Académique Documents
Professionnel Documents
Culture Documents
By
Presented by
Fiona Sofrà
fhend@unimelb.edu.au
CONTENTS
1. INTRODUCTION ...................................................................................................2
2. DETERMINING THE EFFECT OF ORE VARIABILITY .........................................3
3. DEFINITION OF BASELINE RHEOLOGY TESTWORK PROGRAM ....................5
4. TESTING METHODS AND ISSUES......................................................................9
5. DATA ANALYSIS AND APPLICATION ...............................................................10
6. SUMMARY ROADMAP .......................................................................................11
7. CONCLUSION.....................................................................................................13
8. REFERENCES ....................................................................................................13
1. INTRODUCTION
2
Some nickel laterite slurries possess unique rheological characteristics rarely seen in the minerals
industry relating to shear history effects, whilst others possess characteristics commonly observed
in mineral suspensions. As both unique and common behaviour may be evident in one ore body, it
is essential that the variations in the deposit are identified and appropriate strategies are employed
to ensure that the plant will accommodate the feed presented.
3
1,400 Limonite 1
Limonite 2
1,200 Limonite 3
Saprolite 1
Yield Stress (Pa )
1,000 Saprolite 2
Blend 1
Blend 1 flocculated
800
600
400
200
0
0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.7
Solids Mass Fraction (x )
4.5 100
Limonite 1 90
4.0
Saprolite 2 80
3.5
70
3.0
60
2.5
50
2.0
40
1.5
30
1.0 20
0.5 10
0.0 0
0.1 1 10 100 1000
Particle Diameter ( µ m)
4
Sample aging is particularly important for flocculated samples where the flocculant may degrade
over time, samples generated at elevated temperature where cooling may affect the rheology and
samples containing clays, where clays may delaminate and swell over time. In these cases, on-site
testing is recommended at the time of sample generation and at the process temperature.
During transportation to a testing facility both aging and shear history effects may be significant. As
the sample is transported it is inevitable that the shear history experienced will differ from plant
conditions. Obviously, in the case of shear history dependent materials (where the rheology varies
with time of shear as for many nickel laterites) this will result in variations in the measured rheology
compared with plant conditions. Settling and particle size segregation is also likely, requiring the
sample to be homogenised and resuspended prior to testing.
Although extensive efforts are made to minimise the effects mentioned, they are sometimes
unavoidable and often the only prudent approach is to ensure the data is utilised with awareness of
the limitations imposed by sample preparation.
800
700
600
Yield Stress (Pa)
500
400 Limonite 1
300 Saprolite 2
200
100
0
0 50 100 150 200
Time (min)
5
There are times when it is not possible to replicate the shear history conditions anticipated in reality
(they are generally not known a priori) so understanding the rate and extent of variation in the
rheology is important for informed use of data for design or optimisation.
Although the behaviour shown in Figure 3 is common, there are instances where the effect of shear
history varies as a function of the rate of applied shear. The presence of high aspect ratio particles
in some nickel laterites results in the observed yield stress either increasing or decreasing
depending on the shear history imparted. An example is shown in Figure 4. The apparent
reversibility and range of potential structural states suggests that definition of an equilibrium
condition is purely subjective and shear history dependent. In cases where this type of behaviour is
evident, it is important to ensure that the shear conditions that will be experienced in the plant are
well understood and reproduced as closely as possible during sampling and testing.
500
Vane yield stress (Pa)
450 400rpm
400
Hand
350
mixing 450rpm
300
250
200
150
100
50 1400rpm
1400rpm
0
0 10 20 30 40 50 60
Time of shear (min)
6
1,000
Limonite 1
900 unsheared
800
Limonite 1
700 sheared
Yield Stress (Pa)
600
Saprolite 2
500 unsheared and
sheared
400
300
200
100
0
0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65
Solids Mass Fraction (x)
Figure 5: Yield stress profiles - unsheared and sheared limonite 1 and saprolite 2.
As shown in Figure 5, yield stress profiles generally display exponential behaviour. The yield stress
profile should be determined over a wide range of solids concentrations extending beyond the
anticipated operating concentration to indicate where on the curve the operational point lies. A
design operating point near the ‘elbow’ of the curve, where the yield stress increases dramatically
with minor variations in solids concentration, could be problematic because of the narrow operable
window and difficulty controlling the paste concentration to the required precision.
