IREJEST. Vol. 10. No. 1. June, 2013 PP.

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ISSN: 1597-5258

CONCENTRATION OF ITAKPE IRON ORE

C. C. Ugwuegbu, O. O. Onyemaobi, C. C. Obi Department of Materials and Metallurgical Engineering, Federal University of Technology, P. M. B. 1526, Owerri, Imo State Corresponding authors email: cugwuegbu@gmail.com ABSTRACT The concentration of Itakpe iron ore was studied in this work. Chemical analysis, grinding test and sieve analysis, riffle tabling (shaking table), magnetic separation and froth flotation were carried out on the ore sample. The results of the screen analysis showed that the 125 m sieve size retained the highest weight of ore particle of 70.43 g while the 355 m and 250 m sieve sizes showed the highest %Fe content of 35.20% each. More particles were retained in the range of 510 + 63 m and %Fe content read more in this range as well. The best result obtained for riffle tabling was 64.00% Fe content. This value was obtained at minimum water pressure and low angle of inclination (30o). Using the Davies tube magnetic separator at a current of 1.5 A and instrument minimum rate of oscillation, a concentrate with 64.96% Fe content was obtained. Concentrate from the shaking table, when separated magnetically, gave 69.44% Fe content. For concentration of processed ore using froth flotation, best results can be achieved at pH values of 8 11. Concentrates in the size range of 90 + 63 m from raw ore, when floated, gave 54.00% Fe content. Concentrates from the shaking table gave 66% Fe content, and 68.00% Fe content for concentrates from the Davies tube magnetic separator. agents) required to produce hot metal in the 1.0 Introduction blast furnace. These slag materials will also Iron ores come in the form of rocks and reduce the amount of hot metal produced minerals from which iron (Fe) can be from the blast furnace as they will dominate economically recovered. They are usually rich the burden materials. Thus to increase the in iron oxides and vary in colour from dark productivity in a modern blast furnace and grey, bright yellow, deep purple, to rusty red. also to produce hot metal economically, iron The iron itself is usually found in the form of ores should be concentrated or beneficiated. magnetite (Fe3O4), hematite (Fe2O3), goethite Beneficiation of iron ore can be defined as a (Fe2O3.H2O), limonite (2Fe2O3.3H2O) or series of processing steps, which improve the siderite (FeCO3). physical and chemical properties of ore Iron ores are the primary raw material for hot (Babich et al., 2008). High-grade iron is metal production in the blast furnace crushed for sizing, producing both fine ore as oxygen converter steelmaking route. The well as lump ore. To beneficiate low-grade modern blast furnace technology requires the ore, different methods can be used preparation of raw materials in order to ensure individually or step by step: washing, a cost-effective hot metal production (Babich screening, magnetic separation and et al., 2008). According to Delwig et al. concentration etc (Babich et al., 2008). (2007), the operation of large blast furnaces Nigeria is blessed with a large deposit of iron with low reducing agent consumption and ore at Itakpe in Kogi state. The Itakpe iron ore high output is only possible when burden belongs to the metamorphic ore not fully materials of superior quality are used. banded. The ore body is made up of banded Iron ores contain slag materials such as SiO2, schistose and granular ores (Ogbuanya, 1987). Al203, P2O5, MgO and CaO which if not The dominant minerals (iron oxide) likely to removed will increase the energy be encountered in the ore are magnetite and (consumption of carbon or other reducing hematite. The ratio of these two minerals

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Concentration of Itakpe Iron Ore

