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A STUDY OF LEACHING OF COPPER OXIDE ORE BY SULPHURIC ACID

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 Hydrometallurgy:
Materials and Equipment
 Hosted by

PROCEEDINGS OF THE 52nd CONFERENCE OF METALLURGISTS (COM),

Hosting by MATERIALS SCIENCE TECHNOLOGY CONFERENCE (MS&T)
OCTOBER 27 to 31, 2013, MONTRÉAL, QUÉBEC, CANADA

Hydrometallurgy:
Materials and Equipment

Editors

Akram M. Alfantazi
University of British Columba, Vancouver, Canada

Nosrat Behnood
Process Technology Materials Consultant Inc., Pierrefonds, Canada

Gordon Copper
SNC Lavalin Inc. (Mining & Metallurgy), Montreal, Canada

Wilson Pascheto
XPS Consulting & Testwork Services, Falconbridge, Canada

Symposium Organized by the Hydrometallurgy Section of the Metallurgy and Materials Society
of the Canadian Institute of Mining, Metallurgy and Petroleum
 A Publication of The
Canadian Institute of Mining, Metallurgy and Petroleum
1250 - 3500 de Maisonneuve Blvd. West
Westmount, Québec, Canada H3Z 3C1
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Copyright ©2013

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call: (514) 939-2710, ext. 1327
www.metsoc.org
Foreword

This volume includes papers presented at the International Symposium on Hydrometallurgy:

Materials & Equipment during the 52nd Annual conference of Metallurgist (COM 213) being
held in Montreal, Quebec, Canada on October 27 to 31st, 2013.

The symposium features over thirty papers from Canadian and international scientist and
engineers reporting recent developments in process, equipment, materials of construction, and
corrosion in the hydrometallurgical industry.

The success of the Symposium is due to the scientists and engineers reporting their findings. We
wish to thank them for taking precious time to document their work and making the publication
of these proceeding possible.

Akram M. Alfantazi
Nosrat Behnood
Gordon Copper
Wilson Pascheto
Editors

v
Editors’ Biographies

Akram M. Alfantazi is currently a professor in the Materials Engineering Department and

Associate Dean Research and Graduate Studies in the Faculty of Applied Science at the
University of British Columbia (UBC), Vancouver, Canada. Dr. Alfantazi obtained his B.Eng in
Metallurgical Engineering from Laurentian University in 1989, and M.A.Sc. and PhD degrees in
Materials Engineering from Queen’s University in 1991 and 1994, respectively. He then held a
2-year Postdoctoral fellowship at UBC. In 1996, he joined Falconbridge Ltd., where he worked
as a Project Metallurgist for several years before returning to UBC as an assistant professor in
2001, where he has been teaching and conducting research in corrosion, electrometallurgy and
electrochemical processes in materials engineering. Dr. Alfantazi has more than 250 publications
including over 100 refereed journal publications. He has also co-edited several books. He has
served as a consultant to a wide variety of companies in the chemical, metallurgical, and
petroleum industries. He is a Fellow of the Canadian Institute of Mining, Metallurgy and
Petroleum, NACE International, and the Engineering Institute of Canada. He regularly gives
industrial short courses on corrosion and electrometallurgy at conferences and to industry in
many parts of the world. He has received a number of awards for his work including a UBC
Killam Award, the Professional Engineers and Geoscientists of BC Teaching Award of
Excellence, and the Canadian Materials Chemistry Award.

Nosrat Behnood is a consultant at Process Technology Materials Consultant Inc (PTMC Inc)
serving mining & metallurgical and engineering companies for over ten years. Prior to joining
PTMC Inc, he served as Sr. Materials Engineer and Sr. Scientist for Falconbridge & Noranda
Technology Centers (Xstrata-Glencore) for 16 years. Before moving to Canada, he spent 10
years teaching material science in Iran. His expertise focuses on Material science, selection of
materials of construction for mining & metallurgical industries, failure analysis, corrosion,
foundry technology, surface modification, and testing & evaluation of materials. Nosrat has a
master degree in metallurgical engineering from Technical University of Istanbul, Turkey and
MSc & Ph.D. from the University of Newcastle, England. Nosrat holds a U.S. patent and co-
author of over 15 technical articles and a significant number of reports on major issues on
materials engineering, failure investigation, and corrosion for clients.

