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School of Information Science and Engineering, Central South University, 410083, China
Institute of Control Engineering, Central South University, 410083, China
Department of Electrical and Computer Engineering, Polytechnic School of Engineering, New York University, 11201, United States
d
Department of Computer Science and Engineering, Polytechnic School of Engineering, New York University, 11201, United States
b
c
art ic l e i nf o
a b s t r a c t
Article history:
Received 1 June 2014
Received in revised form
12 July 2015
Accepted 13 July 2015
Available online 12 August 2015
This paper presents a two-layer control scheme to address the difculties in the modeling and control of
solution purication process. Two concepts are extracted from the characteristics of solution purication
process: additive utilization efciency (AUE) and impurity removal ratio (IRR). The idea of gradient
optimization of solution purication process, which transforms the economical optimization problem of
solution purication process into nding an optimal decline gradient of the impurity ion concentration
along the reactors, is proposed. A robust adaptive controller is designed to track the optimized impurity
ion concentration in the presence of process uncertainties, disturbance and saturation. Oxidation reduction potential (ORP), which is a signicant parameter of solution purication process, is also used in
the scheme. The ability of the gradient optimization scheme is illustrated with a simulated case study of a
cobalt removal process.
& 2015 Published by Elsevier Ltd.
Keywords:
Solution purication
Gradient optimization
Additive utilization efciency
Impurity removal ratio
Robust adaptive control
Oxidation reduction potential
1. Introduction
Solution purication, which belongs to the more general area of
separation science and technology, is a key step in hydrometallurgy (Flett, 1992). As a widely used approach to obtain pure
metals from their raw ores, hydrometallurgy involves phase and
status transforms of metal elements. Typically, a hydrometallurgy
process is composed of leaching, purication and electrowinning.
The raw ore is rst treated in the leaching process, in which the
valuable metal in the solid state ore is extracted and converted
into soluble salts in liquid solution. As leaching process is not
completely selective, pregnant leaching solution inevitably contains undesired impurity ions. The presence of these impurity ions
would decrease the current efciency in the subsequent electrowinning process in which pure metal is recovered, resulting in
energy waste and downgrade of product quality (Bckman &
stvold, 2000). Therefore, the pregnant leaching solution is required to be puried to a certain degree prior to nal metal
winning.
Owing to the heterogeneous property of raw ores, the types of
impurity ions in the leaching solution are not unique. Consequently, a solution purication process is composed of several substeps designed to remove different impurities. For example,
n
Corresponding author at: School of Information Science and Engineering,
Central South University, 410083, China. Fax: 86 731 88876677.
E-mail address: gwh@mail.csu.edu.cn (W. Gui).
http://dx.doi.org/10.1016/j.conengprac.2015.07.008
0967-0661/& 2015 Published by Elsevier Ltd.
90
2. Process analysis
Solution purication process is a continuous process composed
of N ( N 1, N Z ) consecutive reactors and a thickener in which
the liquidsolid separation takes place (Fig. 2 shows a solution
purication process composed of four reactors and a thickener).
Consider the reaction described by Eq. (1), along the reactors,
impurity ion B is gradually reduced by reaction with additive A
under specic reaction conditions and the assistance of catalyst.
The overow of the thickener is delivered to subsequent process.
The underow which contains crystal nucleus benecial to impurity removal is recycled to promote cementation
mB n + + nA = nAm + + mB
(1)
The technical index and the economical index of solution purication process are the impurity ion concentration of the puried
solution which reects the purication performance, and additive
consumption which relates to the production cost, respectively.
2.1. Process model
The reaction kinetics of Eq. (1) can be described by a rst-order
kinetic equation
dc
= kA s c
dt
(2)
dc1
Fin
Fin + Fu
=
c0
c1 k1A s1c1
dt
V
V
dci
Fin + Fu
Fin + Fu
=
ci 1
ci ki A si ci
dt
V
V
i = 2, 3, 4
(3)
91
mixed potential and determines the rate of all the electrode reactions by affecting the electron transfer rate between oxidant and
reductant.
