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Significant reduction in collector consumption by implementing ultrafine

bubbles in lead and zinc rougher flotation

Article in Powder Technology · November 2022

DOI: 10.1016/j.powtec.2022.118096

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Significant reduction in collector consumption by implementing ultrafine bubbles in lead and

zinc rougher flotation

Mahdi Shadman, Mohammad Raouf Hosseini*, Zahra Taghavi zinjenab, Ebrahim Azimi
Department of Mining Engineering, Isfahan University of Technology, Isfahan 8415683111, Iran

Abstract

Ultrafine bubbles were applied to the rougher flotation of the lead and zinc minerals, and the effects

of the particle size (-38, -75, and -106 µm) and collector concentration (potassium ethyl xanthate: 60,

80, 100, and potassium amyl xanthate: 10, 20, 30 g/t) were investigated on the lead and zinc recovery

by implementing central composite and two-level full factorial designs, respectively. Considering the

results, particle size was the most effective variable which substantially enhanced the lead recovery

from 27.6 to 63.65%, and the zinc recovery from 59.92 to 84.88%. Also, the introduction of ultrafine

bubbles improved the lead and zinc recoveries by about 7.41 and 1.22%, respectively. It could be

concluded that the adsorbed ultrafine bubbles helped collectors in making the particle surface

hydrophobic, and consequently reduced the reagent consumption. In conclusion, the application of

ultrafine bubbles to the lead-zinc flotation proved to be beneficial from the metal recovery aspect.

Keywords: Flotation, Lead, Recovery, Ultrafine bubbles, Zinc

* Corresponding author (M.R. Hosseini):

Email: [email protected],

Tel: +98 31 3391 5171,

Fax: +98 31 3391 2754

1. Introduction

Basically, mineral processing consists of two main stages, generally known as comminution, reducing

particle size, and enrichment where valuables are separated from gangues to produce a marketable

product or concentrate. Froth flotation (i.e., flotation), as one of the physicochemical separation

methods, is undoubtedly one of the most commonly utilized methods of mineral processing [1].

Fine particles or slimes (less than 10 microns) may be naturally generated by weathering or produced

during the comminution and grinding of the ore for satisfying the necessary criteria for mineral

liberations. Therefore, in many instances, slimes cannot be avoided and removed due to economic or

practical reasons [2]. Moreover, mineral processing tailings, which are mainly constituted of fine

particles, are becoming a critical issue for the mining industry, because of environmental concerns.

Improvements in the flotation of fine particles through bubble size reduction, fine particle

aggregation, and modification of the flow conditions have been brought to notice in recent years. The

flotation process involves the interaction between particles and bubbles with three sub-processes

(probabilities) of particle-bubble collision, attachment, and stability. The flotation rate is a function

of these sub-processes [2-6]. The poor flotation of fine particles is often due to the low bubble-particle

collision efficiency, affected by the ratio of the particle to bubble diameter. Studies showed that

decreasing bubble size can result in increasing the efficiency of fine particle flotation [7-10].

Nanobubbles (NBs) are tiny gaseous domains within an aqueous solution that are between 50 and

500 nm in radius. The formation of NBs is often achieved when a homogenous liquid phase undergoes

a phase change caused by a sudden pressure fall below its critical value, which is known as cavitation.

NBs improve coarse and fine particle flotation performances and reduce reagent consumption through

various mechanisms. The bridging of bubbles between hydrophobic surfaces favors fine particle

flotation. Coating the fine particles with NBs will lead to the generation of agglomerates which are

more easily recovered due to an increase in the collision probability. In addition, NBs increase the

particle hydrophobicity and thus the bubble-particle attachment probability, which decreases the

detachment chance [11-14].

2
The history of sulfide ore flotation in the industry dates back to the beginning of the 20th century.

Sulfide ores are the major sources of base metals like copper, lead, zinc, nickel, cobalt, etc.

Beneficiation of the base metal sulfide minerals is predominating through the flotation technique.

Generally, two different strategies are employed for Pb-Zn ores beneficiation through flotation, i.e.,

differential and bulk lead-zinc flotation. In the differential flotation; lead minerals firstly are

recovered after depressing zinc minerals, and subsequently, zinc concentrate is activated after

activation. If the associated sulfide minerals, e.g., galena, and sphalerite have distinct surface

properties, floatability, and adequate liberation, this method is adopted. In the bulk flotation strategy,

suitable for intergrown fine-grain low-grade sulfide ores, both lead and zinc minerals are recovered

simultaneously [15-17].

