Cellular concrete with addition of aluminum recycled foil powders Edval Gonçalves de Araújo(1), Jorge Alberto Soares Tenório(1) (1) Departamento de Engenharia Metalúrgica e de Materiais da Escola Politécnica USP Av. Prof. Mello Moraes, 2463 – Cidade Universitária, CEP: 05508-900, São Paulo, Brasil Key words: cellular concrete, aluminum recycling, aluminum milling ABSTRACT Considering its advantage of low density and favorable insulation properties, there are several applications for lightweight autoclaved aerated concrete of uniform cellular structure. The raw materials for the manufacturing of cellular concrete are Portland cement, finely grounded sand and lime. These are batched and mixed with water and metallic aluminum powder finely divided. There is a reaction between the aluminum powder and hydroxides forming millions of hydrogen bubbles throughout the mixture. The aluminum powder is the highest cost component, and the objective of this work is replacing it for another gas forming agent, like recycled foil. The foils are grinded in a high energy ball mill (attritor). Quartz sand is mixed with aluminum foil to reduce the time required for grinding, obtaining spherical particles and ensuring a uniform distribution of aluminum in the gas forming agent. The activity of this gas forming agent was determined by the gas volumetric technique. Average particle size and compressive strength of the samples were measured. The relationship between volume of the gas released during the reaction and milling conditions are presented, showing its viability for producing a high quality cellular concrete. 1. INTRODUCTION The gas developing agent commonly used in manufacturing autoclaved cellular concretes is made of aluminum powder prepared by fine particulation of pure metallic aluminum. However, in order to reduce the cost to produce cellular concrete, a process is being developed, which replaces aluminum powder by powder from recycled scrap. This recycled aluminum powder costs half as much as pure aluminum powder. 2. OBJECTIVE In the present work, the relationship between the average particle size and the H2 release potential of powders produced from recycled aluminum foil was investigated. In order to evaluate the possibility of replacing Al powder by recycled foil in autoclaved cellular concrete, blocks were molded and their compressive strength was measured as a function of apparent bulk density. 3. METHODS Scrap aluminum foil had to be reduced into granules of 10mm length and thickness less than 1mm by a knife crusher. This material was processed in an attritor mill Netzsch Molinex PE075 of 0.25 litter capacity, high density polyethylene vial, with 50g of granules, 3g Acrawax lubricant and 900g of steel spheres. The milling times were 1h, 2h, 4h, 10h and 15h. To intensify the grinding process, the aluminum granules were mixed before grinding with an abrasive material such as quartz sand in an aluminum-to-sand ratio of 1:2 (by weight). The average particle size of sand was equal to 51µm. Both systems, Al foils and Al foils with silica, were studied. The activity of the gas developing agent was determined by the gas volumetric method, that is, by the amount of gas released when the gas developing agent was mixed with Ca(OH)2 as compared with the volume released from 1g of degreased aluminum powder. The volume of the gas evolved from a 1g batch of pure aluminum powder, calculated from the equation (1) is 1245 cm3 [1], under normal conditions: 25°C and 1atm. 2Al + 3Ca(OH)2 → 3(CaO).Al2O3 + 3H2 (1) After each milling time, a sample of 1g of Al powder from foil or another sample of 3g of Al-SiO2 (because the ratio is 1Al:2SiO2, for measuring the effect of 1g of Al contained) was extracted. The parameters for analysis of effects of mill variables are: ball to powder ratio, steel ball diameter and impeller rotation. The results are the average particle size obtained by laser diffraction (Malvern Instruments Model 2600LC) and the volume of evolved gas. In statistic planning, a 23 complete factorial with two variables levels was used, the higher level with plus signal (+) and lower level with minus signal (-) [2]. Table 1 shows the notation for each variable level and Table 2 shows the coding from a complete factorial design, for each milling time (1h, 2h, 4h, 10h and 15h). Table 1 – Levels of variables of 23 factorial design. variables ball / powder ratio, by weight ball diameter impeller rotation (+) 10:1 7.50mm 1400rpm (-) 5:1 6.35mm 800rpm Table 2 – Coding from a 23 factorial design, for each milling time. test number 1 2 3 4 5 6 7 8 b/p ratio (-) (+) (-) (+) (-) (+) (-) (+) φe (-) (-) (+) (+) (-) (-) (+) (+) rpm (-) (-) (-) (-) (+) (+) (+) (+) For the evaluation of mechanical properties of cellular concrete specimens, these were molded with addition of the gas forming agents (Al and Al-SiO2). Industrial tests were carried out with a mixture comprising the following components: 249kg/m3 of sand grounded to a specific surface of 3000 cm2/g, 84kg/m3 of cement Portland, 58kg/m3 of lime and 10kg/m3 of gypsum. This cellular concrete was molded in blocks, autoclaved under 200°C and 10atm. Tests of apparent density and compressive strength were carried out following ABNT 13440 [3] and ABNT 13439 [4], respectively. 