Gordon Copper is a Senior Process Specialist with over 30 years of experience in the design,
operation and commissioning of metallurgical plants. He has extensive plant operation
experience in magnesium, copper, nickel, lead, zinc and precious metals, and has been
responsible for the process design and commissioning of a variety of smelting and refining
installations. His background includes a wide range of smelting methods as well as
hydrometallurgical and concentration processes. He has worked at Cominco (now Teck), Inco
(now Vale) and has been with SNC-Lavalin for the past 15 years.

Wilson Pascheto is currently the Manager of the Materials Technology Group of XPS Testing
and Consulting Services, a Glencore divison, located in Sudbury, Ontario. He holds a Bachelor
of Metallurgical Engineering from Mackenzie University in Brazil and a Master’s of Materials
Engineering from McMaster University in Hamilton, Ontario. Wilson has over twenty-five years
of plant and laboratory experience in the fields of corrosion, wear, welding, mechanical

vii
properties of materials, materials testing and selection, failure investigations, research and
development in the areas of metals, polymers, ceramics and composites. Wilson has been
directly involved in quality assurance activities for major capital projects in the mining industry,
such as Koniambo Nickel, Sudbury Smelter Calciner, Sudbury and Raglan Mill Expansions,
Kidd Creek Zinc leaching plant, Codelco Copper and CCR slime leaching. He trains company
engineers in QA/QC for capital projects as part of Design for Six Sigma. Wilson has performed
over 1,000 failure investigations ranging from small components to heavy industry machinery
from smelters, mines, concentrators, refineries and hydrometallurgical operations.

viii
Symposium Chairs

Chairman

A.M. Alfantazi, The University of British Columbia, Vancouver, Canada

Co-Chairmen

N. Benhood, Process Technology Materials Consultant Inc., Pierrefonds, Canada

W. Pascheto, Xstrata Process Support, Falconbridge, Canada
G. Cooper, SNC-Lavalin Inc., Montreal, Canada

ix
Table of Contents

Hydrometallurgy: Materials and Equipment

Foreword ......................................................................................................................................... v
Editors’ Biographies ..................................................................................................................... vii
Symposium Chairs ......................................................................................................................... ix

SOLVENT EXTRACTION, ELECTROWINNING AND RELATED TECHNOLOGIES

Large Phase Ratio Extraction and Enrichment of Rare Earth Ions by a Novel
Gas-assistant Column Extractor ...................................................................................................... 3
K. Huang, H. Liu

A Novel Mixer-settler-mixer Three Chamber Integrated Extractor for

Three-liquid-phase Extraction of Li, B and Mg from Salt-Lake Brines ......................................... 9
K. Huang, H. Liu

Optimization of the Usable Life of Lead Electrowinning Anodes ............................................... 17

A. Mirza, M. Burr, T. Ellis, E. Lombard, L. Webb,
F. Leclercq

Alternative Low-cost Composite Coated Anodes for Base Metal Electrowinning ...................... 33
M.J. Barmi, A.N. Nikoloski

LEACHING TECHNOLOGIES, EQUIPMENT AND DESIGN

Best Practices in Material Choice for Design and Construction of

Hydrometallurgical Equipment ..................................................................................................... 47
T. Johnson, J. Graham, D. Kelley

Incorporating Radiant Heat Exchange into Finite Element Model of

Hydrometallurgical Process Equipment ....................................................................................... 57
D. McMullen

Technical Risk Mitigation Through Rheometallurgical Generation of Process

and Equipment Design Criteria ..................................................................................................... 69
A. Mezei, M. Ashbury