ORP, which represents the comparative oxidability or reducibility of the solution and the extent of oxidation reduction
reaction, is highly related to the mixed potential of electrode reactions. The relation between ORP and reaction rate has been
studied in Sun et al. (2013). It is found that in a certain range, a
more negative ORP represents a faster reaction rate and vice versa
Ee + 2F (emix eeq )
k = A f exp
RTc
(4)
Fig. 4. Internal and external environments of purication process.
emix = peorp + q
(5)
1.6
1.4
1.2
Reaction rate (s )
where k is the reaction rate, emix is the mixed potential, eorp is ORP
of the solution, Af is the frequency factor, Ee is the standard activation energy, F is the Faraday constant, R is the ideal gas constant,
Tc is the reaction temperature, eeq is the equilibrium potential, is
the inuence factor of electrode potential variation to cathode
activation energy, p and q are the linear approximation parameters
to be identied.
Due to its signicance, in some plants (Fugleberg & Jarvinen,
1993; Sun et al., 2014), the reaction rate is controlled by adjusting
the setting value of ORP which can be monitored online continuously and controlled by changing the dosage of additive
(Fig. 3). Thus, from the above discussion, ORP is an external representation of the mixed potential, and an intermediate variable
between reaction rate and additive dosage.
x 10
0.8
0.6
0.4
0.2
0
500
510
520
530
540
ORP (mv)
550
560
570
Fig. 5. Relation between ORP and reaction rate under different conditions.
92
x 10
1.5
zw =
0.5
zi =
i=1
where z w0 =
0
500
520
540
560
580
ORP (mv)
600
620
z real
=
z all
(6)
z i = i 1
MA
V (ci 1 ci )
MB
(7)
ci 1 ci
i =
c0
(8)
MA
Vc0
MB
MA
Vc0
MB
i 1 i = z w 0 i 1 i
i=1
i=1
(9)
min
z w (1, 2, , N ) = z w0
i 1 i
i=1
st.
0 < c N = c0 1
mini i maxi ,
i cdp
i=1
N
i = 1, 2, , N
(10)
93
Gradient optimization
c0
Gradient 1
Gradient 2
Gradient 3
Gradient 4
Required technical index
out of predefined range of IRR
failed to meet the required
purification performance
within
predefined
range of IRR
0
0
t1
output value of the ith neuron in the hidden layer. The most
commonly used radial basis function is the Gaussian function:
t2
time
t3
t4
Fig. 7. Gradient optimization along reactors (ti means the time when solution
outows from reactor i (i = 1, 2, , N )).
2 / 2
i
i ( ) = e ci
(12)
min J =
i i ( )
i=1
di |2
i=1
y=
|yi
(11)
(13)
94
x = s 0 + Ax F (x) g (v)
(14)
a 0
0
a a 0
0
a a
A=
0 0
0 0
0
0
0
a
0
0
0
a 0
a a
x 0 = f0 (, p, t )
x1 = a 0 x 0 ax1 x1ga1 (v1) + d1 ( , v1, t )
x j = ax j 1 ax j x j ga j (v j ) + d j ( , v j , t )
(22)
(15)
F +F
In which, a = inV u . F (x) and g (v) are functions of state and input
variables, respectively
x1
0
F (x) =
0 0
x2 0
0 xN
(16)
g1 (v1)
g (v2 )
g (v) = 2
g
N (vN )
(17)
In which,
parameter
set
(18)
of
reactor
gi (vi ) = gi (vi ) + d g i ( , t )
(19)
]T ,
In which, = [ p, c
g i (vi ) and d g i ( , t ) are the deterministic part
and the uncertain part of gi (vi ), respectively.