Zhou et al. (1997) showed that in-situ bubble formation by hydrodynamic cavitation could induce

particle aggregation through gas nucleus bridging with the larger particles having a higher collection

rate. As a result, the flotation kinetics of fine silica and zinc sulfide precipitates were significantly

increased [18]. The effect of nano-microbubbles on the flotation recovery of fine and ultrafine

chalcopyrite particles was investigated by Ahmadi et al. (2014). They proved that the presence of

nano-microbubbles increased the recovery of chalcopyrite fine and ultrafine particles by 16–21%,

and also reduced the consumption of collector and frother by 75% and 50%, respectively. The process

was more efficient for the ultrafine particles than for the fines [19]. Kursuna and Ulusoy (2014)

revealed that zinc concentrate grade and recovery were increased by ultrasonically assisted column

flotation. They explained that ultrasound waves produced small bubbles through hydrodynamic

cavitation. Attachment of the small bubbles to the particle surface increased contact angle and

hydrophobicity and consequently improved collector adsorption [20]. Rulyov et al (2017) found that

the application of microbubbles as the carrier in the flotation of finely dispersed Cu–Pb–Zn– Fe–

sulfide minerals increased the process rate by a factor of 2–4 and the recovery by 0.5–3% [21].

Mikhlin et al. (2020) found that nanobubbles generated by the temperature elevation from 0 to 80℃

increased the contact angle of sphalerite and silica. Also, a maximum contact angle was achieved for

3
galena and pyrite at 40–60℃. The temperature pretreatment depressed sulfide minerals in collector-

less flotation, while improving the collector-assisted flotation of Pb-Zn ore [22]. Chipakwe et al.

(2022) conducted research on the flotation of -150 and -38 µm complex lead-copper-zinc sulfide

particles with the help of 100-200 nm nanobubbles produced by a venturi tube. Nanobubbles

improved the selectivity of coarser particles, where mass recovery and flotation kinetics for the fine

particles were enhanced [23].

The Goushfil lead-zinc mine is an epigenetic Pb, Zn, and Ba Mississippi valley-type deposit which is

located in the Irankuh mining district, 20 km southwest of Isfahan city in Iran. In this study, ultrafine

bubbles (nano-microbubbles) were employed to increase the flotation recovery of coarse (-75 μm, -

106 μm) and fine (-38 μm) lead and zinc mineral particles obtained from Goushfil mine and to

estimate the collector consumption in the presence and absence of ultrafine bubbles.

2. Materials and methods

2.1. Head sample properties

The lead-zinc ore sample utilized in this investigation was obtained from the Goushfil mine, located

southwest of Isfahan, Iran. X-ray diffraction (XRD) examination was done on materials using an

Asenware AW/XDM 300, China, in the 10°–90° range (step size: 0.05° 2, step time: 1 s, slit width:

0.5°) with CuK radiation k=1.5405 at 40 kV, 30 mA. To determine the chemical composition of the

sample, an S4 Pioneer X-ray fluorescence (XRF) analyzer from Bruker (Germany) was used. Also,

atomic absorption spectroscopy (AAS) was implemented to measure the Zn, Pb, and Fe grades of the

sample. Metal recovery calculations were performed based on the result of the AAS analysis. To carry

out the flotation experiments, the feed ore sample was crushed and ground into three size fractions of

-106, -75, and -38 µm using three different grinding times. Also, for the mineral liberation

investigations, polished sections were prepared from +106, -106+38, and -38 µm fractions, and

studied using an Olympus polarized microscope. Dynamic light scattering (DLS) technique was

employed to obtain the size of the -38 µm particles using Horiba SZ-100.

4
2.2. Reagents

The chemical reagents used in this research work were zinc sulfate (ZnSO₄) 32% and sodium cyanide

(NaCN) 98% as zinc inhibitors, dextrin as the iron inhibitor, copper sulfate (CuSO4, XH2O) 24% as

the zinc activator, methyl isobutyl carbinol (MIBC) as the frother, potassium amyl xanthate (PAX)

90% and potassium ethyl xanthate (PEX) 90% as the collector for sphalerite and galena, respectively.

Also, water containing bubbles with diameters of 55-250 nm was used for the flotation tests.

