Journal of Molecular Liquids 225 (2017) 260–264

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Journal of Molecular Liquids

journal homepage: www.elsevier.com/locate/molliq

Review

Various flotation techniques for metal ions removal

Eleni A. Deliyanni a, George Z. Kyzas b,c, Kostas A. Matis a,⁎
a
Division of Chemical Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR 54124, Thessaloniki, Greece
b
Department of Oenology and Beverage Technology, Eastern Macedonia and Thrace Institute of Technology, Kavala, GR 654 04, Greece
c
Hephaestus Advanced Laboratory, Eastern Macedonia and Thrace Institute of Technology, Kavala, GR 654 04, Greece

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

Article history: The importance of the flotation process to the economies of the entire industrial world is considered to be enor-
Received 20 October 2016 mous; it is a gravity separation method, which is based on the idea of applying rising gas bubbles as the transport
Received in revised form 12 November 2016 medium. Usually following the selective attachment of bubbles to particles, those solids are transferred from the
Accepted 17 November 2016
body of water to the surface, where foam is formed. Hence, as opposed to settling, flotation is a solid–liquid sep-
Available online 24 November 2016
aration technique that is applied to particles of which the density is lower, or has been made lower, than the liq-
Keywords:
uid they are in, by collectors and modifiers. Thus, flotation initially originated from the field of mineral processing
Metals recovery but for many years, various particulate solids, in addition to minerals, have been extracted from water by using
Membranes this effective process. These flotation applications mainly include the treatment of water and wastewater, mainly
Water containing heavy metals, being the scope of the present. The techniques followed were that of ion, precipitate
Adsorbents and/or sorptive flotation, including the biosorptive one, summarizing to a dispersed-air flotation – microfiltration
Precipitation hybrid unit. Mention with certain examples will be given to the flotation separation (dispersed or dissolved-air)
Biosorption and recovery of the following pollutants, as selectivity was often the focus: Zn, Cd, Cu, Ni, Fe, Mn, Mo, P, As, Si.
© 2016 Elsevier B.V. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 260
2. Ion and precipitate flotation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 261
3. Sorptive and biosorptive flotation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 262
4. Hybrid flotation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263
5. Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263
References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263

1. Introduction wide applications, particularly, to industrial wastewater treatment, i.e.

Flotation constitutes a gravity separation process that certainly orig-
inated from minerals processing (usually termed froth flotation), a typ-
ical application is certainly with sulphide minerals. The importance of
flotation to the economy of the whole industrial world is considered
to be enormous [1–4]. Without this separation process, many familiar
metals and inorganic raw materials would be exceedingly scarce and
costly, because the high-grade ores that could be processed by simple
physical and mechanical methods have long since been used up. Apart
from adsorption techniques [5–19], flotation has also nowadays found
⁎ Corresponding author.
E-mail address: kamatis@chem.auth.gr (K.A. Matis).
metal ions recovery (in paper recycling, too). A wide variety of heavy
metal bearing waste streams requires treatment [20–22]. Sustainability
in the field of water separation processes (basically, flotation), and its
significance for the chemical and process industry, were commented.
Two broad categories of the process exist, according to the method
used in flotation for the generation of bubbles [23]: (i) dispersed-air flo-
tation that includes froth flotation, also electroflotation, and (ii) dis-
solved-air flotation (denoted often as DAF), which is typical for water
and effluent treatment.
The first generates bubbles by introducing air directly into the flota-
tion cell. In larger agitated cells, air is usually introduced through the
bottom of the agitator shaft and small bubbles are obtained mainly by
the shearing effect of impellers. In smaller cells, however, as well in

