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Slurry Rheology Prediction Based On Hyperspectral Character 2017 Minerals en
Slurry Rheology Prediction Based On Hyperspectral Character 2017 Minerals en
Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng
A R T I C L E I N F O A B S T R A C T
Keywords: The presence of clays in mineral processing offers a number of challenges that range from valuable species
Rheology recovery to the transport of tailings. In particular, when the abundance of one or more clay types increases, the
Suspension rheology may be significantly affected. In this paper, the feasibility of using hyperspectral characterization to
Spectroscopy estimate rheological properties of mineral suspensions was studied. Towards this purpose, a set of rheology
Clay
measurements was made for slurries of different composition, combining up to three out of five minerals: three
Mineral processing
clay minerals (two bentonites from different sources and kaolin), quartz and white mica, which are the main
Geometallurgy
gangue minerals present in the Chilean copper mining industry. Using a Bingham Plastic flow model, a set of
ternary plots for Bingham viscosity and yield stress was obtained. Results show counter-intuitive behavior for
kaolin-white mica mixtures, showing a minimum for viscosity at a 2:3 ratio respectively. In addition,
mechanisms for lowering the high viscosity reached by bentonite slurries were assessed. Modelling of the
hyperspectral data produced high accuracy estimates of the mineral abundances, enabling an accurate
determination of the respective samples position in the ternary mineralogy-rheology diagrams.
⁎
Corresponding author.
E-mail address: javier.merrill@csiro.au (J. Merrill).
http://dx.doi.org/10.1016/j.mineng.2017.03.009
Received 30 June 2016; Received in revised form 22 November 2016; Accepted 25 March 2017
Available online 26 April 2017
0892-6875/ © 2017 Elsevier Ltd. All rights reserved.
J. Merrill et al. Minerals Engineering 109 (2017) 126–134
with high clay/colloidal contents the DLVO equation is highly relevant, Table 1
showing non-Newtonian flow that can have viscous, viscoelastic or Mixture design for each ternary plot, A, B and C being any three minerals from the five
selected.
elastic response. Moreover, EDL repulsion and Van der Waals attraction
effect upon the rheology of clay bearing suspensions has been acknowl- Mineral A (vol.%) Mineral B (vol.%) Mineral C (vol.%)
edged by multiple studies, through the relation observed between the
yield stress and the zeta potential due to pH (Goh et al., 2011) and other 100 – –
67.7 – 33.3
ions concentrations (Addai-Mensah, 2007).
33.3 – 67.7
Previous work (Ndlovu et al., 2014) indicates that suspensions – – 100
rheology is highly dependent on the specific clay species present in the 60 20 20
solid phase. As well, correlation has been found between the clay micro- 20 20 60
structures and rheological behavior, attributed in some part to the 67.7 33.3 –
33.3 33.3 33.3
natural shape and charge asymmetry of clay particles (Goh et al., 2011).
– 33.3 67.7
For example, bentonite slurries which are predominantly smectite in 33.3 67.7 –
composition, have been reported (Zhang and Peng, 2014; Cruz and 20 60 20
Peng, 2016; Zhang et al., 2015; Luckham and Rossi, 1999) to have – 67.7 33.3
– 100 –
greater influence on rheological properties when compared to kaolinite-
dominated slurries. This has been attributed to the face-edge and edge-
edge particles micro-structures, which contrast with kaolinite which
tend to form more compact face-face aggregates. Although the precise
nature of the physicochemical interactions of clay species is beyond the
scope of this investigation, the recognition of the complex interactions
involved plays a role in understanding rheological variability in ores
and synthetic mineral mixtures.
The present work studies the feasibility of estimating the rheological
behavior of slurries from mineral quantification models based on
hyperspectral data, which can be obtained at lower cost and time in
comparison to other characterization techniques such as XRD, SEM. The
ability to anticipate rheological behavior opens the possibility towards
developing efficient control systems for slurry holding and transport.