2.3. Equipment

To generate -2 mm particles, a laboratory roll crusher (in a closed circuit) was employed. The samples

were then combined, split, and packaged for the flotation tests. Grinding periods of 55, 65, and 175

min were used in an open circuit laboratory rod mill to reach the particle sizes of 100% under 106,

75, and 38 μm, respectively. For the flotation experiments, a laboratory Denver flotation machine

with a 2.3 L cell was employed.

(a)
(b)

Fig. 1. The two-phase vortex pump: (a) Schematic of the pump function, (b) The pump structure
includes (1) cover, (2) O-ring, (3) mixing blade, (4) mechanical seal, (5) motor shaft, (6) main body,
(7) motor

A two-phase vortex pump (SVP40 S 22-B), developed by Dantek Company (Isfahan, Iran) was used

to create ultrafine bubbles containing water at the pressure of 3.5 bar, and inlet air flow rate of 7 m3/h

5
and 0.48 Nm3/h, respectively, and a power of 2.2 kW. Fig. 1a. depicts a schematic of the described

pump, which has two inlets (for water and the desired gas) and one outlet (for the produced gasified

fluid). The input water is taken from a reservoir tank, which also accepts the water-containing

ultrafine bubbles from the pump output. As a result, the water circulates between the pump and the

tank and enhances the bubble concentration.

Gas is mixed with the liquid in the pump, then ultrafine bubbles with the size of <50 µm

(microbubbles) and <200 nm (nanobubbles) are formed. The dispersed gas may also be dissolved in

the liquid to some extent. This type of generator uses a regenerative pump that has a very simple and

inexpensive structure, as can be seen in Fig. 1b. The pump is composed of a regenerative impeller

with multiple blades, a casing, and a tank for discharging the pressurized and mixed bubble water.

The fluid passes through each impeller blade which induces a pressure that is higher at the inlet than

at the outlet. The local recirculation flow at each blade passage produces microbubbles by mixing

and crushing the water and air supplied. Therefore, a regenerative pump can achieve lower mass

fluxes but higher-pressure differences in contrast to the other pumps at the same circumferential

velocity. Fine bubbles would be obtained at the outlet of the impeller due to the super-saturated

condition between gas and fluid [24, 25].

2.4. Flotation

Flotation experiments were carried out at natural pH using 900 g samples. The factors investigated

were particle size, the percentage of the ultrafine bubble containing water (UFBW), and the

concentrations of PEX and PAX in the pulp. The mineral samples with 35% solid were conditioned

in different UFBW fractions (0, 0.5, and 1). As zinc depressants, 120 g/t zinc sulfate and 66 g/t sodium

cyanide were added, and the solution was conditioned for 9 min. Dextrin and PEX were added to the

cell and conditioned for an additional 2 min.

6
 Fig. 2. The schematic presentation of the performed flotation process and the equipment applied

Finally, the flotation process began 1 min after the addition of 25 g/t frother. Finally, a lead-rich froth

was collected for 2.5 min. The pulp volume was then restored to its original level by adding

UFBW/tap water and was conditioned for another 2 min with copper sulfate and PAX. Zinc flotation

started 1 min after conditioning the pulp with a 25 g/t frother, and finally, the zinc-rich froth was

collected for 4 min. The gained concentrates and tailings were filtered, dried, weighed, sampled, and

analyzed for the total Pb and Zn contents, and the replicates yielded an error value of 0.4%. The

flotation experiment is schematically displayed in Fig. 2. As is seen, the necessary volume of UFBW

for each experiment was obtained after recycling tap water between the pump and reservoir. After

conducting experiments, the flotation products, as well as the remained tailing in the cell, were dried,

weighted, and analyzed for Pb and Zn contents. Finally, the obtained results were collected and

analyzed, if necessary Stat-Ease design expert software was also used in the analysis.

2.5. Experimental design and data analysis

The Design Expert software (version 7.0, trial version) was used to assess the influence of factors on

lead and zinc recoveries. A central composite design (CCD) with 3 factors at three levels and a 2-

7
level factorial design with four factors at three levels were used in this investigation for the lead and

zinc minerals, respectively. To identify the best conditions, many factors such as UFBW percentage,

collector concentration (PEX or PAX), and feed particle size were investigated. The investigated

parameters and their related real and coded values are listed in Table 1 for the lead and zinc flotation

experiments. The Pb and Zn recoveries were investigated as the response variable to achieve the

optimal UFBW fraction, particle size, PEX, and PAX dosages. Analysis of variance (ANOVA) was

employed to determine the effective variables and their influences on the response, and to assess the

obtained model and the interactions between the parameters. A 95% confidence level was considered

to evaluate the significance of the model terms.

