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IWA Publishing 2014 Water Science & Technology

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2014

Recovery of water and acid from leach solutions using

direct contact membrane distillation
Uchenna K. Kesieme, Nicholas Milne, Chu Yong Cheng, Hal Aral
and Mikel Duke

ABSTRACT
This paper describes for the rst time the use of direct contact membrane distillation (DCMD) for acid
and water recovery from a real leach solution generated by a hydrometallurgical plant. The leach
solutions considered contained H2SO4 or HCl. In all tests the temperature of the feed solution was
kept at 60 C. The test work showed that uxes were within the range of 1833 kg/m2/h and 15
W

35 kg/m /h for the H2SO4 and HCl systems, respectively. In the H2SO4 leach system, the nal
concentration of free acid in the sample solution increased on the concentrate side of the DCMD
system from 1.04 M up to 4.60 M. The sulfate separation efciency was over 99.9% and overall water
recovery exceeded 80%. In the HCl leach system, HCl vapour passed through the membrane from the
feed side to the permeate. The concentration of HCl captured in the permeate was about 1.10 M
leaving behind only 0.41 M in the feed from the initial concentration of 2.13 M. In all the experiments,
salt rejection was >99.9%. DCMD is clearly viable for high recovery of high quality water and
concentrated H2SO4 from spent sulfuric acid leach solution where solvent extraction could then
be applied to recover the sulfuric acid and metals. While HCl can be recovered for reuse using
only DCMD.
Key words

Uchenna K. Kesieme (corresponding author)

Nicholas Milne
Hal Aral
Mikel Duke
Institute for Sustainability and Innovation,
College of Engineering and Science,
Victoria University,
P.O. Box 14428, Melbourne,
Vic 8001,
Australia
E-mail: uchennakennedy.kesieme@live.vu.edu.au
Uchenna K. Kesieme
Chu Yong Cheng
CSIRO,
Process Science and Engineering/CSIRO Minerals
Down Under National Flagship, Australia,
P.O. Box 7229 Karawara, WA 6152,
Australia
Hal Aral
Jervois Mining Limited,
10 Jamieson Street,
Cheltenham, Vic 3192,
Australia

| acid recovery, DCMD, direct distillation, leaching

INTRODUCTION
Leaching is the process of dissolving a soluble mineral or
metal from an ore. The process requires variety of lixiviants
or leach-uids, and operating conditions which are dependent on the mineralogy of the ore to be processed. This
technique is commonly used in mining to recover valuable
metals (such as nickel, gold, copper, and cobalt) from geological materials (Zhu et al. ). Different acids such as HCl and
H2SO4 are often used as leaching uid to dissolve mineral or
metal from their ores. After treatment, the loaded leach solution often contains a high concentration of residual acid
and valuable metals. A conventional and popular method
to treat acid solutions is neutralization of which large
amounts of alkaline reagents such as calcium carbonate; calcium oxide; calcium hydroxide; magnesium hydroxide and
sodium hydroxide are used (Greben & Maree ). This
also produces a sludge containing heavy metal compounds
that must be disposed of. Furthermore, valuable acid is lost
during the neutralization process which could be recovered
doi: 10.2166/wst.2013.788

and reused. Industries are now giving serious consideration

to acid recovery from leach solution considering its economic
and environmental benets. Several methods other than the
direct neutralization method have been developed including
both active and passive treatment technologies to mitigate the
problems of acid and salt accumulation in waste acidic efuents. Various treatment options are membrane distillation
(MD), reverse osmosis (RO), solvent extraction (SX), ion
exchange, electrodialysis, electrolysis, and biosorption
(Shelp et al. ; Ramstedt et al. ; Sarangi et al. ;
Haghshenas et al. ; Kesieme et al. a). Essentially,
these processes work either through separation of acid and
salts through a membrane or using an organic system to
recover the metals, while others are applied to lower the bioavailability of metals in solution, and to lower dissolved metal
and sulphate concentrations.
MD is an emerging thermally driven membrane process
and can be applied to recover acid and fresh water from

