IOP Conference Series: Materials Science and Engineering

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Optimisation of process parameter using Response Surface

Methodology to recover ceramic materials from bauxite mining waste
rocks
To cite this article: Ranjita Swain Mohanty et al 2018 IOP Conf. Ser.: Mater. Sci. Eng. 455 012085

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ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

Optimisation of process parameter using Response Surface

Methodology to recover ceramic materials from bauxite
mining waste rocks

1
Ranjita Swain Mohanty, 2Sunita Routray and 3Rudra Narayan Mohapatro
1,2,3
Assistant Professor, C V Raman College of Engineering, Bhubaneswar
752054, India

Abstract

The bauxite mining waste rocks is also referred as Partially LaterizedKhondalite

(PLK) a rock that is generated during mining of bauxite. PLK rocks that associated
with kaolinized khondalite rocks are being generated and dumped at the mine site as
waste material or sometimes used for back filling of abandoned mines.These rocks
contain 36.14% Al2O3, 29.57% SiO2, 15.87% of Fe2O3, 2.37% of TiO2and 15.60%
LOI.This rock cannot be used as a valuable material for any industry due to the
presence of high iron content as well as not suitable for Bayer’s process as it contains
reactive silica. Physical methods such as magnetic separation, flotation, scrubbing etc.
are not fully successful for removal of iron from PLK rocks. Leaching techniques are
the only alternative method to minimize iron content in it. This present paper deals
with leaching studies of mining waste PLK rocks during bauxite mining, is carried
out on different parameters like temperature, concentration, pulp density and time.
The brightness of the product is increased to 80% which is desirable for high valued
ceramicproducts. Hence, the optimized parameters of the leaching can be scaled up to
the industrial trials for further viability.

Keywords: Bauxite mining waste (PLK) rock, Leaching, Pulp density, Concentration,
Temperature, Time

1. Introduction

NALCO is a major aluminium producer in Odisha, India which is located at Panchpatmali,

Koraput, Odisha. In order to produce around 2.1 million tonnes of alumina per year by National
Aluminium Company (NALCO), about 6.34 million tonnes per annum of bauxite is being mined.
About 6.3 million tons per annum of Partially Laterised Khondalite (PLK) rock is also generated
during bauxite mining at NALCO, Damanjodi mine area. Bauxite mining waste contains on an
average 41–57% of Al2O3, 1–30% of Fe2O3, 1–30% of TiO2, 20–35% of SiO2 and 20–35% of loss of
ignition (LOI). This waste is not used or recycle in the present period. It is also a problem that it
cannot be used for the production of alumina. Hence, it can be used for other industrial applications
and a major resource for the industries like paint, pigment, rubber, cosmetics, ceramics, refractory and

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ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

fillers. This can be converted as a valuable material after a suitable beneficiation to remove iron,
illimanite etc.
The less number of work has been carried out on this sample, hence the literature is collected on
the basis of bauxite and clay materials. The researchers worked on bauxite and clay for removal iron
oxide using different methods like physical and chemical process techniques.
Kuys et al. (1990) studied aboutthe acid leaching of ultrafine materials such as kaolinite, boehmite
and gibbsite etc. The surface iron was removed by this process. It is also found that the removal
depends on the geological part of minerals. Goethite and hematite removed by reductive leaching. The
total iron removed of 67% using HCl from present in ROM without affecting the structure.
Rao et al. (2005) reported in their paper about the leaching of iron from PLK rock samples. The
fine grade sample leached using HCl at higher concentration and with high temperature. It is also
shown that it can be suitable for the industries.
Swain and Rao (2012) studied on kinetic study on leaching of PLK rocks to remove iron oxide.
This study was carried on leaching of fine sample containing less iron content about 5.39%. This is
suitable for filler industries as the brightness is around 80%.
The aim of this work is to optimise the leaching study using ANOVA at different conditions such
as pulp density, acid concentration, time and temperature. The developed product from bauxite mining
waste containing 15.87% of iron oxide content. The raw material produced from the bauxite mining
waste can be used in the industries like high valued ceramicmaterial.
2. MATERIALS AND METHODS
Bauxite mining waste (PLK) rock collected from the mine site of NALCO, Damanjodi from
Easternghat of Odisha. Figure 1 indicates the sample from mining to lab and prepared for leaching
study.ROM was crushed and screened through 150 µm sieve.