Table 1. The applied variables and their associated levels used in the CCD and the 2-level factorial
designs

Factor Name Units Low (-1) Middle (0) High (+1)

CCD for lead recovery
A Size μm -38 -75 -106
B UFBW fraction % 0 50 100
C PEX g/t 60 80 100
2-level factorial design for zinc recovery
A Size μm -38 -75 -106
B UFBW fraction % 0 50 100
C PEX g/t 60 80 100
D PAX g/t 10 20 30

3. Results and discussion

3.1. Sample properties

As shown in Table 2, quartz and dolomite exist in the ore as the major phases, while sphalerite and

galena are classified as the minor phases. Also, according to the XRF investigations (Table 3), the

head sample includes 0.4% Pb, and 1.8% Zn.

Chemical analysis of the ore using AAS showed that Pb and Zn assays are 0.53 and 1.85%,

respectively. 0.41% of lead and 1.70% of zinc are from galena and sphalerite, and the rest is in the

oxidized form.

8
 Table 2. The mineralogical composition of the head sample obtained by XRD
Major phases Quartz Dolomite

Sphalerite Galena
Minor phases
calcite blende

Table 3. The chemical composition of the head sample obtained by XRF

Compounds SiO2 Al2O3 CaO Fe2O3 K 2O MgO SO3 TiO2 BaO Na2O Zn Pb

Amount (%) 47.1 14.1 10.2 3.9 3.7 3.6 2.9 0.7 0.4 0.3 1.8 0.4

Studies carried out on mineral liberation indicate that the degrees of liberation for sphalerite are 65,

83, and 99% for the +106, -106+38, and -38 µm fractions, respectively. Considering galena mineral,

20, 50, and 95% degrees of liberation were calculated for the same three particle size fractions.

Furthermore, DLS analysis revealed that D80 of the -38 µm size fraction was about 12 µm. This

measurement proves that the last fraction contains fine particles.

3.2. Results of the experimental designs

Table 4 and Table 5 provide the intended matrix and parameter values utilized in the lead and zinc

experiments and responses (Pb and Zn recoveries). According to Table 4, by increasing the UFBW

percentage from 0% to 100%, Pb recovery increases by 9-14.1% for -38 µm, 7.8% for -75 µm, and

14.3-15.5% for -106 µm feeds. The highest lead recovery (77.9%) was obtained in run 4 by applying

100% UFBW, 100 g/t PEX, and for -106 μm feed. On the contrary, the lowest lead recovery (20%),

was achieved when using no UFBW, 60 g/t PEX, and -38 μm feed (Run 10). Also, it can be seen from

Table 5 that increasing UFBW content from 0% to 100% increases Zn recovery by 2.7-19.2% for -

38 µm, and 2.3-5.3% for -106 µm feed. The best zinc recovery (92.2%) was obtained in run 12,

employing 100% UFBW, 60 g/t PEX, 10 g/t PAX, and for -106 μm feed.

9
 Table 1. Results of the CCD design obtained in the lead mineral flotation

Run UFBW fraction (%) feed size (μm) PEX (g/t) Recovery (%)
1 0 -106 60 55.75
2 0 -106 100 63.62
3 50 -106 80 61.77
4 100 -106 100 77.94
5 0 -38 100 28.00
6 100 -106 60 71.24
7 100 -75 80 57.30
8 50 -75 100 65.31
9 50 -75 80 61.96
10 0 -38 60 20.00
11 50 -75 80 59.58
12 50 -75 80 57.55
13 50 -38 80 29.04
14 0 -75 80 65.11
15 50 -75 80 57.30
16 50 -75 80 67.43
17 100 -38 60 34.07
18 100 -38 100 36.99
19 50 -75 60 59.06

Table 2. Results of the 2-factorial design obtained in the zinc mineral flotation