2.1. Methodology
Fig. 1. Mixture design over ternary plot.
Quartz (SiO2) and white mica were chosen as gangue minerals
because they are the main components in the feed of many Chilean
mineral in a sample, leading to a point on a ternary plot for viscosity
metallurgical plants. Bentonite and kaolin were used as sources of
and another for yield stress obtained from a fitted Bingham Plastic
montmorillonite and kaolinite, respectively.
Model (Kwak et al., 2005).
Rheology flow curve measurements were conducted at a bulk solids
concentration by volume of 30% (54% in weight approx.). Due to the
high viscosity and yield stress of one of the bentonites, suspensions 2.2. Materials
were restricted to 15 vol.% (Blakey and James, 2003).
Hyperspectral characterization was carried out using the Hylogger3 Five minerals were used for this study: bentonite from a deposit in
(Huntington et al., 2010). The samples were briquettes made from dry northern Chile (Bentonite A), COMACSA® bentonite (Bentonite C)
duplicates of the samples used for the suspensions. After thorough COMACSA, 2016, ground COMACSA® white mica, COMACSA® kaolin
mixing, the various mineral mixtures received no other treatment aside and finely ground quartz.
from pressure before scanning. Several spectral measurements were Quantitative X-ray diffraction analysis was conducted to determine
taken from each sample; some were used for creating models for the mineralogical composition of each material used (Table 3). All XRD
detecting the presence and the volumetric fraction of each of the five data was collected under the same experimental conditions, in the
minerals used, others were used for the evaluation of the models. angular range 2° < 2θ < 80° using Bruker® D8 equipment. These
In order to build all ternary plots, a mixture design (Ayadi et al., data compared favorably with hyperspectral analysis (see below) of the
2013) with 13 experiments was selected, as shown in Table 1 and Fig. 1. samples.
Considering that the measurements for ternary plots containing the To study the particle size distribution, a laser granulometry analysis
high viscosity bentonite were carried out with 15 vol.% and the rest at was performed for every material using Malvern® MasterSizer2000
30 vol.%, and the fact that some vertices and edges were common to equipment. These measurements were conducted in a wet environment
some triple mixture ternary diagrams, a total of 81 rheology measure- (distilled water) to replicate their true in-pulp size.
ments were made.
The density of the samples was determined using pycnometry. 2.3. Preparation of slurries
Humidity tests were performed to determine moisture contents and the
exact amounts of mineral and water to be added when preparing the Slurries were prepared by mixing specific amounts of minerals with
slurries and the briquettes. distilled and demineralized water. The pH of the synthetic slurries was
The same mixture design (Table 1 and Fig. 1) was used for the controlled by adding concentrated sulfuric acid or sodium hydroxide
hyperspectral characterization. Finally, using spectral features, mathe- solutions. The corresponding minerals were weighed according to the
matical models have been developed for detecting the presence of any requirements of each experiment. Subsequently, water was poured into
of the five minerals, and once detected, another model was applied a measuring cylinder. The weighed solids were mixed into the
towards estimating the abundance (volumetric fraction) of that specific corresponding flask with the water and manually shaken until all solids
127
J. Merrill et al. Minerals Engineering 109 (2017) 126–134
were wet. Flasks with the slurries were placed into a mechanical stirring
device for 3 h at 200 RPM to ensure their homogeneity and disaggrega-
tion, after which each flask was withdrawn for pH adjustment and
subsequent rheological measurement. No pre-shearing has been made
protocol was not conducted due to buffer effects altering the pH of the
suspension. Instead, pH equivalence has been prioritized.
Neither the temperature effect, studied by other authors (Yang
et al., 2001), nor a temperature control mechanism was considered
herein, since the room was always kept between 21 and 23 °C, meaning
no significant perturbation for the experiments.
128
J. Merrill et al. Minerals Engineering 109 (2017) 126–134
Table 3
XRD and hyperspectral characterization results.
