RESUMO
Mullite-cordierite ceramic saggar is a necessary consumable material used in the synthesis process of LiCoO2 that is easily eroded during application. In our study, we systematically investigated the characteristics and surface corrosion behavior of waste saggar samples. We divided the cross sections of waste saggar into the attached layer, hardened layer, permeability layer, and matrix layer. Then, we examined the high-temperature solid-state reactions between saggar powder and lithium carbonate or cobalt oxide to identify erosion reactants correlating with an increase in the number of recycled saggars. The results of time-of-flight secondary ion mass spectrometric analysis (TOF-SIMS) prove that the maximum erosion penetration of lithium can reach 2 mm. However, our morphology and elemental distribution analysis results show that the erosion penetration of cobalt was only 200 µm. When enough lithium carbonate reacted, lithium aluminate and lithium silicate were the main phases. Our X-ray computed tomography (X-ray CT) analysis results show that the change in phase volume before and after the reaction, including the generation of oxygen and carbon dioxide gas, led to the internal crack expansion of the material-saggar interface. Our results can contribute to improving saggar and upgrading waste saggar utilization technology.
RESUMO
Secondary aluminum dross (SAD) refers to hazardous waste from secondary aluminum refinement. It contains a large amount of aluminum nitride and fluorides that cause serious environmental pollution for direct discharge and hinder the resource utilization of SAD. However, it is difficult to remove nitride and fluoride simultaneously for their complicated phases. In this paper, the catalytic hydrolysis of SAD using NaOH as a catalyst to remove nitrides and fluorides synchronously was investigated systemically through single factor and response surface experiments. In addition, the chemical speciation and transformation of nitrides and fluorides were analyzed systematically. The catalytic hydrolysis removal mechanism was summarized. The optimal conditions for catalytic hydrolysis were established as follows: reaction temperature 96.60 °C; reaction time 2.85 h; liquid-solid ratio 9.28 mL/g and catalyst addition 12.62 wt %; and removal efficiency of nitrides and fluorides reached 99.03% and 81.93%, respectively. The mechanism of nitrides removal was that aluminum nitride was hydrolyzed to Al(OH)3 and NH3. NaOH reacting with Al(OH)3 covering on the surface of AlN and the rapid escape of NH3 promoted the hydrolysis of AlN under the catalysis of NaOH. The mechanism of fluorides removal was that the encapsulated fluoride particles were opened by catalytic hydrolysis to be dissolved in the solution. In this research, nitrides and fluorides were removed efficiently and synchronously. The hydrolysis residues can be used to prepare polyaluminum chloride (PAC) and ceramic materials. The hydrolysate can be prepared NH3·H2O by evaporative in alkaline solution. Then the solution without NH4 + was prepared Al(OH)3 by precipitation of adjusting pH value using HCl. And the remained liquid after removing NaAlO2 was used to prepare refining agent by evaporative crystallization. The work in this paper was beneficial for the utilization of SAD.