Run UFBW fraction (%) Size (μm) PEX (g/t) PAX (g/t) Recovery (%)
1 100 -106 100 10 91.39
2 50 -75 80 20 85.28
3 0 -106 60 30 85.51
4 100 -106 60 30 87.76
5 0 -106 100 10 82.43
6 100 -38 100 10 62.40
7 0 -38 100 10 59.28
8 0 -106 100 30 84.87
9 100 -106 100 30 81.40
10 50 -75 80 20 83.88
11 0 -38 60 10 60.41
12 100 -106 60 10 92.20
13 100 -38 60 30 67.03
14 100 -38 100 30 48.23
15 0 -38 100 30 67.47
16 100 -38 60 10 63.12
17 0 -106 60 10 86.87
18 0 -38 60 30 56.97
19 50 -75 80 20 85.13

Fig. 3a and b present the average values of the lead and zinc concentrate grades and recoveries in the

presence of 0, 50, and 100% of the UFBW. Fig. 3a and b indicate that including 50% UFBW in the
10
pulp improves both the grade and recovery of either lead or zinc minerals. Application of 50% UFBW

rises lead recovery from 46.5 to 57.7% and increases lead concentrate assay from 2.5 to 2.8%. On the

other hand, improvements in zinc recovery and grade from 62.7 to 84.8%, and 5.4 to 8.9% are

discernable, respectively. However, the application of UFBW instead of tap water (100% UFBW) in

the flotation cell causes a decline in the grade and recovery of both minerals. Recoveries of lead and

zinc fall to 55.5 and 76.6%, respectively. Also, regarding concentrate grades, 2.2% lead and 5.3%

zinc are achieved after 100% UFBW addition.

60 3 90 10
(a) (b) 9
Lead recovery (%)

Zinc grade (%)

2.8 80
Zinc recovery (%)
Lead grade (%)

55 8
2.6 70 7
50 6
2.4 60 5
45 4
2.2 50
Recovery Grade 3
Recovery Grade
40 2 40 2
0 50 100 0 50 100
UFBW fraction (%) UFBW fraction (%)

Fig. 3. Average concentrate grades and recoveries of (a) lead (b) zinc as a function of UFBW
fraction

It is possible that when using 100% UFBW, the excess nanobubbles which are adsorbed on the

particle surfaces attract the collector molecules from their hydrocarbon chain due to the presence of

hydrophobic force between collectors and nanobubbles. Therefore, the polar solidophilic group of the

collector is exposed to water and makes the particles hydrophilic at higher UMFB concentrations.

This phenomenon leads to a reduction in concentrate grade and recovery.

3.3. Statistical analysis of the lead flotation (CCD)

The relationship between UFBW percentage, PEX dosage, and particle size on the response

(Recovery) of the lead and zinc flotation process was investigated using a central composite design.

11
The analysis of variance (ANOVA) of the quadratic model for lead flotation is shown in Table 6, and

the statistics of the proposed model are shown in Table 7. The presented data show that the model is

significant at a 99.99% confidence level. The F-values of lack of Fit (1.36) show that lack of fit is not

significant in contrast with the actual pure error. Regarding the tabulated F-values of the variables,

particle size (A) is the most effective parameter followed by UFBW percentage (B) and PEX

concentration (C), respectively.

Table 3. The results of ANOVA on the lead flotation design

Source Sum of squares Mean square F-value p-value

Model 4475.91 745.99 41.78 <0.0001
A- Particle size 3319.92 3319.92 155.14 <0.0001
B- UFBW 203.18 203.18 9.49 0.0088
C- PEX 100.84 100.84 4.71 0.0491
A2 637.94 637.94 29.81 0.0001
B2 7.91 7.91 0.37 0.5538
Residual 272.52 22.71 - -
Lack of Fit 204.12 25.51 1.36 0.4084
Pure Error 68.40 17.10 - -

Furthermore, Table 7 shows the summary of the statistical data of the obtained model (Eq. 1). As

discerned from the table, the mean value (54.15) is about 12 times larger than the standard deviation

(4.63). The R-squared of the model is 94% which indicates that the model has matched the

experimental data very well. Also, the adjusted R-squared (92%) of the model is at a close distance

from the R-squared value. Adequate precision is 19.93, where ratios larger than 4 suggest sufficient

model discrimination.