varies throughout the ore deposit (Ola et al., 2009). Apart from the iron oxide content of the ore, other oxides present in the ore are collectively regarded as gangue materials and thus should be reduced to reasonable level of tolerance if high productivity and costeffective hot metals are to be produced from the ore. Itakpe iron ore is a low-grade ore as its iron (Fe) content is about 36% (Ola et al., 2009). For cost-effective use in the blast furnace of Nigerias Ajaokuta Steel Complex, the ore needs to be concentrated or beneficiated in order to increase its iron content. This is what this study aims to achieve. 2.0 Materials and Methods 2.1 Materials Materials used for the study include Itakpe iron ore (with chemical composition of the ore shown in Table 1), resin powder, calcium silicate powder, lead oxide powder, hydrochloric acid, water, 10% starch solution, sodium silicate, aerofloat, oleic acid, calcium chloride, sodium hydroxide, hydrofluoric acid, tin chloride, potassium permanganate, stannous chloride (SnCl2), sulphuric acid, mercuric chloride, Fe indicator, potassium dichromate, sodium carbonate, orthophosphoric acid, and hydrogen peroxide. 2.2 Experimental Methods 2.2.1 Equipment The equipment used include Denver blake jaw crusher, gyratory crusher, roll crusher, riffle divider, grinding morter and pestle, universal sieving machine, Wifley shaking table, Davies tube magnetic separator with a current control panel, Denver 12 flotation machine, pH meter with pH electrode, rod mill, electronic weighing machine, desiccator, beakers, evaporating dish. 2.2.2 Crushing The ore sample in the form of lumps of rock of size 20 cm to 30 cm, weighing about 4 kg was crushed to about 10 cm in a Denver blake jaw crusher (Primary crushing). The product from the crusher was fed into the gyratory

crusher to obtain sizes of 20 to 40 mm in diameter. The product from the gyratory crusher was fed into the roll crusher to obtain sizes below 20 mm in diameter (secondary crushing). Sizes far below 20 mm in diameter were made possible by recycling in the roll crusher as many times as possible. 2.2.3 Grinding Test and Sieve Analysis The first grinding test in the rod mill was performed on a high charge with a pneumatic discharge and without control grill. 400 g of sample (crushing product) was ground. The product of the grinding operation was then placed in a universal sieving machine and after vibrating for 15 minutes, the different sieve fractions obtained were tabulated. Chemical analysis was carried out on the size fractions obtained to determine their percentage iron content. In order to obtain a coarser grain size and a wider particle size distribution, a second grinding test was performed using a peripheral discharge at 10 mm grill. The result of the sieve analysis for this grinding test was also tabulated. 2.2.4 Concentration on the Shaking Table (Gravity Concentration) The Wifely shaking table was used for this experiment. 700 g each of different ore sizes were concentrated on the shaking table at two different inclination angles (45o and 30o). For each of the angle of inclination, the water tap was made to flow at its minimum rate. Results obtained were tabulated. Chemical analysis was carried out on the concentrates and middlings obtained, to determine their percentage iron content. 2.2.5 Concentration Separation by Magnetic

The raw ore sample and the Wifely shaking table products (concentrates and middlings) were concentrated (50 g each of different sieve sizes) in the Davis tube magnetic separator at a current of 1.5 A and minimum instrument rate of oscillation, respectively. Results obtained were tabulated. Chemical analysis was also carried out on the

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concentrates and tailings obtained, determine their percentage iron content. 2.2.6 Froth Flotation

to

10 ml sodium silicate, 200 ml water, 10 ml starch solution and 200 g ore sample were ground in the rod mill for 30 minutes. The ground product was totally fed into the Denver 12 flotation cell. The pH of the mixture was observed using the pH meter and its electrode and, when necessary, sodium hydroxide was added to increase its alkalinity or hydrogen chloride added to increase its acidity. The flotation cell was set to revolve at 150 rpm and after 3 minutes of flotation, 3 ml of oleic acid was added. 4 drops of aerofloat were added to obtain enough froth. A maximum time of 15 to 20 minutes was allowed for each flotation. When the flotation reaction seemed too slow, about 0.5 g of calcium chloride was added to activate the reaction. The whole procedure was repeated for pH 6, 7, 8, 9, 10, and 11 for each ore sample being floated. This procedure was also carried out for flotation of concentrates of shaking table and magnetic separation. Results obtained were tabulated. Chemical analysis was carried out on the concentrates and tailings obtained, to determine their percentage iron content. 3.0 Results and Discussion 3.1 Grinding Test and Sieve Analysis The results of the particle size analysis are shown in Tables 2 and 3. Table 2 shows that the highest percentage weight of particles retained is 17.8% and of norminal size of 125 microns. It implies that most of the particles were retained by the 125 micron screen. This contradicts the work done by Ogbuanya (1987), in which he stated that most of the particles in Itakpe iron ore are retained by 250 micron sieve. However, it is important to note that the 250 micron sieve also retained a large amount of the ore particles (16.1% as shown in Table 2). The wider particle size distribution result (Table 3) also shows that the different constituents of the ore sample are easier to crush or grind to a particular size than others and when screened, particular

