Minerals Engineering 96–97 (2016) 123–129

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

The effect of biopolymer dispersants on copper flotation in the presence

of kaolinite
Yanhong Wang a,⇑, Rolf Andreas Lauten b, Yongjun Peng a,⇑
a
School of Chemical Engineering, University of Queensland, St. Lucia, QLD 4072, Australia
b
Pionera, Hjalmar Wesselsvei 6, Sarpsborg, Norway

a r t i c l e i n f o a b s t r a c t

Article history: In this study, three lignosulfonate-based biopolymers, DP1775, DP1777 and DP1778 with different com-
Received 25 December 2015 positions were examined as dispersants in copper flotation in the presence of kaolinite. While rheological
Revised 13 May 2016 measurements indicated that these biopolymers dispersed the kaolinite aggregates, flotation results
Accepted 13 May 2016
revealed that the three biopolymers increased the copper recovery, with a decline in copper grade, which
Available online 20 May 2016
was attributed to an interaction of biopolymers with the frother modifying the froth and enhancing the
mechanical entrainment. Two-phase foam characterisation revealed a larger height in the blends of
Keywords:
biopolymer and frother, which in turn promoted the mechanical entrainment in flotation. The dispersing
Copper flotation
Biopolymers
and foaming abilities of biopolymers were governed by their structural features such as the content of
Kaolinite functional groups, the molecular weight and counterions. This study indicates that when selecting a poly-
Entrainment meric dispersant in flotation to deal with clay minerals, its froth property should also be taken into
Foam stability consideration.
Ó 2016 Elsevier Ltd. All rights reserved.

1. Introduction and Peng (2014) found that higher froth stability offset the down-
ward gravitational settling of particles and reduced their drainage
In mineral flotation, entrainment is a mechanical mass transfer from froth thereby increasing flotation recovery. They also found
process where particles suspended in water between bubbles enter that higher froth stability increased mechanical entrainment,
the flotation froth from the top of the pulp region and are trans- resulting in the higher recovery of gangue minerals. An ideal froth
ferred to the concentrate (L. Wang et al., 2015). Several factors should not be too stable with low coalescence or of too low viscos-
including water recovery, pulp density, particle size, gas flow rate, ity with high coalescence, which is targeted to achieve a balance
rheology, froth structure etc. may affect entrainment, however, between optimal recovery and minimal mechanical entrainment.
particle size and froth stability are predominant (Smith and According to Moolman et al. (1996), the froth should consist of clo-
Warren, 1989). It has been found that coarse particles drain more sely packed bubbles with clear areas on top of some of the bubbles.
readily from the voids between bubbles than fine particles. In addi- Clay minerals include phyllosilicate and non-phyllosilicate min-
tion, fine particles are easily suspended in the water or the water erals (Guggenheim and Martin, 1995). Basically, the structural
films surrounding the bubbles in the region below the pulp/froth framework of clay minerals consists of layers comprising silica
interface. Hence, fine particles have more chances to travel up tetrahedral (T) sheets and alumina octahedral (O) sheets joining
through the froth to the concentrate (Subrahmanyam and together in certain proportions (Theng, 2012). Clay minerals pre-
Forssberg, 1988). Generally, it is believed that mineral particles sent in froth flotation processes normally have colloidal dimension,
smaller than 50 lm are readily recovered by entrainment. well below the 50 lm limit mentioned above. Therefore, clay min-
Froth stability refers to the rate of bubble coalescence and bub- erals are often entrained mechanically and report to the concen-
ble bursting. It is known that froth with relatively low coalescence trate. Kaolinite as a non-swelling clay mineral with a 1:1
and small bubbles implies high stability which not only facilitates structure, composed of one tetrahedral sheet with one octahedral
the recovery of attached particles, but also promotes the recovery sheet, is the most common clay mineral that occurs in mineral pro-
of gangue minerals by entrainment (Wang and Peng, 2013). Wang cessing (Wang and Peng, 2013). Liu and Peng (2014) tested poorly
crystallized kaolinite, Q38, in flotation and found a near linear rela-
⇑ Corresponding authors. tionship between mass and water recovery in both tap water and
E-mail addresses: [email protected] (Y. Wang), [email protected] saline water. Kaolinite was reported to the flotation concentrate
(Y. Peng).

http://dx.doi.org/10.1016/j.mineng.2016.05.010
0892-6875/Ó 2016 Elsevier Ltd. All rights reserved.
124 Y. Wang et al. / Minerals Engineering 96–97 (2016) 123–129

by entrainment in both cases. The previous study found that the Table 3
copper grade gradually decreased with increasing kaolinite content Composition and molecular weight of biopolymers used in this study.

