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Vol. 26, No. 1, Feb 2007, p . 89
E-mail: rm@ustb.edu.cn AT ScienceDirect

Influences of solid particles on the formation of

the third phase crud during solvent extraction

ZHENG Qi, RUAN Renman, WEN Jiunkang, SONG Yongsheng, DONG Qinghai, WU Minglin,
and Y40 Guocheng
General Research hrtitute fot Nonferrous Metals, Belling 1ooOX8, China
(Received 2005 11-18)

Abstract: The influences of solid particles in leach solution on the formation of the third phase crud during solvent extrac-
tion of :upper were studied. Analyzed fiom the point of view of pH value and surface tension, the study results showed that
the soli 1particle is one of the most important contributors for the formation of the third phase crud. During solvent extrac-
tion, if he pH value was greater than 2.30, the number of solid particles in the mother solution increased, in which case the
possibility of forming the third phase crud could also increase, and the interface tension value might grow in pace with the
quantit: of the third phase crud.
Key wc,rds: solvent extraction; solid particle; the third phase crud; surface tcnsion

wpptrrred by the “973”National Basic Research of China (No. 2004CB619206).]

[This tr~idji~jinunciull~

tion, and influence the balance of copper ion be-

1. Introduction
During solvent extraction, the solvent extraction
rate depends on the chemical reaction rate and mass
transfer speed on phase interface. To improve the
area of contact interface, both phases must be ade-
quately mixed to form an emulsion, that is, one
phase uniformly disperses into another phase in the
form of micro drops with the diameter usually more
than 0.1 p n . However, this emulsion could be un-
stable, when the mixing ceases. The dispersed phase
(i.e.. micro drop) must be aggregated and both
phases stratified rapidly. If the dispersed phase is not
aggregated and stratified for a long period (for ex-
ample, of the order of several ten minutes). this
phennmcnnn is callcd criiuldication, and its product
is the third phnre crud; in cothar W O I ~ ~klhuillly
, tllc
third phase may be formed between the organic
phase and the aqueous phase. Its generation may not
only impede the interaction between the organic
phase and the aqueous phase during solvent extrac-
tween both the phases, that is, the solvent extraction
rate of copper, but also has adverse effects on the
phase splitting speed and even impede the normal
production progress. Moreover, because of the en-
trainment of the third phase, a loss of the organic ex-
tracting agent may accompany it. And the formation
of large quantity of crud is very unfavorable to nor-
mal production. Thus, how to effectively reduce or
prevent the generation of the third phase becomes an
important study topic during solvent extraction of
copper.
In the solvent extraction circuit, the causes of
forming the third phase crud are complex, such as
the solids in leach solution, composition of solvent
(cxtractmg agent a d diluting agent etc.), and ex-
pci-iiirciit opcraiiun CIC. may present adverxe effects
on chemical and physical behaviors during solvent
extraction and lead to the formation of the third
phase crud. Assuming that the interface reaction of a
solid particle occurs between the aqueous phase and

Correqponding author: 7HFYG Q1 E-mail: qir65@’aind L o r n

90
organic phase to stabilize the emulsion and form the
crud [I], the third phase crud is defined as a solid
stable emulsion resulting from mixing an aqueous
phase containing some fine suspended solids such as
a pregnant leach solution with an organic extractant
phase; in other words, the formation of crud is
caused by the affinity of some solid particles in a
leach solution to some components in the organic
surface behaviors of solid particles may be divided
into hydrophilic, hydrophobic, or both at the same
time.
Factors responsible for the stability of the third
phase crud are surfacerinterface tension, interface
charge, and strength of the interfacial film. Similar to
the surface-active agent, the solid particles are dis-
tributed at the interface of the solution to stabilize
the third phase and mainly increase the strength of
the interfacial film.