constituents settle at particular size ranges of the sieve. The particle size distribution of the ore is shown in Fig. 1. The value of P80 of the ore is about 586 microns and P50 about 234 microns. The results of chemical analysis for %Fe content of the different sieve fractions obtained from the sieve analysis of the ore are shown in Table 4. Fig. 2 shows the histogram of %Fe distribution among the sieve sizes. It was generated from Table 4. As can be seen from the histogram, the size ranges between 355 and 180 m possess particles of high %Fe content (about 35%). The size ranges 500 + 355 m and 180 + 125 m also gave high % Fe content (about 31%). These size ranges would yield better results if used for beneficiation. 3.2 Concentration on the Shaking Table Concentration on the shaking table or flowing film concentration was carried out at angle of inclination of 45o and 30o, and also at a minimum water flow rate in each case. The results obtained are shown in Tables 5 and 6. As can be seen from the tables, very little or no tailings were recovered in all cases. Percentage recovery was slightly more for the 30o angle of inclination. Recovery of concentrate was virtually the same in both cases. The results obtained from the 30o angle of inclination were analyzed to determine the %Fe content of the concentrates and middlings at different sieve sizes. The results obtained are shown in Table 7. The 250 + 180 m sieve size gave the highest %Fe composition of 64.00% in the concentrate. The least of 59.64 %Fe composition was obtained from 1000 + 710 m sieve size. The middlings gave percentage iron compositions ranging from 19.88% to 24.98%. Fig. 3 is the graph of %Fe content versus particle size plotted for the concentrates and middlings recovered from the shaking table at an inclination angle of 30o. It shows that %Fe content decreases with increasing particle size, especially for the tailings. The effect of

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Concentration of Itakpe Iron Ore

particle size on %Fe content of concentrate is not much remarkable. 3.3 Magnetic Separation The results obtained from the magnetic separation of the raw ore and the concentrates obtained from the shaking table are shown in Tables 8 and 9. As can be seen from the tables, tailings have higher weight than the concentrates. This means that the ore is rich in hematite which is a paramagnetic mineral. To recover the hematite mineral via magnetic separation, a high-intensity magnetic separation is required. Also shown in Tables 8 and 9 are the results of chemical analysis of %Fe content of the raw ore and magnetic separation concentrate. %Fe content appreciated in both cases. An average of 63% Fe was obtained for concentrate of raw ore sample. The +710 m sieve size gave the lowest value of %Fe content (58.11%) and +63 m sieve size the highest (64.96%). Highest results were obtained with samples of concentrates from shaking table (an average of 67% Fe, with +710 m sieve size yielding the lowest value of 65.32% Fe and +355 m sieve size given the highest value of 69.44% Fe the highest value obtained for all the beneficiated ore samples in this study). Fig. 4 shows critically the effect of particle size on the grade of concentrate recovered by magnetic separation of the unprocessed ore and concentrates from shaking table concentration. For tailings of both cases, the %Fe content increased with increasing particle size. This could be as a result of larger particles of the tailings being nonmagnetic iron particles which obviously were not attracted by the magnet in the Davies tube. It is important to note that hematite mineral has a high hardness when compared to magnetite. This thus confirms that the ore is more of hematite. For the concentrates of magnetic separation and riffle tabling, %Fe content decreased with increasing particle size for both cases.

