You are on page 1of 29

Froth Flotation

Froth Flotation
1
Introduction

Froth flotation is a surface-chemistry based process of separation of fine solids that takes

advantage of the differences in wettability at solid particle-surfaces. Solid surfaces are

often naturally wettable by water and termed hydrophilic. A surface that is non-wettable

is water repelling and termed hydrophobic. If a surface is hydrophobic, it is also

typically air attracting, termed aerophilic, and is strongly attracted to an air interface,

which readily displaces water at the solid’s surface. In froth flotation, separation of a

binary solids mixture may be accomplished by the selective attachment of hydrophobic

solid particles to gas bubbles (typically air). The other hydrophilic solid particles remain

in the liquid (typically water). The difference in the density between the air bubbles and

water provides buoyancy that preferentially lifts the hydrophobic solid particles to the

surface where they remain entrained in a froth which can be drained off or mechanically

skimmed away, thus, effecting the separation.

Froth flotation is often used to separate solids of similar densities and sizes, which

prevent other types of separations based upon gravity that might otherwise be employed.

It is especially useful for particle sizes below 100ìm (150 mesh), which are typically too

small for gravity separation using jigging and tabling. The lower-size limit for flotation

separation is approximately 35 ìm (400 mesh); however, particles as small as 1 ìm have

been separated. At these small particle sizes, it may be difficult to take advantage of

surface-property differences to induce selective hydrophobicity. On the other hand,

particles greater than 200 ìm (65 mesh) tend to be readily sheared from the bubble

surfaces by collision with other particles or vessel walls. However, relatively low-density

Froth Flotation
2
materials, such as coal, may be successfully separated up to 1600 ìm (10 mesh) in some

systems.

Froth flotation has been used in the minerals processing industry since the mid-1800’s

with many of its broad-based applications to mineral recovery extensively developed

between 1900 and 1925. Today, at least 100 different minerals, including almost all of

the world’s copper, lead, zinc, nickel, silver, molybdenum, manganese, chromium,

cobalt, tungsten, and titanium, are processed using froth flotation. In 1997, the estimated

worldwide mineral production, using froth flotation, was two billion tons. Another major

usage of froth flotation is by the coal industry for desulferization and the recovery of fine

coal, once discarded as waste. Since the 1950's, flotation has also been applied in many

non-mineral industries including sewage treatment; water purification; paper de-inking;

and chemical, plastics, and food processing. The development of froth flotation

continues today with the need to recover minerals from increasingly poorer grades of ore,

as well as its non-traditional application to other types of materials.

There are several different types of froth flotation systems in use today including the

mechanical type, of which there are many subtypes, and the flotation column. The type

of froth-flotation apparatus to be used in this experimentation is the batch, sub-aerated

mechanical type shown in Figure 1. While this is a laboratory scale unit capable of

handling up to 5 L (5 x 10-6 m3), the same equipment type and principals are used at the

industrial level up to 7,000 ft3 (200 m3). A photograph of a 1000 ft3 unit is shown on the

title page (source: Mining Engineering, 31, 1979, p. 785).

Froth Flotation
3
Rotating Shaft
Air

Froth
Layer

Frothing
Tank Froth Effluent

Hydrophobic Particle
Hydrophilic Particle
Agitator Air Bubble

Figure 1. Sub-Aerated Mechanical Froth Flotation Apparatus.

The froth-flotation apparatus to be used consists of a frothing tank containing the solution

and solid-particle mixture. A shrouded impeller or agitator provides continuous

recirculatory mixing of the solids and solution. Air is introduced through the shaft and

exits into the solution at the bottom of the agitator (sub-aerated). The introduction of air

creates bubbles that are stabilized by an added frothing agent. The hydrophobic particles,

activated by an added collector agent, adhere to the air bubbles (frothers and collectors

will be discussed in subsequent sections). Due to the density differences, the air bubbles

rise to the surface of the solution where they collect as a froth layer (the concentrate

stream) which spills over into a froth-collection tray. The froth may also be mechanically

skimmed off. The hydrophilic particles remain in solution, which is eventually decanted

off as waste (the tailing stream). Typically, the concentrating stream contains the desired,

or more valuable, component and the tailing stream, the gangue.