The behavior of a solid particle at the interface
depends on its wettability to water and the organic
phase, that is, depends on three interface tensions:
interface tension c&,bd.w&r between solid-water, in-
terface tension c&,Mq,",c phase between solid-organic
phase, interface tension o,,~, phase-water between or-
ganic phase-water. The interface tension of solid
particles at interface may be calculated according to
the formula below:
qohd-orgamc phase - qsohd-water = oxgmc phase-~ate&~s@
where Bis the contact angle, used for measuring the
wettability of solid to water or to the organic phase.
Fig. I shows the distribution of solid particles be-
tween the interface of the organic phase-aqueous
phase.
Although some researchers have given their in-
terpretation on the causes of forming the third phase.
their opinions are quite different. The authors studied
the formation of the h r d phase crud during solvent
extraction of copper from the point of view of inter-
RARE METALS, Vol. 26, No. 1, Feh 2007
facial chemistry (such as surfacehnterface tension),
especially the influences of solid particle. in the
leach solution (solvent extraction mother solution)
on the third phase crud, analyzed the components of
the third phase crud and the influences of surface
tension on the formation of the third phase mid, and
finally found a means to control or reduce the for-
mation of the third phase crud.
e > 900
- __ O = 90" f3< 90"
Fig. 1.. Three forms of the distribution of solid parti-
cles at the interface of organic-aqueousphase.
2. Experimental
2.1. Materials and reagents
Tlie experimental materials were obtained from
the copper leach solution in the leach expansion ex-
periment. Part of the third phase crud was also taken
from the solvent extraction loop in the laboratory.
Reagent: the extracting agent was Lix983N pro-
duced by Cognis Corporation, German; and the di-
luting agent was commercial sulfonated kerosene;
all other reagents such as sulfuric acid, sodium hy-
droxide, copper sulfate, sodium silicate, aluminum
sulfate, ferric sulfate, etc. were technically pure or
chemically pure.
2.2. Methods
The extractant (organic phase) and leach solution
(aqueous phase) were filled into a separating funnel
according to the specified proportion. After being
vibrated and mixed with a vibrator for 3 nun, it was
allowed to rest, to stratify. The extracted residual
solution (aqueous phase) was taken for anal! zing the
concentration of metallic ion.
Eimulsion separation: emulsion samples were
loaded into 50 mL centrifuge tubes and then centri-
fug;ihzed at about 9000 r/min for 1 h at 26 'C.
Zheng Q., et al., Influences of solid particles on the formation of the third phase crud during..
2.3. Analysis and test
The main testing instruments included a F’roces-
sor Tensiometer KlOO full-auto surface tensiometer
produced by Germany KRUSS Company, U.S.
Thermo Orion MODEL868 acidometer, Hitachi
GGX-9 atomic absorption spectral photometer, 722
visible raster spectrophotometer, Philips PW2400
XRPX fluorescence spectrometer, Germany OP-
TON polarization microscope, and JSM-840 scan-
ning electron microscope. The content of metallic
ion was measured using the atomic absorption
method and Gravimetric method. The pH value of
the aqueous phase or acid strength was measured
with the acidometer using the acid-base titration
method, and the surface tensiodinterface tension
was measured with a tensiometer. The shape, granu-
larity, and component were detected using scanning
electron microscopy with an energy spectrometer.
3. Results and discussion
3.1. Analysis on the component of the third phase
crud
The third phase crud is a mixture of organic sol-
vent, aqueous solution, and solid substances formed
during the mixing of solvent extraction, which is a
physical and not a chemical process [6]. When the
third phase forms, its stratification is relatively slow,
with the upper layer black and the lower layer yel-
low, and a large quantity of white floccus between
the upper and lower layers, mixed with emulsion.
Although the crud is a relatively stable multi-
ple-phase system, after deposition for a long period,
some organic phase or aqueous phase may slowly
separate. The third phase crud during solvent extrac-
tion has water-in-oil (wh) type or oil-in-water (o/w)
type. The type of the third phase crud depends on the
causes of crud formation. Both types of crud may be
present during the production of copper extraction.