XRD HyLogger/TSA
Fig. 4. Spectral sample of bentonite A. Dashed lines mark montmorillonite main spectral
features.
the white mica, quartz and kaolin, but seems to have problems
detecting montmorillonite, maybe confusing it with an amorphous
phase, but hyperspectral analysis confirmed the presence of montmor-
illonite in both bentonites.
The XRD characterization of the materials revealed that the white
mica was primarily muscovite (KAl2(Si3Al)O10(OH,F)2), whilst both
dickite and kaolinite (both Al2(Si2O5)(OH)4), along with minor quartz
and pyrophyllite were identified in the kaolin. Both bentonite samples
contained montmorillonite (Na,Ca)0.3(Al,Mg)2Si4O10(OH)2·nH2O, but
Fig. 5. Rheogram for bentonite A at 30 vol.%, pH 7.00.
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J. Merrill et al. Minerals Engineering 109 (2017) 126–134
would be between 100 and 200 s−1, giving a viscosity of 6.2 mPa·s and
Fig. 7. Viscosity ternary plot in vol. fraction for bentonite A, bentonite C and white mica
a yield stress of 0.16 Pa. Note that in this case the yield stress is close to at 15% Cv and pH 7.
0, resembling a Newtonian fluid.
After adjusting a Bingham Plastic flow model for each one of the 81
rheometry measurements, the results were plotted in ternary contour
diagrams, where sometimes counter-intuitive results, such as sharp
increases in viscosity and yield stress and other synergic behaviors
between minerals, are observed. From all 20 ternary plots created, two
were chosen for this work due to their outstanding non-linear mixing
effects. This corresponding phenomena is discussed in the following
sections of this work.
Table 4 presents the parameters for the Bingham model for the five
minerals used. A steep increment in Bingham viscosity and yield stress
from 15% to 30% Cv as slurries get closer to the maximum fraction of
packing is found (Alejo and Barrientos, 2009). It is noted that
rheological tests could not be performed to pure bentonite C at solids
concentrations above 10% Cv, because of the high viscosity and yield
stress. In particular, the slurry could not be poured from the flask to the
cup.
Even in small amounts, bentonite C caused a significant increase in Fig. 8. Viscosity ternary plot in vol. fraction for white mica, kaolin and quartz at 30% Cv
viscosity and yield stress, as previously found for bentonite concentra- and pH 7.
tions above 6% by weight (Bekkour et al., 2005). As indicated by Fig. 7.
Unexpectedly, bentonite A was the only mineral that dropped this sharp of suspensions with the same minerals alone. In this case, a slurry at
rise, even when there is more smectite minerals added to the pulp. This 30% Cv with pure white mica and pure kaolin, showed higher viscosity
suggests that even a minor amount of impurities in this mineral exerts a values that when combined, reaching a minimum when the ratio of
rheology modification mechanism for bentonite, being orthoclase, kaolin and white mica is 2/3 respectively.
anhydrite and andesine the candidates for this behavior or maybe a This may be explained by structure formation of white mica
synergic effect between two or more of them. Discarding kaolin and particles while bonding each other, which is cause of strong time
muscovite can take place, since these minerals were present in the other dependency for rheological properties and shear thinning behavior
materials used in this study, and no other steep drops of the rheological (Nosrati et al., 2011). Kaolin might affect these structures because of its
parameters were identified for bentonite C. fine particle size and the edge-face charge heterogeneity of the kaolinite
Another synergistic effect can be seen between white mica and particles. Quartz does not affect this behavior, keeping the minimum
kaolin (Fig. 8). In most cases, the viscosity of a suspension with viscosity at a kaolin-white mica ratio of 2/3, reaffirming the hypothesis
combined minerals has an intermediate value between the viscosities of structures being affected by electrostatic unbalances, having silica a
well-balanced crystal structure. Another hypothesis suggests that this
non-intuitive rheological behavior relies on competitive ion adsorption
Table 4
(Goldberg, 2002) due to the presence of more than one species,
Bingham model parameters adjusted for ternary vertices (pure minerals).
generating non-DLVO interactions. Synergistic effects were not ob-
Cv 30% Cv 15% served in the corresponding Bingham yield stress ternary plot, but since
Bingham flow model is inaccurate for the low shear rate region for most
Viscosity Yield stress Viscosity Yield stress suspensions in this study, it is not conclusive.