4. RESULTS AND DISCUSSION 4.1.– Particle Size Analysis The average particle size of aluminum powders obtained from foil comminution is shown in Figure 1(A). These data indicate that in all processing conditions an accentuated decrease of particle size of aluminum powder has occurred. In each milling time, it was observed that the impeller rotation was more significant in decreasing the particle size. However, this effect was not constant, reaching its maximum at 4h. Other principal effects, b/p and φe, were significant and constant between 2 and 15h, with prevalence of ball to powder ratio effect compared to ball diameter. The two-factor and three-factor interactions were not significant. 70 (A) 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 50 40 30 20 10 0 2 4 6 8 10 Time (h) 12 14 16 (B) 1200 1100 1 2 3 4 5 6 7 8 1 2 3 4 5 6 7 8 1000 900 Gas volume(ml) µm) 60 Average particle size ( 1300 800 700 600 500 400 300 200 100 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Time (h) Figure 1 – (A) Particle Size as a function of milling time. (B) Volume of evolved gas as a function of milling time. Al System: solid line curves, Al-SiO2 System: dot line curves. The numbers 1 to 8 correspond to the notation presented in Table II. The experimental procedure with the aluminum-silica system was the same used with aluminum. The dot line curves in Figure 1(A) present the particle size as a function of milling time. In this graphic it can be observed that with time increase there is an accentuated decrease of average particle size until 4h, and with a lower rate, for 10 and 15h. The Al-SiO2 particle size was smaller than in Al system. This occurred because the sand is more fragile and inserted in the aluminum foil. This sand features have contributed to a maximum rapid grinding of the mixture to the required degree of dispersity. Moreover, due to the bigger grindability of the sand and its amount, the laser diffractions results of particle size of aluminumsand system could not be compared to aluminum ones, as the diffraction analysis showed a greater number of sand particles than Al. Thus, the experiments with or without sand addition provided the aluminum particle size and the particle size of composite aluminum-silica, respectively. In the analysis of results of the variable effects it was noted that the impeller rotation velocity was once more significant. The value of this effect reached its maximum at 2h and decreased with increasing milling time. Other main effects, b/p and φe, were similar, even though smaller, to the rpm variable. Each of these effects had a peak at 2h, and their values decreased in higher milling times. The analysis of influence of atritor mill variables in both systems showed the prevalence of the impeller rotation velocity over other parameters. In fact, rpm variable was directly related to kinetic energy of the system (spheres + powder), and so, ball size and ball quantity also contributed to the final results. But, in this study, the rpm variation level from 800 to 1400 was more effective for diminishing of particle size than the variation of the two other variables, in both systems. 4.2 – Volumetric Gas Analysis The volume of hydrogen released in both systems had a similar behaviour, as shown in Figure 1(B). In the beginning of the milling there was an increase in the quantity of released gas and, after this peak, there was a gradual reduction of the H2 released. The volume released by AlSiO2 was greater than in the Al system and the maximum occurred between 2 and 4h for Al- SiO2 and around 10h in the Al system. Gas release increased with milling time (decreasing particle size). However, aluminum oxidation also increased with decreasing particle size. After the peak related above, the specific surface area was enough for oxidation to be prevalent and so gas release decreased. Then, oxidation of aluminum particles became the process controller and probably the greater alumina thickness contributed to the reduction of chemical reaction of the aluminum with lime. Therefore, the particle size and oxidation are the main factors in the reaction of bubbles production. 