(Y. Wang et al., 2015). By using Cryo-SEM, Zhang et al. (2015) iden- Counterion Molecular Main function groups
tified that the entrainment of kaolinite in copper-gold flotation weight
was due to the formation of loose kaolinite aggregates by edge- Mw Mn Sulfur (%) Carboxylic (%)
to-edge (E-E) associations in the pulp phase. Moreover, these DP-1775 Na+ 39,000 2400 6.1 8.7
aggregate structures were easily transported from pulp to froth DP-1777 Na+ 13,700 2000 8.5 9.5
phase owing to their low densities, which was also observed by DP-1778 Ca2+ 6000 800 4.8 14.5
Cruz et al. (2015). Obviously, the formation of kaolinite association
structures imposes a detrimental effect on flotation grade. weight, the largest proportion of carboxylic groups, 14.5% and
In industry, polymeric dispersants have been used to reduce the the smallest proportion of sulfonic groups 4.8%. DP-1775 and DP-
negative impact of clay minerals in flotation. For instance, at New- 1777 are sodium-based polyelectrolytes while DP-1778 is a
crest’s Telfer Operation, three polymers, Polyacrylate A, modified calcium-based polyelectrolyte.
carboxylic acid and lignosulfonate-based F-100 biopolymer, were Potassium isoamyl xanthate (PAX) obtained from Orica, Aus-
tested in the laboratory to mitigate the negative effects of clay tralia Pty Ltd, was used as the collector. The frother DSF004 used
minerals on copper-gold flotation. It was found that all three poly- at the Telfer plant, an aliphatic alcohol based mixture, was used
mers showed positive results with F-100 biopolymer producing the as received in laboratory tests without further purification. The
greatest improvement in copper recovery and grade (Seaman et al., pH value of slurry in flotation was controlled by lime. Brisbane
2012). Wei et al. (2013) further studied the effect of F-100 on the tap water with minor ion concentrations was used throughout
flotation of low and high clay ores obtained from Telfer. They found the flotation process. This water was described elsewhere (Liu
that the addition of F-100 in the flotation of the high clay ore and Peng, 2014).
improved the flotation recovery significantly with a decrease in
pulp viscosity.
2.2. Rheology measurements
In this study, three lignosulfonate-based biopolymers with dif-
ferent compositions, DP-1775, DP-1777 and DP-1778, were exam-
Rheology measurements were conducted by an Ares rheometer
ined as kaolinite dispersants in the flotation of a copper-gold ore. It
(TA Instruments Ltd., U.S.). All tests were conducted with a 42 mm
is expected that these biopolymers disperse kaolinite aggregates,
diameter cup and a vane with a diameter of 28 mm. Each time
and thus reduce the entrainment of kaolinite in flotation.
40 mL kaolinite slurry was poured into the cup and the rotor was