Froth Flotation
4
Objectives

The purpose of this experiment is to investigate the various aspects of the froth-flotation

separation of materials using a batch, laboratory-scale mechanical flotation apparatus

commonly used in industry for separation research and development. Experimental

parameters will be varied to determine their effect on the froth-flotation separation

including the types and concentrations of collectors, frothers, and modifiers (depressants,

activators, and pH regulators). The conditioning times; solids loading and weight

fractions; agitator speed; aeration rate; particle densities, sizes, and shapes; and the

temperature may be varied. Data analyses will include determination of the grade and

recoveries of the more desired material with respect to the effect of the experimental

parameters, as well as determination of the kinetics of the separation process. Qualitative

observations should also be documented to serve as bases for additional conclusions

concerning possible behavior of the system with respect to the quantitative results. Based

upon the experimental results, the different separation outcomes should be compared and

contrasted and optimal parameter ranges should be postulated for the separations. Scale-

up considerations of these laboratory results to larger flotation systems and their use with

multi-stage separations may also be investigated. As an experimenter, you are to decide

what to investigate and are responsible to develop the appropriate experimental

methodology to achieve viable separations, data, and analyses. It will be easy to identify

numerous hydrophilic feeds. An excellent selection for a hydrophobic solid is fine

activated carbon. Characterize your feed by composition and by particle size of each

component. Use sieves to characterize particle sizes.

Froth Flotation
5
Background

Wettability

Froth flotation involves three phases – solid, liquid, and gas – and the corresponding

potential phase interfaces – solid-liquid, solid-gas, liquid-gas, and solid-liquid-gas. The

hydrophobic (aerophilic) or hydrophilic nature of the solids at the solid-liquid-gas

interfacial region is determined by the wettability of the solid. A parameter that

characterizes wettability is the contact angle at the three-phase interface (Figure 2). The

contact angle, è, is related to the respective interfacial surface tensions, ãSG, ãSL, and ãLG,

by Young’s equilibrium equation,

ãSG = ãSL + ãLG cos è . (Eq. 1)

Air

ãLG ãLG ãLG


Water Drop
è ãSG è P ãSG
è P ãSG P
ãSL ãSL Solid ãSL

Hydophylic Regime Intermediate Regime Hydophobic Regime


0o < è < 90o è = 90o 90o < è < 180o

Figure 2. Relative Equilibrium States for a Water Droplet at a


Solid Surface Indicating Various Wettability Regimes.

In Figure 2, point P is the solid-liquid-gas interfacial region. If the liquid-water drop

spreads over the solid, the solid is hydrophilic – characterized by a contact angle of 0o < è

< 90o between the water drop and the solid surface at P. At these angles, air bubbles do

not readily adhere to hydrophilic solids in water. Conversely, when the solids are not

Froth Flotation
6
readily wetted by water, the solids adhere to the air bubbles and the characteristic contact

angle is 90o < è < 180o, and these solids are said to be hydrophobic (or aerophylic). An

intermediate regime, è = 90o, may exist where the solid does not exhibit either strong

hydrophilic or hydrophobic character.

The hydrophilic or hydrophobic character of the solid expressed by the contact angle is

an idealized representation in its application to froth flotation. In practice, it is not

necessary to actually obtain a hydrophobic solid as defined by a è > 90o. Contact angles

in flotation systems typically do not exceed 100o. What is more important is that the

system is operated in such a manner that one of the solid components has a greater –

preferably a substantially greater – hydrophobicity than the other solids from which it is

to be separated. It has been found that a è of at least 20o is necessary for bubble

attachment and successful flotation, and è’s > 20o are desirable for effective separation.

Many materials, such as minerals, are nonpolar and are more naturally hydrophilic than

hydrophobic in water. However, there are also many exceptions such as coal with a

natural è = 45-60o and talc with a natural è = 88o (see the bottom of Table 1 in next

section).

Thus, in order to obtain a successful separation using froth flotation, it is usually

necessary to selectively enhance the hydrophobicity of one of the solid components that

is otherwise hydrophilic or not strongly hydrophobic. This selective modification of the

wettability of solids in froth flotation is obtained using additional reagents termed

collectors.

Froth Flotation
7
Collectors

To invoke selective hydrophobicity, substances know as collectors are used. Collectors

are typically heteropolar organic substances – they contain both nonpolar and polar

chemical groups. The nonpolar end is almost always a long-chain or cyclic hydrocarbon

group that is hydrophobic. The collector must be able to attach to the solid, and it does so

through its polar end, which is typically an ionic group termed the solidophil group.

When the solidophil group of a suitable collector contacts a mineral at a surface site that

can chemically interact with the solidophil group, the collector bonds to the surface of the

mineral via chemisorption or ionic bonding. The nonpolar end of the collector then

orients outward from the solid surface forming a nonpolar chemical envelope

surrounding the solid particle, inducing hydrophobic behavior on an otherwise

hydrophilic solid surface. The solid particle can then more readily attach to an air bubble

(Figure 3) via the hydrophobic end of the collector.

