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Autoclave Design and Scale-up from Batch Test Data: A Review of Sizing Methods and Their Bases
Khosrow Nikkhah, H.A. Simons Ltd., Mining Group, 111 Dunsmuir Street, Suite 400, Vancouver V6B 5W3, BC, CANADA
ABSTRACT
A comprehensive understanding of the effects of autoclave
configuration (batch, semi-batch, continuous) on the residence
time necessary to achieve a target conversion is a prerequisite
for design of commercial scale autoclaves. Particle size
distribution, mineral and reagent concentrations, temperature
and mixing also influence the conversion.
This paper outlines the bases of using test data to predict
performance of commercial scale autoclaves. Recommendations
for coordinating test program design with selection of scale-up
method are provided. Examples are given to illustrate the
different levels of engineering effort needed to meet
corresponding levels of design optimization and accuracy.
INTRODUCTION
Commercial pressure leaching autoclaves have been in
operation since mid 1950s. Historical production data suggest
that these early autoclaves were originally designed with excess
capacity (Berezowsky, Collins, Kerfoot, and Torres, 1991).
Process development initially consisted of tests in batch
autoclaves. While in some cases this stage had been followed by
continuous pilot plant tests in multi-compartment autoclaves, in
many cases the batch test residence times were extended to the
continuous commercial stage using some factor, resulting in an
over estimation of the required autoclave volume. In some other
instances the continuous stage of testing had not been performed
or its results could not be interpreted as a continuation of batch
tests due to differences in ore composition, grind size and
reactor conditions. In such cases, it would be important to be
able to scale-up the batch test data to a multi-compartment
continuous mode using a sound approach that takes into account
both the physical and chemical aspects of the leaching reaction
as well as the reactor configuration.
Today, the fraction of capital cost of a hydrometallurgical plant
associated with the pressure autoclaves could be as high as 30%
of the total capital expenditure. Moderate over-estimation of
volume requirements can significantly drive-up such costs,
either through buying larger autoclaves or (since transporting
such units can be difficult) unneeded extra units. This can be
avoided by a thorough understanding of the effects of autoclave
configurations on scale-up to the commercial-scale units. While
it is important to avoid over-design and its associated costs, the
engineer must also ensure that possible variations in ore grade
and quantities will not lead to shortfalls in extraction efficiency
for the design residence time.
FACTORS AFFECTING AUTOCLAVE SIZE
In a recent paper on design of autoclaves for pressure leaching
of nickel laterites (King, 1996), the following have been listed
as the determining factors in the pressure autoclave size:
temperature
number of operating trains
shipping restrictions.
2
reactions in hydrometallurgy are prime candidates for analytical
treatment in this manner.
Assuming that minerals are in the form of spherical particles
that react in an aqueous phase, this treatment can be applied to
pressure leaching operations that operate under batch and
continuous configurations. In this way a more accurate model
of a leaching operation can be developed.
For both homogeneous and heterogeneous systems reaction
rate can be described to be a function of both composition and
temperature. In heterogeneous systems concentration can be
represented by the size of the spherical solid particle. For a
component A(q) in the liquid phase reacting with a solid B(s) by
the chemical equation:
Figure 1. Graphical Calculation of Reaction per Stage,
(OKane, 1963).
(1)
b dN A
1 dN B
=
= bk s C Aq
2
4rc dt
4rc2 dt
(2)
dr
1
2 drc
= b c = bk s C Aq
2 b 4rc
dt
dt
4rc
(3)
b R
bk s C Aq
(4)
= 1
rc
= 1 (1 X B )1/ 3
R
(5)
2/ 3
r
= 1 c = 1 (1 X B )
(6)
(7)
(Das)CSTR = /(1-)2/3
(8)
(9)
1 (1 X )1/ 3
M
( rs )t
c
=
Ri
(10)
M
1
1 (1 X )1/3 = ( kc C An )t
Ri
c
(11)
1 X = 1
(12)
R
1 X = 1 i
( Ri )
(Ri) =
, and
Ri
(13)
( M / c )( rs )
1
E ( t ) = e t / t
t
(14)
(15)
E (t ) =
j (t / t )
_
j 1
j (t /t )
t ( j 1)!
5
volume of each compartment was slightly short of 2 gallons.
Heating was provided to each compartment by a direct gas
burner.
Figures 2 and 3 show the batch and continuous leach curves
for the pressure oxidation tests. Figure 2 illustrates the rate of
sulfur oxidation for the batch test at 165 and 175 oC. It was
shown that in a similar fashion to first order shrinking core
reactions under surface reaction control, the reaction rate while
increasing with temperature, decreases with % sulfur converted.
90
80
160 C
175 C
60
50
100
40
90
30
80
20
70
10
0
0
20
40
60
80
100
120
% S Oxidation
% S Oxidation
100
70
60
Continuous Test
50
Model
40
30
80.00
160 C
175 C
20
40
60
80
100
120
50.00
100
40.00
90
30.00
80
20.00
70
10.00
0.00
0
20
40
60
80
100
120
% S Oxidation
% S Oxidation
60.00
90.00
70.00
10
60
Continuous Test
50
Model
40
30
20
10
0
0
20
40
60
80
100
120
140
6
1
0.98
0.96
Conversion
0.94
0.92
0.9
Model Compartment 1
Test Compartment 1
Test Compartment 2
Model Compartment 2
Test Compartment 3
Model Compartment 3
Test Compartment 4
Model Compartment 4
0.88
0.86
0.84
0.82
0.75
0.8
0.85
0.9
0.95
1.05
1.1
1.15
2.
