a proof of principle. In order to fulfil requirements of both methods, a sapphire single-crystal is used as a sample holder. Practical considerations for successful simultaneous in situ neutron diffraction and Raman spectroscopic measurements are given.

Lead Electrodeposition from Triethylenetetramine Solution Containing Inhibitors

Lead can be efficiently electrodeposited from a number of common leaching agents such as mineral acids, carboxylic acids, and bases (hydroxides and ammonia). This paper reports the possibility to deposit lead from a triethylenetetramine solution, which is also a powerful extracting agent for lead sulfate. The high affinity of triethylenetetramine towards lead sulfate molecules makes it a promising candidate for lead recovery from various solid materials, including industrial secondary resources, sewages, and wastes. A popular methodology that can be found in the literature to recover metal from amine is based on purging a solution with carbon dioxide, resulting in lead carbonate precipitation. Here, the direct electrodeposition of lead from an amine solution was reported. The effects of the main process parameters, i.e., current density, temperature, and presence of additives, were examined to enhance the product quality. Bone glue, ethylene glycol, and polyvinylpyrolidone were used as perspective inhibitors of dendritic lead formation. It was shown that the addition of ethylene glycol can significantly reduce their formation as well as discoloration resulting from amine, producing lead metal with a 99.9% purity.

Adaptive process for improving leaching efficiency of germanium from secondary zinc oxide

Adaptive process was used to treat germanium-containing secondary zinc oxide. The leaching parameters were determined by batch experiment, and continuous experiment was conducted and the stability of the process was verified. The leaching efficiency of Zn and Ge in the batch experiments were 92.51 and 90.67%, respectively, while the leaching efficiencies of Zn and Ge in the continuous experiment were 93.53 and 88.47%, respectively. In the neutralization process, the Fe3+ concentration in the neutralized solution is within 0.025 g/L. The Fe2+in the leaching solution increased gradually, as the neutralized residue was returned to the leaching process, the Zn in leaching residue reduce and the leaching efficiency of Zn increased. The residue mainly contained zinc sulfide and lead sulfate, with some fluffy structures on the surface. The process is promising for industrial application from indicators, economy, and applicability.