Figure 3. Collector Alignment at the Solids Surface.

Consequently, a key to successful froth flotation is to selectively induce, using a suitable

collector, hydrophobicity on the desired material to be recovered while retaining

Froth Flotation
8
hydrophilicity of the nondesirable material. It should also be noted that the strength of

the induced hydrophobicity of the mineral via the collector is directly relatable to the

length of the hydrocarbon group while the strength and selectivity of the collector’s ionic

bonding is controlled by the type of solidophil group.

There are many different types of collectors, and they are classified as to the type of ion

(anionic or cationic) that is formed upon their dissociation in aqueous solutions. For

example, sodium oleate, C17H33COONa, is a widely used collector for minerals

separation. It is comprised of a long-chain, nonpolar hydrocarbon group, R = [C17H33],

which is hydrophobic and a polar carboxyl group, [COONa], which is the solidophil

group. Upon dissociation in water, the solidophil group is anionic or

R C

This anionic carboxyl group will bond with minerals that contain alkali-earth metal

cations such as Ca, Ba, and Mg, as well as carbonate, oxide, and sulfate minerals.

Other widely employed anionic collectors include the xanthates, containing bivalent

sulfur, that are highly selective collectors in the separation of sulfide minerals. The

xanthate anion is

R O C

S
Froth Flotation
9
Other types of collectors are used in froth flotation including dithiophosphates and alkyl

sulfuric salts that are also anionic collectors. The later include sodium dodecyl sulfate and

sodium lauryl sulfate, used in detergents. The later have the sulfo-solidophil group

O O

R O O

Cationic collectors are less widely used. The most common types contain amine groups,

such as aniline and pyridine, but cation attachment to most minerals is typically weak.

They are also typically water insoluble and require the presence of acids to induce

solubility. However, cation collectors are used for silicates and other oxides, including

some rare earth oxides.

As previously discussed, the effect of collectors on the hydrophobicity of solids can be

related to the contact angle, è. Examples of contact angles modified by various collectors

for various minerals are indicated in Table 1, as well as those for naturally hydrophobic

materials for comparison.

Froth Flotation
10
Table 1. Contact Angles for Various Solids and Collectors
(adapted from Encyclopedia of Chemical Technology 4th Edition, Vol. 11 (1997) p. 88.

Solid Collector and Conditions Ł (degs)


-3
colemanite 5 x 10 M sodium oleate 43
copper metal 1.5 x 10-4 M sodium oleate 93
fluorite 1 x 10-5 M sodium oleate, pH = 8.1 91
galena 1 x 10-3 M potassium ethyl xanthate 60
ilmenite 1.3 x 10–3 M sodium oleate solution, T = 75oC, pH = 8 80
silica 1.1 x 10-5 M dodecylammonium chloride, pH = 10 81
graphite water 86-96
coal water 20-60
stibnite water 84
sulfur water 85
molybdenite water 75
talc water 88
iodyrite water 20

Frothers

In addition to collectors, another important component in successful flotation is the

presence of frothers. Once its surface is rendered hydrophobic, a solid particle must be

able to attach to an air bubble. While it may be possible to initially obtain solid particle

attachment to air bubbles in an agitated liquid under aeration alone, these air bubbles are

unstable and quickly break down due to collisions with other bubbles, solid particles, and

the vessel walls. In addition, the bubble size may not be sufficient to effectively carry a

solid particle to the surface of the liquid. Consequently, additional materials, termed

frothers, are added to promote the formation of stable air bubbles under aeration.

Frothers, like collectors, are typically comprised of both a polar and nonpolar end. The

nonpolar hydrophobic ends orient themselves into the air phase. Bubble wall strength is

enhanced by simultaneous strong polar-group and water-dipole reaction (hydration) at the

air-liquid interface resulting in greater bubble stability due to a localized increase in

surface tension.

Froth Flotation
11
Frothers are generally classified by their polar groups with the most common being the

hydroxyl (–OH), carboxyl (–COOH), carbonyl (=C=O), amino (–NH3), and sulfo (–

OSO2OH and–SO2OH) groups. Table 2 lists some common frothers according to their

chemical grouping. Effective frothers typically contain at least five or six carbon atoms

in their straight-chain, nonpolar group to obtain sufficient and stable interaction with the

air phase. For branched-chain hydrocarbons, the number of carbon atoms in the nonpolar

group may range up to sixteen. However, a frother must be at least slightly soluble in the

liquid medium and increasing the straight-chain-hydrocarbon length (perhaps up to a

maximum of eight, e.g., octyl alcohol) will eventually lead to too low of a solubility for

effective frothing. Thus, a suitable frother must provide a balance between sufficient

nonpolar interaction with air and solubility in water. With respect to the polar groups,

one or two are usually sufficient to interact at the liquid-air interface to provide sufficient

frothing properties, and additional polar groups provide little benefit.