3.4 Froth Flotation Ore samples floated include samples of raw ore, samples of concentrate of magnetic separation and samples of concentrates obtained from the shaking table experiment. Table of results (Table 10 13) show clearly that the higher the pH value (starting from pH 6), the higher the weight of flotation concentrate. This is more obvious in the results obtained by separating concentration of magnetic separation and riffle tabling. As shown in Tables 10 13 (percentage recovery of concentrates), more of the concentrates were recovered at pH values of 8 to 11. From the assay of results in Tables 14 to 16, %Fe content was higher when samples of magnetic separation and riffle tabling were separated. Samples of 250 +125 m gave a better result than those of 90 + 63 m of raw ore samples. On the average, samples of concentrates of magnetic separation had the highest %Fe concentration of 68%, followed by samples of concentrates of riffle tabling which had 66% and then raw ore samples which had 54%. In the graph of %Fe content versus pH (Fig. 5) for all cases, %Fe concentration is prominent at increasing pH (markedly at pH value of 8). In some cases it remained constant, increasing or decreasing very slightly up to pH value of 10 or 11. In summary, Itakpe iron ore responded well to flotation concentration at pH values of 8 11. 4.0 Conclusion Based on the findings of this study, the following conclusions have been drawn: 1. The liberation size of Itakpe iron ore is between 355 + 250 m and 250 + 180 m and is most suitable for concentration. 2. Low angles of tables inclination (below 30o) and minimum water pressure is best for flowing film (shaking table) concentration of Itakpe iron ore. 3. Hematite content of Itakpe iron ore is higher when compared to the composition of magnetite. For concentration of the ore

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through magnetic separation, highintensity magnetic separation is required. 4. Low pH values (6 to 7) are suitable for concentrating raw Itakpe iron ore via froth flotation. 5. High pH values (8 to 11) are suitable for concentrating processed Itakpe iron ore via froth flotation. 6. Itakpe iron ore concentration can best be achieved by using a combination of different ore concentrating techniques. References Babich, A., Senk, D., Gudenau, H. W., and Mavrommatis, K. Th. (2008).Ironmaking Textbook. RWTH Aachen University, Department of Ferrous Metallurgy, Germany Delwig, C., Hrtig, W., Hoffmann, M., and Lungen, H. B. (2007).Stahl Und Eisen 127. No. 6/7, S51-s66

Ogbuanya, A. D. (1987). Beneficiation of Itakpe Iron Ore. Unpublished B. Eng. Thesis, Federal University of Technology, Akure, Nigeria Ola, S. A., Usman, G. A., Odunaike, A. A., Kollere, S. M., Ajiboye, P. O., and Adeleke, A. O. (2009). Pilot Scale Froth Flotation Studies to Upgrade Nigerian Itakpe Sinter Grade Iron Ore to a MidrexGrade Super-Concentrate. Journal of Minerals and Materials Characterization and Engineering, Vol. 8, No. 5, pp 405-416 Olubambi, P. A. and Potgieter, J. H. (2005). Effectiveness of Gravity Concentration for the Beneficiation of Itakpe (Nigeria) Iron Ore Achieved through Jigging Operation, Journal of Minerals and Materials Characterization and Engineering, Vol. 4, No. 1, pp 21-30

Table 1 Chemical Composition of Itakpe Iron Ore (Olubambi and Potgieter, 2005) Mineral Fe2O3 Composition 30.88 Fe3O4 19.05 SiO2 42.05 CaO 1.25 Al2O3 3.20 MgO 0.37 TiO2 0.20

Table 2 Sieve analysis using the universal sieving machine Size fraction (m) + 1400 - 1400 + 1000 - 1000 + 710 - 710 + 500 - 500 + 355 - 355 + 250 - 250 + 180 - 180 + 125 - 125 + 90 - 90 + 63 - 63 TOTAL Weight retained (g) 3.64 9.92 23.00 37.20 45.74 63.66 49.42 70.43 31.80 27.35 33.83 395.99 Weight retained (%) 0.919 2.505 5.808 9.394 11.551 16.076 12.480 17.786 8.031 6.907 8.543 100.000 Norminalapature size (mm) 1400 1000 710 500 355 250 180 125 90 63 Cumulative Wt% of Oversize 0.919 3.424 9.233 18.627 30.178 46.254 58.734 76.520 84.550 91.457 100.000 Cumulative Wt% of Undersize 99.081 96.576 90.767 81.373 69.822 53.746 41.266 23.480 15.450 8.543 0.000

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Concentration of Itakpe Iron Ore