RPb (%) = 60.80 + 18.22A + 4.5B + 3.18C - 14.22A2 + 1.58B2 Eq. 1

Table 4. Statistics of the lead recovery model

Statistics Value
Standard Deviation 4.63
Mean 54.15
Coefficient of Variation 8.54
R-Squared 0.94
Adjusted R-Squared 0.92
Adequate Precision 19.93

12
The Box-Cox plot (Fig. 4a) of the lead recovery model was used to evaluate the best transformation

to be applied to the response data. It displays the minimal lambda values as well as lambdas at the

95% confidence level. The low and high confidence intervals are 0.02 and 1.62, respectively. Also,

the present confidence interval is 1, indicating that standard transformation and model reform is

unnecessary.

The perturbation plot is useful for comparing the effects of all the variables at a certain point in the

design space. Only one element is changed across its range while the other factors remain fixed at the

pre-determined level. Fig. 4b demonstrates the perturbation diagram of lead recovery where the

reference point is set to the midpoint (coded 0) of all components. According to the figure, raising all

three parameters from -1 to +1 level enhances the lead recovery, and as previously stated in Eq. 1,

the slope of the curve for the particle size is more than the ultrafine bubble fraction and PEX. Raising

the concentration of UFBW from 0 to 100% increases lead recovery by 10.9%. Also, raising particle

size from -38 to -106 μm improves lead recovery by 37.2%. Increasing the PEX dosage from 60 to

100 g/t augments the lead recovery by 4.5%.

11 (a) 80 (b)
A: Particle size
B: UFBW fraction
10 70 C: PEX concentration B
CA
BC
Pb recovery (%)
Ln(ResidualSS)

9 60

8 50

7 40

6 5 .8861 7
30 A
5 20

-3 -2 -1 0 1 2 3 -1.000 -0.500 0.000 0.500 1.000

Lambda Deviation from reference point

Fig. 4. The plots of (a) Box-Cox and (b) perturbation for the lead recovery

3.4. Statistical analysis of the zinc flotation (factorial design)

13
The effects of particle size, UFBW fraction, PEX, and PAX dosage on the zinc recovery as the

response variable were studied by applying a 2-level factorial design. The ANOVA result of the

factorial design is shown in Table 8. According to the table, the models are significant at a 99.7%

confidence level. Considering the tabulated F- and p-values, the significant model variables are

particle size (A), PEX (C), PAX (D) concentration, and UFBW (B), in the order given. Also, the two-

factor interactions BC, BD, and AB are significant with more than 95% confidence level. The

curvature F-value of 536.83 indicates that there is a considerable bend in the design space.

Table 5. The results of ANOVA on the zinc flotation design

Source Sum of Squares Mean Square F- Value p-value

Model 3060.69 255.05 448.17 0.0029
A- Particle size 2691.76 2691.76 4729.84 0.0002
B- UFBW 5.93 5.93 10.43 0.0232
C- PEX 31.39 31.39 55.17 0.0007
D- PAX 22.20 22.20 39.01 0.0015
AB 16.88 16.88 29.66 0.0028
AD 3.85 3.85 6.76 0.0482
BC 60.05 60.05 105.52 0.0002
BD 58.19 58.19 102.25 0.0002
CD 4.19 4.19 7.37 0.0420
ABC 44.88 44.88 78.87 0.0003
BCD 95.37 95.37 167.59 <0.0001
ABCD 25.93 25.93 45.57 0.0011
Curvature 315.73 315.73 554.79 <0.0001

Table 9 presents the statistical summary of the model. The zinc recovery model is presented in Eq. 2.

As inferred, the value of the standard deviation (0.75) is small compared with the mean (75.35) of the

proposed model. Also, the R-squared and adjusted R-squared are both at the maximum values.

Finally, the term “Adequate precision” which refers to the signal-to-noise ratio is 67.05 which is

considered a large value.

RZn (%) = 73.58 + 12.97A + 0.61B - 1.40C - 1.18D + 1.03AB - 0.49AD - 1.94BC -
Eq. 2
1.91BD - 0.51CD + 1.67ABC - 2.44BCD + 1.27ABCD

As shown in Eq. 2, the coefficient of the parameter A (particle size) is greater than all others,

indicating that size has the greatest impact on the zinc recovery and using large particle size leads to
14
improved zinc recoveries. The second component is UFBW fraction (B) which boosts zinc recovery.

Because of its lower coefficient, the significance of the UFBW fraction on the zinc recovery is after

the PEX (C) and PAX (D) collectors. Due to the negative coefficients of PAX and PEX, increasing

their concentration adversely influences zinc recovery.