Most of the frothers in Table 2 are hydroxyl-group-type frothers, and, thus, have little

collector properties. However, because of the inherent heteropolarity of collectors, a

collector can also serve as a frother in some systems. This is true of the carboxyl-type

frother, sodium oleate, and the sulfo-solidophil fatty acids. Certain collector/frother

combinations may also exhibit a synergistic separation effect. However, one designs a

flotation system based upon a collector specific to the modification of the surface

properties of the solids required for separation. The type of frothing agent is a secondary

consideration that is chosen after the collector to provide suitable frothing conditions and

noninterference with the collector or separation system.

Froth Flotation
12
Table 2. Examples of Frothers.

Frother Formula
Aliphatic Alcohols CH3(CH2)nCH2OH, n = 3–5
MIBC (4-methyl-2-pentanol) CH3CH(CH3)CH2CH(OH)CH3
di-acetone alcohol (CH3)2(OH)CH2COCH3
2-ethyl 3-hexanol CH3(CH2)3CH(C2H5)CH2OH
Cyclic Alcohols
pine oil (terpineol) C10H17OH
eucalyptus oil (cineole) C10H16O
Phenols
cresol CH3C6H4OH
xylenol (e.g., xylitol) HOCH(CHOH)3CH2OH
Alkoxyparaffins
1,1,3-triethoxybutane CH3CH2CH(OC2H5)CH(OC2H5)2
Polyglycols
poly(propylene glycol) monalkyl ethers R(OC3H6)nOH, n = 2–5, R = CH3, C4H9
poly(ethylene glycol)s R(OC2H4)nOC2H4OH, n = 2-5
Other
sulfo-cetyl alcohol CH3(CH2)14CH2OSO2OH

Modifiers

Additional modifiers such as activators, depressants, dispersants, and pH regulators are

also commonly used in froth flotation. Activators may be added to chemically

“resurface” the solid to increase the interaction with collectors that are otherwise

ineffective alone. Depressants form a polar chemical envelope around the solid particle

that enhances hydrophilicity or selectively prevents interaction with collectors that may

induce unwanted hydrophobicity. Dispersants act to break agglomerated particles apart

so that single particles interact with the collectors and air bubbles. Regulators are

commonly used to control the pH since the hydrophobicity of systems is often optimal

within a certain pH range. Frothers also often need a certain pH range in order to form

stable bubbles. The presence of reducing agents may also serve to prevent the presence

of soluble ions due to oxidation that may undesirably activate certain minerals.

Froth Flotation
13
Separation Kinetics

It should be emphasized that the overall dynamics and kinetics of froth flotation

separation involves the surface phenomena of the collector’s chemical envelope

surrounding the solid particles and its hydrophobic nature. While one must still consider

the particle size and mass of the material since these affect the ability of the bubbles to

successfully transport the solid particle, the type of material that lies beneath the

hydrophobic envelope, once it is established, has little affect on the separation.

Consequently, if enough conditioning time has been provided for collector action to

selectively render the desired solid particles hydrophobic, the remaining overall

separation is essentially dependent only upon the efficiency of the bubble and solid-

particle interactions (assuming the particle size and density are within a suitable range).

The overall flotation efficiency, EF, of the separation system may be defined by

EF = EC • EA • ES (Eq. 2)

where EC is the collision efficiency, EA is the attachment efficiency, and ES is the stability

efficiency of the bubble-solid interaction. It is convenient to express the overall

separation or flotation rate, rs, by

 dC 
rs = −   = k C n (Eq. 3)
 dt 

where C is the concentration of the desired component (the hydrophobic component) in

the frothing tank; t is time; n is the order of the process, n = 0, 1, 2,…; and k is the

flotation rate constant. This approach to flotation rate modeling is analogous to that used

in chemical-reaction kinetics. It must be re-stressed that this rate expression is for the

overall separation process and not the reaction of the collector at the solids surface.

Froth Flotation
14
In kinetic modeling, one often assumes a reaction order and subsequently determines the

accuracy of that assumption based upon the experimental data. However, in practice for

all but the simplest processes, there are often undeterminable or unknown system

relationships. Kinetic modeling assuming a first-order process permits one to at least

compare systems. This is often termed a pseudo-first-order assumption, and Eq. 3 with n

= 1 has been found to adequately model most flotation systems comprised of a single

solid-particle size and hydrophobic strength.