4.3 – Relationship between average particle size and volumetric analysis The Figure 2 shows the results of released gas as a function of average particle size. There was no direct correlation, but this data could be divided in three zones. In zone I an increase of gas release with decrease of particle size occurred. In particle size between 35 and 40µm there was a high dispersion of the values and a decrease of gas releasing rate with the decrease of particle size was observed in zone II. The zone III, with particle size smaller than 25µm, was characterized by decrease of gas volume with decrease of particle size. In the Zone I the limitation of the gas released reaction was due to the high aluminum particle size, so the milling time was not enough. In zone II, there was a balance between decrease of the particle size and powder oxidation. Finally, in zone III a decrease of particle size continued to occur, but the oxidation was so intense that promoted a low efficiency in the gas production reaction. 1200 Al Al-SiO2 Gas volume (ml) 1000 800 600 400 200 zone III zone II zone I 0 10 20 30 40 50 60 70 Average particle size (µm) Figure 2 – Average particle size in function of gas volume released. 5. Mechanical Behaviour: Apparent Density and Compressive Strength In Figure 3(A) the curves of gas released volume (by gram of contained aluminum) versus density can be observed. In the Figure 3(B) the results of density in function of compressive strength are illustrated. In both cases, the minimum squares method for the correlation analysis was used. The results show an inverse correlation between density and gas released, with the lower gas volume occurring in 1 to 2h and 10 to 15h. 1100 Al Al-SiO2 1000 Y=1078,91-0,785X+3,08E-4 X , R=0.95 Y =-178,76437+2,72292 X-0,00181 X2, R=0,96 3 ) 900 Density (kg/m (A) 2 800 700 600 500 400 0 200 400 600 800 1000 1200 Gas Volume (ml) 9 Al-SiO2 Al 8 7 Compressive Strength (MPa) (B) 2 Y=1,32449-0,00602 X+1,31855E-5 X , R=0,93 Y=-3,99947X+0,01178, R=0,98 6 5 4 3 2 1 0 400 500 600 700 800 900 1000 1100 1200 Density (kg/m3) Figure 3 – (A) Gas evolved in function of apparent density for Al and Al-SiO2. (B) Density in function of compressive strength for Al and Al-SiO2. Minimum Square Correlation. The correlation between density and compressive strength was direct. Nevertheless, only two points of the Al-SiO2 system processed for 2h, as shown in Table 3, reached the conditions established by ABNT (C12: 1,2MPa; d ≤ 450kg/m3). In the majority of the other Al-SiO2 system samples and in all Al system (Table 4), much higher densities were obtained due to the low quantity of bubbles, which were not enough to promote the required expansion. Some of the denser samples could even be classified in other strength levels of cellular concrete (C15: 1,5MPa; d ≤ 500kg/m3; C25: 2,5MPa; d ≤ 550kg/m3; C45: 4,5MPa and d ≤ 650kg/m3). Thus, the particle size and the aluminum powder agent oxidation level must be adjusted by the milling variables. The other process variables, which can be altered to obtain a certain concrete class, are the water temperature in the process and the quantity of Al agent added. Table 3 – Data of compressive strength of blocks for Al-SiO2 gas forming agent. condition (-)(-)(-) (+)(-)(-) (-)(+)(-) (+)(+)(-) (-)(-)(+) 1h 4.1±0.4 3.2±0.3 3.8±0.3 3.2±0.3 2.1±0.25 2h 4.1±0.25 3.15±0.25 2.5±0.1 3.0±0.2 1.55±0.05 4h 2.6±0.3 1.7±0.17 1.9±0.2 1.3±0.05 3.35±0.35 10h 3.35±0.25 2.9±0.1 4.0±0.3 3.3±015 5.15±0.4 15h 4.7±0.35 5.0±0.4 4.1±0.7 5.1±0.8 6.2±0.85 (+)(-)(+) 0.8±0.15 1.2±0.05 3.55±0.25 4.75±0.35 5.85±0.45 (-)(+)(+) 1.7±0.2 1.45±0.1 3±0.2 6.05±0.6 6.5±0.3 (+)(+)(+) 0.6±0.15 1.35±0.1 4.2±0.27 4.9±0.5 5.8±0.8 Table 4 - Data of compressive strength of blocks for Al gas forming agent. condition (-)(-)(-) (+)(-)(-) (-)(+)(-) (+)(+)(-) (-)(-)(+) (+)(-)(+) (-)(+)(+) (+)(+)(+) 1h 8.25±1 7.15±0.9 8.1±1.3 7.5±1 7.0±0.9 5.9±0.7 6.6±0.7 5.55±0.6 2h 6.2±0.65 5.85±0.35 5.4±0.4 6.1±0.55 5.6±0.2 4.75±0.35 4.9±0.3 4.5±0.3 4h 5.2±0.4 4.25±0.35 5.1±0.5 4.6±0.3 3.8±0.3 3.5±0.2 4.05±0.3 2.65±0.25 10h 3.1±0.25 3.05±0.3 3.8±0.2 3.5±0.2 4.5±0.5 4.35±0.35 4.1±0.7 4.2±0.45 15h 4.1±0.45 4.4±0.6 3.65±0.4 3.55±0.35 4.75±0.8 4.35±0.5 4.5±0.6 4.4±0.5 6. – Conclusion The particle size and evolved gas volume permit the milling conditions mapping, chosen the best values of process variables rpm, b/p, φe and milling time. The impeller rotation proportionated the greater effect. It is possible to produce cellular concrete blocks using powder from aluminum recycled foil. For a required density and strength combination the main parameters are milling time, oxidation level and hard particles addition. Acknowledgment: This research was supported by FAPESP under project number 00/00219-2. References: 1. B. V. Grishin, US PATENT 4,119,476, 8p., 1978 2. G. E. P. Box, W.G. Hunter, J. S. Hunter. Statistics for Experimenters, p. 307-351, 1978 3. ABNT STANDART 13440; 4p; 1995. 4. ABNT STANDART13439, 4p., 1995.
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