Table 6. Statistics of the zinc recovery model

Statistics Value
Standard Deviation 0.75
Mean 75.35
Coefficient of Variation 1.00
R-Squared 1.00
Adjusted R-Squared 1.00
Adequate Precision 67.05

Fig. 5a shows the Box-Cox diagram of the zinc recovery. It displays the minimal lambda values as

well as lambdas at the 95% confidence level. The low and high confidence intervals are 0.21 and

1.81, respectively. The present confidence interval is 1. So, as seen in Eq. 2, the model is proposed

without transformation.

6 (a) 100 A: Particle size (b)

B: UFBW fraction
C: PEX concentration
5
90
D: PAX concentration A
Zn recovery (%)
Ln(ResidualSS)

80
C
BD DB
4
C
70

3 A
60

2 1.8116 3
50

1 40

-3 -2 -1 0 1 2 3 -1.000 -0.500 0.000 0.500 1.000

Lambda Deviation from reference point

Fig. 5. The plots of (a) Box-Cox and (b) perturbation for the zinc recovery

15
Fig. 5b illustrates the perturbation plot of the zinc recovery at the midpoint (coded 0) of all other

variables. Clearly, changing the coded value of parameter A (particle size) from -1 to 1 enhances zinc

recovery owing to its positive line slope. Furthermore, considering the positive small slope of

parameter B (UFBW fraction), zinc recovery increases by augmenting the UFBW fraction in the pulp.

However, as can be seen, boosting both parameters C and D from -1 to 1 results in a negative slope

of the lines, indicating a reduction in zinc recovery. Therefore, increasing the concentration of the

ultrafine bubbles from 0 to 100% improves zinc recovery by 1.8%, and raising the feed particle size

from -38 to -106 μm improves zinc recovery by 24.8%. The elevation of PEX dosage from 60 to 100

g/t lowers the zinc recovery by 3.7%. Similarly, increasing PAX dosage from 10 to 30 g/t decreases

zinc recovery by 3.5%.

(a) (b)

Fig. 6. Interaction plot of the UFBW fraction and particle size on the zinc recovery: (a) contour
plot, (b) 3D plot

Fig. 6a and b present 2D and 3D plots of the effects of particle size and UFBW fraction as the

independent parameters on the zinc recovery as the response variable, while keeping other factors

constant at the midpoint (coded 0). It is evident from the figures that at the highest level of UFBW

fraction (100%), increasing the size of particles from -38 to -106 μm leads to an improvement in zinc

recovery from 60 to 87.8% while PEX and PAX concentrations were at 80 and 20 g/t. It can also be

understood that UFBW has a greater impact on the coarse (-106 μm) than the fine particles (-38 μm).

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Increasing the UFBW fraction from 0 to 100% increases zinc recovery from 86.1 to 87.8% for

particles with a size of -106 μm, and from 60 to 61.7% for the -38 μm particles.

Fig. 7 can be used to make the two-factor interactions more understandable. The interaction is shown

as two non-parallel lines when the response differs depending on the settings of both parameters.

According to the studies [26, 27], since ultrafine bubbles act as a secondary collector, a decrease in

collector consumption in the presence of ultrafine bubbles is discrete. Therefore, here the interactions

between the UFBW and both collector concentrations (BC, BD) on the zinc recovery are examined.

Fig. 7a and b depict the interaction of the UFBW fraction and the PEX collector for the particle sizes

of -38 and -106 µm when the PAX concentration is constant and equals 30 g/t (high level, +1). In the

absence of ultrafine bubbles (0%), zinc recovery in the presence of 100 g/t PEX equals 67.7%, and a

decrease in PEX concentration reduces zinc recovery to 56.8%. When the proportion of UFBW in

the pulp increases, a reduction in the collector concentration enhances the zinc recovery so that, at

the UFBW fraction of 36%, zinc recovery at the low PEX exceeds the high PEX concentration.