Contrary to the behaviour shown in Figure 5, the application of shear may result in an increase in
the yield stress at a given solids concentration. In the case of particularly friable ores, the
application of shear may cause particle degradation and an increase in the proportion of fine
particles. An increase in the fine fraction will shift the yield stress curve to the left i.e. a higher yield
stress for a given solids concentration as shown for a laterite ore in Figure 6. Conversely, a coarse
PSD will shift the curve to the right, but with a more abrupt transition from liquid to solid-like
behaviour i.e. a sharper ‘elbow’ in the curve.
200
180 laterite ore -53 micron
laterite ore -212 micron
160
laterite ore -500 micron
Yield Stress (Pa )
140
120
100
80
60
40
20
0
0.5 0.55 0.6 0.65 0.7 0.75 0.8
Solids Mass Fraction (x )
7
3.3. SHEAR STRESS VS SHEAR RATE
A flow curve, or rheogram shows the shear stress as a function of shear rate and therefore the
viscosity as a function of shear rate. Flow curves need to be measured over the anticipated
operating range indicated by yield stress profiles and may also need to encompass a range of shear
histories (from unsheared to fully sheared). Figure 7 demonstrates the importance of testing under
the appropriate conditions by showing the effect of shear and mineralogy on the flow behaviour of
three samples. All three materials in Figure 5 are at the same yield stress of 100 Pa, however the
solids concentration required to achieve this yield stress ranges from 39wt% to 52wt% and is a
function of shear history and ore type. Although these three materials possess the same yield
stress, the rheograms clearly show how different the flow characteristics are. The saprolite is best
described as a Bingham plastic and is insensitive to shear history whereas the limonite is highly
shear thinning and shear history sensitive.
The ramifications of insufficient investigation into the flow behaviour could be dramatic. If for
example, the design yield stress for autoclave feed was 100 Pa and only the saprolite rheology was
known, the pre-autoclave thickener would be operated to produce an underflow at 52wt% solids.
Clearly, the autoclave feed preparation system would fail if it was attempted to thicken the limonite
to 52wt% solids concentration as the unsheared material would behave as a paste with a yield
stress >1200 Pa (solid like and un-pumpable). The unsheared limonite has a yield stress of 100 Pa
at only 39wt% solids. However, with an understanding of the shear sensitive nature of the limonite,
it would be possible to process a sheared limonite at concentrations up to 49wt%.
250
200
Shear Stress (Pa)
150
100
Figure 7. Flow curves for sheared and unsheared laterite 1 and saprolite 2.
8
1.00 0.387
50Pa
Fraction of Lim 1 blended with Sap 2 100Pa
200Pa
0.75 0.408 0.421
Linear 100Pa Blend
0.00 0.524
Some testing methods are more appropriate for a particular application than others. However, what
is more important is that those conducting measurements and those applying the data generated
have an understanding of the issues associated with various testing methods. Rather than describe
particular test methods in detail, this section aims to comparatively discuss critical issues for each
method.
Table 1: Yield stress and pipeline pressure drop for a fixed slump height (Clayton, 2003)
Coal Tails Au Tails Pb/Zn Tails
Solids SG (kg/m3) 1450 2800 4100 *dP Prediction assumes
Solids conc. %w/w 36 75 75 Bingham viscosity=1Pa.s
Slump Height (mm) 203 (8”) 203 (8”) 203 (8”) Pipe ID = 200mm
Yield Stress (Pa) 160 275 330 Pipeline Velocity = 1m/s
Predicted Pressure 5.07 8.13 9.6 Horizontal pipeline
Drop (kPa/m)*
9
Each measurement is dependent on the shear rate and duration of shear of preceding
measurements in the sweep. As many nickel laterites are sensitive to shear history, this
approach results in the material being in a different structural state for each measurement –
essentially the same material is not being tested at each shear rate.
Particle migration away from the shearing surface may take place over the duration of the test
resulting in measurement of a low concentration region not representative of the bulk sample.
For smooth bobs rotating in a cup, slip may occur at the bob surface, again resulting in
measurement of a low concentration region not representative of the bulk sample.
For shear thinning or thixotropic slurries, the reduction in the viscosity over the duration of the
test may result in particle settling and the formation of a concentration gradient along the length
of the shearing surface.
Evaporation at high temperature may be significant, thereby increasing the concentration of the
sample being tested over the duration of a test. As most nickel laterites are processed at
elevated temperature and the yield stress and viscosity are temperature dependent, it is
important that rheology testing is conducted at the process temperature.