http://dx.doi.org/10.1016/j.molliq.2016.11.069
0167-7322/© 2016 Elsevier B.V. All rights reserved.
 E.A. Deliyanni et al. / Journal of Molecular Liquids 225 (2017) 260–264
flotation columns, a “sparger” is often used. The material used for the
sparger may be rigid (e.g. porous ceramic, stainless-steel or polyethyl-
ene) or soft (filter cloth, rubber etc.), whereas its shape may vary
(plate or cylinder). The size of the bubbles depends upon the sparger
pore size; the performance of rigid porous spargers has tended to dete-
riorate, due to pore plugging [24].
Dissolved-air (or pressure) flotation is based on the varying solubil-
ity of air in water, according to the pressure in the vessel; the arrange-
ment follows typically the idea of a recycle reactor configuration.
Initially, water (usually part of the outlet) is saturated with air at a rel-
atively high pressure. When this water is introduced in the flotation
vessel, the change to normal (atmospheric) pressure releases the air
bubbles. Alternatively, vacuum may be used to decrease the pressure,
after first saturating the water at atmospheric pressure. The amount of
air dissolved in water for a given pressure may be easily calculated
using Henry's law.
It is believed that the control of both particle - i.e. by size reduction -
and bubble size is of paramount interest in affecting the process; noting
that a large amount of valuable minerals was in the past discarded as
fines and ultrafines, because of inadequate technology to process
them economically [25]. Although much attention, perhaps for obvious
reasons, has been paid in-depth to the particle size, the role of bubble
size was somehow comparatively disregarded, deserving more atten-
tion [21]. Certainly, there are practical reasons involved in the gas (usu-
ally, air) bubble size change. However, various alternative bubble
generation methods, quite unconventional, utilize fine bubbles [26].
Updating the recent literature in the relevant scientific area perhaps
mention may be given, among other, to the following papers: Selectivity
coefficients between metal ions were evaluated from ion flotation re-
sults, using a polyethoxy-carboxylate surfactant [27]. Sugar based che-
lating surfactants were used elsewhere for metal recovery from water
phases; the importance of the adsorption phenomenon explained the
differences obtained for flotation experiments at different pH [28]. The
removal of sulphate ions from wastewater, being an environmental
challenge faced by several industrial sectors (i.e. acid mine drainage),
was examined; the results showed that the removal of these ions by flo-
tation depended on their precipitation and flocculation [29]. Different
mechanisms (such as foam fractionation, ion flotation, precipitate flota-
tion, and adsorbing colloid flotation) were found to occur during the
separation of gallium from leach liquors [30]. Optimal results for the re-
covery of nickel and zinc ions, obtained from a first experimental step,
conducted in a Hallimond tube were then evaluated in a mechanical flo-
tation cell [31]. The successful separation of the arsenic-bearing min-
erals from contaminated soils was also reported, using oil agglomerate
flotation, i.e. an agglomerate method by the addition of oil [32]. A
leaching-flotation-precipitation process was finally adopted to recycle
metals (Li/Fe/Mn ions) from spent battery cathodes [33].
Hereafter, the flotation research work has been reviewed and classi-
fied according to the relative process mechanism followed each time
[34] - this being, in the meantime, the title of the following chapters.
So, investigations are briefly described for ion, precipitate (i.e. as metal
hydroxide or xanthate) and sorptive flotation; the latter onto zeolite,
hydroxyapatite or biosorbents.
2. Ion and precipitate flotation
Ion flotation involves the removal of surface-inactive ions from
aqueous solutions by adding surfactants or collectors and the subse-
quent passage of gas bubbles through the solutions; the surfactant is
usually an ion having a charge opposite to that of the metal ion to be re-
moved. As a result of this procedure, on the surface appears a fine solid
particle containing the surfactant as a chemical constituent, which per-
mits the separation and concentration of the ionic species in a small vol-
ume of collapsed foam [35]. Hence, sometimes the process was termed
foam flotation, too. The surfactants are generally recoverable from the
product and may be recycled as also the clean water.
261
The potential of Cd(II) removal from aqueous solution with a
rhamnolipid biosurfactant sample was studied in the literature [36].
Synthetic surfactants have been replaced by microbial ones (i.e. yeasts)
to treat acid mine drainage [37], due to the advantages they offer, in-
cluding biodegradability. The recovery of gallium and indium halide
complexes and the respective thermodynamics of the process mecha-
nism were reported [38]. Removing also Cd(II) by ion flotation [39],
the advantages for treating wastewaters by this technique were raised
- i.e. low energy consumption, small space requirements, small volume
of sludge and acting selectively.
Namely, selective metals separation could be achieved, too. Fig. 1
presents an example. The flotation removal of phosphate, arsenate
and silicate anions was shown to be independent of the initial concen-
tration of molybdate ions, remaining in the underflow [40]. At low con-
centrations, the loss on Mo anions was increasing.
The metals (including molybdenum), of course, are non-renewable
resources - being consumed at an exponential rate as a result of popula-
tion and capital growth - Ion flotation will be further commented below.
Noting that a development of the technique, termed often adsorbing
colloid flotation, was applied in the given figure; this involves the re-
moval of a solute, like a metal ion, by adsorption on, co-precipitation
with or occlusion into a carrier floc, as ferric hydroxide. The latter is
then floated after usually the addition of a suitable surfactant (i.e.
dodecylamine), unless the product is enough hydrophobic or may be
well flocculated [41]. A modified Jameson (jet) cell was elsewhere
used for this technique, removing copper, zinc and nickel ions from syn-
thetic wastewater [42].
Following the aforementioned description of ion flotation, let us
continue saying that raising the respective concentrations may lead to
precipitation of the ion-surfactant floatable product, before air is passed.
This means that it is not a solution anymore but rather a dispersion.
Different “kinds” of precipitate flotation were categorized [43]. Fig. 2
gives here an example for the precipitate flotation of zinc ion
(1.53 × 10−4 M), where the best results were noticed at the pH value
of ~10 [44]; there was an agreement between the data and the optimum
precipitation area of the respective hydroxide [45].
Similar conclusions were reached for lead precipitate flotation [46].
The traditional chemical precipitation processes not only produce
large amounts of sludge, but also make it difficult to recycle the waste
metals.
R (%)
100
80
60 Mo
P
As
40 Si
20
0
0 200 400 600 800
[Mo(VI)] (mg/L)
Fig. 1. Selective separation by flotation of molybdate oxyanions from impurities (P, As and
Si): effect of initial molybdate concentrations. Reprinted with permission from Elsevier
[40].
262 E.A. Deliyanni et al. / Journal of Molecular Liquids 225 (2017) 260–264