In Eq. (19), g i (vi ) is saturated when input vi exceeded certain
value as shown in Fig. 6. There is a sharp corner when the saturation happens, thus backstepping technique cannot be directly
applied. In order to remove this barrier, the saturation is approximated by a smooth function (Wen, Zhou, Liu, & Su, 2011)
ai vi + bi vi2 + ci if vi vMi
gai (vi ) =
if vi < vMi
gi (vi )
x 0 = f0 (, p, t )
x1 = a 0 x 0 ax1 h1 + d1 (t )
h1 =
where h1 = x1ga1 (v1),
(23)
z1 = x1 x r1
z2 = h1 1
(24)
Vz1 =
1 2
z1
2
(25)
Vz 1 = z1z1
= z1 [a 0 x 0 ax1 z2 1 + d1 (t ) xr1]
(26)
(20)
Design
(21)
(27)
1 as
^
1 = c1z1 ax1 xr1 + a 0 sgn (z1) x^0 + sgn (z1) D1
(28)
x^0 = 0 a 0 |z1|
(29)
V1 = Vz1 +
(30)
1
x 0 x 0
0
(31)
(32)
z 3 cv if z 3 cv
sgv (z 3 ) = 0
if |z 3 | < cv
z 3 + cv if z 3 cv
(33)
^
Thus, for the following Lyapunov function, where D 3 = D3 D3
is the estimation error of D3, Theorem 2 can be obtained
(34)
(35)
1 2
D1
21
V2 = V1 + Vz2 +
(36)
V2 = z1z1 + z2 z2 +
1
1
x 0 x 0 + D 1D 1
0
1
c2 z22
(37)
h1 =
1
2
2
2 (z 3 cv ) + D3 /(23 ) if z 3 cv
2
V3 = D 3 /(23 )
if |z 3 | < cv
2
1
(z + c )2 + D /(2 ) if z c
3
v
v
3
3
2 3
v1 = g a1 1(h1/x1)
sgn (z 3 ) if |z 3 | cv
sat (z 3 ) =
if |z 3 | < cv
z 3/cv
Design
(40)
^
+ a 0 sgn (z1) x^0 c1xr1 x r(12) + sgn (z1) D1]}
^
D3 = 3 |sgv (z 3 )|
which is the bound of 1 (x1, , v1, t ), function sgv (z3 ) and sat (z3 ) are
dened as
with
Vz 2 = z2 z2 = z2 ( 1 )
(39)
^
v^1 = fv (u1) + c3 sgv (z 3 ) + D3 sat (z 3 )
1 2
z2
2
c1z12
Vz2 =
1 2
x 0
2 0
V1 = z1z1 +
95
(38)
V3 = sgv (z 3 ) z 3 +
1
D3 D3
3
(41)
(42)
96
^
V3 c3 sgv (z 3 )2 sgv (z 3 ) sgn (z 3 ) D3 + |sgv (z 3 )|D3
1
^
^
^
D 3 D3 + sgv (z 3 )[sgn (z 3 ) D3 sat (z 3 ) D3 ]
3
c3 sgv (z 3 )2 +
1
^
D3 (3 |sgv (z 3 )| D3 )
3
^
^
+ sgv (z 3 )[sgn (z 3 ) D3 sat (z 3 ) D3 ]
(43)
^
^
Notice that sgv (z3 )[sgn (z3 ) D3 sat (z3 ) D3 ] = 0, so
V3 c3 sgv (z 3 )2
(44)
z5 = vr1 v1
= vr1 v^1 + v^1 v1
= z4 z3
(45)
copper, cobalt, nickel, cadmium, indium, gallium, arsenic, antimony, and germanium. The presence of these metal ion impurities
would cause large drops of current efciency during electrowinning in which metallic zinc is recovered, resulting in energy waste
and downgrade of product quality. Thus, before electrowinning,
these metal ion impurities need to be removed to an acceptable
level. Among the impurity ions, cobalt ion is difcult to be removed and has the most detrimental effect to electrowinning, so
the result of cobalt removal is used as an index of solution purication performance.