To determine the type of crud, apart fi-om direct ob-
servation, it may also be observed through the dye-
ing method; that is, after it is dyed with wa-
ter-soluble methylene blue, the third phase crud is
observed with a microscope. Under the microscope,
it may be clearly distinguishable, because the aque-
. 91
ous phase is easier to dye, but the organic phase is
difficult to dye. The wholly-dyed crud is the wa-
ter-in-oil type; on the contrary, only the drop dyed is
the oil-in-water type. Using this method it was found
that the third phafe crud formed by solid particles
exists either in the oil-in-water type or in the wa-
ter-in-oil type.
The component analysis was carried out for the
third phase crud sampled from the laboratory, and
the results are shown in Tables 1 and 2.
Table 1. Component analysis for the third phase crud
%
Organic phase Aqueous phase
-___ Solid -
phase
~ ~~ ~ -
65.7 25.8 8.5
Table 2. Composition of the solid phase in the crud
%
SiO? Fe A1203 Cu ~~~
CaO ~~
MgO-
45.84 30.36 14.78 1.38 0.98 0.60
Tables 1 and 2 show that the main components of
the crud include organic solvent, relatively small
quantity of solid phase, and solid phase mainly con-
sists of SiOz and Fe, secondly of A1203, Cu, CaO,
MgO, etc. Thus it is deemed that the solid particles
in the mother solution are one of the main causes in
the formation of the third phase crud.
The shape and gain size of solid particles sus-
pended in the mother solution were observed using
the scanning electron microscope and the results are
shown in Fig. 2. As seen in Fig. 2, the solid particles
are irregular, with the grain size less than 1 pm.
3.2. Sources of solid particles and influences on
the formation of third phase crud
The surface tension or specific surface energy of
solid particles is very high, hence easier to absorb
the organic solvent which reduces its surface energy
so as to form the stable third phase crud. In the leach
solution, the solid particles usually exist in solid
suspensions and charged colloidal particles (buch as
colloidal silicon settlement). Certainly both have no
clear dividing line, and for the purpose of conven-
ience, the effects of both types of solid particles on
92
Fig. 2. SEM of solid particles in mother solution.
the formation of the third phase crud are elucidated
a5 shown below.
(1) Functions of solid suspensions in the leach
solution.
The undecomposed ores in the leach solution,
some insoluble fine solid particles such as hydrate
from metallic ion hydrolysis, salt based sulfates of
Fe and Cu, aluminum sulfate, calcium sulfate (gyp-
sum), soluble silicon, aluminum, suspensions of
mud, and dust etc. usually easily form the diffi-
cult-to-stratified emulsion with organic phase and
lead to the formation of the third phase crud. Espe-
cially from the devotion of Si02 in solution: from
the common practices, it is known that the content of
SiOz in the aqueous phase will be less than 0.1 g L .
If it is greater, for the stabilization of S O 2 to
oil-in-water type emulsion, usually the emulsifica-
Table 3. Influences of solid suspensions on the formation of crud
~~~~~~~
State Clarified time / h ~
Solid suspensions / (mg.L-’)
~ ~
Before clarifying 0 85
After clarifying 24
(2) Influences of colloidal particles on the forma-
tion of the third phase crud.
The colloidal materials in the leach solution are
inainly caused by improper control of the pH value
of the leach solution. If the pH value is very high,
the colloids such as Fe(OH)3, AI(OH)?, and H2Si03
may be formed. For example, the silicate dissolved
RARE METALS, Vol. 26, No. 1, Feh 2007
tion may present 171. There are some large porous
surface-active agents such as minerals and clay in
the leach solution, some of them are hydrcyhilic,
and the others hydrophobic. These solid particles
help t;o stabilize the emulsion to form the crud.
Moreover, the solid particle in the leach solution
may not only accelerate the formation of cnd, once
absorbed in the crud, it may also become a srabiliz-
ing agent to stabilize the emulsification structure of
the crud. The types of third phase cruds formed de-
pend on the hydrophobic and hydrophilic h:haviors
of solid particles. If the solid particles art hydro-
philic, the oil-in-water type may appear; if they are
hydrophobic, the water-in-oil type crud forms.