lowered until the gap between the rotor and the bottom of the
2. Experimental cup was 4 mm. Rheograms were generated in the shear rate inter-
val between 1 and 300 s
1 for 60 s. Three duplicates were mea-
2.1. Material and reagents sured for each sample and the results were similar. During
measurements, the temperature was maintained at 25 °C with an
A copper-gold ore with a minimum amount of clay minerals accuracy of ±1 °C.
was supplied from the Telfer mine. This ore was referred to as
‘‘clean ore” and was used as a reference. The mineral composition
of this ore as analysed by quantitative X-ray Diffraction (XRD) is 2.3. Mineral grinding and flotation
listed in Table 1. The major valuable mineral in the ore is chalcopy-
rite, with pyrite, quartz, albite, muscovite, dolomite and other The clean ore was crushed to a size of
2.36 mm using jaw and
amorphous contents being the gangue minerals. Key element com- roll crushers. Then 800 g crushed ore sample was ground in a lab-
positions of the ore are shown in Table 2. It can be seen that the oratory rod mill with stainless steel rods at 62% solids to obtain an
copper originates from chalcopyrite. The ore does not contain sec- 80% passing of 106 lm (P80 = 106 lm). The ground slurry was
ondary copper sulphide minerals which may cause slime coating transferred to a 2.5 L J.K. flotation cell, with an agitation speed of
due to electrostatic attraction (Peng and Zhao, 2011). Kaolinite 1000 rpm. 200 g dry kaolinite mixed in tap water was added to
Q38 which contains 85% kaolinite with 4% quartz and 11% mus- make an artificial kaolinite-ore slurry with 80% clean ore and 20%
covite, was purchased from Sibelco Group, Australia. 70% of the kaolinite. The solid content in the flotation cell was about 30 wt
Q38 sample particles were smaller than 10 lm. %. The slurry pH was adjusted to 9.0 with lime, and then condi-
The characteristics of the three biopolymers, supplied by Pion- tioned with or without the addition of any biopolymer for 3 min.
era, used in this study are listed in Table 3, with product numbers 60 g/t collector and 30 g/t frother were added and the slurry was
of DP-1775, DP-1777 and DP1778. DP-1775 has the highest molec- conditioned for another 3 min. Flotation froth was scraped every
ular weight, 8.7% carboxyl groups and 6.1% sulfonic groups, while 10 s. Four concentrates were collected after a cumulative time of
DP-1777 has a lower molecular weight with a higher content of 1, 3, 6 and 10 min with an air flow rate of 3.0 L/min. After the first
functional groups, 9.5% carboxyl group and 8.5% sulfonic groups, 3 min flotation, additional amounts of 30 g/t collector and 15 g/t
compared with DP-1775. DP-1778 has the lowest molecular frother were added.