A Study of Leaching of Copper Oxide Ore by Sulphuric Acid .................................................... 83

M. Clotilde Apua, M.B. Kime, M.P. Mubiayi

xi
Approach for Early Evaluation of Pressure Oxidation for a Refractory Gold
Ore Deposit ................................................................................................................................... 93
S. Singh, M. Eichhorn, K.S. Fraser

Capacity Enhancement at Newmont Mining Corporation’s Twin Creeks

Whole Ore Pressure Oxidation Facility ...................................................................................... 111
M. Eichhorn, T. Krumins, L. Zunti, F.C. Ruff

Mercury Removal From Pressure Oxidation Vent Gas at Newmont Mining

Corporation’s Twin Creeks Facility............................................................................................ 129
T. Krumins, C. Stunguris, L. Zunti, S. Blaskovich

Thermal Design of Refractory Lined Pressure Oxidation

Autoclaves................................................................................................................................... 145
I. Donohue, P. Lauzon, M. Pearson

Optimum Condition of Vanadium Recovery From Power Plant Fly-ash with

Considering Nickel Behavior During the Acidic Leaching Process Using
Orthogonal Array Design............................................................................................................ 157
E. Nazari, F. Rashchi, M. Saba

MATERIALS CORROSION IN HYDROMETALLURGICAL

APPLICATIONS

An Experimental Study on the Effect of Halides on the Corrosion of Aluminum .................... 167
C. Curtis, N. Gao, J. Alberto Gonzalez, D.Y.H. Liu

Corrosion Evaluation of Anodized and Unanodized Titanium for Application in

Pressure Leaching ....................................................................................................................... 179
J. Liu, A. Alfantazi, E. Asselin

The Combined Effect of Fluorides and Ferric Ions on the Uniform Corrosion of
Titanium and Titanium Alloys in Sulfuric Acid ......................................................................... 193
P. Laihonen, M. Lindgren

Corrosion Studies at Teck’s Hydrometallurgical Facility (CESL): Identification

of an Alloy Substitute for Titanium in Certain Applications...................................................... 203
J. Riha, R. Bruce, D. Schwartz

The Role of Thiosulfate on the Pitting Behavior of Stainless Steel 316 as a Material
of Construction in Near-neutral Solutions Containing Chloride Ions Relevant to
Gold Leaching ............................................................................................................................. 215
M. Roushanafshar, A. Alfantazi

xii
 POSTER

Developing Alternative Industrial Materials From Mining Waste ............................................. 233

J. Hernández A., J. Flores B., F. Patiño, C.N.Y. Trápala P., M. Pérez L.,
I. Rivera L., J.C. Juárez T., G. Juárez-López

Author Index ............................................................................................................................... 241

xiii
 83

A STUDY OF LEACHING OF COPPER OXIDE ORE BY SULPHURIC

ACID

M. Clotilde Apua 1, M.B. Kime2, Mukuna P. Mubiayi 3

1
Process, Energy, and Environmental Technology Station, Faculty of Engineering and the Built
Environment, University of Johannesburg, South Africa
2
Extraction Metallurgy, Faculty of Engineering and the Built Environment, University of
Johannesburg, South Africa
3
Mechanical Engineering Science, Faculty of Engineering and the Built Environment, University
of Johannesburg, South Africa

Keywords: Copper Oxide Ore, Leaching, Sulphuric Acid

Abstract

The Democratic Republic of Congo copper oxide ore containing mainly malachite was leached
in sulphuric acid. The effects of leaching time, pH, stirring speed, and temperature on the
dissolution rate were studied. The results show that recoveries of 98.17 % copper, 84.68 %
cobalt, and 37.99 % iron can be obtained using experimental optimal conditions of 1 h leaching
period at a temperature of 70 oC with a stirring speed of 500 rpm, at pH 1, H2SO4 concentration
of 75 g/L, and a solid to liquid ratio of 13 %.

