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J. Cent. South Univ.

(2014) 21: 1077−1084


DOI: 10.1007/s11771-014-2039-8

Effect of some operational variables on


bubble size in a pilot-scale mechanical flotation machine

ZHANG Wei(张炜)1, 2, J.E. Nesset2, J.A. Finch2

1. Mining and Mineral Resources Division, Department of Business Administration,


Chinalco China Copper Corporation Limited, Beijing 100082, China;
2. Department of Mining and Materials Engineering, McGill University, Montreal, QC, H3A OC5, Canada
© Central South University Press and Springer-Verlag Berlin Heidelberg 2014

Abstract: This work aims to provide a relationship of how the key operational variables of frother type and impeller speed affect the
size of bubble (D32). The study was performed using pilot-scale equipment (0.8 m3) that is up to two orders of magnitude larger than
equipment used for studies performed to date by others, and incorporated the key process variables of frother type and impeller speed.
The results show that each frother family exhibits a unique CCC95-HLB relationship dependent on n (number of C-atoms in alkyl
group) and m (number of propylene oxide group). Empirical models were developed to predict CCC95 from HLB associated with
other two parameters α and β. The impeller speed-bubble size tests show that D32 is unaffected by increased impeller tip speed across
the range of 4.6 to 9.2 m/s (representing the industrial operating range), although D32 starts to increase below 4.6 m/s. The finding is
valid for both coalescing and non-coalescing conditions. The results suggest that the bubble size and bubble size distribution (BSD)
being created do not change with increasing impeller speed in the quiescent zone of the flotation.

Key words: flotation; bubble size; operational variables; critical coalescence concentration; hydrophile-lipophile balance; impeller
speed

almost never controlled in plants. They offered the


1 Introduction opinion that sub-500 μm bubbles would be required to
significantly improve the collection efficiency. Although
Froth flotation is a versatile and extremely complex the importance of the bubble size was established as
physico-chemical process that has been widely used in early as 1970’s, these studies and their outcomes might
recovering valuable minerals. During the flotation be inadequate since the effects of many key variables
process, bubbles play a fundamental role and it is well affecting the flotation process have not been fully
documented that the bubble size or bubble size considered. These key variables which govern the
distribution (BSD) have a direct influence on the flotation process are classified into two general groups:
flotation performance [1−3]. The importance of the “ituational” variables (e.g., water quality, gas/air density,
bubble size in flotation has been investigated by a pulp viscosity, etc.) and “operational” variables (e.g.,
number of researchers in the 1960’s and 1970’s. REAY frother type and concentration, gas rate, impeller speed,
and RATCLIFF [4] showed that collection efficiency of etc.). The operational variables comprise of two aspects:
particles by bubbles would strongly depend on the chemical-related and machine-related. In the past, the
bubble to particle size ratio. They concluded that, within role of operational variables has received less attention
practical constraints, there was a powerful incentive to [7−8] than situational variables, even though they are a
make bubble size as small as possible. More specifically, vital part of the flotation process. The review of literature
ANFRUNS and KITCHENER [5] demonstrated the has highlighted that there currently exists no generally
strong dependence of particle collection efficiency on accepted relationships and models between bubble size
this ratio, and the need for small, sub-1 mm bubbles in and operational variables, nor is the extent to which these
collecting sub-40 μm particles. In a major review of the relationships can be predicted from phenomenological or
physical factors affecting flotation, JAMESON [6] more fundamental understandings of the bubble
concluded that bubble size is an important key which is formation processes. This research attempts to address