Regarding the -38 µm particles, at the fraction of 100% UFBW, the zinc recovery (66.8%) using 60

g/t PEX concentration is approximately equivalent to the recovery (67.7%) gained at 100 g/t PEX

without UFBW. This indicates a 40% decline in PEX consumption. Considering the -106 µm

particles, the low concentration of the PEX outperforms its high concentration when the proportion

of UFBW in the pulp is raised. In fact, zinc recovery increased from 85.6 at 0% UFBW to 87.9% at

100% UFBW. Inversely, at high PEX concentrations (100 g/t) elevating UFBW fraction from 0 to

100% drops zinc recovery from 84.7 to 81.3%. This evidences that ultrafine bubbles have a positive

influence on the low concentration of PEX for either fine or coarse particles.

Fig. 7c, and d represent the relationship between the PAX concentration and the UFBW fraction in

the presence of an 80 g/t (midpoint) PEX concentration for the -38 µm and -106 µm particle sizes.

Regarding the -38 µm particles (Fig. 7c), the zinc recovery at the UFBW fraction of 0% in the

presence of a 30 g/t PAX collector is 62.3%. However, when the UFBW fraction becomes 100%, 10

g/t PAX concentration leads to the zinc recovery of 62.8% which is even more than that obtained at

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30 g/t collector concentration. Therefore, using the UFBW fraction decreases collector consumption

by 67%. Moreover, Fig. 7d shows that if the particle size of -106 µm is used, increasing the UFBW

fraction from 0 to 100% enhances the zinc recovery from 84.7 to 91.8% at the PAX concentration of

10 g/t, while for the high concentration of PAX (30 g/t), the recovery reduces from 85.2 to 84.6% by

increasing UFBW fraction from 0 to 100%. As a result, ultrafine bubble application can also reduce

PAX consumption at coarse particles.

(a) (b)

(c) (d)

Fig. 7. Interaction plot of the UFBW fraction and both collectors concentrations on the zinc
recovery. (Red lines: higher concentration; black lines: lower concentrations)

3.5. Process optimization

The following variables were considered in the numerical optimization of the evaluated model to

maximize the lead and zinc recovery in the presence of ultrafine bubbles: particle size (-38 to -106

µm), UFBW fraction (0–100%), PEX (60–100 g/t), and PAX (10–30 g/t), and the optimal levels of

the variables were established. The optimal levels of the operational variables to achieve maximum

lead recovery based on the reduced quadratic model with desirability levels of 70% are: particle size
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of 94 µm, UFBW fraction of 100%, and PEX concentration of 100 g/t. Based on such optimization,

a lead recovery of 69.66-82.14% confidence interval with a 95% confidence level is projected.

Furthermore, according to the factorial model, the optimal levels of the operational variables to

achieve maximum zinc recovery with desirability levels of 84% are as follows: particle size (-106

µm), UFBW fraction (100%), PEX (100 g/t) and PAX concentration (10 g/t). A zinc recovery

between 90.05 and 93.52% confidence interval with a 95% confidence level is estimated after

optimization. The flotation experiments conducted in the obtained optimum conditions, gained the

lead and zinc recoveries of 80.31 and 91.88%, respectively, which are in the predicted confidence

intervals.

4. Conclusion

Investigating the influence of ultrafine bubbles (UFBW fraction) on lead and zinc rougher flotation

performance, in terms of valuables recovery to the concentrates, was the goal of this study. The

experimental design data revealed that size is the most influential parameter on the lead and zinc

recoveries. Other influencing parameters are UFBW fraction and collector dosage (PAX and PEX).

The lead recovery was enhanced in the presence of a high concentration of PEX collector (100 g/t).

Also, a low dosage of PEX and PAX collectors (PEX: 60 g/t, PAX: 10 g/t) improved the recovery of

zinc mineral to the concentrate. The ultrafine bubbles playing the secondary collector role might be

the reason. The recovery of lead raised significantly from 24.9 to 32.5% as the UFBW fraction

increased from 0 to 100% at -38 µm particle size, and from 59.5 to 70.2% at -106 µm particle size.

Increasing the fraction of UFBW from 0 to 100% improves zinc recovery from 84.7 to 91.8% for -

106 µm particles and from 59.8 to 62.8% for the particle size of -38 µm. The introduction of ultrafine

bubbles meaningfully reduced the consumption of PEX and PAX collectors by up to 40 g/t and 20

g/t, respectively. By optimizing the key parameters, it is expected that lead and zinc recoveries

increase to 75.9 and 91.8%, respectively, when the ultrafine bubbles are used.

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Acknowledgment

Bama lead and zinc company is greatly acknowledged for providing mineral samples, laboratory

facilities, and technical support for this research project.

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