(a) (b)
Fig.1 (a) ROM Sample, (b) Homogonise sample
Leaching experiments were carried out in leaching reactor attached with a magnetic stirrer and a
thermometer. The variables were pulp density, acid concentration, time and temperature. Iron analysis
was carried out by using wet chemical method.
Conditions for leaching experiments
Conc. of HCl, M -[x1]: 1, 2, 3and 4
Pulp density (S/L) - [x2]: 5, 10, 15
Volume of the solid liquid solution: 100
Temperature, °C - [x3]: 40, 70,100
Time period, minute - [x4]: 60, 120,180, and 240

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ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

3. RESULTS AND DISCUSSIONS

The size analysis is shown in Fig.2 which indicates 50% of the sample passed in a screen size
below 100-micron. The physio-chemical analysis of PLK rock sample is given in Table 1that indicates
the bulk density is 1.28 gm/cc, true density is 2.6 gm/cc whereas the porosity is 52.3% and angle of
repose is 37.9º.The chemical analysis is represented in Table 1 shows that sample contains 36.14%
Al2O3, 29.57% SiO2, 15.87% of Fe2O3, 2.37% of TiO2and 15.60% LOI.

120

100
Cum. wt. percent passing

80

60

40

20

0
0 100 200 300 400
Size, micron
Fig.2 Cumulative percent passing of ground sample of PLK rocks

Table 1. Physico-chemical analysis of bauxite mining waste rock samples

Details Physical properties of the samples
Bulk density, g/cc True density, g/cc Porosity, % Angle of repose, °
PLK rock bulk material 1.28 2.6 52.3 37.9

Chemical analysis of the samples

Al2O3% SiO2% Fe2O3% TiO2% LOI%
PLK rock bulk material 36.14 29.57 15.87 2.37 15.60

During the leaching period, following minerals are being leached out with HCl.
………………………………[1]
………………………………..[2]
…………………………………..[3]

The leaching study at different variables is tabulated in Table 2. This experiment is designed using
RSM in Design Expert software. As per the design, the experiments were carried out at different
conditions. Then, the predicted result is compared to actual result by using ANOVA software.
The statistical design shows one regression analysis for the removal of iron oxide. The equation is
being presented in the coded form:

3
ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

.............................................(1)

The data indicate that the regression analysis shows the actual and predicted values match each
other. This can be very sure by seeing the R 2 value. The R2 value is 0.91 which is approaching 1. This
value shows a good relation between the predicted and actual value, this shows in Fig.3.

Table 2. Leaching study of bauxite mining waste rockswith different variables

Si. Pulp density, Concentration of Temperature, Time, hr Fe2O3,
No. % [x1] HCl, M [x2] °C [x3] [x4] %
1 5 3 70 4 62.6
2 10 3 100 4 72
3 10 3 70 3 84
4 10 4 70 4 53
5 15 2 70 3 65.2
6 10 2 40 3 2.6
7 5 3 40 3 6.3
8 15 4 70 3 99.4
9 10 2 70 4 65.6
10 10 3 40 2 6.7
11 10 2 70 2 45.5
12 15 3 40 3 25.2
13 10 3 40 4 20.2
14 10 2 100 3 95.6
15 10 3 70 3 84
16 10 3 70 3 84
17 10 3 100 2 66.4
18 5 4 70 3 62.3
19 10 3 70 3 84
20 10 4 70 2 82
21 10 4 40 3 27.2
22 15 3 70 4 99.5
23 10 4 100 3 85
24 10 3 70 3 84
25 15 3 100 3 95.1
26 15 3 70 2 99.2
27 5 3 70 2 27.2
28 5 3 100 3 95.5
29 5 2 70 3 25.6

The data shown in Table 2 indicates that the pulp density plays an important role to dissolve the
iron in HCl. At higher pulp density with lower leaching time and medium temperature the iron
dissolution is maximum. It is clearly seen that with 15% PD and at 3M HCl concentration for two

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ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

hours leaching duration, 99.2% of iron leached out. The tabulated data also indicates that the iron
leaching is constant with increase in molarity and leaching time at constant temperature.
Optimisation of the process parameter has been carried out by using MATLAB 7.0. The data from
equation 1 is being used for the optimisation. In the programme the optimisation is done on quadratic
programme for the process parameters by achieving the maximum value of the response (removal of
Fe2O3%). The minimum and maximum value for the parameters is also given in the software for
optimum removal of Fe2O3 from bauxite mining waste rocks. The optimum conditions achieved for
99% of removal of iron oxide is 15% PD with 3 M HCl concentration at 70°C for 2 hours of time
duration.