Foundation item: Project supported by the Collaborative Research and Development Program of NSERC (Natural Sciences and Engineering Research
Council of Canada) with Industrial Sponsorship from Vale, Teck Cominco, Xstrata Process Support, Agnico-Eagle, Shell Canada, Barrick
Gold, COREM, SGS Lakefield Research and Flottec
Received date: 2012−10−15; Accepted date: 2013−03−25
Corresponding author: ZHANG Wei, PhD; Tel: +86−13521508736; E-mail: zhang_wei@chalco.com.cn
1078 J. Cent. South Univ. (2014) 21: 1077−1084
this shortcoming, which has eluded researchers up to improved with increased power input in scavenging
now. applications [21]. This is achieved by increasing the
Frothers are heteropolar surfactants, comprising impeller rotational speed: values of 5−10 kW/m3 have
polar and non-polar groups, which are used to promote been reported. Apparently effective, it is a costly way to
flotation performance through control of hydrodynamic improve the recovery of fine particles. Plant operators
and froth properties [9−14]. The most commonly used often consider the impeller rotational speed of the
frothers fall in two main categories: Aliphatic Alcohols flotation machine as an adjustment that can be used to
(CnH2n+1OH) and Polyglycols (CnH2n+1(OC3H6)mOH) change the pumping rate of slurry, impact particle
[9−10]. The frother functions in some manner must suspension and bubble particle contact, or more
depend on the frother structure [9], e.g., the relative importantly, change bubble size. Recent laboratory
strength of the hydrophobic to hydrophilic groups. In investigations by GRAU and HEISKANEN [1] on 50
each frother family, the relative strength can be modified and 70 L laboratory flotation machines in air-water,
by changing the number of —CH2— groups (represented determined that bubble size was dependent on impeller
by n) in the Alkyl chain in the case of Alcohols and tip speed to the power, −0.41 and −0.55 for the 50 L unit,
Polyglycols, and/or number of Propylene Oxide (PO, for an impeller tip speed range of 2 to 5 m/s. However,
represented by m) groups in the case of Polyglycols. similar test on the 70 L unit showed no significant
Varying the relative strength of the hydrophobic to relationship, which possibly reason for the lack of a
hydrophilic groups in the molecule changes its similar dependency. It is important note that the range of
hydrophile-lipophile balance, or HLB. The common impeller tip speeds in these tests is largely below those
calculation of HLB is the Davies method where group typically used in industrial units, 5 to 7 m/s [21]. The
numbers are assigned and summed [15]. There have been literatures reveal that the relationship between impeller
some attempts to link frother functions to HLB [9, speed (or power intensity) and bubble size is incomplete
16−19]. and has not gained acceptance as evidenced by the
Based on other researchers, GORAIN et al [20] observation. It is therefore deemed as an important
recognized that frother is the single most important variable in this work.
variable affecting bubble size. GORAIN’s work has been Based on the above discussion, knowledge of how
seminal in that it was the first to clearly link chemical key operational variables affect the bubble size is seen as
variables such as frother type as an important variable to an essential component of process understanding and
bubble size, or more clearly, flotation recovery. As optimization. This work attempts to provide new insights
frother concentration increases, the bubble size into the effects of chemical (frother type) and machine
distribution (BSD) narrows and becomes finer. The (impeller speed) related operational variables on bubble
Sauter mean size vs. frother concentration (D32−C) size in a mechanically agitated flotation cell. The
relationship shows an exponential decay to a minimum proposed testing will make use of a pilot-sized flotation
(limiting) size (DL) at a concentration characteristic of machine considerably larger than a standard lab unit,
the frother. This concentration is referred to as the critical approximately 0.8 to 1 m3 in volume, to limit
coalescence concentration (CCC) [16]. Noting the dimensional effects associated with smaller laboratory
difficulty in defining the end point of an exponential cells. The ability to have a distinct separation zone above
function, NESSET et al [18−19] refined the estimation the mixing zone around the impeller is important for
by fitting a three-parameter model to the D32−C and sampling the bubble size and gas rate exiting the cell
determining the CCC95, i.e., the concentration giving cross-sectional area. Uniformity of bubble distribution
95% size reduction in D32 relative to water alone (D0). within the larger cell is also expected to be better.
The CCC95 was selected as the bubble size function Locating the McGill Bubble Size Analyzer (MBSA)
parameter. In this work, the frother type-bubble size tests [2−3, 22] will also be easier in the larger cell. Testing
were conducted on 36 frothers in three different families will initially be conducted in the two-phase water-air
and the ambition is to provide fundamental input to the system and will be followed by tests using slurries in the
selection of frother for an optimum bubble size, such as next stage.
establishing a correlation between CCC and HLB, which
remains a largely empirical exercise. 2 Experimental
Typically, the larger flotation machines have a
power input of 1−2 kW/m3 of cell volume, with 1 kW/m3 2.1 Apparatus and methods
being the more typical for Outokumpu, Bateman, Dorr The same rig as previously described in Ref. [22]
Oliver and Metso designs. Recent reports from the South was used. It consists of a mechanical flotation cell (0.8
African platinum industry suggest that metallurgical m3 in volume) with a McGill Bubble Size Analyzer
recovery of small, sub-10 μm PGM particles can be (MBSA) (Fig. 1). The flotation cell will be fitted with a
J. Cent. South Univ. (2014) 21: 1077−1084 1079
meter and a Jg device adapted for the cell.
The unit was operated with 700 L water at room
temperature (22−24 °C) with air dispersed through the
21 cm diameter at a superficial air rate Jg (volumetric air
rate divided by cell cross-sectional area) of 0.5 cm/s
(both of 0.5 and 1.0 cm/s air rates were applied in
impeller speed-bubble size tests). Bubbles were sampled
20 cm below the water surface, well above the
turbulence of the impeller–stator region. The images
were processed using in-house software to give D32.
Further details are given in Ref. [19].