Zn Removal %
100
80
60
40
20
0 phide minerals. Thermodynamic equilibrium diagrams and software
2 4 6 8 10 12
pH
Fig. 2. Flotation (dispersed-air) of zinc hydroxide precipitate by dodecylamine surfactant:
influence of solution pH; comparison with the theoretical optimum precipitation area.
Reprinted with permission from Gordon and Breach Sci [44].
Acid mine drainage is known to cause severe environmental pollu-
tion because of its high heavy metal content and strong acidity. A new
and comprehensive technology for wastewater treatment was pro-
posed, based on flotation, to reduce pollution and recycle resources
[47]. Rhamnolipid was also applied as a collector in the flotation of chro-
mium containing precipitates in aqueous solution, following a two level
full factorial design [48]; this is a biosurfactant that is produced by the
bacterial species Pseudomonas aeruginosa.
3. Sorptive and biosorptive flotation
The method involves the preliminary abstraction or scavenging of
metal ions using proper “sorbents”, which exist at the fine or ultrafine
particle-size range, followed by a subsequent flotation stage for the sep-
aration of metal-loaded sorbent particles from the treated (cleaned) so-
lution [49]. An example is presented as Fig. 3.
In the range investigated (up to 2 g/L. HAP), flotation was effective
and recoveries of the order of 90% were found for hydroxyapatite
Re (%)
100
(denoted as HAP) particles, while cadmium removals were over 95%
10
-6
[50]; calcium hydroxyapatite being the prototype of an inorganic crys-
talline constituent in human calcified tissues. The combined zinc re-
moval by common ion exchange resins (of Lewatit-type) and their
efficient separation by application of flotation during multicycle opera-
tion mode were elsewhere examined, including the regeneration of
resins; the particle size of resins during these experiments was reduced
Zn in size, as compared with the original [51]. Cost is an important param-
(M) eter for comparing the sorbent materials [52].
The impact of chemical speciation was stressed during various flota-
-4
10 tion applications for metal separation from the effluent [53]. The study
of the electrokinetic behaviour of the respective system involved, usual-
ly assisted by zeta-potential measurements, helped in the clarification
of the present flotation technique. Various examples were given, includ-
ing the removal of chromates and the classical in flotation, that of sul-
packages were employed to interpret the removal mechanism involved.
Biosorption is the process that makes use of dead biomass, usually
from fermentation wastes or by-products [54,55]; dead biomass does
not require nutrients and can be exposed to environments of high tox-
icity. The ability of microorganisms to remove metal ions from solution
is a well known phenomenon. Further, centrifugation and sedimenta-
tion, the conventional separation techniques, are not suitable to be
employed in the case of metal-bearing biosorbent due to the small
size of solid particles present in the solution, while in sedimentation
large settling tanks are needed due the low settling rate [56].
In the latter work, a novel material, air-filled emulsion introducing
high surface area between metal ions and biosorbent was used for cop-
per removal. Dissolved-air flotation has been recently reported to be
successfully applied after copper biosorption (onto inactive dry baker's
yeast Saccharomyces cerevisiae) resulting thereby a rapid, effective, and
relatively low-cost process [57]. The experimental results were support-
ed by the physicochemical characteristics of the surfactants used as col-
lector reagents - including dodecylamine.
A related example for the biosorptive flotation technique is shown as
Fig. 4, where metals and biomass removal were presented. A pro-
nounced indication for possible selective recovery of copper was ob-
served [58]; the existing difference in biomass floatability over the pH
of 8 was due to the deprotonation of surfactant. The biomass, here Strep-
tomyces rimosus, was previously modified by a polyelectrolyte. The
scope was to examine the effectiveness of potential low cost sorbent
materials, which may be applied in the preliminary stage of the process;
100

