International Laterite Nickel Symposium - 2004 k e s s Develo~mEdited by W.P. Imrie. D.M. Lane. S.C.C. Baniett. R.M. Berezowsb, E.J.M.

Jahnsen. P.G. Mason.

J.A. Murray, R.C. Osborne. J.G. Reid. J.G. Schofield. L.E. Seeley, I.G. Skipper and Y.M. Torres
TMS (The Minerals, Metals & Materials Sociew), 2004

A COMPLETE APPROACH TO FLOWSHEET DEVELOPMENT NIQUEL DO VERMELHO (CVRD) CASE STUDY

Mike

dams'; Dwight van der ~ e u l e n ' John

;
~n~ove'

'SGS Lakefield Oretest, 43 1 Victoria Rd, Malaga, Western Australia 6090 Australia
Keywords: Flowsheet, CVRD, Nickel, Piloting, Pressure, Leach, Refining.
Abstract

A comprehensive pre-feasibility study has been conducted by Companhia Vale do Rio Doce
(CVRD) for Niquel do Vermelho nickel laterite deposit. Within this study, five integrated
flowsheet options were evaluated via batch and pilot campaigns at Lakefield Oretest, over an
intensive six-month period from receipt of ore to final reporting. Key technical objectives set by
the client included demonstrating the technical viability of the beneficiation of several ore
types, processing through integrated pressure acid leachlmixed hydroxide precipitation
(PALIMI-IP) and mixed sulfide precipitation (PALIMSP) circuits, and the treatment of barren
liquors to meet stringent environmental requirements. Refining of the MHP was by ammonia
re-leach and solvent extraction (SX) to produce LME-grade nickel cathodes, NiCO,, NiO and
CoS. LME grade nickel and cobalt was also produced by oxidation of the MSP and hydrogen
reduction on the leachate. The database and data acquisition system, along with web-based
reporting, enabled rapid turnaround on both daily and more comprehensive run reports, making
it possible for speedy and confident decisions on operating conditions of the complex
flowsheets. The high value of developing such data is emphasized and discussed as pivotal in
the successful progression of laterite projects through to sustainable commercial viability.
Introduction

Development of metallurgical flowsheets for the recovery of metal values from ores has often
been a lengthy process. Moreover, if the testwork program has been inadequately planned, there
is a risk that inappropriate strategic decisions may be made to meet tight schedule deadlines.
SGS Lakefield Oretest has developed a sound basis to assist resource companies during their
flowsheet development. Integration of process flowsheet definition, batch and pilot testwork
with state-of-the-art facilities and modem data acquisition and reporting systems, ensures the
rapid delivery of tested process flowsheet appropriate for the ore. This paper presents a case
study covering a testwork program designed for such an approach.
Lakefield Oretest was commissioned by CVRD to conduct a comprehensive piloting campaign
to study the different hydrometallurgical routes associated with processing Niquel do Vermelho
nickel laterite ore through beneficiation, pressure acid leaching, and subsequent production of a
mixed hydroxide intermediate product (MI-IP), and a mixed sulphide intermediate product
(MSP). Both intermediate products were further processed through different downstream
refining routes to produce nickel cathode, cobalt sulphide, nickel carbonate, nickel oxide, as
well as nickel and cobalt powders, all as finished products.
Five flowsheets were devised by CVRD, covering both key routes (MHP and MSP). The prime
objective of the program was to demonstrate the technical viability of the PALNHP and
161

PALlMSP process routes on Niquel do Vermelho laterite ores, for producing a range of final
and intermediate products.
The program covered a six-month schedule, from receipt of the ore to issue of the final report.
This included flowsheet definition, batch testwork for definition of process conditions, pilot
testwork and comprehensive ongoing reporting throughout the campaign. The schedule is
summarized in Table I.
Table I. CVRD Program Schedule
Duration or Tonnage

Item
Batch testwork
Beneficiation Runs
PALlMHP Run 1
PALlMHP Run 2
PALlMSP Run
SXIEW Run
Final Report

Date
Nov 2002 -May 2003
Nov 2002
Dec 2002
Jan 2003
Mar 2003
Mar 2003
May 2003

4 x lot
7 days
7 days
7 days
7 days

Process Flowsheet Definition

The testwork program to be evaluated in the pre-feasibility study was initially prepared by
CVRD, and was designed to cover proven industrial-scale options for processing of nickel
laterites through acid leaching. Atter the contract was awarded and prior to commencement of
the campaign, a series of discussions was held with the client. A detailed proposal covering all
aspects of the program, discussed below in more detail, was developed with the client's
requirements and Oretest experience.
A schematic process flowsheet diagram for the campaign is given in Figure 1 .