For the majority of slurries and pastes, ramped measurements are inappropriate and a superior
approach is to conduct individual measurements at successive shear rates with minimal, gentle
homogenisation of the sample between measurements.
A good way to check the validity of flow data from rotational testing (or any testing for that matter) is
to compare the low shear rate data with an independently measured vane yield stress. If the low
shear rate data do not coincide with the yield stress this indicates that one or more of the above
factors may be prevalent.
No matter how ‘good’ the rheological data, it is imperative that the end-user ensure that rheological
information is applied appropriately. One of the first things to consider is whether the data are
relative or absolute. Relative data, for example slump heights for a particular material or flow data
obtained for a different shear history condition to that of the process, can be useful in it’s own right,
but the user must be aware that the information may be best for ranking, comparative or ‘indication
of change’ purposes rather than direct design input.
10
Bingham Model; τ = τ yB + η B γ& (1)
The Bingham Model has historically been used for prediction of pipeline transport requirements,
where the shear rates of interest are of the order of 10 to 100s-1. For pipeline start-up conditions,
rake drive requirements and vessel agitation, the shear rates of interest are much lower (zero for
pipeline start-up conditions and rake drive requirements and 5 to 15s-1 for agitation), so the
Bingham parameters are largely unsuitable.
Although fluid models are convenient the constants τyB, τyHB, ηB,, K and n are fitting parameters only,
and may not be representative of the true flow characteristics of the material. This is particularly
relevant in the case where a highly shear thinning material is described using a Bingham model. At
high solids loadings, few slurries/pastes display true Bingham behaviour, yet Bingham parameters
are often quoted. The Bingham model extrapolates high shear rate data to zero shear rate and may
result in a significant overestimation of the true yield stress (the stress required for flow to occur)
while the constant Bingham viscosity (ηB) does not indicate the variation in the true viscosity,
defined as the ratio of the shear stress to the shear rate at a particular shear rate, especially at low
shear rates. Figure 9 shows the discrepancy between the true, vane yield stress (shown in the
legend) and the extrapolated Bingham yield stress (τyB) for three samples. Clearly, designing based
on the Bingham yield stress would result in excessive conservatism, especially at high solids
concentrations, where the Bingham yield stress may indicate unfeasible or uneconomic operation.
The Herschel-Bulkley model generally provides a far better representation of the actual material
behaviour.
800
600
Shear Stress (Pa)
500
τyB = 352Pa
400
200
Sample A. Vane yield stress 350 Pa
100 Sample B. Vane yield stress 250 Pa
Sample C. Vane yield stress 150 Pa
0
0 100 200 300 400 500 600 700
-1
Shear Rate (s )
6. SUMMARY ROADMAP
A roadmap has been developed to assist designers and operators to navigate through the
rheological questions to ask and issues to address - from sampling to testing protocols, data
analysis and informed data application. Figure 10 simplifies the complex process of rheological
characterisation by considering the effect of ore mineralogy, sample preparation and management,
baseline tests required and test methods and data analysis and application.
11
Mineralogy assessment – XRD and PSD
No
Yes
Yes
Develop shear
No Is shear history important for particular application? Yes
history test matrix
No
For further
Does rheology need to be modified by altering Yes discussion
chemistry elsewhere
No
12
7. CONCLUSION
For maximisation of the feed to a PAL process and subsequent minimisation of equipment costs for
a given throughput, a thorough understanding of the range of rheological behaviour that will be
encountered is required. A comprehensive ore characterisation and rheology testwork programme
will highlight opportunities for feed optimisation and highlight problematic issues which may be
alleviated through prudent ore blending and / or physical treatment.
It is important that nickel laterite PAL plant designers and operators are cognisant of the range of
rheological phenomena that may be encountered and the testwork required to quantify these
phenomena. The effect of concentration, temperature, shear history, shear rate, flocculation
conditions and blending must all be well understood and incorporated into the testwork programme.
A systematic framework for rheological assessment has been developed which is presented in this
paper to ensure that data obtained is relevant to the autoclave feed thickening and handling
systems and to guide the reader through a checklist of rheological questions to ask and issues to
address.
8. REFERENCES
1. Clayton, 2003 "The Importance of Rheology in Paste Fill Operations", S. Clayton (PhD) 2003.
The Univeristy of Melbourne
2. Sofrà, 2006. Rheological Assessment – A roadmap for plant designers and operators. Paste
2006. F. Sofra. Proceedings of the International Seminar on Paste and Thickened Tailings 3-7
April 2006, Limerick Ireland.
13