Introduction

Copper is widely used in electrical materials, electronic, mechanical, architecture and military
industries. The demand of copper products in the world has been increased due to the progress in
science and technology and the development of economy [1, 2, 3]. Mainly two methods,
pyrometallurgical and hydrometallurgical, are used worldwide to process copper ore for metal
production. The first method is used for sulphide flotation concentrates, and it is economically
achievable for high grade copper ores and large-scale operations. Nevertheless, this process has
several disadvantages, including the production of hazardous gases and high energy consumption
[4].

At this time, sulphuric acid and ammonia solutions are generally mostly used to leach copper
minerals; hydrochloric acid medium is also used. Sulphuric acid lixiviant is currently used to
extract copper from a copper oxide ore of the Democratic Republic of Congo [5, 6]. Copper
oxide minerals such as malachite (Cu2(OH)2CO3), azurite (Cu3(OH)2(CO3)2), chrysocolla
(CuSiO3.2H2O), tenorite (CuO) are soluble in sulphuric acid. The typical dissolution reaction of
malachite with sulphuric acid can be given as follows [7]:

Cu2(OH)2CO3 + 2H2SO4 → 2CuSO4 + CO2 + 3H2O (1)

84 COM 2013 hosted by MS&T'13

The present study aimed to the optimization of the leaching of copper from the copper oxide ore
in sulphuric acid solution. While kept constant one of the variables, the effect of leaching period,
pH, stirring speed, and temperature were separately studied.

Experimental
Materials

The copper oxide ore used in this study was from Kamfundwa in the Democratic Republic of
Congo. The ground ore was first split using the spinning riffler to obtain a representative sample
that will be used for the leaching experiments. The particle size distribution (PSD) of the sample
was analyzed by a Microtrac S3500. The mineral phases of the ore were analyzed by a Rigaku
Ultima IV X-ray diffractometre (XRD). A Rigaku ZSX Primus II X-ray fluorescence was used
for the elemental composition of the ore. The mineral distribution in the residues was determined
by a Tescan 3XMU scanning electron microscope and X-ray energy dispersive spectrometer
(SEM / EDS).

Methods

Batch leaching tests were conducted in a 400 ml conical flask. A required amount of 75 g/L
sulphuric acid solution was used and 5 g of the ground copper oxide ore with a solid to liquid
ratio of 13%. Leaching parameters such as leaching time from 0.25 – 4 h, pH range 0.5 – 4,
stirring speed from 500 – 800 rpm, and temperature in the range of 23 – 70 oC were investigated
to obtain the optimal experimental conditions. After filtration, the pregnant leach solution (PLS)
samples were analysed by AAS for copper, cobalt, and iron. Specific leaching residues samples
were collected, washed with distilled water, dried, re-ground in a mortar prior SEM/EDS
analysis and the particle size distribution.

Results

Characterization of the Feed

The particle size distribution of the sample in Figure 1 shows that the ore sample has a P80
particle diameter of 62.23 µm.
 HYDROMETALLURGY: MATERIALS & EQUIPMENT 85

100
90
80
Passing (wt%) 70
60
50
40
30
20
10
0
0.01 0.1 1 10 100 1000 10000
Size (µm)

Figure 1. Curve of particle size distribution of the ore.

The main chemical analysis of the ore sample is presented in Table I. High copper content of
10.07% were found in the ore.
6000
Quartz

5000

4000
Intensity (cps)

3000
Malachite Quartz

2000
Malachite

Malachite
Quartz
Malachite
Malachite

Malachite
Malachite

Malachite
Malachite

Malachite

Quartz
Malachite

1000
Quartz

Quartz

Quartz
Quartz

0
0 20 40 60 80
2-theta (deg)

Figure 2. XRD pattern of the ore.