Cobalt removal process studied in this section is composed of
four consecutive continuous stirred tank reactors and a thickener
(Fig. 2). Spent acid is supplied to provide an acid reaction environment. The solution is heated to around 80 C to guarantee
enough reaction impetus. Zinc dust and arsenic trioxide are added
into the reactors to conduct complex chemical and electrochemical
reactions with cobalt ions and residual copper ions from previous
copper removal process.
The main reactions taking place in cobalt removal process include the following:
Cu2 + + Zn = Zn2 + + Cu
(49)
(50)
(51)
z 4 = vr 1 v^1
^
= vr 1 fv (u1) c3 sgv (z 3 ) D3 sat (z 3 )
^
= 11u1 1x 0 c3 sgv (z 3 ) D3 sat (z 3 ) + vr 1
(46)
If
u1 =
1
^
[1x 0 + c3 sgv (z 3 ) + D3 sat (z 3 ) vr 1 c4 z 4 ]
11
(47)
then
z 4 = c4 z 4
(48)
4. Experimental study
In order to evaluate the feasibility and ability of the proposed
scheme, an experimental study of a cobalt removal process in a
zinc hydrometallurgy plant (Sun et al., 2014) is investigated in this
section.
4.1. Process description
Cobalt removal is an intermediary step of the solution purication process in zinc hydrometallurgy (Fig. 1). Due to the impurity of zinc concentrate, zinc sulfate solution after leaching
contains not only zinc ion, but also other metal ions, such as
dx1
Fin
Fin + Fu
=
x0
x1 k1A s1x1
dt
V
V
dxi
Fin + Fu
Fin + Fu
=
xi 1
x i ki A si x i
dt
V
V
i = 2, 3, 4
in which V is the volume of the reactor, Fin is the ow rate of the
leaching solution, Fu is the ow rate of the underow, x0 is the
impurity ion concentration of the leaching solution, xi is the efuent impurity ion concentration of the ith ( i = 1, 2, 3, 4 ) reactor,
ki and A s i are the reaction rate and reaction surface area in unit
volume of the ith ( i = 1, 2, 3, 4 ) reactor, respectively, and
Ee + 2F [(peorp + q) eeq ]
k = A f exp
RTc
(52)
A s = g s
(53)
where Af is the frequency factor, Ee is the standard activation energy, eeq is the equilibrium potential of cobalt reduction, Tc is the
reaction temperature, R is the idea gas constant, F is the Faraday
constant, gs is the precipitant content in unit volume of reactor,
eorp is the oxidationreduction potential, is the inuence factor of
electrode potential variation to cathode activation energy, is the
relation factor between surface area in unit volume of reactor and
gs, p and q are the approximation terms between oxidationreduction potential and mixed potential. The details of these
min
z w (u1, u2 , u3, u4 ) =
ui
i=1
st.
cout cindex
(54)
Table 1
Parameters in kinetic model.
Parameter Physical meaning
Unit
Value
V
gs
m3
450
A0
R
Volume of reactor
Precipitant content in unit volume of the
reactor
Relation parameter between surface area
and gs
Frequency factor of cobalt removal reaction
Ideal gas constant
Tc
F
Reaction temperature
Faraday constant
Ee
emix
eorp
eeq
p
q
97
kg/m3
m2m3/kg
1/s
J/(molK)
K
C/mol
8.314472
96485
kJ/mol
V
V
V
1
1
1
Fig. 10. Hinder effect caused by excessive zinc dust dosage.