Solution of this equation assuming pseudo-first-order kinetics, n = 1, yields the integrated

rate expression

Ct − Co = e − kt (Eq. 4)
or
C 
ln  t  = − k t (Eq. 5)
 Co 

where Ct is the concentration of the desired component (the hydrophobic component) in

the frothing tank at time t and Co is the concentration of the desired component at t = 0,

the beginning of the separation. Note that the ratio Ct/Co is the fraction of the desired

component remaining in the tank at time t.

Based upon bubble-particle capture modeling, the flotation rate constant may be

expressed by

3 G EF h
k= (Eq. 6)
2 db V

Froth Flotation
15
where G is the gas flow rate; db is the average bubble diameter; and V and h are the

volume and depth, respectively, of the particle suspension. If k is known, then the

flotation efficiency, EF, can be estimated from Eq. 6 for a given system with known db.

The flotation rate constant, k, can be determined from a plot of ln [Ct/Co] vs. t (see Eq. 5)

from experimental data. If this plot is linear, then the assumption of overall first-order

separation kinetics is valid. However, in actual systems this plot often exhibits

nonlinearity that is usually attributable to a distribution of particle sizes and varying

hydrophobic strengths of the solids. The result is a distribution of flotation rate constant

values. The recovery rate is then represented by a sum of a series of exponential terms,

and the plot of ln [Ct/Co] vs. t will exhibit curvature.

Froth Flotation
16
Experimental Equipment

The principal experimental apparatus used for this lab is the D-12 Lab Flotation Machine

manufactured by the Denver Equipment Company. A general schematic of the apparatus

appears in Figure 4. Further details about this unit are provided in the manufacturer’s

equipment manual available in the lab. The apparatus provides recirculation and

agitation to maintain thorough mixing and solid/liquid suspension. Other types of

agitators/mixer heads are supplied with the equipment; however, all experimentation

should be done with the installed agitator unless directed otherwise by the instructor.

Speed-Adjustment
Knob RPM Indicator

Speed Adjustment Belt Housing


Lock Ring

Motor

Aeration Valve

Agitator Shaft
Housing
Power Switch

Height-Adjustment
Handle
Height-Adjustment
Stop Knob Agitator Assembly

Support Column Frothing Tank


Effluent Lip

Base
Frothing Tank

Figure 4. Details of the Denver D-12 Lab Flotation Machine


(photo by John Murphy).

Froth Flotation
17
The vertical position of the agitator is adjusted by pulling out the stop knob on the left-

hand side of the unit and turning the lever on the right-hand side (Caution – the agitator

assembly is heavy). The rotation speed (rpm’s) of the agitator is varied by turning the

knob at the top of the motor at the back of the unit (Caution – only change the motor

speed with the motor running). An rpm tachometer is located at the top of the unit. To

change the agitator rpm’s, back off the lock ring (the knurled ring) and turn the top knob

clockwise to decrease the speed and counterclockwise to increase the speed. Retighten

the lock ring. Air, via a petcock valve located near the top of the agitator shaft, is

introduced through the shaft into the aqueous solution to promote frothing. This aeration

is controlled and metered using a rotameter and needle valve.

Flotation tanks are available in various sizes ranging from 1.5 to 5 L. The flotation tanks

are designed with an effluent lip to allow the froth to exit for collection in the froth-

collection trays. Both stainless-steel and acrylic tanks are available. The acrylic tank

may be used to qualitatively view the particle, bubble, and fluid behavior under agitation.

The 1.5 L stainless steel tanks (2 are available) should be used for all other

experimentation unless directed otherwise by the instructor.

A temperature-controlled, heated water bath is available for operation at elevated

temperature using the 1.5 L tanks. Only distilled water (available in the lab) should be

used in the heating bath. The temperature set point is chosen via a dial located at the top

of the immersion heater. A temperature meter and thermocouple are used to monitor the

heating bath and flotation tank.

Froth Flotation
18
A pH meter is available to measure the pH of the various flotation solutions before and

after the addition of various collectors, frothers, inhibitors, promoters, and pH regulators.

Calibration solutions are available (see the instructor).

Other equipment required for the experiment includes appropriately sized sieves,

distilled- water wash bottles, weight balance, weighing pans or paper, graduated cylinder

of volumetric flask, hot plate, beakers, stirring rod, and filter paper (coffee filters work

well).

Froth Flotation
19
General Methodology

The following procedures outline the general methodology for running most froth

flotation experiments with the equipment in the lab (see next section for specific

separations).