Variables, such as reactor temperature and pressure, overpressure of the gaseous reactant, slurry density and grind
size are fixed either by relying on published data or
performing preliminary tests where one or more of these
variables are varied for a fixed residence time.
7
Having optimized the reaction conditions, the next step is to
perform a series of tests at varying residence times to produce a
leach curve showing the progression of mineral dissolution with
residence time. Performance of repeat tests to prove the
reproducibility of results is also important.
Other test results worth following are residual solids
constituents, other metal values and acid in solution. In
performing autoclave batch test programs, it is important to
maintain the focus on the goal of the entire process. For
example, when performing high pressure sulfuric acid leach tests
for a laterite, it is important to limit the acid addition to the point
where the quantity of nickel in solution reaches a maximum.
Similar high dissolution of nickel and cobalt may be achieved
by continuing to add acid, while larger quantities of other ore
constituents (e.g., iron and aluminum) are being dissolved. It is
required to follow the dissolution of these metals as well, as
high concentration in the leach solution would adversely affect
the usage of acid and neutralization reagents.
In leaching reactions, it is always necessary to consider the
complex chemistry of the process in its entirety, before deciding
on the range of results that is adequate for a batch test program.
For example, in the case of high pressure acid leach of a laterite,
while dissolution reactions are the focus, the precipitation
reaction of iron which results in the formation of hematite also
needs to be completed for a useful set of results to be obtained
for scale-up.
If the test program is performed in a batch mode, it can be
theoretically analyzed and related to a continuous operation, for
the purposes of design and scale-up. However, if the procedures
used in the laboratory tests are unnecessarily too complex, it
would be difficult to quantify the results and use them as the
basis of scale-up.
In a recent paper, (Gathje, Oberg and Simmons, 1995) a new
approach to laboratory testing for autoclave design and scale-up
is proposed, which suggests that the mode of testing should be
semi-continuous in order to be able to obtain a better
understanding of scale-up to the continuous operation. This
method starts with a normal batch test as described for the
McLaughlin sample. This test provides the initial sample for the
semi-continuous method. Then a portion of the slurry is
discharged from the batch test autoclave and replaced with fresh
feed. Each cycle is repeated until an equilibrium is reached.
The problem with this method is that it cannot be quantitatively
treated as either a batch or a continuous operation. It is
therefore difficult for it to be considered as the basis of scale-up,
unless it is used in conjunction with an unnecessarily complex
theoretical treatment which takes into account the addition and
withdrawals of mass into the reactor. This approach replaces
neither the batch nor the continuous pilot plant stage of testing.
Reactor
Temp.
Oxygen,
OverPressure
-
Ni, gpl
Co, gpl
Fe, gpl
Species
Solids,
Wt. %
Reactor
Pressure
Ni
Co
Fe
Mn
50
5
0.2
0.01
Slurry,
Wt. %:
Time,
minutes
30
45
60
75
90
105
120
120+
Repeat
Runs
10.5
Solids
Wt. %
-
CONCLUSIONS
Scale-up of leaching reactions have been performed using
models based on the shrinking core principle with and without
consideration of the particle size distribution. While models
based on the monosized particle distribution are of adequate
degree of accuracy for pre-feasibility and feasibility studies, it is
essential to consider particle size distribution in more detailed
engineering designs. Complete batch test data must be available
for the development of these models. Performance of laboratory
tests and the equipment used should be such that scale-up to
continuous operation could be achieved by a relatively simple
quantitative treatment.
Because of complexities of the reactions involved in pressure
leaching and characteristics that are particular to different modes
of operation, scale-up models cannot replace pilot plant
campaigns based on continuous operation.
8
REFERENCES
Baldwin, S.A. and Demopoulos, G.P., 1995, Assessment of
Alternative Iron Sources in the Pressure Leaching of Zinc
Concentrates Using A Reactor Model, Hydrometallurgy, 39,
pp. 147-162.
Baldwin, S.A., Demopoulos, G.P., and Papengelakis, V.G.,
1995, Mathematical Modeling of the Zinc Pressure Leach
Process, Metall. and Mat. Trans., B 26B, pp. 1035-1047.
Bartlett, R.W., 1971, Conversion and Extraction Efficiencies
for Ground Particles in Heterogeneous Process Reactors,
Metall. Trans., B 2B, pp.2999-3006.
Berezowsky, R. M. G. S., Collins, M.J., Kerfoot, D.G.E and
Torres, N., 1991, The Commercial Status of Autoclave
Technology, JOM, February, pp.9-15.
Caddel, J.R. and Hurt, D. M., 1951, Principles of Reactor
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Particulate Leaching Reactors- the Population Balance
Approach, Hydrometallurgy, 29, pp. 275-295.
Dixon, D.,1996, The Multiple Convolution Integral: A New
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Gathje, J., Oberg, K.C., and Simmons, G., 1995, Pressure
Oxidation Process Development: Beware of Laboratory Testing
Results!, Presentation at the SME Annual Meeting, Denver,
Colorado, March 6-9.
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King, D. H., 1996, Autoclave Design for Pressure Leaching of
Laterites, Presentation at Nickel/Cobalt Pressure Leaching and
Hydrometallurgy Forum, Perth, Australia, May 13-14.
Lievenspiel, 1972, Chemical Reaction Engineering, 2nd
Edition, John Wiley and Sons.
OKane, P.T., 1963, Pressure Leaching Autoclave Design,
Presentation at the 13th Annual Canadian Chemical Engineering
Conference, Montreal, Quebec, October.