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Recovery of water and acid from leach solution using DCMD

acidic leach solutions. In MD processes, a micro-porous

hydrophobic membrane is used to separate two aqueous solutions at different temperatures, and selective mass transfer
occurs. This process takes place at atmospheric pressure and
a temperature which may be much lower than the boiling
point. The hydrophobicity of the membrane prevents the
transport of liquid across the pores of the partition while
water vapour and volatiles can be transported from the
warm side, condensing at the cold surface. In comparison
with other separation methods, MD has several advantages
including very high rates of rejection for non-volatile components, lower operating pressure than pressure-driven
membrane processes, much larger membrane pore size
than that of (RO) and typically larger than that of ultra-ltration membranes, less sensitivity to fouling than RO, and
low sensitivity to feed salinity and low feed temperature
requirements (4080 C) as compared to other thermal distillation method such as multi-effect distillation (Zhang et al.
). MD is a promising technique for minimizing RO concentrate discharge. It has been demonstrated that salt
concentration in the feed has a relatively small effect on
the mass ux of MD processes in comparison to RO processes, indicating that MD can effectively deal with high
concentrations of brines (Kesieme et al. c), and also
can be applied for desalination and wastewater recycling
in places where waste heat, solar or geothermal sources
are available (Banat & Jwaied ). MD processes have
several congurations which are as follows: (1) direct contact membrane distillation (DCMD), (2) air gap membrane
distillation, (3) sweeping gas membrane distillation, and
(4) vacuum membrane distillation (VMD). Among these
congurations, DCMD, is the most widely used because it
is convenient to set-up and gives high water ux (Cath
et al. ; Kesieme et al. c).
MD has potential applications in many areas of scientic and industrial interest to obtain highly puried permeates
from solutions containing contaminants. Tomaszewska &
Mientka () studied separation of H2SO4 and HCl from
a synthetic solution containing only H2SO4 and HCl. It
was reported that the presence of sulfuric acid in the
feed decreases the solubility of HCl, and hence increases
HCl ux as H2SO4 concentration increases in the feed.
Tomaszewska et al. () also reported a salting out effect
using MD for synthetic and a real metal pickling solution
containing both HCl and salts, respectively. Furthermore,
in a similar study (Kesieme et al. ), the inuence of
acid concentration and the presence of inorganic salts
were investigated using DCMD for three synthetic solutions:
(a) 0.5 M H2SO4, (b) 0.5 M H2SO40.2 M NaCl and
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(c) 0.5 M H2SO40.2 M Na2SO40.2 M NaCl. It was

reported that the presence of NaCl in the feed solutions of
(b) and (c) resulted in signicant transfer of HCl vapour to
the permeate. In the work reported by Zhang et al. ()
and Tang & Zhou (), acid recovery from different process acidic solutions using MD technique was also
reported. These studies of DCMD for acid recovery focus
on treatment of primarily synthetic and specic real solutions. However to the best of the authors knowledge,
treatment of real leach solutions by MD to recover acid generated from hydrometallurgical plant have not been
reported. The treatment of real leach solutions containing
H2SO4 or HCl using DCMD is a novel concept of value in
recovering acid from metal or salt solutions.
Conceptual ow-sheets to recover acids and water from
leach solutions containing H2SO4 or HCl are shown in
Figure 1(a) and 1(b). For H2SO4 leach solution, DCMD can
be applied to recover fresh water and concentrate sulfuric
acid solution and metals. The concentrated acidic solution
can be recovered using SX (Kesieme et al. a, b).
The fresh water recovered by MD can be also used for scrubbing the entrained metals and stripping the extracted acid
(Kesieme et al. a, b). For HCl leach solutions, DCMD
can be applied to recover HCl solution and also, concentrate
the non-volatiles such as ferrous ion. The aim of this study
was to assess the opportunity of DCMD to recover fresh
water and acids from real acid leach solution generated
from hydrometallurgical plants. The concentrated sulfuric
acid can be recovered by SX and recycled to the leaching
circuit for reuse.