The following data may explain the influences of
solid suspensions on the formation of crud. In the
column leach expansion experiment solution with
the solid suspensions of 85 mgL, filtered after clari-
fication for 24 h, the content of solid suspensions in
the leached solution is reduced to 18 mg/L. T&e the
leached solution before and after filtering respec-
tively, and carry out the solvent extraction test under
the Sine test conditions. Before filtering, the quan-
tity of crud is 3-4 times more than that after filtering
(see Table 3 for details). Observations ti-on I the test
show that for an organic solvent, before purification,
there are large quantities of netted bubbles ;it the in-
terface during the solvent extraction. and after puri-
fication, the interface of the organic solverit is very
clear during the solvent extraction. The duration of
phase separating is only 32 s.
~ ~~~~
Quantity of crud / mL Phase separatiori time
-~
/s
1.o I97
18 3.2 32
by acid may be turned into silicic acid (,Si(OH)j),
and silica gel finally.
Dui-ing the physical mixing in two mutual insolu-
ble liquids systems, it is inevitable that there is “fric-
tion” between both phaqes. This “friction” may gen-
erate a static charge on the surface of drop.;. When
the liurface of the dispersed drops is charged, these
Zheng Q.. et af., Influences of solid particles on the formation of the third phase crud during
chargcd drops may repel mutually and they will be
unable to aggregate to keep at suspension state. This
is one of the main causes in the formation of an
emulsion. One case is that the drop is composed of
an uncharged nucleating center (micro particles such
as SKI2) for absorption effect. The negative charge
on its drop surface is mainly caused by ”friction”.
Another case is that the nucleating center of the drop
is composed of a charged ionic colloidal group (such
as multinuclear hydrocarbon complex ion of Fe) or
solid particles. Under the effect of its charges, the
polar 2nd of the organic phase or aqueous phase
molec dar is absorbed on its surface, and the surface
of the drops form the whole potential to let the drops
repel r iutually.
During the solvent extraction, if the surface film
absorbed a solid particle. especially the charged par-
ticle , ind a new-formed colloidal particle, the
strengl h and tightness of the film may be improved
considxably. The colloid charged and let the drops
repel ( ne another and therefore it was uneasy to ag-
pegatt:. thus the emulsification phenomenon oc-
curred [6].
During the solvent extraction experiment, it was
found hat when the pH value of leach solution was
more han 3.0, the third phase crud formed, but
Table 4. Intluences of pH value on the formation of the third phase crud
~
Mother solution
~
Solvent extraction
Content 01 solid Intcrfacid
pH ohenomenon
I .52 0 L.ittle foam
1.97 0 Little foam
7.30 20 Interface clear
-3. I4 85 Much foam
3.91
-~ 100 Much foam
As shown in Table 4, with the pH value increas-
ing in tilt mother solution. the copper extraction rate
also increases when the pH value is lower, However.
when the pH value reaches up to 7.30. the quantity
1 1 1 IIii- f l t l i C l Idlii>c ciud iiicicasrs gicatly. ‘ r h i h is
caused by a high content of foreign materials such as
Fe. Al. Si etc. in the mother solution. If the pH value
is highcr than that for hydrolysis purpose. the col-
loidal substance is generated during solvent extrac-
... Y3
when the pH value of this leach solution was ad-
justed to 1.7-2.5 with sulfuric acid and the extraction
test was carried out under the same test conditions,
its results showed that the colloid would be damaged
effectively by adjusting the pH value of the leach
solution below 2.3 and allowing the Fe, Al, Si, etc.
present in the ionic states. Thus, the control of the
pH value in the leach solution to reduce the genera-
tion of colloidal materials is crucial to prevent the
formation of the third phase crud.
3.3. Influences of pH value on the formation of
the third phase crud
Observing from everything mentioned above,
during the solvent extraction, if the pH value is too
high, especially over that of hydrolysis of Fe. A1 etc.,
sediments such as Fe(OH)3 and AI(OH)3 etc. may be
formed. Under these conditions, the formation of the
third phase crud is easier.
