Ida De Michelis

Study on the influence of various factors in the hydrometallurgical processing of waste printed circuit boards for copper and gold recovery

The present lab-scale experimental study presents the process of leaching waste printed circuit boards (WPCBs) in order to recover gold by thioureation. Preliminary tests have shown that copper adversely affects gold extraction; therefore an oxidative leaching pre-treatment was performed in order to remove base metals. The effects of sulfuric acid concentration, hydrogen peroxide volume and temperature on the metal extraction yield were studied by analysis of variance (ANOVA). The highest copper extraction yields were 76.12% for sample A and 18.29% for sample D, after leaching with 2M H2SO4, 20 ml of 30% H2O2 at 30°C for 3h. In order to improve Cu removal, a second leaching was performed only on sample A, resulting in a Cu extraction yield of 90%. Other experiments have shown the negative effect of the stirring rate on copper dissolution. The conditions used for the process of gold extraction by thiourea were: 20 g/L thiourea, 6g/L ferric ion, 10 g/L sulfuric acid, 600 rpm stirring rate. To study the influence of temperature and particle size, this process was tested on pins manually removed from computer central processing units (CPUs) and on waste CPU for 3½ h. A gold extraction yield of 69% was obtained after 75% of Cu was removed by a double oxidative leaching treatment of WPCBs with particle sizes smaller than 2 mm.

Treatment of exhaust fluorescent lamps to recover yttrium: Experimental and process analyses

The paper deals with recovery of yttrium from fluorescent powder coming from dismantling of spent fluorescent tubes. Metals are leached by using different acids (nitric, hydrochloric and sulphuric) and ammonia in different leaching tests. These tests show that ammonia is not suitable to recover yttrium, whereas HNO(3) produces toxic vapours. A full factorial design is carried out with HCl and H(2)SO(4) to evaluate the influence of operating factors. HCl and H(2)SO(4) leaching systems give similar results in terms of yttrium extraction yield, but the last one allows to reduce calcium extraction with subsequent advantage during recovery of yttrium compounds in the downstream. The greatest extraction of yttrium is obtained by 20% w/v S/L ratio, 4N H(2)SO(4) concentration and 90°C. Yttrium and calcium yields are nearly 85% and 5%, respectively. The analysis of variance shows that acid concentration alone and interaction between acid and pulp density have a significant positive effect on yttrium solubilization for both HCl and H(2)SO(4) medium. Two models are empirically developed to estimate yttrium and calcium concentration during leaching. Precipitation tests demonstrate that at least the stoichiometric amount of oxalic acid is necessary to recover yttrium efficiently and a pure yttrium oxalate n-hydrate can be produced (99% grade). The process is economically feasible if other components of the fluorescent lamps (glass, ferrous and non-ferrous scraps) are recovered after the equipment dismantling and valorized, besides the cost that is usually paid to recycling companies for collection, treatment or final disposal of such fluorescent powders.

Fenton treatment of complex industrial wastewater: optimization of process conditions by surface response method.

Remediation of industrial wastewaters represents a stringent problem in modern society, which requires particular understanding and ad hoc solutions. In this work, we performed extensive experimental study of chemical Fenton oxidation in order to understand the optimal operative conditions to be applied in real industrial wastewaters treatment. We analyzed the effectiveness of chemical oxygen demand (COD) removal from different wastewaters within a wide range of initial COD content. We observed a maximum COD % removal of about 80%, assessing the efficiency of the process. In order to understand the role of different reagents in the final yield, we performed a factorial experimental approach on the Fentons reagents (H(2)O(2) and Fe(2+)) and analyzed the results developing an analytical second-order model. The model depends on three variables, namely: the initial [COD(i)] of the sample, the [COD(i)]/[H(2)O(2)] ratio and [H(2)O(2)]/[Fe(2+)] ratio. We obtained an accurate description of the COD % removal in different initial conditions, with a R(2)=0.85. In particular, we observed that optimal quantities of Fentons reagents are a function of the initial COD of the treated wastes.