METHODS
Experiments were conducted in DCMD mode to conrm
the viability of MD to recover acid from two different real
leach solutions containing HCl or H2SO4. The leach solutions were from a Jervois Mining process plant in
Melbourne, and had composition as shown in Table 1.
The ow diagram of the experimental rig is shown in
Figure 2. The membranes used were at sheet PTFE supported on polypropylene scrim backing as optimised in
previous work by Zhang et al. (). The membranes had
an active area of 0.0169 m2, pore size of 0.45 m and were
supplied by Ningbo Chanqi, China. A cartridge lter with ltration size of 0.5 m was used on the hot loop to collect
precipitated matter prior to entering the MD module. The
ow rate into the module hot and cold sides were
900 mL/min. The feed temperature was 60 C and the cold
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U. K. Kesieme et al.

Figure 1

Table 1

Recovery of water and acid from leach solution using DCMD

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A conceptual ow-sheet to recover water, acid, and metal values from H2SO4 or HCl leach solutions.

Feed compositions of the leach liquor for H2SO4 and HCl systems

Species

H2SO4 leach solution

HCl leach solution

Aluminium (mg/L)

4,400

5,590

Calcium (mg/L)

248

Cobalt (mg/L)

21.9

30.8

Copper (mg/L)

6.7

27.1

Iron (mg/L)

15,700

20,000

Magnesium (mg/L)

1,830

5,900

Manganese (mg/L)

265

342

Nickel (mg/L)

341

1,310

Scandium (mg/L)

26

10

Zinc (mg/L)

28

24.7

Free acid (H) mol/L

1.08

2.13
Figure 2

temperature was maintained at 20 C. The choice of feed

temperature and ow rate affects the efciencies of the
MD process. The feed temperature of 60 C is a representative of a waste heat situation based on the previous study
(Kesieme et al. c) and the feed and permeate owrate
was selected based on the study of DCMD testing for RO
brine solution (Zhang et al. ). For the solution
W

DCMD experimental ow diagram.

containing non-volatile substances only water vapour is

transferred across the membrane and the non-volatile compounds such as H2SO4 are retained by the membrane.
Solutions containing volatiles compounds such as HCl and
water vapour can pass through the membrane to the permeate. The vapour was condensed directly in the solution
(distillate) in the permeate in which HCl was dissolved.

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Recovery of water and acid from leach solution using DCMD

The cold cycle was initially supplied by distilled water.

Permeate build-up was measured by the accumulated mass
of water in the permeate tank. The HCl ux was calculated
from the material balance of HCl in the distillate performed
every hour taking into account the changes of volume and
the acid concentration in the distillate and well described
in the previous work (Tomaszewska & Mientka ). The
water ux is calculated based on Equation (1). Recovery is
calculated as shown in Equation (2)

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2014

matrix buffering @ 5 g/L and Cs internal standard was

employed to accommodate the wide range of matrix variation in the dilutions. Free acid was determined at pH
4.20 in sodium EDTA matrix with standardised 0.1 M
NaOH.

RESULTS AND DISCUSSION

MD concentration step for the H2SO4 leach solution

FWater

Mass of permeate (kg)

Effective membrane area (m2 ) operating time (hr)
(1)

Recovery (%)

Permeate produced (L) 100

Initial feed volume (L)

(2)

Electrical conductivity was measured using a conductivity

metre in the permeate tank to ensure membrane intactness.
For H2SO4 leach solution conductivity <80 S/cm and was
decreasing over time in the permeate while the HCl leach
solution conductivity increased with time and went out of
scale due to the ow of the HCl vapour in the permeate.
Cations in samples were determined by ICP OES analysis,
which was performed on a range of serial dilutions to reduce
the concentration of each species to a suitable level. Cs

Figure 3

Table 2

Water ux and recovery over time for H2SO4 loaded leach solution.