80
80

60
Re (%)

60

40
40

20
20 Streptomyces
HAP Cd Cu
Zn
0
Ni
0.0 0.5 1.0 1.5 2.0 0
[HAP], (g/L) 0 2 4 6 8 10
pH
Fig. 3. Sorption of cadmium ions on hydroxyapatite ultrafines and downstream flotation
(dissolved-air) by sodium oleate: effect of used initial hydroxyapatite concentration; Fig. 4. Metals removal from aqueous solution by (two cycles) biosorption-flotation
aluminum sulphate as flocculant was also applied. Reprinted with permission from operation: loaded biomass recovery vs. pH, with collector dodecylamine added only in
Taylor and Francis [50]. the first cycle. Reprinted with permission from Elsevier [58].
 E.A. Deliyanni et al. / Journal of Molecular Liquids 225 (2017) 260–264 263

as the various biosorbents, i.e. biomass, are produced in thousands of Table 1

tons as a solid waste (or by-product) from industrial fermentations. Cleaning with the hybrid unit an industrial effluent (Assarel mine), by sorptive flotation
using zeolite particles as adsorbents, sodium oleate as the necessary collector and an ap-
propriate flocculant to enhance the solid/liquid separation process. Reprinted with per-
4. Hybrid flotation mission from Elsevier [62].

pH Zeolite R% flotation Cu(II)rem. Fe(III)rem. Mn(II)rem.

Copper recovery was finally investigated thoroughly by various flo-
(g/L) (mg/L) (mg/L) (mg/L)
tation techniques, see for instance [59], as funded by an EU research
Natural (~6) 4 80.56 1.54 0.28 21.54
programme focusing to an industrial wastewater (from the Assarel-
Natural (~6.4) 8 81.56 0.38 0.14 4.64
Medet open pit copper mine, near Panagyurishte, Bulgaria). Fig. 5 6.5 4 81.6 0.85 0.14 9.94
given as an example from this area, shows copper ion flotation, where 6.5 8 80.76 0.25 0.14 3.25
almost complete copper removal was obvious for all cases. O-alkyl
dithiocarbonates, called usually xanthates in minerals engineering,
and other thio reagents are known flotation collectors for mineral sul- stream fed into the cell by flotation, allowing thus to achieve the double
phides; the xanthates exhibit a high level of chemical reactivity for goal of producing a clean effluent while at the same time recovering the
heavy metals. The reaction of certain dissolved metal ions, such as contents of the feed stream. Assuming that flotation achieves a solids re-
Cu2+, with xanthate anions gives an unstable complex that decomposes covery of about 90% (typical value), this can be advantageous to a MF/UF
to produce dixanthogen and cuprous xanthate [60]. filtration unit (even a separate one). It has been demonstrated that it
The feasibility of the hybrid cell was proven; stable fluxes of up to was possible to reduce substantially the fouling process by combining
80 L/m2 h1 were achieved with the ceramic flat-sheet multichannel membrane microfiltration with flotation.
membranes applied at low transmembrane pressure (b100 mbar)
[61]. Cake resistance was generally of the same magnitude as mem-
5. Conclusions
brane resistance and thus, quite low that could be attributed to a highly
permeable zeolites cake layer formed. No energy, additional to that
Concluding, it is believed that the various flotation techniques (de-
needed for flotation, was necessary for fouling control of the mem-
scribed briefly above) may deserve wider attention, because they com-
branes, leading to low operation costs of the process. Backflushing (gen-
bine both the need for effluent treatment and the recovery of metals
tle) contribution had no important influence and rather improved the
and raw materials, many of them being anymore exceedingly scarce
operation. Table 1 gives another indication of results (being a part of an-
and costly. Moreover, flotation techniques could be beneficial in sus-
other examined flowsheet) for the same industrial effluent following
tainable development during conventional water and wastewater treat-
sorptive flotation by zeolites [62]. The residual copper in solution was
ment, especially when no other or harmful chemical reagents are added
always inside the accepted standards, while the copper content in the
to help the pollutant separation. By-product recovery is a potentially
froth obtained through the flotation approached 6.0 weight-%, being re-
profitable aspect of treatment. Hybrid units are perhaps the future in
coverable. Noting that experimental series simulating in the laboratory
plant design. The one explored, having downstream applied membrane
a real flotation process, consisting a rougher, a scavenger and a cleaner,
filtration technology following flotation (even compact) for solid-liquid
is usual in mineral processing; for instance, see [63,64]. Detailed eco-
separation purposes, was shown promising, achieving energy savings
nomic considerations of our hybrid unit were published [59,62,65].
too.
In the later paper, it was also reported that various hybrid systems
include membrane separation processes which were presented in the
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