2.2 Reagents
The surfactants from the three frother families are
identified in Table 1 which shows the range in n and m
and corresponding range in HLB (note, Polypropylene
Fig. 1 Metso RCSTM 0.8 m3 mechanical cell assembly and Glycol Ethyl Ethers (i.e., n=2) and Monopropylene
McGill Bubble Size Analyzer (clamped on cell beams) Glycol (m=1) are not available). All were reagent grade
from Aldrich-Sigma (98%−99.9% purity). Several
gas-flow meter and valve on the air intake, a transmitting commercial frothers were included and are listed in
torque-meter (strain gauge) for measuring power input Table 2.
on the rotor drive shaft, automatic level control, variable
speed motor, changeable rotors, and an ability to operate 3 Results and discussion
in either self-aerated or forced air mode. The ability to
alter chemistry (frother type/concentration) and machine 3.1 Reliability
(impeller speed) variables in a test program that Figure 2 shows Sauter mean bubble size (D32) as a
accurately establishes the effect on bubble size function of concentration (C) for three repeats for the
distribution is primary. Bubble size distributions will be commercial frother DowFroth 250 (DF250). Replicate
measured using McGill’s bubble viewer technology [22]. tests (i.e., starting from solution preparation) were
Gas rate will be measured by both the installed flow conducted by two different operators (inter-operator)

Table 1 Frother families and range of surfactants (n, m and HLB) used in this work
Frother family Chemical structure n m HLB
alkyl group
 
Aliphatic alcohols C n H 2 n1 OH
 3−8 — 5−7.5
hydroxyl group
Propylene oxide group
 
Polypropylene glycols (PPG) H(OC 3 H 6 ) m OH
 0 3−17 7.4−9.3
hydroxyl group
Propylene oxide group
 
Polypropylene glycol alkyl C n H 2 n 1 (OC3H 6 ) OH
  m  1, 3, 4 1−7 6.5−8.3
ethers (PPGAE) hydroxyl group
alky lg roup

Table 2 Commercial frothers used in this work


Frother Family Commercial frother type Supplier n m Relative molecular mass HLB
Aliphatic alcohols FX120-01 Flottec 6 — 102 6.05
Polypropylene glycol (PPG) F150 Flottec 0 7 425 8.625
DowFroth 250 Dow Chemical 1 4 264 7.83
DowFroth 1012 Dow Chemical 1 6.7 398 7.48
Polypropylene glycol alkyl
FX160-01 Flottec 1 3.8 251 7.86
ether (PPGAE)
FX160-05 Flottec 3 2.5 207 7.11
F160 Flottec 4 2.5 217 6.63
1080 J. Cent. South Univ. (2014) 21: 1077−1084
surfactants. The estimation of CCC95 from the
three-parameter model fit to the D32 vs. C data proved
the reliability based on replicated tests (Fig. 2).
Efforts along this structure-function approach by
LASKOWSKI [16] and NESSET et al [18−19] laid a
foundation. The pursuit revealed a family-based
CCC-HLB pattern, confirming the possibility entertained
by PUGH [9]. Figure 4(a) shows the CCC95-HLB
relationship for the Aliphatic Alcohols. Starting with
Propanol there is a sharp decrease in CCC95 as HLB
decreases (i.e., n increases), which levels off above 6
carbons (n=6 or C-6). Previous studies on inhibition of
bubble coalescence by Alcohols reveal a similar trend.
Fig. 2 Reliability: inter-operator and intra-operator replicated The concentration required decreases with increasing n
experiments at same conditions for DF250 to approach a limiting value for n>6 [23−24]. For n<6,
there is an increasing isomer effect, i.e., effect of position
at three different times (intra-operator). The D32−C of the OH group, which is illustrated by comparing
curves were consistent and the 95% confidence interval Hexanol and Pentanol in Fig. 4(b). For practical purposes,
on the calculated CCC95 was 0.6×10−6 or 0.0024 however, since such short chain Alcohols are not
mmol/L, which is too small to indicate on subsequent employed as frothers, the isomer effect is later ignored.
plots. The results (Fig. 2) show high precision. The commercial frother FX120-01 is seen to fit the trend
(Fig. 4(a)).
3.2 Effect of frother type and concentration (CCC95 Figure 5 shows the relationship of CCC95 vs. HLB
vs. HLB) for the two Polyglycol families, in this case, as a function
In many flotation systems, frothers have the key
function of controlling bubble size. Consequently,
understanding and predicting their action are of interest
to modellers and plant operators alike. The approach here
was to explore a structure-function relationship. To
quantify structure, HLB was used as it encompasses the
hydrophilic-hydrophobic (amphipathic) character that
controls adsorption at the air-water interface, which
arguably is the basis for frother action. The function,
bubble size reduction, was quantified through the CCC
concept derived from the plot of Sauter mean diameter
(D32) versus concentration (C). D32 was calculated from
bubble size distribution using a sampling-for-imaging
technique and was validated in Fig. 2. The trend in Fig. 2
was seen for all frothers, illustrated in Fig. 3 for three