1.) For ambient temperature operation, choose the desired frothing-tank size and
place it under the agitator. A cutout under the frothing tank will center it. Lower
the agitator to the desired height (typically ½ to ¾”. from the frothin g-tank
floor). Caution – firmly grasp the adjusting handle before disengaging the stop
knob and ensure that the stop knob is fully engaged when finished.

2.) If using the heating bath for elevated temperature operation, only the 1.5 L
stainless-steel tanks can be used. Insert the frothing tank into the empty heating
bath, centering it on the standoff on the floor of the heating bath. The frothing-
tank effluent lip should nestle over the cutout along the top of the heating bath.
Place the 1 in. high tray support under the heating bath and position the heating
bath against the back of the flotation unit’s main-support column. Lower the
agitator to the desired height (typically ½ to ¾”. from the frothing -tank floor).
Adjust to center the agitator in the frothing tank. The frothing tank will first
need to be filled with water to enable it to settle in the heating bath. Thus, do the
following in conjunction with Step 3 – fill the heating bath with distilled water to
within 1 to 2” from the top of the heating bath. Place the froth diverter (a bent
aluminum panel) over the lip of the frothing tank with the bent, side supports
facing down.

3.) Measure out a suitable amount of distilled water and fill the frothing tank with
the agitator in place. For a 1.5 L tank, this amount is ~1.3 L of distilled water
yielding a liquid height approximately ½”below the effluent lip of the frothing
tank.

4.) Place a froth-collection tray (3 or 4 plastic ones are available) under the effluent
lip of the frothing tank. Position several other froth-collection trays nearby so
that they can be readily replaced during a run.

5.) Turn on the agitator and set the desired agitator speed using the set knob and
rpm-indicator dial. Caution – change the agitator speed only with the motor
running and always retighten the lock ring when finished with the adjustment.

6.) Open the aeration petcock valve at the top of the agitator shaft and the ball valve
on the rotameter-inlet line, and set the airflow to the desired setpoint using the
needle valve on the rotameter inlet line. Calibrate and record the airflow.

Froth Flotation
20
7.) Adjust the liquid height in the frothing tank if excessive spillage occurs at a
given speed and airflow. Record the new volume.

8.) Turn off the aeration at the ball valve on the rotameter-inlet line. Leave the
aeration petcock valve open.

9.) Pre-sieve the desirable-component and gangue solids to obtain particle sizes that
enable subsequent separation by sieving and quantitative weight analyses after
flotation. Record all sizes.

10.) Weigh out the desirable-component and gangue solids to obtain the desired
weight fraction. If a pre-mixed solids sample is used, determine the weight
fraction. Record all weights.

11.) Weigh out the desired amounts of collector, frother, depressant, promoter, etc. If
liquid, measure out using a graduated cylinder or volumetric flask. Record all
values.

12.) Record the temperature of the frothing tank using the thermocouple. If using the
heating bath, set the heating bath to the desired temperature using the immersion
heater set-point dial (calibrated in oF). Maximum operating temperature should
not exceed 75oC. Monitor the heated-bath and frothing-tank temperatures until
the desired temperature is obtained.

13.) Calibrate the pH meter using suitable calibration solutions (see the instructor).
Record the pH in the frothing tank.

14.) Pour the solids mixture to be separated into the frothing tank and allow mixing.

15.) With the aeration still off, separately add any promoters, inhibitors, pH
modifiers, collectors, and frothers and record the time, temperature, and pH after
each addition. A conditioning time (~typically 1 to 2 min. although it may be an
im) should follow each addition, and the sequence of the additions and their
conditioning times recorded. Note any qualitative observations of the frothing
tank solution such as dispersion or coalescence of solids, bubble formation, etc.

16.) To begin froth-flotation separation, turn on the ball valve at the rotameter-inlet
line and record the time. Froth should build and begin to elute over the effluent
lip of the frothing tank and into the froth-collection tray. A plastic spatula may
be used to sweep the froth off the top of the frothing tank and into the froth-
collection tray, especially if it tends to froth over the sides of the frothing tank.
Depending upon the amount of froth, the froth-collection tray may need to be
switched over time. Record the times for froth-collection-tray switches to obtain
time-based, separation information. Note any qualitative observations during the
separation with time including froth amounts, discernable presence of solids in
the froth, bubble-size distribution, bubble stability, etc.

Froth Flotation
21
17.) When frothing ceases, shut off the aeration at the ball valve on the rotameter-
inlet line and record the time. Record any final qualitative observations.

18.) Separately wash out each froth-collection tray with distilled water into filter
paper (coffee filters work well) placed in a suitably fine sieve to prevent any
solids loss.

