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Eco-friendly process for beneficiation of iron ore slimes

Conference Paper · October 2014

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Beena Rai Venugopal Tammishetti


Tata Consultancy Services Limited Tata Research Development and Design Centre
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Kaustubh vijaykumar Joshi Patel Pradip


Tata Chemicals Ltd., Innovation Centre, Pune, India Alembic Pharmaceuticals
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Eco-friendly process for beneficiation of iron ore
slimes
Beena Rai, Venugopal Tammishetti, Kaustubh Joshi and Pradip
Tata Research Development and Design Centre, a division of Tata Consultancy Services, India

ABSTRACT
Rapid depletion of high grade iron ores coupled with the increasing demand for the blast furnace
grade iron ore in recent times has shifted the research focus on the development of appropriate
technologies for the utilization of low - grade alumina rich iron ore slimes. These slimes are
currently being dumped into tailing ponds owing to their high alumina content. Typical constituent
minerals present in the Indian iron ore slimes are hematite, goethite, gibbsite and kaolinite.
Considering the fine particle size distribution (<37 microns) in the slimes, selective dispersion-
flocculation seems to be one of the most appropriate process which has been explored by us.
We present our successful results on a natural iron ore slime sample obtained from one of the mines
in India. We have been able to achieve a concentrate assaying >67% Fe, and <3% Al 2O3 and 2.8% loss
on ignition (LOI) from the slime sample assaying 60.4% Fe, 7.7% Al2O3 and 5.45% LOI with an Fe
recovery of 62-69% simply by adjusting the pulp pH. We have scaled up the process to a semi batch
scale as a prelude to commercialize it for the beneficiation of low grade iron ore slimes.
INTRODUCTION
India has rich iron ore deposits. However, the presence of relatively higher content of alumina in Indian
iron ores leads to several problems in its utilization. During mining and washing of iron ores large
amount of low-grade fines and slimes are generated which are dumped in tailing ponds as a waste. With
ever increasing demand for iron ore, industry is now looking for possible options to beneficiate these low-
grade iron ore slimes and fines. Several research groups are engaged in developing separation processes
for the beneficiation of fines and slimes (Tripathy, Singh & Bhagat, 2001; Mathur, Singh & Moudgil, 2000;
Pradip & Rai, 2000; Thella, Mukherjee & Rajashekar, 2010; Rocha, Cançado & Peres, 2010; Raghu kumar et
al., 2011; Mukherjee, Mishra & Vijay kumar, 2009; Song, Lu & Lopez-Valdivieso, 2002).
Several groups have reported on the dispersion –flocculation of iron minerals (Pradip, 2006; Pradip et al.,
1993; Pradip, 1994; Pradip, 1997; Krishnan & Iwasaki, 1983; Mathur & Moudgil, 1997; Ravishankar &
Pradip, 1988; Hanumantha Rao & Narasimhan, 1985; Weissonborn, Warren & Dunn, 1994; Liu, Zhang &
Laskowski, 2000; Laskowski, Liu & Connor, 2007; Shibata & Fuerstenau, 2003; Pascoe & Doherty, 1997;
Jain et al., 2013). However, the presence of gibbsite in the iron ores makes it difficult to separate it from
iron oxide due to their similar surface properties (Pradip, 2006). There are also reports on gravity
separation by utilizing the specific gravity differences between desired and gangue mineral (Burt, 1994;
Roy, 2009; Bazin et al., 2012; Raghukumar, Tripathy & Mohanan, 2012) as well as magnetic separation
(Svoboda, 1987). However, both gravity and magnetic separation are not effective in the beneficiation of
slimes which are typically much finer (< 37 microns). All beneficiation flow sheets have a de-sliming step
before gravity and magnetic separation since slimes hinder separation, our processes address the problem
of discarded slimes (<37 microns).
We are working on a research program focused on finding/designing of selective reagents for iron oxide –
gibbsite - kaolinite separation based on a molecular modeling computational approach developed by us
(Jain et al., 2013). In this communication we report a separation process wherein only pH of the slurry has
been used as a parameter to achieve acceptable grades without addition of any reagents.