Figure 3 shows ux and recovery over time using DCMD to

concentrate the H2SO4 leach solution and recover fresh
water. Within 8 hours of the batch MD experiment, ux
decreases from 3318 kg/m2/h. The choice of feed temperature affects ux of an MD system. Generally, increases in
feed temperature also increases ux. The feed temperature
of 60 C is selected as a representative of the waste heat situation for MD based on the previous study of the waste heat
situation for MD (Kesieme et al. c). The performance of
MD was also proven to be optimal at this temperature
(Zhang et al. ). In previous work (Kesieme et al.
c), it was observed that the mass ux of MD appeared
only slightly dependent on feed water salinity up to
361 g/L total dissolved solids. Therefore ux decline
appears to be related more to membrane scaling effects
than vapour pressure reduction due to salinity. The water
recovery exceeded 80%, and the initial feed volume of
3,950 mL was reduced to less than 500 mL.
Table 2 shows the concentration of various species at
the start and end of the MD batch experiment. The salt rejection exceeded 99.9% and the free acid was concentrated
from the initial concentration of 1.08 M to about 4.60 M.
Similar observation was reported in the literature of using
DCMD to concentrate sulfuric acid from process acidic solutions (Kesieme et al. ; Zhang et al. ; Tomaszewska
and Mientka ). The nal permeate acid concentration is
<0.001 M, which is equivalent to an acid separation efciency >99.9%. The concentrations factor for all metals
except calcium was found to be greater than 4. This is
attributable to the high water recovery achieved (>80%).
W

Concentration of the major species of the H2SO4 leach solution in the feed after treatment using DCMD

Species

Al

Ca

Co

Cu

Fe

Mg

Mn

Ni

Sc

Free H [mol/L]

Zn

Initial feed [mg/L]

4,400

248

21.9

6.7

15,700

1,830

265

341

26

28

1.08

Final feed [mg/L]

19,100

310

94.1

32.6

66,100

8,000

1,140

1,460

111

117

4.6

Concentration factor

4.34

1.25

4.29

4.78

4.21

4.37

4.30

4.28

4.27

4.18

4.26

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Recovery of water and acid from leach solution using DCMD

The concentration factor achieved for calcium is more limited because it was precipitating. As the concentrate side
salinity increases the saturation point for various dissolved
species is exceeded causing conditions suitable for various
types of scale and salt precipitation. At low pH, sulfate
ions tend to be present as bisulfate ion, which reduces the
tendency for gypsum scale to form. Iron scale due to the formation of iron hydroxides and/or carbonates may be
eliminated because the pH is sufciently low to reduce
hydroxide and carbonate alkalinities. Furthermore, iron
may predominantly be in the ferrous form with little tendency to oxidise to the ferric form. Manganese scale and
fouling potential can be avoided by keeping the manganous
ion in solution at low pH (Bourke & Mack ). Aluminium is also retained in solution at low pH because it is
almost entirely in the dissolved aluminium ion form at low
pH. Other heavy metals are also retained and rejected by
the membrane. No signicant scale was observed on the
membrane, but was observed in the 0.5 m lter and
hence the salt precipitation and scaling were efciently captured at the highest temperature point in the hot cycle
minimising membrane scaling. An interesting feature of
MD as a thermal process is the separation of the saline
water heating zone (heat exchanger) from the evaporation
zone (membrane). The separation has allowed the convenient placement of the lter between the zones to
capture precipitating salts made up of ferrous compounds
and calcium immediately after heating, but prior to evaporation. As the water enters the membrane module, it begins to
cool due to evaporation. Also, the membrane surface itself is
cooled by the cold permeate side leading to the temperature
polarisation effect. Both effects assist in the avoidance of
calcium scaling of the membrane (Kesieme et al. c).
The solubility of calcium scaling salts has an inverse
relationship with temperature meaning they are less soluble
at higher temperature.
MD can operate at high salinities where RO fails and
may be applied to effectively concentrate sulfuric acid solution and also recover fresh water from a H2SO4 leach
liquor from a hydrometallurgical plant. Therefore for process waste solutions containing sulfuric acid, iron,
aluminium, magnesium, scandium, nickel, cobalt, manganese and sulfates, MD is well suited to recover water and
concentrate sulfuric acid. The nal product can be separated
into (1) pure water with water recovery exceeding 80%
(permeate) and (2) concentrate containing sulfuric acid
and sulfates. The concentrate containing valuable components such as H2SO4, and Ni/Co hydroxide can be
selectively be recovered using SX as shown in Figure 1(a).