Beneficlation

R1
R2
R3
R4

Blend
ore1
Ore 2
Ore 3

R l PAUMHP
R2 P A U M H P l

*m
productlon

Steam strip

NH strip

Acid strip

)-

Batch H- redn

NiCO ppbr

calcination

Figure I. Schematic process flowsheet diagram for the campaign

Drill core samples were received and blended into four representative ore types comprising
three different silica grades and a blend. Batch testwork to define the conditions preceded pilot

beneficiation testwork to determine beneficiation response and produce thickened products with
grade and size suitable for feed to the autoclave.
Batch hydrometallurgical testwork was conducted on representative sub-samples of the various
feeds to define conditions for PALMHP Run I in the pilot plant. This was a run to confirm the
operating conditions, to fill the circuit and to produce sufficient PAL discharge for batch
testwork on the downstream unit operations. This testwork was completed while ensuring
sufficient time to implement changes and improvements in process design and determine
conditions from the batch work on actual PAL discharge sample for the integrated PALMHP
Run 2, and PALIMSP Run 3. [ntermediate MI-IP and MSP products were further processed by
continuous and batch testing, to produce the range of final products.
Batch Testwork - Process Development

Batch Beneficiation
A series of scrubbing and attritioning tests were carried out to define the process flowsheet and
required piloting conditions. Several samples were wet screened and shipped to CVRD for
successful comparison of methodologies, enabling correlations with earlier batch testwork
conducted at CVRD. Spiral testwork successfully produced a chromite concentrate while the
use of a Kelsey jig for this duty proved less effective.
Settling. Rheologv and Flocculant Screening
Settling and rheology tests were conducted on autoclave feed samples and revealed no
significant slurry handling issues. A selection of flocculants were successfully compared using
2 m column settling tests to assist in the choice and dosage of an appropriate reagent.
Batch Pressure Acid Leach
~ e v e i a batch
l
PAL tests were conducted using a 4.5 L autoclave, to define the leach conditions
for piloting, which specifically included acid addition levels and expected retention times.
MHP Process Route Definition
Batch testwork was conducted on the major downstream unit operations for the MI-IP circuit to
hclp define process flowsheet and conditions for piloting. This work included primary
neutralisation, iron removal, MI-IP, ammonia re-leach, partial steam strip, SX, NiC03
precipitation and calcination, and excess barren liquor neutralisation.
MSP Process Route Definition and Seed Production
Batch testwork was conducted on the major downstream unit operations for the MSP circuit to
help define process flowsheet and conditions for piloting. This work included pre-reduction,
neutralisation, MSP, pressure oxidation (POX), impurity removal, SX (Cyanex 272), hydrogen
reduction, and excess barren liquor neutralisation. A CVRD mixed sulphide precipitation seed
to initiate MSP production in the MSP pilot-plant, was initiated using a 20L batch autoclave.

Pilot Testwork
Beneficiation Piloting
Three runs with -10 tonnes of each of HighIMidlLow Silica samples were conducted after a
preliminary run on a blend of all three ore types. Overall mass accountability was 100.0 k 1.5%.
The Niquel do Vermelho samples represent a deposit with good nickel grades and impurity
levels. Rejection of silica and significant nickel upgrading using conventional scrubbing, size
separation and attritioning were demonstrated. A series of conceptual mass balances for a fullscale plant were carried out at several product particle sizes. Results are reported elsewhere [I].
A schematic process flowsheet diagram for the beneficiation pilot plant is given in Figure 2.

Recycle process water

Scrubbing

I .'-Screening

Scrubbing

+6 rnrn +0.5 rnrn

rejects rejects

product

rejects

Figure 2. Process flowsheet diagram for beneficiation

Hvdrometalluraical Piloting to MHP and MSP Intermediate Products
Three separate continuous pressure acid leach runs, each demonstrating the amenability of
blended, beneficiated Niquel do Vermelho ores to pressure sulphuric acid leaching (PAL), were
successfully piloted. Pressure acid leaching of nickel laterite ores is well establishcd at the
commercial scale, minimising project risks associated with this established technology.
Excellent extractions for both Ni and Co were consistently achieved. The consumption of acid
was relatively low as compared to the broad range of other nickel laterite operations.
A schematic process flowsheet diagram for the hydrometallurgical piloting to MHP and MSP
intermediates is given in Figure 3.
Two piloting runs to produce a mixed hydroxide intermediate product were successfully
completed. Re-leaching of the residue from the iron removal stage and secondary hydroxide
precipitation circuits, in the second of these runs, was also demonstrated.
The two piloting runs produced a combined mixed hydroxide intermediate precipitate product
of good quality.