19.) Raise the agitator and rinse any remaining froth and solids back into the frothing
tank using distilled water. Remove the frothing tank.

20.) Separately wash out the frothing tank with distilled water into filter paper (coffee
filters work well) placed in a suitably fine sieve to prevent any solids loss.

21.) Remove the filter paper from the sieve, seal with tape, and label accordingly.

22.) Dry the samples in the filter paper in a drying oven at 75–100 oC. Record the
drying time and temperature.

23.) When dry, re-sieve each sample based upon the initial sieve-size distribution to
obtain separation of the solids. Alternatively, if one of the solids is magnetic,
use a magnetic plunger or magnetic separator to separate.

24.) Weigh each separated sample and calculate recovery and grade (purity) obtained
in the separation. Note any total sample loss.

25.) Empty the water bath at the end of the experimental period, and return all
samples, reagents, and equipment to their proper place.

Froth Flotation
22
Suggested Separations

Your group or your instructor can identify a synthetic mixture to study.

Fluid Phase
Water (do not use other liquids)

Frothing Agents
Dowfroth
MIBC
Others that you identify (have the technician or instructor order them if necessary)

Hydrophilic Particles
Each group has the responsibility of selecting a hydrophilic particle. Use the sieves to
characterize the size of the particles (dry).

Hydrophobic Particles
An excellent hydrophobic particle is extremely fine activated carbon. Use the mortar and
pestal to crush the activated carbon, and use the sieves to characterize the size of the
particles (dry).

Froth Flotation
23
Suggested Separation Experiments for Copper and Ilmenite

Sodium oleate, C17H33COONa, which is soluble in water serves as both a collector and

frother in a number of metal and mineral separations. It can be used in the separation of

copper metal from gangue, such as sand, and ilmenite from zircon in water. Table 3 lists

the various sample and reagent materials available in the lab (Caution – note the

warnings at the bottom of this table). Sodium oleic acid is used as the reagent to prepare

the sodium oleate solution. Please note that this reagent is relatively expensive.

Maximum molar concentrations up to 3 x 10-4 M (which is ~0.1g of oleic acid for the 1.5

L tank) should be used for each run, but less if possible (1.5 x 10-4 M usually works

well). Copper metal is available in two presized samples (–150 mesh and –40,+60 mesh).

Presized sand is available (–50,+70 mesh), as well as common beach sand which may be

sieved. Ilmenite and zircon are available both as a mixture (~22% by weight ilmenite)

and as separate samples, all unsized. Other reagents listed in Table 3 are potential

frothers, pH regulators, and depressants that may be used.

A total solids loading of 50 g of material is suggested for the 1.5 L cell using sodium

oleate concentrations up to 3 x 10-4 M. Typical weight fractions of 10–40 % for the

desirable component are also suggested to minimize sample usage.

Froth Flotation
24
Table 3. Materials for Froth Flotation of Cu/Sand and Ilmenite/Zircon

Material Aldrich # or Other CAS #


Sodium Oleic Acid** 23,397-8 143-19-1
Copper (-150 mesh)*** 26,607-8 7440-50-8
Copper (-40, +60 mesh)*** 26,608-6 7440-59-9
Sand (-50, +70 mesh)*** 27,473-9 -
Beach Sand (common, unsized) - -
Ilmenite (FeTiO3) DuPont -
Zircon (ZrO2•SiO2) DuPont -
Ilmenite(~22%) – Zircon mixture InProsys (DuPont) -
Starblast – staurolite (FeO•Al2O3•SiO2•H2O) DuPont -
Sodium hydroxide** VWR # VW6720-1 1310-73-2
Calcium Oxide - -
Hydrochloric acid*, ** - -
Sodium metasilicate*** 30,781-5 6834-92-0
Sodium dodecyl sulfate** 86,201-0 151-21-3
Poly (propylene glycol) monobutyl ether 43,810-3 9003-13-8
Propylene glycol amyl ester (DowFroth-250TM) Dow -
*Please see the instructor before handling this reagent.
**Gloves should be worn when handling any of these reagents or their solutions.
***Avoid breathing any of the fine powders especially copper.

The following are suggested froth-flotation experiments using sodium oleate solution

(maximum of 3 x 10-4 M) for copper and ilmenite separation from sand and zircon,

respectively.

• Investigate the effect of pH and pH regulator concentration and determine the

optimum pH range for separation – alkaline pH regulators such as caustic soda

(NaOH), lime (CaO), or soda ash (Na2CO3) may be used. Note that it will be

necessary to first dissolve these reagents in water on a hot plate at ~75 oC before

addition to the frothing tank. Operation in the acidic range may also be investigated

using hydrochloric (HCL) or sulfuric (H2SO4) acids. These pH modifiers may also

serve as dispersants, depressants, and activators in some systems.