Fig. 4 CCC95 versus HLB for aliphatic alcohols and their


isomers (1-alcohol, 2-alcohol and 3-alcohol) (a) and effect of
Fig. 3 Effect of frother addition on D32 for 3 frother types —OH group position on CCC95 for pentanol and hexanol
(CCC95 is noted by the vertical dashed line) isomers (b)
J. Cent. South Univ. (2014) 21: 1077−1084 1081
also possible to deduce CCC95 knowing n and m, from
HLB via Eqs. (2) and (3). This approach represents a
significant step towards a structure-based prediction of
the impact of frother on bubble size in flotation machines
which was illustrated for the commercial frothers.
At present, the prediction relates directly to
mechanical flotation cells but the trends are likely
applicable to all machines. Future work may see a
relationship between CCC and machine type enabling the
present results to be generalized.

3.3 Effect of impeller speed (power intensity)


Of particular interest to the industry is the extent to
Fig. 5 CCC95 versus HLB for polyglycols as function of m which bubble size can be manipulated by either chemical
and n means (e.g., frother change) or machine means (e.g.,
higher power intensity via rotor design or a change in
of m for a given n. There is a pattern: CCC95 decreases impeller rotational speed). Therefore, one goal of this
with increasing m in a series of parallel or self-similar work is to investigate the effectiveness of machine means
plots which trend to lower HLB with increasing n. such as increasing impeller speed in order to reduce the
Although the PPGAEs and PPGs are usually considered bubble size.
as separate families, the pattern suggests that they can be There have been two opportunities to date to
treated as one. The commercial frothers are shown to fit examine the effect of increased power intensity on
the pattern. bubble size. Figure 6 shows the Jg−D32 comparison
The trends in Figs. 4(a) and 5 show consistent between the Lac des Iles 130 m3 Outokumpu tank cells
patterns that can be fitted to the following exponential having 1 kW/m3, and 75 L Denver pilot cells having
equation: approximately 3 kW/m3 of input power. The chemistry of
CCC95    exp(   HLB) (1) both systems was identical so the majority of the
difference is likely due to the difference in power
where α and β are constants that depend on the family
intensity. An opportunity also presens itself at the South
(i.e., n and m). Table 2 gives the values for the
African Impala plant where new Metso 30 m3 RCS tank
polyglycols and 1-alcohols.
cells have just been installed on a tailings re-treatment
For polyglycols, α and β can be linked to n as
duty using oversized (70 m3) mechanisms. A good
  4.74 1017  exp(3.497  n)  1.956 1019  comparison on similar feed with upstream Bateman
exp(0.001452  n) (2) 50 m3 tank cells and no additional frother added is
therefore possible during downtime of half the plant.
6.985  n  4.814 Figure 7 shows the comparison of bubble size versus gas
 (3)
1.455  n rate for the Metso unit at 3 kW/m3 versus the Bateman
The large database permitted development of cell at 1 kW/m3. In both Figs. 6 and 7, there is a clear
empirical models, which well describe the results in reduction in bubble size, seemingly due to the higher
Eq. (1) and Table 2 for polyglycols and 1-alcohols. It is power intensity (impeller speed). Some assumptions