(mPa·s) (Pa) (mPa·s) (Pa)
The knowledge of the aforementioned effects could lead to bene-
Bentonite A 296.1 146.7 5.9 0.87 ficial decision making in a processing plant, allowing to control high
Bentonite C – – 440.7a 293.6a viscosities and yield stress in case they are present, possibly, with the
White Mica 52.6 14.4 6.6 0 minerals available in the mineral deposit itself.
Kaolin 57.5 35.1 5.7 1.21
Putting these features in the context of a slurry transport system,
Quartz 6.2 0.16 5.0 0
present results expose the potential to reduce water consumption via
a
For plotting purposes the missing value was replaced by 1.1 times the maximum raising the solids concentration, maintaining rheological properties
value measured, that corresponded to 400.63 mPa·s for viscosity and 266.94 Pa for yield within desired ranges, increasing the treatment capacity of the unit
stress, reached by the 66.67% bentonite C and 33.33% white mica mixture slurry, giving processes.
440.693 and 293.63 Pa for the missing values.
130
J. Merrill et al. Minerals Engineering 109 (2017) 126–134
Table 5
Mineral recognition parameters and errors in 447 samples.
Mineral Spectral feature Height/deepness limit Position limit False negatives False positives
131
J. Merrill et al. Minerals Engineering 109 (2017) 126–134
Fig. 10. White mica abundance (volumetric fraction) vs. Energy absorption in the 2300
3.4.1. Model evaluation
and 2500 nm wavelength range. The first evaluation process was to compare values given by linear
and non-linear models, using the real abundances, and then plotting the
results in ternary diagrams for visual comparison. Table 8 shows the
real abundances for the three minerals, along with measured and
modelled viscosity and yield stress.
In Fig. 12, the linear model shows a loss of curvature, occluding the
synergic effect between kaolin and white mica, while the non-linear
model shows a good fit.
For yield stress, Fig. 13 shows a large overestimation for high
values, again showing a better fit in the non-linear model.
Finally, hyperspectral data was used as an input for linear and non-
linear models towards calculating the Mean Absolute Deviation (MAD)
of the rheological properties estimation. Results are shown in Table 9.
MAD values are lower for non-linear models. These values are small
in comparison with the high viscosity or yield stress values reached by
slurries, indicating an appropriate estimation process starting from
hyper-spectral characterization and finally obtaining estimated rheolo-
gical properties.
Fig. 11. White mica abundance vs. MCscalar2. This scheme of rheology control model might be adopted in an
online hyperspectral sampling of the crusher output, towards improved
Table 6 decision making in real time to optimize the use of water or additives
Linear model fitted for white mica volumetric fraction.
for the milling or other downstream processes. Alternatively, applica-
Linear model fitted m c R2 tion of the approach in geometallurgical models might enable improved
feasibility studying, when considering predictions of rheological prop-
y = mx + c 0.2675 −0.0485 0.952 erties for the slurries that will be treated, while at the same time,
making profitable the extraction of metals from deposits with high
contents of clay minerals, through the incorporation of rheology control
Table 7
systems.
Mean absolute deviation.
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J. Merrill et al. Minerals Engineering 109 (2017) 126–134
Table 8
Data and results for fitted viscosity and yield stress models.
White Mica (vol.%) Kaolin (vol.%) Quartz (vol.%) τ (Pa) η (mPa·s) τ (Pa) η (mPa·s) τ (Pa) η (mPa·s)
Table 9
Mean Absolute Deviation for rheological properties using abundances from hyperspectral
quantification models in linear and non-linear models for viscosity and yield stress.
Acknowledgements
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