INCORPORATION OF ALUMINUM-RICH SALT SALG IN BAUXITIC-TYPE REFRACTORIES. 193 Aveiro, Portugal

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1 INCORPORATION OF ALUMINUM-RICH SALT SALG IN BAUXITIC-TYPE REFRACTORIES D.A. Pereira 1, J.A. Labrincha 2 1 Mechanical Engineering Dept., ISEP, 4200 Porto, Portugal 2 Ceramics and Glass Engineering Dept., UIMC, University of Aveiro, Aveiro, Portugal The aluminum industry is affected by pressure from society to reduce its negative impact on the environment. This has resulted in tremendous efforts to cut energy consumption and to reduce waste by improving production methods and by introducing new technologies 1. Salt slags produced from aluminum scrap re-melting processes are generally considered as toxic and hazardous wastes, and a suitable washing treatment is required to allow its use 2. The large amount normally produced and the difficulties on reducing their volume by proper drying or filter-pressing methods, results in high costs for their transport for disposal. The average composition of the slag seems favorable for recycling 3, to recover aluminumbased compounds, such as alumina, or for incorporation in other products. In this last field, several materials have been tried as inertization matrix, such as concrete, glass and ceramics 4-8. In the present work, the use of a bauxitic-type refractory material as an inertization matrix is attempted. 1

2 Experimental A salt slag from an aluminum-alloy producing industry (Alpor Braga, Portugal) was used in this work. The adaptability of the residue to the washing by water process was firstly studied, by doing leaching tests in several conditions and by measuring the compositions of the insoluble part and of the solution. This method is previously mentioned in the literature 2. After using a proper washing process, the toxicity classification of the slag changes from hazardous to inert. Grain size distribution of the washed residue was obtained by sieving and only the finer fraction (under 180µm, corresponding to 60wt%) was used. Its mineralogical composition was obtained by XRD and includes corundum, aluminum hydroxides as major components, and minor phases MgAl 2 O 4 and Al 2 Si 4 O 10. The average chemical composition was estimated by XRF. Finally, the thermal behavior was predicted from thermal differential (DTA) and gravimetric (TGA) analyses. The clay-based refractory formulation was also characterized, corresponding to the typical industrial processing conditions preferably followed. One industrially pre-extruded refractory paste was used as incorporation matrix (Cerâmica do Fojo - Vila Nova de Gaia, Portugal). Its chemical composition (XRF) is typical of an alumina-rich refractory product (bauxitic). All samples were fired in industrial environment, following the usual long cycle (37 hours) for such type of bricks. Two different formulations containing 11 and 18wt% salt slag were prepared. For comparison, a free-residue formulation was also tested. After 2

3 drying and firing, a common evaluation of the ceramic-based product was made, including mechanical tests, water absorption, shrinkage, and presence/leaching of soluble salts that normally exist in the wet slag. The efficiency of the inertization method was evaluated by the confirmation that only minor changes in the ceramic material properties and on processing conditions were caused by the sludge addition. The direct addition of the wet residue is attractive from a technological point of view, but after drying a preferable migration of very fine aluminum-rich particles (transported by the water) to the surface of the material was observed. This phenomenon is more evident with increasing slag contents. Preliminary drying of the residue at about 100 C strongly prevents the occurrence of this segregation, due to the formation of aluminum-rich agglomerates. However, this drying operation is strongly penalizing from an economical point of view. The mixing operation is critical in determining a good homogeneity of the batch. In order to improve the dispersibility of the slag into the ceramic matrix, the paste was consecutively extruded (three or four times) before final shaping of samples. Water addition was needed to adjust plasticity levels. The slag acts as a fluxing agent and tends to improve liquid phase formation in the matrix. For a fixed temperature, the shrinkage tends to increase with increasing slag content improving mechanical strength. Similar characteristics to the undoped composition might be obtained at lower temperatures and this improved reactivity might cause energy savings with regards to lower firing temperatures. This confirms the potential of such recycled material, not only for economical and environmental reasons but also from a 3