The mother solution for the experiment is taken
from the column leach expansion test. Dilute sulfu-
ric acid or sodium hydroxide solution may be re-
spectively used for adjusting the pH value of the
mother solution to 1.52, 1.97, 2.30, 3.14, and 3.91.
The other conditions are identical. Table 4 shows the
test results.
~ ~ ~ Quantity of Recovery of
Phase scparating crud I mL copper I %
time I s
40 0 x0.05
35 1 8 I .57
35 1 95.10
I97 3.2 90.36
150 3.8 75.56
tion, and the crnulsification is presented easily and
forms the third phase. Reducing the pH value dam-
ages the colloid and postpones the formiltion of thr
third phiixe crud. The text has proven that controlling
die pH valuc oi rhc morhcr soiurion ~ C I O W~ . .i
iiisy
reduce 2/3 of the total formation of the third phase.
Because the contents of Ca and Mg are higher in the
mother solution, if the pH value is too low, during
the solvent extraction, calcium and magnesium may
94 RARE METALS, Vol. 26, No. 1, Feb 2007

be separated out in the sulfate, to increase the quan-
tity of interface floccus and cause the third phase to
increase. Table 4 shows that decrease in the pH
value of the mother solution may increase the ex-
traction rate of copper (pH > 2.3). If the pH value is
too low, however, the extraction rate of copper may
be decreased again. Thus the pH value shall be con-
trolled at about 2.3.
3.4. Influences of surface tension on the forma-
tion of the third phase crud
General speaking, the formation of the third
phase crud mainly depends on the surface tension of
the drop and the strength and tightness of the surface
film. During generation of the third phase crud or
emulsion, the influence of surface tension is signifi-
cant; both the water-in-oil or oil-in-water types have
interface reaction. Apart from the behavior of the
drop itself (such as medium properties and concen-
tration). the surface tension also depends on whether
there are surface-active substances in the solvent ex-
traction system. Usually the existence of sur-
face-active substances may cause the formation of
stable emulsion. According to the surface chemical
principle, the higher the surface energy of molecular,
the less the surface area of drop, which shrinks
automatically; that is, the drops may aggregate.
However, if the molecular of some surface active
substances are absorbed on the surface of drops, its
surface free energy may be reduced considerably,
because the molecular of surface active substances is
an organic compound composed of a hydrophilic
polar group (such as OH group) and hydrmophobic
non-polar group (such as alkyl group). Its polar
group faces the water and its non-polar group faces
the organic phase. This regular orientation mange-
ment lets the unsaturated force field on the iurface
balance, and thus reduce the surface tension. There-
fore, the surface tension may be reduced ~.mlyif
there are surface-active substances which allow the
emulsion to stabilize. Certainly, if the solvent extrac-
tion :system is entrained with surface-acti\.e sub-
stancm such as solid particles, the surface tension
will be lowered and will form the stable emulsion,
that is, the third phase crud.
The surfacehnterface tension may be nicasured
through the platinum plate methodplatin urn ring
method, respectively. The mother solution. extract-
ing agent, extracted residual solution, and loaded
organic phase are taken for measuring. Table 5
shows the results and phenomenon of the surface
tension test. Table 6 shows the influences of the pH
value of solvent extraction on the surface tension.