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Figure 4

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2014

Electrical conductivity and pH reading in the permeate over time.

Figure 4 shows the changes to electrical conductivity

and pH in the permeate over time for the H2SO4 leach solution during the MD batch experiment. Electrical
conductivity reading in the permeate was found to be
decreasing over time in the range of 7451 S/cm throughout the experiment. The pH reading was stable within the
range of 6.977.00. Conrming membrane effectiveness to
reject non-volatiles such as sulfuric acid as no acid was
detected in the permeate tank but rather concentrating in
the feed concentrate.
Experimental viability of MD to recover HCl solution
from HCl leach liquor
Figure 5 shows the total ux and HCl ux for the MD process on HCl leach liquor. It is important to note, that while
non-volatile compounds such as H2SO4 are virtually completely retained by MD technique, volatile compounds
such as HCl can pass through the membrane to the permeate. The selectivity of an MD system is determined by the

Figure 5

HCl ux and total ux for HCl loaded leach solution.

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Recovery of water and acid from leach solution using DCMD

liquid/vapour equilibrium of the feed (Tomaszewska &

Mientka ). The composition of the permeate will
depend on the values of the volatility and/or different diffusion rates for the respective components of the feed. This
means that the component with higher vapour pressure
will diffuse faster through the membrane. Therefore,
during the MD experiment of an HCl leach solution, the
ux containing both HCl and water vapour across the
membrane as shown in Figure 5. The HCl ux was slow
at the beginning of the experiment and increased gradually
until after 100 min, where the ux increase was sharp.
This may be due to uxing of water vapour through the
membrane prior to HCl ux at the beginning of the experiment. The HCl ux was increasing over time in the
permeate up to about 90 mol/m2/d. However, the total
ux was found to be decreasing from 3515 kg/m2/h
within about 4 h of the batch experiment. The ux changes
are similar to that reported for the MD batch experiment
on H2SO4 leach solution and the same experimental condition of temperature and owrate. A higher feed
temperature results in an increase of the driving force of
DCMD. The uxes of the volatile compounds such as

Figure 6

HCl (free acid) permeate concentration and recovery for HCl loaded leach
solution.

Table 3

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water vapour and HCl rise exponentially according to the

vapour pressures. The temperature of the feed and distillate
(60 and 20 C) were sufcient to obtain a good ux as
shown in Figure 5. HCl vapour was almost depleted in
the feed and successfully captured in the permeate. Free
acid in the permeate after the MD experiment is higher
than in the feed, and about 1.10 M was recovered leaving
behind only 0.41 M in the feed from the initial concentration of 2.13 M. Tomaszewska et al. () also
reported HCl ux increases in the permeate up to
870 mol/m2/d as the salt concentration was increasing in
the feed. To achieve a better performance of HCl recovery,
the VMD conguration was recommended (Bandini et al.
; Camacho et al. ). The VMD conguration is
useful when volatiles such as HCl are being removed
from an aqueous solution. However, it is interesting to
observe the performance of DCMD for HCl removal/
recovery as it is a much simpler setup than VMD, not relying on an external condenser or vacuum pump.
Figure 6 shows HCl (free acid) permeate concentration
and recovery over time for HCl-loaded leach solution.
About 70% of the total solution was recovered in the permeate. The concentration factors achieved for the major ions
are shown in Table 3. The result shows that the concentration factors were not uniform as in the case of H2SO4
leach solution. The reason may be due to changes in the
pH and more importantly most metal ions particularly Al,
Fe and Mn are not very stable in a chloride medium. The
concentration factors achieved for Fe, Al, Mn and Mg
were 3.17, 2.3, 3.30 and 2.31, respectively, and the individual salt rejections were generally greater than 99.9%.
Therefore, MD can be applied for the treatment of industrial
efuents containing HCl and salts. The salts were completely retained in the feed, and only pure hydrochloric acid
captured in the permeate. The useful products might be
hydrochloric acid and salts after crystallization from the
supersaturated feed.
W