4 functional point of view. However, compositional specifications of refractories respecting to some elements (e.g., maximum alkalines contents) might impose incorporation limits. Water absorption evolution as a function of slag content is not coherent with the changes in the previous discussed parameters. Theoretically, stronger consolidated samples are obtained for highly contracted materials that tend to present superior mechanical resistance. At the same time, the amount of open pores should decrease and, consequently, smaller water absorption levels should be expected. The opposite trend was observed for slag-containing samples. A probable explanation for this unexpected dependence might be given by the occurrence of decomposition reactions during firing, mostly caused by the slag. Weight loss evolution with residue content supports this argument. In fact, decomposition reactions correspond to material loss and might create open pores in the structure that can persist at high temperatures if the maturing process is far from completion, as seems to happen with current samples. Higher shrinkage levels observed on heavily doped samples resulted from stronger contractions on the first stages of the firing process or even upon drying. Conclusions It is possibly within limits to incorporate washed aluminum salt slags in bauxitic-type refractories. In general, the final characteristics of the fired material tend to be better with increasing slag contents, as shown by the enhancement of the flexural strength. The fluxing characteristics of the slag might explain this 4

5 effect, as they contribute to a stronger maturing structural process. From a functional point of view, significant incorporation levels (18wt%) are permitted. However, a careful study of the final composition (e.g., admissible levels of some minor elements) and relevant special refractory characteristics should be conducted to confirm the respect for the required specifications. Acknowledgement The collaboration of Cerâmica do Fojo (Gaia, Portugal), and Alpor (Braga, Portugal) Industries is greatly appreciated. References 1. I. Alfaro, R. Ballhord, The applications of aluminium-oxide obtained from the recycling of aluminium, Proceedings of Third ASM International Conference on the Recycling of Metals, p , Ed. I Alfaro, Barcelona, Spain (1997). 2. D.A. Pereira, F. Castro, M.F. Almeida, Characterization of aluminum salt slag, Proceedings of 8th Meeting of Portuguese Materials Society, p , Ed. L.G. Rosa, Marinha Grande, Portugal (1997). 3. F. Delmas, L. Gonçalves, A. Natário, Production of alumina from Al-rich anodizing sludge, Proceedings of 8th Meeting of Portuguese Materials Society, p , Ed. L.G. Rosa, Marinha Grande, Portugal (1997). 4. Y. Carrie, Cement kiln recycling: an industrial solution to an environmental issue, Advances Instrumentation Control, (1996). 5. C.H. Drummond, R.D. Blume, P. Nevatia, Z. Gao, Vitrified glass-ceramic product development from industrial wastes. Key Engineering Materials 132-5

6 (1997). 6. M. Dondi, M. Marsigli, B. Fabbri, Recycling of industrial and urban wastes in brick production: a review, Tile & Brick Int., 13 [4] (1997). 7. J.A. Perez, R. Terradas, M.R. Manent, M. Seijas, S. Martinez, Inertization of industrial wastes in ceramic materials, Industrial Ceramics, 16 [1] 7-10 (1996). 8. D.M.S. Couto, R.F. Silva, F. Castro, J.A. Labrincha, Inertization of metallurgical sludges in clay-based ceramics, Proceeding of the 2 nd Mediterranean Clay Meeting, Vol. 2, p , Ed. C.S. Gomes, Fundação J.J. Magalhães, Aveiro, Portugal (1998). 6

7 Table I Average chemical composition (%) of washed salt slag (XRF) and bauxitic-type refractory (EDS). Fe 2 O Material SiO 2 Al 2 O 3 3 CaO MgO Na 2 O K 2 O TiO 2 Salt salg Refractory

8 Table II Relevant characteristics of dried and fired samples, as a function of slag content. R corresponds to the free-slag formulation. Formulation Shrinkage on Drying (%) Shrinkage on Firing (%) Flexural Strength After Firing (MPa) Water Absorption (%) Weight Loss (%) R R + 11% Slag R + 18% Slag Figure captions: 8

9 Figure 1 - Scheme of relevant steps used for samples preparation. Figure 2 - DTA/TGA analyses of washed salt slag. Figure 3 - Shrinkage on firing and flexural strength of final bodies, as a function of slag content. 9

10 Sludge Clay Paste Drying? Wet Mixing Plasticity Setting (water addition/removal) Extrusion (Ø1x13cm cylinders) Drying (40ºC/24hr C/12 hr) Firing (1420ºC; 3.5h) 10

11 Weight Loss (%) EXO ENDO Temperature ( C) Temperature Differential (µv) 11

12 Shrinkage (%) 2,5 2 1,5 1 0, % Slag Flexural Strength (MPa) 12

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