Yttrium recovery from primary and secondary sources: A review of main hydrometallurgical processes

Yttrium is important rare earths (REs) used in numerous fields, mainly in the phosphor powders for low-energy lighting. The uses of these elements, especially for high-tech products are increased in recent years and combined with the scarcity of the resources and the environmental impact of the technologies to extract them from ores make the recycling waste, that contain Y and other RE, a priority. The present review summarized the main hydrometallurgical technologies to extract Y from ores, contaminated solutions, WEEE and generic wastes. Before to discuss the works about the treatment of wastes, the processes to retrieval Y from ores are discussed, since the processes are similar and derived from those already developed for the extraction from primary sources. Particular attention was given to the recovery of Y from WEEE because the recycle of them is important not only for economical point of view, considering its value, but also for environmental impact that this could be generated if not properly disposal.

Recovery of yttrium from fluorescent powder of cathode ray tube, CRT: Zn removal by sulphide precipitation

This work is focused on the recovery of yttrium and zinc from fluorescent powder of cathode ray tube (CRT). Metals are extracted by sulphuric acid in the presence of hydrogen peroxide. Leaching tests are carried out according to a 2(2) full factorial plan and the highest extraction yields for yttrium and zinc equal to 100% are observed under the following conditions: 3M of sulphuric acid, 10% v/v of H2O2 concentrated solution at 30% v/v, 10% w/w pulp density, 70°C and 3h of reaction. Two series of precipitation tests for zinc are carried out: a 2(2) full factorial design and a completely randomized factorial design. In these series the factors investigated are pH of solution during the precipitation and the amount of sodium sulphide added to precipitate zinc sulphide. The data of these tests are used to describe two empirical mathematical models for zinc and yttrium precipitation yields by regression analysis. The highest precipitation yields for zinc are obtained under the following conditions: pH equal to 2-2.5% and 10-12%v/v of Na2S concentrated solution at 10%w/v. In these conditions the coprecipitation of yttrium is of 15-20%. Finally further yttrium precipitation experiments by oxalic acid on the residual solutions, after removing of zinc, show that yttrium could be recovered and calcined to obtain the final product as yttrium oxide. The achieved results allow to propose a CRT recycling process based on leaching of fluorescent powder from cathode ray tube and recovery of yttrium oxide after removing of zinc by precipitation. The final recovery of yttrium is 75-80%.

Separation and recovery of glass, plastic and indium from spent LCD panels

The present paper deals with physico-mechanical pre-treatments for dismantling of spent liquid crystal displays (LCDs) and further recovery of valuable fractions like plastic, glass and indium. After a wide experimental campaign, two processes were designed, tested and optimized. In the wet process, 20%, 15% and 40% by weight of the feeding panels are recovered as plastic, glass and indium concentrate, respectively. Instead, in the dry process, only two fractions were separated: around 11% and 85% by weight are recovered as plastic and glass/indium mixture. Indium, that concentrated in the -212μm fraction, was completely dissolved by sulphuric acid leaching (0.75molL-1 H2SO4 solution, 80°C, 10%vol H2O2, pulp density 10%wt/vol, leaching time 3h). 100% of indium can be extracted from the pregnant solution with 5%wt/vol Amberlite™ resin, at room temperature and pH 3 in 24h. Indium was thus re-extracted from the resin by means of a 2molL-1 H2SO4 solution, at room temperature and S/L of 40%wt/vol.

Extraction of Zinc and Manganese from Alkaline and Zinc-Carbon Spent Batteries by Citric-Sulphuric Acid Solution

The paper is focused on the recovery of zinc and manganese from alkaline and zinc-carbon spent batteries. Metals are extracted by sulphuric acid leaching in the presence of citric acid as reducing agent. Leaching tests are carried out according to a full factorial design, and empirical equations for Mn and Zn extraction yields are determined from experimental data as a function of pulp density, sulphuric acid concentration, temperature, and citric acid concentration. The highest values experimentally observed for extraction yields were 97% of manganese and 100% of zinc, under the following operating conditions: temperature , pulp density 20%, sulphuric acid concentration 1.8 M, and citric acid 40 g . A second series of leaching tests is also performed to derive other empirical models to predict zinc and manganese extraction. Precipitation tests, aimed both at investigating precipitation of zinc during leaching and at evaluating recovery options of zinc and manganese, show that a quantitative precipitation of zinc can be reached but a coprecipitation of nearly 30% of manganese also takes place. The achieved results allow to propose a battery recycling process based on a countercurrent reducing leaching by citric acid in sulphuric solution.