98
0.7
Outlet cobalt ion concentration (mg/L)
4.5
Kinetic model
Practical value
3.5
Kinetic model
Practical value
0.6
0.5
0.4
0.3
0.2
10
20
30
40
50
60
70
10
80
60
70
80
40
Cobalt ion concentration
Kinetic model
Practical value
2.5
2
1.5
1
10
20
30
40
50
test point
60
70
35
30
25
20
80
10 12 14 16 18 20 22 24
time (h)
1.2
320
Kinetic model
Practical value
40
50
test point
0.5
30
20
0.8
0.6
0.4
0.2
280
260
240
220
10
20
30
40
50
test point
60
70
80
200
10
12 14
time (h)
16
18
20
22
24
99
Disturbance
50%
Disturbance
40%
Impurity removal ratio
Disturbance
30%
Reactor 1
Reactor 2
Reactor 3
Reactor 4
20%
10%
10 12 14
time (h)
16
18
20
0%
22 24
10 12 14
time (h)
16
18
20
22 24
AUE of reactor 2
100%
100%
Practical value
RBFNN
80%
60%
AUE
AUE
80%
60%
40%
40%
20%
20%
0%
12
time (h)
16
20
Practical value
RBFNN
0%
24
AUE of reactor 3
20
24
100%
Practical value
RBFNN
80%
60%
60%
40%
40%
20%
20%
12
time (h)
16
20
Practical value
RBFNN
80%
AUE
AUE
16
AUE of reactor 4
100%
0%
12
time (h)
24
0%
12
time (h)
16
20
24
100
15
Reactor1
Reactor2
Reactor3
Reactor4
10
10 12 14
time (h)
16
18
20
22 24
Fig. 20. Setting value of the impurity ion concentration of each reactor.
Table 2
Constraints on IRR of each reactor.
Reactor
Reactor 1
Reactor 2
Reactor 3
Reactor 4
Constraint on IRR
[55% 70%]
[20% 40%]
[2.5% 5%]
[1% 3%]
560
610
ORP (mv)
ORP (mv)
550
540
600
590
580
530
570
520
12
time (h)
16
20
560
24
660
650
650
640
640
630
620
610
610
4
12
time (h)
16
16
20
24
20
24
630
620
600
12
time (h)
660
ORP (mv)
ORP (mv)
20
24
600
12
time (h)
16
Another important phenomenon is that the uctuation in cobalt ion concentration is gradually attenuated from reactor 1 to
reactor 4. This is due to the constraints on the IRR of each reactor
and the use of robust adaptive controller. By using the controller,
the zinc dust dosage is neither kept constant nor changed drastically. As a result, the nal cobalt ion concentration is more stable
compared with the open loop control manner adopted in Sun et al.
(2014).
Dosage (kg/m3)
0.40
Dosage (kg/m3)
101
0.35
0.30
0.25
0.20
0.15
0.25
12
time (h)
16
20
0.10
24
0.10
0.08
0.08
0.06
0.04
0.02
0
12
time (h)
16
20
24
20
24
0.10
Dosage (kg/m3)
Dosage (kg/m3)
0.06
0.04
0.02
12
time (h)
16
20
24
12
time (h)
16
ORP of reactor 1
560
ORP of reactor 2
620
610
ORP (mv)
ORP (mv)
550
540
520
12
time (h)
16
20
590
580
Practical ORP
Reference ORP
530
600
Practical ORP
Reference ORP
570
560
24
660
650
650
640
640
630
620
600
12
time (h)
20
24
16
20
630
620
Practical ORP
Reference ORP
610
16
ORP of reactor 4
660
ORP (mv)
ORP (mv)
ORP of reactor 3
12
time (h)
Practical ORP
Reference ORP
610
24
600
12
time (h)
16
20
24
102
10
10
Control result
Reference value
mg/L
mg/L
12
time (h)
16
20
24
12
time (h)
16
20
24
10
Control result
Reference value
8
6
12
time (h)
16
20
Control result
Reference value
mg/L
mg/L
10
Control result
Reference value
24
12
time (h)
16
20
24
5. Conclusion
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Acknowledgments
This research was supported by Innovation-driven Plan in
Central South University (Grant no. 2015cx007), the National
Natural Science Foundation of China (Grant nos. 61174133,
61273185) and Science Fund for Creative Research Groups of the
National Natural Science Foundation of China (Grant no.
61321003). Bei Sun and Mingfang He would like to thank China
Scholarship Council for the nancial support (Nos. 201206370097
and 201306370089). These are gratefully acknowledged.
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