Se:en from the rest results in Tables 5 and 6, it was
found that the surface tensions of extracted residual
so1ut:ion and loaded organic phase are considerably

Table 5. Test result of surface tension and experiment phenomenon

~ ~

Sudace tension / ( m m-')

~
Phase Quantity
Mother Extracted residual Loaded organic Interface tension ~eparat,on ot crud
Extractant
solution
~ ~~ ~~
solution
~~ ~~
phase ~
of water-organic
~ ~ ~~ __
69.87 52.75 48.67 25.62 13.45 Rapid hl iriim
72.35 52.75 5 1.87 26.04 15.96 Quicker I 1rtle
70.85 52.75 52.24 26.71 15.74 Slower Ab~rnil:tnce
72.21 52.75 49.70 25.83 14.08 Mcdium Abundance

Table 6. Influences of pH on surface tension

Surface tension / (rnn~m-') ~

pH Mother solution Extracting agent Extracted residual solution Loaded organic phase
~~~ ~~~ ~ ~~ -~~ . -~
I .97 69.95 52.75 53.12 26.84
2.30 70.48 52.75 52.33 26.84
3.14 70.85 52.75 52.24 26.7 1
3.91 71.32 52.75 :51.58 26.96 _~
Zheng Q., et al., Influences of solid particles on the formation of the third phase crud during
more r-duced than those of the mother solution and
extracting agent, and the sum of both kept at a stable
value. The interface tension value has the tendency
of keeping step with the variation of the third phase
crud; the higher the pH value, the higher the surface
tension of mother solution. but the less the surface
tension of extracted residual solution. The variation
of loadzd organic phase is not considerable.
4. Measures to prevent and control the
formation of the third phase crud
Becwse the solid particles are the cause of form-
ing the third phase crud, some measures may be
adopted for controlling the aqueous phase to prevent
the formation of the third phase crud. (1) Naturally
clarifj )r filter etc. to eliminate those insoluble solid
particles in the extraction solution, strictly control
the con :ent of solid particles in the aqueous phase. (2)
E l i m k t e those colloids or suspensions such as sili-
con oxide, alumina. and ferric hydroxide etc. in ex-
traction solutions. (3) Keep the extraction solution at
the speified pH value to prevent the existence of
colloid1 particles in leach solution, for example,
when e.;tracted in acid solution, its pH value must be
lower ti) avoid the formation of the third phase for
some metallic ion sediment, and to reduce the nucle-
ating ctmter for the formation of the third phase;
Adjust the pH value of leach solution by adding
sulfuric acid (strong electrolyte), which may effec-
tively dJmage the colloid, and let the Fe, Al, and Si
present in the ion state. (4) Add the flocculating
agent and then filter. The formation of the third
phase or crud during solvent extraction may be re-
duced e3ectively.
5. Conclusions
(1) During copper solvent extraction, the compo-
nents of the measured third phase crud show that the
main ccmponents of solid phase are SiOz and Fe,
followed by A1 and Ca, Mg, Cu, etc. Thus the solid
particles in the mother solution are one of the most
importarit contributor5 for the formation of the thlrd
phase crJd.
... 95
(2) During copper solvent extraction, the solid
particles in the mother solution are the main causes
to form the third phase crud. The solid particle sus-
pensions are usually easier to form in a diffi-
cult-to-stratify emulsion with organic phase and
cause the formation of the third phase crud. These
solid particles may not only accelerate the formation
of crud, once absorbed on the crud, they may also
become stabilizing agents to stabilize the emulsifica-
tion structure of the crud. Hence, the leach solution
with solid suspensions should be filtered to greatly
reduce the quantity of the third phase crud. From all
the above mentioned, it is clear that the suspended
solid particles in the mother solution present great
effects to the formation of crud.
(3) During the solvent extraction, if the surface
film is absorbed with some solid particles, especially
charged particles and new-formed colloidal particles,
the strength and tightness of the film may be im-
proved considerably. Because the colloid is charged
and the drops repel mutually, it is difficult to aggre-
gate. Thus, the third phase crud presented.
(4) During the solvent extraction, if the pH value
is too high, especially above that needed for hy-
drolysis of Fe and A1 etc, the sediments such as
Fe(OH)? and Al(OHh may be accompanied. Under
these conditions, the formation of third phase crud
becomes easier.
(5) After extraction, the surface tensions of the
extracted residual solution and loaded organic phase
are considerably reduced and the sum of both kept at
a stable value. The interface tension value has the
tendency of keeping step with the variation of the
third phase crud; that is, the higher the value of in-
terface tension, the more the quantity of crud; and
the higher the pH value, the higher the surface ten-
sion of the mother solution, but the less the surface
tension of the extracted residual solution.
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