(a) MHP Route

rra
ld

Resldw
R.*.ch

Pmmmum Crld
U.rh

mmy
N.uhall.atlon

I1
o-.o.

--.
YHP
I-*

---

"-

0I.O.w-

+Fin. P

Idllm.

7-m.

(b) MSPRoutr
IW(S

CCD

A
S ~ C C
WPnWa.

"W

St-

1" p.
mb

PAUPWN

!7ryCf

U n m

E-.

U'

Removal

mmn

u w

S-d

0,-

Pllrmlb

0,-

Runoval

~m~unt-.n

RVd.

v
-RnbPr&cl

Tallln~.

lo r d m

l o Id-

Figure 3. Process flowsheets for hydrometallurgical piloting to (a) MHP and (b) MSP
intermediates.
Excess barren liquor bled from the manganese removal circuit as CCD wash water was treated
successfully to produce a relatively pure effluent for potential disposal to the environment.
Impurities in the treated barren liquor from the MHP circuit bleed were well below the
maximum allowable levels provided by CVRD for liquid emuent discharge.
A mixed sulphide precipitation run, decoupled from the pressure acid leach (PAL) run after the
neutralisation stage for safety reasons, was also successfully piloted. Subsequent processing of

the reduced and neutralised pregnant liquor solutions occurred in a mixed-sulphide precipitation
plant using hydrogen sulphide gas. This run successfully demonstrated continuous autoclave
precipitation of mixed sulphides with Ni recoveries greater than 99 %and with total rejection of
Mn and Mg impurities. A good quality mixed sulphide intermediate product was produced.
Excess barren liquor bled from the mixed sulphide barren liquor circuit, was further neutralised
to remove iron and produce a relatively pure effluent for potential disposal to the environment.
The treated barren liquor from the MSP circuit contained impurities well below the maximum
allowable levels provided by CVRD for liquid eMuent discharge.
Ammonia Re-leach and Partial Steam S t r i ~Piloting
A series of bulk batch ammonia re-leach runs was completed, leaching mixed hydroxide
product from the two MHP piloting runs. The leachate produced was of good quality.
Solvent Extraction and Electrowinninrr (SXEW) Piloting
Two separate solvent extraction continuous piloting runs were completed, demonstrating the
technical viability of recovering nickel from the partial steam strip liquor using LIX 841. One
run used an acid strip, the product from which was stored for a separate electrowinning trial.
Several LME-grade cathodes (assaying > 99.99 % Ni) one-tenth of full-scale were produced.
The second run used an ammonium carbonate strip, the product o f which was stored for the
separate production of a nickel carbonate precipitate. The nickel carbonate was subsequently
calcined to produce nickel oxide assaying > 99.5 % NiO.

Batch Testwork - Product Treatment

MHP Product Treatment
The SX pilot-scale testwork on the MHP product produced a pure, high concentration NiS04
electrolyte for EW and nickel ammonium carbonate pregnant liquor. The latter was treated in
further testwork to produce NiO.
MSP Product Treatment
The pilot-scale MSP testwork produced an intermediate mixed sulfide precipitate product,
which was treated in further testwork as follows:
POX leaching to dissolve the MSP.
Impurity removal of Fe, Cu and Zn by precipitation, cementation and SX.
SX batch testwork to produce separate NiS04 and C0S04 pregnant liquors.
H2 reduction of NiS04 to Ni metal powder.
H2 reduction of CoS04 to Co metal powder.

Reporting
Data capture, collation, interpretation and reporting is a crucial activity for an integrated pilot
plant campaign of this size. SGS Lakefield Oretest places great emphasis on this aspect of
piloting, with a data metallurgist team appointed for this area of the program in addition to the
plant operating teams. This approach enables the operating metallurgists to focus on

metallurgical issues based on sound mass balance and concentration and operating profile data.
Likewise, the data metallurgy team can focus on resolving any sample preparation, assaying
and mass-balancing issues without also having to be concerned about operating the plant.