Table 1
Mineral compositions of the clean ore analysed by XRD (wt%).

Quartz Albite Muscovite Dolomite Pyrite Chalcopyrite Amorphous

27.7 35.2 6.8 8.4 2.9 1.4 17.5

Table 2
Key mineral or element compositions of the clean ore (wt%).

Cu Au Al2O3 Bi CaO Cd Co Fe MgO Pb S SiO2 Tl Zn

0.43 1.13(g/t) 10.3 0.019 5.04 0.004 0.007 2.98 2.2 0.01 2.04 63.4 0.048 0.027
 Y. Wang et al. / Minerals Engineering 96–97 (2016) 123–129 125

2.4. Foam characterisation data in Fig. 1(a), (b) and (c) with the addition of DP-1775, DP-1777
and DP-1778, respectively, were best fitted to the Herschel-Bulkley
In this study, the two-phase foam maximum height was model:
selected as a parameter to characterise the foamability of frother,
biopolymers and their mixtures using a modified Bikermann’s s ¼ sy þ Kðc_ Þn
method (Awatey et al., 2013; Tan et al., 2005). A graduated foam
column was used with a cross-sectional area of 100 cm2 and a where c_ (s
1) is the shear rate; sy (Pa) is the yield stress; s (Pa) is the
motor driven agitator extending from the top towards the bottom. shear stress; K (Pasn) is the consistency index and n is the flow
For each test 1.0 L well-mixed solution was poured into the foam behaviour index. Fig. 1(d) shows the Herschel-Bulkley yield stress
column. The impeller speed was constant at 500 rpm. For each test, in the absence and presence of DP-1775, DP-1777 or DP-1778. As
foam was generated by sparging air from the bottom of the col- can be seen, 30 wt% kaolinite suspension in the absence of any
umn. The flow rate of air was kept at 3.0 L/min for all the tests. biopolymer behaved as a non-Newtonian fluid with a yield stress.
At beginning of the test, the foam was allowed to rise until a max- The presence of yield stress often indicates the formation of aggre-
imum height (Hmax) was reached, the foam maximum height was gate structures in a suspension (Ndlovu et al., 2011). Although it has
recorded and the air flow was stopped. been found that both basal and edge faces of kaolinite are nega-
tively charged at pH 9 (Gupta and Miller, 2010), a high kaolinite
concentration can reduce the mobility of particles and force kaolin-
2.5. Dynamic surface tension
ite platelets to adapt E-E association due to the strong repulsion
between the facial platelets (Du et al., 2010).
A KR €USS bubble pressure tensiometer BP50 was used to mea- With increasing biopolymer dosage from 0 to 0.01 wt%, 0.05 wt
sure the dynamic surface tension of the solution of the frother, %, 0.1 wt% and 0.5 wt%, the suspension was gradually transformed
biopolymers, and their mixtures. Air was pumped into a gas reser- towards a Newtonian fluid with a decline in the Herschel-Bulkley
voir and passed through a capillary to produce bubbles in the solu- yield stress. Fig. 1(d) shows that the Herschel-Bulkley yield stress
tions. A sensitive pressure transducer was used to monitor the decreased from 1.4 Pa to nearly 0 Pa when the concentration of
pressure in the bubble at the capillary tip, whilst a computer inter- DP-1775 and DP-1777 increased to 0.5 wt%. DP-1778 decreased
face was connected to control and monitor the process. The the Herschel-Bulkley yield stress to 0.6 Pa at the same concentra-
stopped flow mode, where the air supply to the system was termi- tion. Both the transition towards a Newtonian fluid and the decline
nated and bubble separation occurred due to the decrease in sur- in the Herschel-Bulkley yield stress as the biopolymer concentra-
face tension, was used to determine the dynamic surface tension tion increased suggest a disruption of the kaolinite network struc-
between 10 and 500 s. DI water was used in this experiment to ture. DP-1775 and DP-1777 had a similar ability to reduce the yield
avoid possible interference of ions. stress, and were superior to DP-1778. This difference was more
pronounced at a higher biopolymer concentration. Liu and Peng
3. Results (2015) found that a small amount of lignosulfonate biopolymer
D748 dispersed kaolinite particles and improved coal flotation in
3.1. Effect of biopolymers on the rheology of kaolinite suspensions deionised water. This was ascribed to the adsorption of polymer
molecules onto kaolinite and enhanced electrostatic repulsion
The rheograms of 30 wt% kaolinite suspensions in the absence through polymer anionic functional groups. In the current study,
and presence of biopolymers are shown in Fig. 1. The experimental the yield stress observed in kaolinite slurries in the absence of

Fig. 1. Rheograms of kaolinite suspensions with different dosages of biopolymers: (a) DP-1775; (b) DP-1777; (c) DP-1778; (d) Herschel-Bulkley yield stress in the absence
and presence of DP-1775, DP-1777 and DP-1778.
126 Y. Wang et al. / Minerals Engineering 96–97 (2016) 123–129

biopolymers illustrated the formation of kaolinite aggregates. It

has been reported that in flotation slurries these aggregates pro-
mote mechanical entrainment of kaolinite particles (Cruz et al.,
2015). Since the presence of biopolymers has dispersed kaolinite
aggregates in this section, it is expected that the dispersing effect
might lead to lower mechanical entrainment in flotation. This
was examined in the next section.