MATERIALS AND METHODS

Materials
The natural slime sample used in this study was <400 mesh (-37 micron) and obtained from a mine in
India. The slime sample, as analyzed by wet chemical analysis, contained 60.4% Fe and 7.7% Al 2O3. The
loss on ignition (LOI) was observed to be 5.5%. X-Ray diffraction patterns were recorded using
SHIMADZU XRD 6000 powdered X-ray diffractometer (XRD). The presence of hematite (Fe2O3), goethite
(FeO(OH)), gibbsite (Al(OH)3) and kaolinite (Al2O3 2SiO2 2H2O) minerals was confirmed by XRD analysis
(Figure 1). The aqueous solutions of sodium hydroxide and nitric acid were used for adjusting the pH of
slime slurry prepared by adding dry slime sample to distilled water.
Figure 1 X-ray diffraction pattern for iron ore slimes sample (feed) for a typical test

Separation Experiments

Series Decantation Process (Batch process)


The schematic of the experimental procedure is presented in Figure 2. A slime slurry of 10% pulp density
was prepared in distilled water. The pH of slurry was adjusted to 11.5 and subjected to ultrasonication for
5 minutes. The pH was readjusted to 11.5 if any change was observed after ultrasonication. The slurry was
stirred further for 30 minutes at 100 rpm and for 3 minutes at 40 rpm using an impeller. The stirring was
discontinued and it was allowed to settle for 1 minute. After 1 minute settling, the supernatant was
decanted into another beaker and allowed to settle for another 60-90 seconds. This process of settling and
decantation was repeated for 8-10 times and all the settled portions were mixed together and labeled as
final settled portion. Both final settled portion and final suspended portion (supernatant) were dried and
analyzed by wet chemical analysis.
Figure 2 Schematic of series decantation experiments

Semi-Batch Process
The schematic of semi-batch process is presented in Figure 3. Slime slurry was kept under stirring during
the entire process. Alkaline water was taken in the process tank (tank 1). The impeller speed in the process
tank (2) was kept very low (about 5 -10 rpm) and the slime slurry was supplied to the process tank near
the impeller blade by drawing through a pipe. No pump was used to draw the slurry and height
difference was utilized to assure the flow of the slurry. The supernatant from the process tank is
simultaneously siphoned off from just below the surface of the liquid. The liquid level in the process tank
was maintained constant by adjusting the inlet and outlet flow rates. Once all the slime slurry was fed into
the process tank, additional amount of alkaline water was supplied to the process tank to maintain the
liquid level. After supplying alkaline water for some time, experiment was stopped and the samples from
process tank and gangue collection tank were dried and analyzed.
1

Figure 3 Schematic of semi-batch process

Floatex Density Separator (FDS)


The schematic of lab scale Floatex density separator is presented in Figure 4. The set up consists of two
sections: one container section and the conical bottom section. Slime slurry is fed from the top and gets
distributed in the middle of the container. Water is supplied from teeter line which helps in elutriation of
particles. The overflow is continuously collected. At the end of the experiment, slurry in the container
section and concentrate (underflow) in the conical bottom section are collected separately. All the three
samples i.e., overflow, container slurry and the under flow are dried and analyzed.
Feed

Over flow
30 cm
15 cm
Teeter water

15 cm

Under flow
Figure 4 Schematic of Floatex density separator
RESULTS AND DISCUSSION

Selection of Optimal pH
In order to study the effect of pH on the selectivity, experiments were performed in the pH range 4–12.
Experiments were done with the 800ml slime sample at 10% pulp density for 1 minute of settling. As
presented in Figure 5, the Fe grade in settled portion improved with increase in the basicity and best
results were obtained at 11.5 pH. Accordingly, subsequent experiments were conducted at 11.5 pH only.