100
90
80
70
Predicted value

60
50
40
30
20
10
0
0 20 40 60 80 100
Actual value

Fig.3 ANOVA analysis for leaching of bauxite mining waste at different conditions

Table 3. Evaluation of the optimised result from the model

Si. Pulp density, Concentration of Temperature, Time, hr Fe2O3, Brightness,
No. % [x1] HCl, M [x2] °C [x3] [x4] % %
1 15 3 70 2 99.1 80.08
2 15 3 70 2 99.4 79.98
3 15 3 70 2 99.8 80.69

It is shown in Table 3 that the results obtained from the experiments at the optimum leaching
process parameter. It is observed that the brightness value depends on the removal of iron from the
sample. The experimental data may vary slightly with respect to the same process parameter. The
reason may be the residence time and leaching reaction inside the reactor or may be analysis by the
analyser. The approximate value of iron by using three consecutives is 99.4%. The brightness is
approximately 80.25%. The leached material is very much suitable as a high valued raw material for
ceramic object preparation.

Table 4. Properties of leached residue and comparison with standard of ceramic property used by
industries
Details Product (Leached residue) Standard ceramic property*
Plasticity using water, % 11.4% 32%
Shrink due to drying, % 3.45% 7% (max.)

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ICAAMM IOP Publishing
IOP Conf. Series: Materials Science and Engineering 455 (2018) 012085 doi:10.1088/1757-899X/455/1/012085

Shrink due to firing, % 10.2% 14% (max.)

Colour after calcination White Perfectly white
Grit present, % Nil 2% (max.)
Fe2O3, % 0.79% 1% (max.)
*As per BIS

The product contains 0.79% of Fe2O3and brightness value is 80.25% as given in Table 4. It also
shows that the product has the plasticity within limit. The shrinkage after firing and drying is also
shows a good result. Hence, the product satisfies the ceramic standard used by BIS. This is one of the
high valued ceramic material can be used for preparing This can be used for preparation of capacitors,
cupolas and insulators etc.

4. Conclusions

The bauxite mining waste containing PLK rocks are being generated during bauxite mining. This
waste contains reactive silica and iron content as a discolouring mineral. The optimum conditions for
removal of iron content are PD: 15%, HCl Conc.: 3 molars, Time: 2 hours and Temperature: 70°C.
The acid concentration is less required in the leaching processis more approachable for the industries
as well as in favour of the environment. The high valued leached product can be a new resource for
ceramic industry. This leached product satisfies the Indian standard properties. This ceramic raw
material can also be used for manufacturing of capacitors, cupolas and insulators etc.

5. References
[1] Kuys K, Ralston, J, Smart, R C, Sobieraj S, Wood, R, Turner, P S , 1990 Surface characterization
Iron removal and enrichment of bauxite ultrafine Miner. Eng. 3 (5) 421–435.
[2] Rao R B, Reddy P S R, Das B, Prakash, S., Rao K K, Prasad, A R Das, S K, Rajeev, Mukherjee,
Misra, V N, 2005. Studies on production of value added materials from partially Laterized
khondalite. Collaborative Project Report No T/MPET/515/July/2005, IMMT and NALCO,
Bhubaneswar.
[3] Swain, Ranjita and Rao, R B, 2012. Kinetic study on leaching of iron in Partially
LaterisedKhondalite rocks for ceramic industrial applications. International Journal of Mineral
Processing 112–113 (2012) 77–83
6. Acknowledgement
Authors are thankful to Chairman of C. V. Raman group of Institutions, Bhubaneswar, Odisha,
India for providing support to carry out the research work. One of the authors Dr.Ranjita Swain is
thankful to NALCO for funding and JNARDDC for the support to carry out the work.