Table 3 Sieve Analysis for a Wider Distribution of Particle Sizes Size fraction (m) + 4000 - 4000 + 3150 - 3150 + 2000 - 2000 + 1000 - 1000 + 800 - 800 + 630 - 630 + 500 - 500 + 400 - 400 + 315 - 315 + 250 - 250 + 200 - 200 + 160 - 160 + 125 - 125 + 100 - 100 + 80 - 80 TOTAL Weight retained (g) 0.40 1.00 0.50 1.70 2.70 6.00 9.82 15.91 21.80 35.70 28.10 15.70 37.00 30.80 31.40 9.00 247.53 Weight retained (%) 0.162 0.404 0.202 0.687 1.091 2.424 3.967 6.428 8.807 14.422 11.352 6.343 14.948 12.443 12.685 3.636 100.000 Norminal apature size (mm) 4000 3150 2000 1000 800 630 500 400 315 250 200 160 125 100 80 Cumulative Wt% of Oversize 0.162 0.566 0.768 1.454 2.545 4.969 8.936 15.364 24.171 38.593 49.945 56.288 71.236 83.679 96.364 100.000 Cumulative Wt% of Undersize 99.838 99.434 99.232 98.546 97.455 95.031 91.064 84.636 75.829 61.407 50.055 43.712 28.764 16.321 3.636 0.000

Table 4 Chemical Analysis for %Fe Content of the Different Sieve Fractions Obtained from Sieve Analysis of Raw Ore Size Fraction (m) - 1400 + 1000 - 1000 + 710 - 710 + 500 - 500 + 355 - 355 + 250 - 250 + 180 - 180 + 125 - 125 + 90 - 90 + 63 - 63 Particle Size (m) - 1000 + 710 - 710 + 355 - 355 + 250 - 250 + 180 - 180 + 90 - 90 + 63 Weight of sample (g) 700 700 700 700 700 700 Norminal Size (m) 1000 710 500 355 250 180 125 90 63 %Fe 22.0 24.8 23.2 31.2 35.2 35.2 30.8 21.6 27.2 31.6 Weight of tailings (g) nil nil nil nil nil nil % Recovery

Table 5 Results Obtained by Flowing Film Concentration (Concentration on a Shaking Table) Weight of Concentrate (g) 610 618 586 590 621 625 Weight of middling (g) 62 50 57 55 49 60

96.00 95.43 91.86 92.14 95.71 97.86

* Table inclined at 45o to the horizontal; Water pressure set to the taps minimum

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Table 6 Results Obtained by Flowing Film Concentration (Concentration on a Shaking Table) Particle Size (m) - 1000 + 710 - 710 + 355 - 355 + 250 - 250 + 180 - 180 + 90 - 90 + 63 Weight of sample (g) 700 700 700 700 700 700 Weight of Concentrate (g) 621 626 618 630 628 638 Weight of middling (g) 55 59 61 41 39 37 Weight of tailings (g) 8 5 11 nil nil nil % Recovery

97.71 98.57 98.57 95.86 95.28 96.43

* Table inclined at 30o to the horizontal; Water pressure set to the taps minimum Table 7 Results Obtained by Flowing Film Concentration (Concentration on a Shaking Table) Particle Size (m) - 1000 + 710 - 710 + 355 - 355 + 250 - 250 + 180 - 180 + 90 - 90 + 63 Weight of sample (g) 700 700 700 700 700 700 Weight of Concentrate (g) 621 626 618 630 628 638 Weight of middling (g) 55 59 61 41 39 37 % Fe Content of Concentrate 59.64 63.28 63.44 64.00 62.75 63.84 % Fe Content of Middlings 19.88 24.92 23.44 24.88 25.25 25.62

* Table inclined at 30o to the horizontal; Water pressure set to the taps minimum Table 8 Magnetic Separation of Raw Ore at a Current of 1.5 A Particle Size (m) - 1000 + 710 - 710 + 355 - 355 + 250 - 250 + 180 - 180 + 90 - 90 + 63 Particle Size (m) - 1000 + 710 - 710 + 355 - 355 + 250 - 250 + 180 - 180 + 90 - 90 + 63 Weight of feed (g) 50 50 50 50 50 50 Weight of feed (g) 50 50 50 50 50 50 Weight of Concentrate (g) 12.00 17.50 18.00 16.00 11.00 15.00 Weight of Concentrate (g) 12.00 17.50 18.00 16.00 11.00 15.00 Weight of tailings (g) 34.00 24.00 28.20 25.00 30.20 30.60 Weight of tailings (g) 34.00 24.00 28.20 25.00 30.20 30.60 % Fe Content of Concentrate 58.11 61.63 62.08 60.77 64.22 64.96 % Fe Content of Concentrate 65.32 69.44 65.66 66.43 66.72 68.19 % Fe Content of Tailings 21.00 18.64 20.16 17.88 29.66 26.41 % Fe Content of Tailings 48.16 39.09 43.50 28.22 36.29 33.83