X-ray diffraction pattern in Figure 2 shows that copper is mainly in the form of malachite
mineral CuCO3(OH)2.
86 COM 2013 hosted by MS&T'13

Table I. Main Chemical Composition of the Ore

Component (%)
Cu Co Fe Si Mg Al Ca Mn
10.07 0.71 4.12 74.74 5.29 2.50 1.00 0.48

Leaching

Effect of Time: The effect of time on the leaching of copper oxide ore is shown in Figure 3. It
was mainly observed that the copper dissolution, like the leaching of cobalt and iron, is
completed within 1h. A maximum copper extraction of 92.89% was obtained after 1 h, whilst
cobalt and iron recoveries remained lower than 80%. Practically, 1 h of leaching period was
found to be optimum.

100
90
metal leaching (%)

80
70
60
50 Cu
40 Co
30 Fe
20
10
0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
time (h)

Figure 3. The effect of time on the leaching of copper from the copper oxide ore (acid
concentration, 75 g/L; temperature, RT; the amount of ore, 5 g; particle size, 80% − 62.23 µm;
S/L, 13%; stirring speed, 300 rpm; pH less than 0.35).

Effect of pH: The results in Fig. 4 show that copper recovery of more than 70% was reached at
pH 1 whilst maximum recoveries of more than 90% and more than 70% were obtained for cobalt
and iron, respectively. From pH 1, the leaching of metals (copper, cobalt, and iron) decreased as
the pH value increased. This can be justified by the limited quantity of H2SO4 reactant in
solution.
 HYDROMETALLURGY: MATERIALS & EQUIPMENT 87

100
90
80
70
metal leaching (%)
60
50 Cu
40 Co
30 Fe
20
10
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0
pH

Figure 4. The effect of pH on the leaching of copper from the copper oxide ore (acid
concentration, 75 g/L; the amount of ore, 5 g; particle size, 80% − 62.23 µm; S/L, 13%; leaching
period, 1 h; temperature, RT; stirring speed, 300 rpm).

Effect of Stirring Speed: The effect of stirring speed on the leaching of copper from copper oxide
ore shown in Figure 5 indicates that copper extraction is about 75.89 % when 500 rpm stirring
speed was applied. Cobalt and iron recoveries were 97.01 % and 26.98 %, respectively. With the
increase of stirring from 300 rpm to 500 rpm, the diffusion rate of ion in leaching solution
increase also and decrease for stirring speed greater than 500 rpm because of the formation of the
vortex.

Effect of Temperature: The results presented in Figure 6 show that the copper extraction
increased until the temperature was 70 oC, where 97.41% of copper was recovered. Cobalt and
iron recoveries were 98.08% and 74.06%, respectively. The optimum temperature was found to
be 70oC.

Leaching Under Optimal Experimental Conditions: Figure 7 shows that a copper recovery of
98.17 % was reached after 1 h leaching of copper oxide ore when using optimal conditions.
Cobalt recovery was 84.68 % whereas iron extraction was less than 40 %.
88 COM 2013 hosted by MS&T'13

100
90
80
metal leaching (%) 70
60
50 Cu
40 Co
30
20 Fe
10
0
200 300 400 500 600 700 800
stirring speed (rpm)

Figure 5. The effect of stirring speed on the leaching of copper from the copper oxide ore (acid
concentration, 75 g/L; the amount of ore, 5 g; particle size, 80% − 62.23 µm; S/L, 13%; leaching
time, 1 h; pH, 1; temperature, RT).

100
metal leaching (%)

80

60

Co
40
Cu
Fe
20
20 30 40 50 60 70 80
o
temperature ( C)

Figure 6. The effect of temperature on the leaching of copper from the copper oxide ore (acid
concentration, 75 g/L; the amount of ore, 5 g; particle size, 80% − 62.23 µm; S/L, 13%; leaching
time, 1 h; pH, 1; stirring speed, 500 rpm).
 HYDROMETALLURGY: MATERIALS & EQUIPMENT 89

100
90
80
metal leaching (%)
70
60
50
40
30 Cu
20 Co
10 Fe
0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
time (h)

Figure 7. Leaching of copper from the copper oxide ore under optimal experimental conditions
(acid concentration, 75 g/L; the amount of ore, 5 g; particle size, 80% − 62.23 µm; S/L, 13%;
leaching time up to 4 h; pH, 1; stirring speed, 500 rpm; temperature, 70 oC).