During the piloting campaign, and specifically during the plant operating periods, the data
metallurgists processed all data via databases and spreadsheets so as to build up information
progressively towards the final report. This allowed daily metallurgical and control reports to
be presented in a timely manner based on control assay information representing live plant
conditions with only a few hours lag for sample preparation, assay and data processing. The
data included metallurgical recoveries, operating temperatures, pressures, flows and solution
chemistry, as well as any operating, safety and environmental issues. This provided good
quality key process measurements from which informed decisions were made in time to have a
visible impact on plant performance before the run had finished.
All data was presented in various forms, ranging from Distributive Control System (DCS),
logsheets, raw assays, daily metallurgical and control reports through to trending, campaign
summaries and overall elemental balances and accountabilities:
8

Daily Reporting covering the previous 24 hours of operations, trends and metallurgy.
Weekly Reporting of project management issues.
Comprehensive Run Data Pack within I0 days of run completion.
Final Report, comprising I l volumes.

This approach ensured speedy and confident set point decisions on the various unit operations
in the pilot-plant flowsheets. The quality of the data is enhanced as it is less prone to error by
having a dedicated data team processing it.
The final campaign report was completed about six months from receipt of ore, ensuring a
sound basis for the engineering study.
Data Acquisition Systems
The pilot-plant database was set up at Lakefield Oretest to ensure effective acquisition and
control of data. The diagram in Figure 4 outlines the components of the system. The central
component is the Structured Query Language (SQL) Server database, and both Microsoft (MS)
Access and Microsoft (MS) Excel were used to extract or input data from the central database.
The ability to query the database and instantly plot trends presented the operating metallurgists
with a powerful tool to ensure fine control on the various processes.
Client Access Website
Provision of a secure Client Access Website enabled the rapid communication of key data,
photographs, daily and weekly reports in an easily downloadable form to virtually anywhere in
the world. This meant that client personnel and consultants could at all times take part in the
decision-making process, regardless of other commitments or location.

HiPAL Database
Data Components

Figure 4. Data Acquisition System Components

Campaign Outcomes
Technical Outcomes
Following upfront process flowsheet definition covering the five process options, technical
success was achieved on all process routes piloted. High nickel and cobalt leach recoveries
were achieved, as well as plant and process availabilities in excess of 99 %. Overall
accountabilities for PALIMHP Run 2, as an example, were 101.9 YOfor Ni and 99.0 % for Co.
Autoclave plant stability over a representative seven-day run is illustrated in Figure 5. Plant
stability achieved can be also seen as a clear indication of the amenability of the ore to HPAL
processing. Relatively low pulp viscosity and minimum scale formation or solids accretion
resulted in no process related blockages or instability.
Management Outcomes
The operation integrated both occupational health and safety and environmental management
systems, with excellent records for the period. During the course of the 6-month program some
200,000 assays were carried out on about 15,000 samples, the majority of which were sampled,
assayed and reported within the four seven-day piloting runs.
Comprehensive run data pack reports were released within 10 days of mn completion, including
mass balance, profiles, trends, interpretive comments and recommendations. A final report of
around 5,000 pages was released within 30 days of the final operation.
Program Outcomes
High plant availabilities meant that more information was generated during the testwork
program for CVRD. Tight schedules were met for the entire campaign, including batch, pilot
and reporting aspects. This made for rapid daily and run reporting for effective decisionmaking.

Figure 5. Autoclave control data for a representative 7-day run.

Conclusions

The technical, management and program successes of the campaign ensured the rapid
availability of meaninghl data and other information for use in the pre-feasibility study.
This case study has illustrated the benefits of a complete approach to comprehensive flowsheet
development, envisaged by CVRD since the early stages of the Niquel do Vermelho project.
Lakefield Oretest was able to provide all piloting and bench scale tests required for testing with
high quality procedures, data analysis and results presentation. These benefits are significant,
and provide a sound basis for decision making during the course of developing a resource
project.
Acknowledgements

This paper is published with the permission of CVRD. The success of the campaign was due in
no short measure to the excellent technical and operational expertise of the 71 team members,
as well as 6 clicnt personnel, every one of whom played an invaluable role in achieving the
outcomes of the program. In addition, 13 vendors and consultants were involved to augment
various aspects of the program.
References

Vanessa M. Torres. 'Wiquel do Vermelho Project - Metallurgical Update," ALTA 2003

I.
Nickel/Cobalt-9 Technical Proceedings (Castlemaine, VIC, ALTA Metallurgical Services,
2003), 12 pp.