3.2. Effect of biopolymers on copper flotation

The rheological characterisation in Fig. 1 indicates that at 0.1 wt

% biopolymer concentration the kaolinite suspension was well dis-
Fig. 3. Cumulative mass recovery as a function of water recovery in the flotation of
persed. This concentration corresponds to a dosage of 200 g/t in the ore mixed with 80 wt% clean ore and 20 wt% kaolinite in the absence and
flotation. Fig. 2 shows the effect of the three biopolymers, DP- presence of 200 g/t DP-1775, DP-1777 and DP-1778.
1775, DP-1777 and DP-1778, on the flotation of the ore consisting
of 80 wt% clean ore and 20 wt% kaolinite. Copper recovery
increased from 85% to 90%, 94% and 93% at the end of flotation, the concentrate was considered as entrainment. Fig. 4 shows the
in the presence of DP-1777, DP-1775 and DP-1778, respectively. ENT in the flotation in the absence and presence of biopolymers.
DP-1775 and DP-1778 had a better effect on copper recovery than As can be seen, the ENT of 0.376 was obtained in the absence of
DP-1777. The presence of biopolymers also led to an increase in any biopolymer. This high ENT value was due to the presence of
flotation rate, seen as the higher copper recoveries in the first con- kaolinite particles. However, the ENT further increased to around
centrate. However, the addition of biopolymers decreased copper 0.392 in the presence of biopolymers. There was a small variation
grade. The initial copper grade of the first concentrate decreased of ENT between different biopolymers. The ENT with DP-1775 and
from 4.2% to about 3.5% in the presence of any biopolymer. Obvi- DP-1778 was slightly higher than that with DP-1777.
ously, these biopolymers promoted the recovery of gangue miner- Obviously, the dispersion of kaolinite aggregates, seen as a
als in flotation. reduction in yield stress by biopolymers, did not lower the degree
Fig. 3 shows the mass recovery as a function of water recovery of entrainment in copper flotation. Instead, an increase in entrain-
in the absence and presence of the three biopolymers. As can be ment was observed in the presence of biopolymers. During flota-
seen, after the completion of 10 min flotation, the mass recovery tion, it was observed that biopolymers modified the froth
was relatively low, about 9%, in the absence of any biopolymer. properties. Generally, bubble size in the froth phase appeared
The addition of 200 g/t DP-1777, DP-1775 and DP-1778 increased smaller and more froth formed on top of the flotation cell with
the mass recovery to 10%, 10.5% and 11.5%, respectively. The water the addition of biopolymers. This may contribute to the increased
recovery was also increased from 21% to 22%, 23% and 24.5%, copper recovery and decreased copper grade. It is known that some
respectively. The variations in mass recovery were due to different polymers used in flotation have a foaming ability that modifies the
amounts of water recovered into the concentrate in the presence of froth properties and thereby mineral flotation behaviour
these biopolymers. Thus, the decrease in copper grade may be lar- (Schreithofer et al., 2011). Attention then turned to measure the
gely due to the increased gangue recovery by entrainment with the foaming ability of the biopolymers.
addition of biopolymers.
Entrainment is a strong function of mass recovery and water 3.3. Foamability measurements
recovery. An increase of the slope of curves in Fig. 3 indicates the
accelerated entrainment of gangue minerals. The degree of To understand the foamability of the three biopolymers, two
entrainment (ENT) may be calculated by the following equation phase foam height of a solution containing the frother with or
(Zheng et al., 2006): without a single biopolymer was measured. Results are shown in
  Fig. 5. Fig. 5(a) shows the foam height as a function of biopolymer
Mgangue
or frother concentration. The foam height remained at the same
M water
ENT con:tail ¼  con level with the increase of frother or DP-1777 concentration. In con-
M gangue
Mwater
tail
trast, the foam height increased continually with increasing con-
centration of DP-1778 or DP-1775. Generally, the relative
where M is the mass (g). Copper in the clean ore is present as chal- foamability of these biopolymers is in the order:
copyrite. To determine the ENT, the recovery of all other minerals in
DP-1778 > DP-1775 > DP-1777:

Fig. 2. Copper grade as a function of copper recovery from the flotation of the ore
mixed with 80 wt% clean ore and 20 wt% kaolinite in the absence and presence of Fig. 4. The degree of entrainment (ENT) in the flotation of the ore-kaolinite mixture
200 g/t DP-1775, DP-1777 and DP-1778. in the absence and presence of 200 g/t DP-1775, DP-1777 and DP-1778.
 Y. Wang et al. / Minerals Engineering 96–97 (2016) 123–129 127

Fig. 5. The steady state foam height as a function of the frother or biopolymer concentration: (a) a single biopolymer or frother; (b) the biopolymer mixed with 10 ppm
frother.