Froth Flotation
25
• Investigate the effect of depressants that may inhibit any hydrophobicity of the

gangue material – sodium metasilicate, Na2SiO3, is a potential depressant of

siliceous materials such as sand and zircon. It is also a pH regulator.

• Investigate the effect of particle size on the separation – both the desired component

and the gangue material size may be varied.

• Investigate the effect of agitator speed (rpm’s) on the separation.

• Investigate the effect of aeration on the separation – perhaps allowing separation

using lower sodium oleate concentrations.

• Investigate the effect of conditioning time for various modifiers on the separation.

• Investigate the effect of temperature on the separation – temperature ranges from

room temperature to 75oC may be performed.

• Investigate the viability of using alternative or additional frothers allowing

separation using lower sodium oleate concentrations – high-molecular-weight

alcohols, such as poly (propylene glycol) monoalkyl ethers [R(OC3H6)nOH, where n

= 2-5 and R = CH3, C4H9] such as poly (propylene glycol) monobutyl ether and

propylene glycol amyl ester (Dowfroth-250TM) act as frothers.

• Investigate the rate of separation by determining concentration versus time over

short time intervals – the kinetic effects of particle size; aeration; solids loading;

collector, frother, and modifier types and concentrations; and temperature may be

thoroughly investigated (see Additional Analyses section).

Froth Flotation
26
Data Analysis

The following are outlines of the types of analyses that may be performed. The

application of these analyses will be determined from the types of experiments chosen.

• Calculate the % grade, G, or purity of the concentrate stream (the hydrophobic

 m 
stream) from G =  des  ⋅ 100 where mdes is the weight of the desired component
 mconc 

(usually the more valuable mineral) in the concentrate stream and mtot is the total

weight of the concentrate stream. The % increase in % grade between the original

weight fraction of the desired component and the weight fraction in the concentrate

may also be reported.

• Calculate the % recovery, R, of the desired component in the concentrate stream

m 
(the hydrophobic stream) from R =  des  ⋅100 where mdes is the weight of the
 mfeed 

desired component in the concentrate stream and mfeed was the weight of the desired

component in the feed stream before separation. Percent loss of the desired

component via the tailings stream (the hydrophilic stream) may also be reported.

• Create plots of grade and recovery vs. agitator speed, pH, temperature, and

concentrations of frother, collector, pH regulator, depressant, activator, etc. that

were determined in the experiments. Similarly, create grade vs. recovery plots for

comparisons.

Froth Flotation
27
• Compare the results of other mineral processes – e.g., tabling, mineral jigging,

cycloning, and centrifuging – often used in lieu of, or in conjunction, with that of

froth flotation, specifically with respect to particle size, efficiencies, grade and

recovery, cost, and other factors.

• Apply scale-up design procedures to froth flotation based upon the experimental

results.

Additional Analyses

The following are additional analyses that require more extensive data collection.

• Determine the rate constant, k, of the separation process for a given set of conditions

by experimentally determining concentration versus time and applying the rate

 dC 
expression, rs = −   = kC n , assuming a pseudo-first-order process (n = 1) where
 dt 

C is the concentration of the desired component (the hydrophobic component) in the

C 
frothing tank and t is time. Create a normalized plot of ln  t  vs. t where Ct is the
 Co 

concentration of the desired component at time, t, and Co is the initial concentration

at time, t = 0, the beginning of the separation. Determine the first-order rate

constant, k. If the process is not first order, investigate other possible rate

expressions.

• Determine the rate constant, k, behavior with temperature, T, of the separation

process given a set of conditions and apply the Arrhenius relationship,

k = Ae − E a / RT , where A is the frequency factor, Ea is the activation energy, and R is

Froth Flotation
28
1
the gas constant. Create a plot of ln k vs. 1 . Determine A and Ea and relate these
T

to the dynamics of the separation.

General References

Kirk-Othmer Encyclopedia of Chemical Technology 4th Ed., Vol. 11 (1997) pp. 81-106.

Kirk-Othmer Encyclopedia of Chemical Technology 4th Ed., Vol. 23 (1997) pp. 478-536.

Perry’s Chemical Engineer’s Handbook, 5th Ed., (1984) pp. 21-46.

McKetta, John J., Encyclopedia of Chemical Processing and Design, Vol. 23 (1985) pp.
454-506.

Last Update: August 2001

Froth Flotation
29