Table 9 Magnetic Separation of 30o table concentrate ore at a Current of 1.5 A

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Concentration of Itakpe Iron Ore

Table 10 Flotation Results of Raw Ore at Particle Size Class of 90 + 63 m Sample Size m) Original Weight(g) Weight of Float (g) Weight of Sink/Concentrate (g) % Recovery pH Used Sample Size (m) Original Weight (g) Weight of Float (g) Weight of Sink/Concentrate (g) % Recovery pH Used Sample Size (m) Original Weight (g) Weight of Float (g) Weight of Sink/Concentrate (g) % Recovery pH Used Sample Size (m) Original Weight(g) Weight of Float (g) Weight ofSink/Concentrate(g) % Recovery pH Used - 90 + 63 200 64 128 64.00 6 250 + 25m 200 12 169 84.50 6 - 90+ 63 200 58 108 54.00 6 - 90 + 63 200 70 101 50.50 7 250 + 25m 200 19 157 78.50 7 - 90 + 63 200 49 121 60.50 7 - 90 + 63 200 40 143 71.50 8 - 90 + 63 200 108 91 45.50 9 - 90 + 63 200 42 130 65.00 10 - 90 + 63 200 66 116 58.00 11 250 + 125 m 200 30 144 72.00 11 - 90 + 63 200 16 163 81.50 11

Table 11 Flotation Results of Raw Ore at Particle Size Class of 250 + 125 m 250 + 25m 200 14 155 77.50 8 250 + 125m 200 22 143 71.50 9 250 + 125m 200 16 140 70.00 10 - 90 + 63 200 20 178 89.00 10

Table 12 Flotation Results of Concentrates from Shaking Table (30o) - 90 + 63 200 21 171 85.50 8 - 90 + 63 200 24 169 84.50 9

Table 13 Flotation Results of Concentrates from Magnetic Separation - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 200 200 200 200 200 200 81 69 29 19 13 16 112 130 146 168 171 173 56.00 65.00 73.00 84.00 85.50 86.50 6 7 8 9 10 11

Table 14 Chemical Analysis for %Fe Content of the Floated Raw Ore Samples Size Fraction (m) - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 250 + 125 - 250 + 125 - 250 + 125 - 250 + 125 - 250 + 125 - 250 + 125 pH 6 7 8 9 10 11 6 7 8 9 10 11 %Fe Content of Concentrate 41.22 43.13 56.56 55.25 55.77 54.81 55.86 56.61 58.00 58.24 59.92 65.07 %Fe Content of Tailings 30.00 27.12 21.44 31.40 38.31 43.20 42.66 38.91 43.50 46.76 46.18 46.48

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Table 15 Chemical Analysis for %Fe Content of Concentrate of Shaking Table (30o) Size Fraction (m) - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 pH 6 7 8 9 10 11 %Fe Content of Concentrate 62.10 66.71 65.12 66.81 66.62 66.10 %Fe Content of Tailings 21.44 23.61 32.18 29.92 34.00 26.87

Table 16 Chemical Analysis for %Fe Content of Concentrate of Magnetic Separation Size Fraction (m) - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 - 90 + 63 pH 6 7 8 9 10 11 %Fe Content of Concentrate 67.21 68.04 67.98 68.60 68.66 65.81 %Fe Content of Tailings 31.50 29.50 40.56 35.39 30.18 29.60

Fig. 1 Particle size distribution curve of Itakpe iron ore

Fig. 3 Effect of particle size on %Fe content of riffle table concentrated ore

Fig. 2 Histogram of %Fe distribution of Itakpe iron ore among sieve sizes

Fig. 4 Effect of particle size on %Fe content of magnetic separated ores

Fig. 5 Effect of pH on %Fe content of floated ores