SEM / EDS Analysis of the Residues

A sequence of dissolution experiments on ore sample using optimal experimental conditions

were carried out for leaching time ranging from15 min to 4 h and the SEM / EDS of the residues
were analyzed. Figure 8 shows that the silicon (46.04 %) and iron (2.58 %) contents were all
very high whereas copper (0.10 %) and cobalt (0.05 %) content were very low in the residues of
the ore sample, indicating that the majority of copper and cobalt dissolved when the ore samples
were leached with 75g/L sulphuric acid at 70 °C. Figure 8 shows that the silicon and oxygen
content was very high indicating that silicon was the main constituent of the residues.
90 COM 2013 hosted by MS&T'13

Cu, Co, Fe, Si, O

Cu, Co, Fe, Si, O

Cu, Co, Fe,

F Si, O

Figure 8.
8 SEM of th
he residue (frrom the leaching under optimal
o expeerimental conditions withh 1h
leacching time).

D
Discussion

The increease of time on the leachhing of coppper oxide oree produced an

a increase in
i the leaching of
copper, cobalt,
c and iron. Howevver a maximuum copper recovery
r wass observed after
a 1 h leacching
time.

pH 1 waas found to increase

i the recovery off copper in sulphuric
s accid. However, the increaase in
pH valuee decreased the copper recovery.
r Thhis indicatess the dependdence of leacching on thee acid
concentraation. The acid
a concenttration is higgh at pH 1 than
t at pH greater
g than 1. In a studdy by
Ntengwee [8] and Jan ndova et al. [9],
[ the coppper leaching was w found most
m efficiennt at pH < 2.00 at a
particularr leaching teemperature. This agrees well with thhe findings of
o this studyy. As can be seen,
maximum m copper reccoveries werre obtained after
a 1 h leacching time.

Agitationn keeps uniiform level of the conncentration of copper and therefoore increasess the
exposuree of particlees to sulphuuric acid. Coontinuous sttirring speedd was foundd to increase the
extractionn of copperr however inncreasing sppeed decreassed it [10]. This is whaat resulted inn the
increase of copper reecovery usinng sulphuric acid. In the study by CA AO Zhan-fanng et al. [11], the
leaching efficiency was
w found too increase with
w stirring speed of 5000 rpm. Thiss is in agreeement
with the findings of this
t work.

From thee study on th he effect of temperaturee on leachingg of copper oxide ore produced
p possitive
results. For
F different temperaturees, the generral trend wass that the reccovery of coopper, cobaltt, and
iron fromm the solid orre was increasing with thhe increase in
i temperatuure.
 HYDROMETALLURGY: MATERIALS & EQUIPMENT 91

Conclusion

Copper maximum recovery was obtained after 1 h leaching time. pH 1 was favorable for the
leaching of copper oxide ore than high pH values (pH greater than 1). The leaching of copper
oxide ore was favored at stirring speed of 500 rpm than higher values. The increase in
temperature produced an increase in the copper, cobalt, and iron recoveries. Under the optimal
leaching conditions, the copper, cobalt, and iron recoveries were 98.17%, 84.68%, and 37.99%,
respectively. Using sulphuric acid concentration of 75 g/L, S/L of 13%, and particle size of 80%
− 62.23 µm; in this study the following optimum leaching conditions were determined:
dissolution time, 1 h; pH, 1.0; stirring speed, 500 rpm; temperature, 70 oC.

Acknowledgements

The authors would like to acknowledge the financial support from the Technology Innovation
Agency.
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