Concentration of the major species for the HCl leach solution in the feed and permeate after treatment using DCMD

Species

Al

Co

Initial feed [mg/L]

5,590

30.8

Final feed [mg/L]

12,900

84.1

<0.5

<0.1

Final permeate [mg/L]

4.1

<0.1

Conc factor

2.30

Initial permeate [mg/L]

2.73

Cu

Fe

27.1
118
<0.1

Mg

Mn

Ni

Sc

Zn

Free H [mol/L]

20,000

5,900

342

1,310

10

24.7

2.13

63,400

13,600

1,130

6,000

23

60.4

0.41

<0.1

<0.5

1.69

2.64

4.49

4.35

3.17

2.31

<0.1

<0.1

<0.1

<0.1

<0.001

<0.1

<0.1

<0.1

<0.1

1.095

3.30

4.58

2.30

2.44

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Recovery of water and acid from leach solution using DCMD

Economics, energy analysis and cost evaluation of MD

system
A desalinated water cost assessment for MD, like the benchmark RO and MED systems, is sensitive to several factors
such as energy source, plant capacity, salinity, and design
features (Kesieme et al. c). Among those factors,
energy source and plant capacity have a dominating inuence in addition to feed seawater salinity for the RO
process (Fritzmann et al. ). Unlike RO, energy consumption in MD systems includes both thermal and
electrical energy. The thermal energy requirement of MD
is around 90% of the total energy but can come at a relatively low cost and offers an opportunity for the use of low
cost waste thermal heat (Kesieme et al. c). Therefore
MD is most viable to desalinate water when a low cost
waste heat source is found.

CONCLUSIONS
The experiment conrms MD viability to recover acids and
water from acidic loaded leach liquor.
For H2SO4 loaded leach solution, H2SO4 was concentrated from the initial concentration of 1.08 to 4.6 M
(as free acid) and water recovery >80%. The sulfate
separation efciency was over 99.9%. The concentrated
H2SO4 remaining on the feed may be selectively recovered
using SX.
For the HCl loaded leach solution, HCl was most
depleted in the feed and successfully captured in the permeate tank (as free acid). The concentration of HCl recovered
in the permeate was about 1.10 M leaving behind only
0.41 M in the feed from the initial feed concentration of
2.13 M.
The cartridge lter between the heating zone (heat
exchanger) and the evaporation zone (membrane) was
used to capture precipitating salts immediately after heating,
but prior to evaporation. This reduces the chances of membrane fouling and scaling on the MD system and thus
enhances water recovery.
MD as a thermal process is energy intensive, and is
therefore sensitive to the price of thermal energy indicating
more cost-effective operation if waste heat can be utilised.
MD has benets over RO in its ability to concentrate to
very high salinities without signicant ux loss, and allow
for the recovery of HCl.

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ACKNOWLEDGEMENTS
The authors would like to thank CSIRO Minerals Down
Under National Research Flagship and Victoria University
for providing the PhD scholarship for U.K.K., and also
Jervois Mining for providing the leach solutions.

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First received 24 July 2013; accepted in revised form 2 December 2013. Available online 14 December 2013