Figure 5 Effect of pH on the selectivity

Series Decantation Process (Batch process)


The results of series decantation experiments are summarized in the Table 1. The pH of the system was
maintained at 11.5 throughout the experiment. The overall Fe grade in the settled portion was found to be
67.9% with a Fe recovery of 69.5%. The experiment was also repeated to check the reproducibility.
Table 1 Results of Series Decantation Experiments

Concentrate Tailings

Trial 1 Trial 2 Trial 1 Trial 2

Yield (Wt%) 61.8 56.8 38.2 43.2

Assay (%)

Fe 67.9 67.7 48.3 50.8

Al2O3 3.3 2.9 14.8 14.0

LOI 2.7 2.8 10.0 9.1

Fe recovery (Wt%) 69.5 63.7 30.5 36.3


Mineral-wise Separation Efficiency

A computational tool [unpublished results] was developed in our laboratory to estimate the quantitative
percentage of hematite, goethite, gibbsite and kaolinite minerals in feed, concentrate and tailings samples
based on chemical assays. It is evident from the results summarized in Table 2 that both hematite and
goethite are recovered in the concentrate while gibbsite and kaolinite are rejected in tails.

Table 2 Results of Quantitative Mineral Estimation

Chemical Assay/ Wt% Split

Feed Concentrate Tails

Wt% Split 100 (100) 56 (55.7) 44 (44.3)

Assay (%)

Fe 60.4 (59.7) 67.8 (67.2) 50.5 (50.3)

Al2O3 7.7 (5.9) 2.9 (1.4) 11.9 (11.5)

LOI 5.5 (5.0) 2.8 (2.4) 8.5 (8.3)

Silica 4.2 (3.8) 0.8 (0.2) 8.7 (8.3)

*Numbers in brackets represent reconciled values using our tool


Computed Mineralogical Composition in Wt%

Computed Mineralogical Assay Mineral Recovery in


Mineral the Concentrate, %
Feed Concentrate Tails

Hematite 63.5 81.5 40.9 71.6

Goethite 24.3 16.2 34.5 37.1

Gibbsite 4.1 1.9 6.8 26.1

Kaolinite 8.1 0.4 17.8 2.9

Semi-Batch Process
This experiment was repeated at the pulp density of 20%. The pH of the system was maintained at 11.5.
The settled portion (about 40% of the total weight) was collected as concentrate. The supernatant (tailings)
was collected, dried and analyzed separately. The settled portion comprised of 67.5% Fe and 3% Al 2O3
with a Fe recovery of 42.8%. The tailings contained 54.8% Fe with Al2O3 content of 9% (Table 3).
Table 3 Results of Semi-batch Process

Sample Yield (%) % Fe % Al2O3 % LOI

Concentrate 39.6 67.5 3.0 2.7

Tailings 60.4 54.8 9.0 6.5


Floatex Density Separator (FDS)
The pH adjusted slime slurry (4 liters) at 40% solid loading was fed to the FDS at a flow rate of 0.35 LPM.
The teeter water was supplied at a flow rate of 0.4 LPM. Both the slime slurry and teeter water were
adjusted to a pH of 11.5. At the end of the experiment, samples from overflow, container section and
underflow were collected, dried and analyzed. Results are summarized in Table 4. The improvement is
not as much as in the case of batch or semi-batch processes. The efforts are in progress to find the best
parameters like flow rates of feed slurry and teeter water to improve it further.

Table 4 Results Obtained during FDS Test Work

Sample ID Yield (%) % Fe % Al2O3 % LOI

Feed - 56.6 5.9 5.7

Overflow 6.9 50.4 7.8 9.5

Container section 71.0 55.0 6.5 6.6

Underflow 22.1 63.5 3.7 3.8

CONCLUSIONS
A sample of low grade iron ore slime has been upgraded without using any selective reagents like
dispersants and/or flocculants. This was achieved by utilizing the charges on mineral surface charge by
adjusting pH with sodium hydroxide. An upgraded fraction containing >67% Fe and <3% is obtained with
>50%yield. The yield can be increased further by increasing the number of stages in batch process as well
as number of series operations in semi-batch process. The efforts are on to develop the process further for
an industrial scale device for example, in a Floatex Density Separator.

ACKNOWLEDGEMENTS
The authors would like to thank Dr. Sivakumar Subramanian, Tata Research Development and Design
Centre, Tata Consultancy Services for his kind help in estimation of mineralogical composition from
chemical assay and Mr. K Ananth Krishnan, Chief Technology Officer, Tata Consultancy Services for
supporting this research work.

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