Reducing acid leaching of manganiferous ore: Effect of the iron removal operation on solid waste disposal

The process of reducing acid leaching of manganiferous ore is aimed at the extraction of manganese from low grade manganese ores. This work is focused on the iron removal operation. The following items have been considered in order to investigate the effect of the main operating conditions on solid waste disposal and on the process costs: (i) type and quantity of the base agent used for iron precipitation, (ii) effective need of leaching waste separation prior to the iron removal operation, (iii) presence of a second leaching stage with the roasted ore, which might also act as a preliminary iron removal step, and (iv) effect of tailings washing on the solid waste classification. Different base compounds have been tested, including CaO, CaCO3, NaOH, and Na2CO3. The latter gave the best results concerning both the precipitation process kinetics and the reagent consumption. The filtration of the liquor leach prior to iron removal was not necessary, implying significant savings in capital costs. A reduction of chemical consumption and an increase of manganese concentration in the solution were obtained by introducing secondary leaching tests with the previously roasted ore; this additional step was introduced without a significant decrease of global manganese extraction yield. Finally, toxicity characteristic leaching procedure (TCLP) tests carried out on the leaching solid waste showed: (i) a reduction of arsenic mobility in the presence of iron precipitates, and (ii) the need for a washing step in order to produce a waste that is classifiable as not dangerous, taking into consideration the existing Environmental National Laws.

Removal of tetramethyl ammonium hydroxide from synthetic liquid wastes of electronic industry through micellar enhanced ultrafiltration

ABSTRACT In this paper, the separation of tetramethyl ammonium hydroxide (TMAH) from synthetic liquid wastes of electronic industry is carried out by using a micellar enhanced ultrafiltration (MEUF) process. This treatment represents the first step of an integrated process, aimed at the recovery of TMAH and surfactant and water reuse. The laboratory tests are carried out with an ultrafiltration module using initial solutions having a concentration of pollutant equal to 2 g/L and by adding sodium dodecyl sulfate as a surfactant, at a concentration in the range 4–10 mM/L, that is, under and above its critical micellar concentration (CMC). The experiments have been carried out at a fixed temperature of 25°C. The obtained results showed that very good percentage removals of TMAH are achieved (99%), especially when the surfactant was above the CMC. GRAPHICAL ABSTRACT

Purification of residual leach liquors from hydrometallurgical process of NiMH spent batteries through micellar enhanced ultra filtration

Hydrometallurgical processes for the treatment and recovery of metals from waste electrical and electronic equipment produce wastewaters containing heavy metals. These residual solutions cannot be discharged into the sewer without an appropriate treatment. Specific wastewater treatments integrated with the hydrometallurgical processes ensure a sustainable recycling loops of the electrical wastes to maximize the metals recovery and minimize the amount of wastes and wastewaters produced. In this research activity the efficiency of ultrafiltration combined with surfactant micelles (micellar-enhanced ultrafiltration) was tested to remove metals form leach liquors obtained after leaching of NiMH spent batteries. In the micellar-enhanced ultrafiltration, a surfactant is added into the aqueous stream containing contaminants or solute above its critical micelle concentration. When the surfactant concentration exceeding this critical value, the surfactant monomers will assemble and aggregate to form micelles having diameter larger than the pore diameter of ultrafiltration membrane. Micelles containing contaminants whose diameter is larger than membrane pore size will be rejected during ultrafiltration process, leaving only water, unsolubilized contaminants and surfactant monomers in permeate stream. The experiments are carried out in a lab-scale plant, where a tubular ceramic ultrafiltration membrane is used with adding a surfactant to concentrate heavy metals in the retentate stream, producing a permeate of purified water that can be reused inside the process, thus minimizing the fresh water consumption.