Table 2 Constants in Eq. (1) for range of n and m and goodness-of-fit (precision) statistics
Precision
Family n m α β 2
Data points, N R R2Adjusted SSE RMSE
−10
1-alcohol 3−8 0 1.52×10 3.207 6 0.9815 0.9769 0.002136 0.02311
−17
Polypropylene glycol 0 2−17 4.76×10 3.951 6 0.9615 0.942 0.006069 0.04498
Polypropylene glycol
1 1−7 1.61×10−18 4.855 6 0.9745 0.9682 0.004049 0.03181
methyl ether
Polypropylene glycol
3 1−3 3.15×10−19 5.624 4 0.9937 0.9905 0.0001581 0.008891
propyl ether
Polypropylene glycol
4 1−3 9.58×10−20 6.125 4 0.9972 0.9957 3.027×10−5 0.003891
butyl ether
1082 J. Cent. South Univ. (2014) 21: 1077−1084
and 10×10−5 DF250 at Jg levels of 0.5 and 1 cm/s. These
concentrations represent CCCx levels of 0, 52%, 77%
and 95%. The range was selected so as to maintain
reasonable sensitivity to bubble size change (i.e.,
avoiding very high levels of frother addition). The
purpose of this test was to explore the effect of impeller
speed on bubble size by using different concentrations
DF250 frothers.
vM  d MS 
vIT     π  dI (4)
60  DMS 
where vIT is the impeller speed, vM is the motor speed,
dMS is the motor sheave diameter, DMS is the mechanism
Fig. 6 Jg−D32 relationship for Outokumpu 130 m3 cells
sheave diameter, dI is the impeller diameter.
(1 kW/m3) and Denver 75 L pilot cells (3 kW/m3) at Lac des
The curves which are shown in Fig. 8 are D32 versus
Iles [18]
impeller tip speed (i.e., power intensity) for Jg =0.5 and
1 cm/s and different frother concentrations. First, as
stated in Ref. [8], the bubble size decrease markedly
followed by increasing of the frother concentration or
decreasing of superficial gas velocity (Jg). Second, it is
evident that the conditions in the impeller region are
highly turbulent, and bubble size and BSD are unaffected
by significant changes in impeller speed (and resulting
power intensity) within the full operating region of 4.6 to
9.2 m/s. Below this, as the cell approaches its lower
operating limit, bubble size begins to increase. However,
for practical considerations, the bubble size remains
effectively constant with increasing impeller tip speed.
Fig. 7 Jg−D32 relationship for Bateman 50 m3 cells (1 kW/m3) This suggests that the system is dominated by
and Metso RCS 30 m3 cells fitted with 70 m3 mechanisms coalescence issues and that there is no “breakage” of
(3 kW/m3) at Impala [18] bubbles occurring. It also means that in plants where
speeding up mechanisms (South Africa-Pt fines recovery)
have been made in these comparisons [17], and clearly, has proved beneficial, the effects must be due to
the conclusions would be strengthened by a more particle-collection efficiency related to increase pumping
controlled set of laboratory experiments measuring rates and kinetic energy and not bubble size or increased
power intensity at the shaft for various combinations of bubble surface area flux (Sb).
impeller speed and size. The results may seem at odds with the researches by
However, the above assumption cannot be GRAU and HEISKANEN [1] who have claimed that
conformed by the impeller speed-bubble size tests in
pilot-scale Metso flotation cell. On the Metso unit,
impeller rotational speed is controlled via the frequency
setting (Hz) of the motor’s silicon controlled rectifier
(SCR). The specific power is determined by dividing net
power by 0.7 m3 of water in the cell. To calculate the
impeller tip speed from the motor speed, one needs the
ratio of motor sheave (0.125 m in diameter) to
mechanism sheave (0.356 m in diameter) and the
impeller diameter (0.21), as shown in Eq. (4). The range
of the SCR frequency on the unit is 30 to 80 Hz,
providing a range of impeller rotation speed from 313 to
834, equivalent to tip speed variation from 3.44 to 9.17
m/s. This range extends well-beyond the typical industry Fig. 8 Effect of impeller tip speed on bubble size (D32) for
range of 5 to 7 m/s [21]. The testing was done at 0, 2.5, 5 0.8 m3 metso pilot flotation cell [18]
J. Cent. South Univ. (2014) 21: 1077−1084 1083
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