Fig. 5(b) shows the foam height as a function of biopolymer gradient of the 10 ppm frother solution. Specifically, the addition
concentration in the presence of 10 ppm frother concentration of DP-1778 to the frother solution decreased the surface tension
similar to that used in the flotation process. Clearly, in the mixed to the lowest value, followed by the addition of DP-1775. The addi-
system the foam height was substantially higher than that pro- tion of 100 ppm DP-1777 to 10 ppm frother solution had little
duced by either frother or biopolymer alone. For DP-1778 and effect on the dynamic surface tension. Thus, dynamic surface ten-
DP-1775, the foam heights in the mixed system were even higher sion measurements in Fig. 6(b) also correlated with the foam
than the summation of the foam height produced by the frother height of the mixture containing frother and biopolymers in
and biopolymer alone as shown in Fig. 5(a). For DP-1777, the foam Fig. 5(b).
height of the mixture was similar to that produced by frother
alone. The results in Fig. 5 suggest a synergistic effect of DP-1778
and DP-1775 with the frother, leading to an increased foam height 4. Discussion
when they were mixed.
Measurements of dynamic surface tension were conducted to In this study, the three biopolymers differed in their ability to
see if the biopolymer foamability can be related to the surface disperse kaolinite suspensions and affect flotation performance.
activity. Fig. 6 shows the dynamic surface tension of 100 ppm sin- The reduction of yield stress of kaolinite suspensions was due to
gle biopolymer or 10 ppm frother solution, and their mixtures. As the dispersion effect of biopolymers. Generally, there are two prin-
shown in Fig. 6(a), in the long time scale (10–500 s), the frother cipal mechanisms responsible for the dispersion of anionic poly-
DSF004 was a strong surfactant, with dynamic surface tension dra- mers: electrical double layer repulsion and steric repulsion. At a
matically decreasing from 72.4 to 70.3 mN/m. The dynamic surface low polymer concentration, the adsorption of negatively charged
tension of 100 ppm DP-1777 solution appeared to be constant at polymers on particle surface enhances the electrical double layer
about 72.6 mN/m. The dynamic surface tension of 100 ppm DP- repulsion between particles. At a high polymer concentration,
1775 solution was slightly lower. The dynamic surface tension of steric repulsion may be promoted. In this study, the biopolymers
100 ppm DP-1778 gradually declined to 71.6 mN/m. Hence, the reduced the yield stress of kaolinite suspension to different extents
surface activity of these biopolymers is in the order: DP- at the same concentration. This is associated with their unique
1778 > DP-1775 > DP-1777, which is in agreement with the foam structures. DP-1775 and DP-1777, which reduced the yield stress
height indicated in Fig. 5(a). of kaolinite suspensions similarly as shown in Fig. 1, have a similar
Fig. 6(b) shows that the surface tension gradient of the mixture content of functional groups. They may render the faces of kaolin-
containing 10 ppm frother and 100 ppm biopolymer is below the ite platelets more negative and increase both electrical double

Fig. 6. Dynamic surface tension: (a) 100 ppm single biopolymer or 10 ppm frother; (b) the mixture of 10 ppm frother and 100 ppm biopolymer.
128 Y. Wang et al. / Minerals Engineering 96–97 (2016) 123–129

layer repulsion and steric repulsion between polymer-adsorbed increased the copper recovery, with a decline in copper grade. This
kaolinite particles in a similar way. DP-1778 has the highest num- was attributed to the foamability of the biopolymers. When the
ber of functional groups and should have a greatest capability to biopolymers were mixed with the frother, the foamability
reduce the yield stress of kaolinite suspensions among the three increased, due to an increase in surface activity. The dispersing
biopolymers, but Fig. 1 shows an opposite trend. The discrepancy and foaming abilities of biopolymers are governed by their struc-
may be linked with the counterion, Ca2+, and the low molecular tural features, i.e. content of functional groups, the molecular
weight of DP-1778. The presence of the divalent cation Ca2+ can weight and counterion. This study indicates that when choosing
reduce or neutralize the negative charge on kaolinite surface and a polymer to mitigate the negative effect of kaolinite in flotation,
lower the electrostatic repulsion. It is also known that the molecu- the surface activity of the polymer and its interaction with the
lar weights of polymers determine their adsorption on mineral sur- frother should be considered.
face (Lagaly et al., 2006). DP-1778 has the lowest molecular
weight, which may affect its adsorption on kaolinite surface and Acknowledgements
its ability to disperse kaolinite suspensions. The lower molecular
weight also means it is less likely to extend out from mineral sur- The authors are thankful for the financial support from the Aus-
face with weaker steric repulsion. In general, the three biopoly- tralian Research Council and Pionera (ARC linkage project,
mers showed the potential to disrupt kaolinite aggregates, but LP120200162). Besides, the supply of practical ores from Newcrest
this did not translate into the reduction of mechanical entrainment Telfer operation is greatly appreciated. The first author also thanks
in the flotation of the ore in the presence of kaolinite. Instead, the scholarship provided by the University of Queensland.
higher mechanical entrainment was observed with the addition
of these biopolymers. References
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