Pure Energy Minerals Limited (TSX-V:PE) (FRANKFURT:A111EG) (OTCQB:
PEMIF) (the “Company” or “Pure Energy”) is very pleased to announce
the initial results from Pure Energy’s recently completed
innovative mini-pilot test work. The mini-pilot campaign was
successful on all counts and demonstrated efficient recovery of at
least 85% of the lithium from the tested brine. The mini pilot
trial also produced battery-grade lithium hydroxide monohydrate.
The Company sees this milestone as an important proof-of-concept
for modern, efficient and environmentally sustainable lithium brine
processing techniques without the use of evaporation ponds. The
newly developed flowsheet will be a foundation of Pure Energy’s
forthcoming Preliminary Economic Assessment (PEA), and it will
constitute a key building block for a larger scale continuous pilot
plant. A summary of the main findings is shown below, and greater
detail will be provided in the forthcoming PEA.
Summary of Testing Performed and Results
The testing work performed by Pure Energy and its technology
providers Tenova Bateman Technologies (TBT) and SGS Canada
evaluated a four-stage process:
- Pre-Treatment ⟹removal of divalent ions including alkaline
earth elements by membranes (LiP™) and chemical precipitation;
- Solvent Extraction (LiSX™) ⟹ preferential extraction and
concentration of lithium from the pre-treated brine to make a high
purity lithium sulphate solution;
- Electrolysis (LiEL™) ⟹ conversion of high-purity lithium
sulphate solution into high purity lithium hydroxide solution;
and,
- Crystallization ⟹ evaporation, crystallization and
centrifuge separation of battery-grade lithium hydroxide
crystals.
Important Findings from Mini Pilot Plant
Test
One of the most important work products of the mini pilot plant
is a preliminary process flowsheet, a simplified version of which
is shown below as Figure 1. The test work also supports several key
performance indicators that warrant continued development and
scale-up of the TBT Process for commercial scale lithium production
at the Clayton Valley South Project (“CVS Project”):
- Achieved overall lithium recovery of >85% from the tested
brine;
- Successfully removed the major interfering elements from the
solvent extraction (SX) feed brine: calcium (Ca), magnesium (Mg),
and strontium (Sr);
- Achieved near 100% extraction of lithium by LiSX™;
- Achieved high lithium concentration factors, approximately 38x,
during the LiSX™ stage;
- Crystallized battery-grade lithium hydroxide monohydrate with a
high quality distribution of grain size and morphology; and
- Identified several areas in the process that are ripe for
improvement and optimization of costs and efficiencies in a future
scaled-up operation.
To view Figure 1, please visit:
http://orders.newsfilecorp.com/files/4131/24048_figure1.jpg
Figure 1
– Schematic Summary of Preliminary Flowsheet for Treatment
of CVS Lithium Brine
Patrick Highsmith, Pure Energy Minerals CEO commented, “The TBT
and Pure Energy technical team has done some extraordinary work in
this mini-pilot plant. Not only is this a proof-of-concept for the
use of TBT’s new technology in lithium production, but the team
collaborated and optimized the process on-the-fly. The flowsheet
you see here is a significant improvement upon our projections from
the bench scale tests, and we believe there is a great opportunity
for economic application of this technology to commercial scale
production. The preliminary estimates of lithium recovery by our
process are at least a 70% improvement over the typical 50%
recovery experienced by traditional evaporation. The current
resource drilling that is underway at the CVS Project and the
subsequent update to our mineral resource are the last precursor
steps to our PEA. We look forward to more fully describing the
project and its economics during Q1 of 2017.”
Pre-Treatment
The pre-treatment of the CVS brine to remove key interferents
(particularly Ca and Mg) is a prerequisite if selective solvent
extraction of lithium is to be used. The CVS lithium brine is an
ideal candidate for the direct use of modern membrane technology as
it has relatively low concentrations of Ca and Mg (compared to
other brine deposits globally), and is not saturated with other
solutes that may cause problems with membranes (e.g. gypsum). In
order to test the use of membranes for pre-treating the brine ahead
of solvent extraction, TBT tested a synthetic brine with the same
composition as brine recovered during bulk sampling from
exploration well CV-1 (from the CVS Project). They tested an array
of commercially available membranes from several suppliers to
determine whether the main interferents (Ca, Mg and Sr) could be
effectively reduced to acceptable levels. The first part of the
test work consisted of screening 8 different membranes in a
flat-sheet configuration at an operating pressure of 60 bar, and
evaluating how the various membranes transmitted lithium whilst
rejecting alkaline earth elements. Following completion of the
flat-sheet testing, TBT selected a single membrane based on its
superior relative performance and proceeded with testing it in a
spiral-wound module test rig, again at 60 bar.
The recently completed test work demonstrated that even in a
relatively simple, ‘single-pass’ arrangement (i.e. brine being
passed once through a single set of membranes), approximately
85-90% of the lithium is recovered, while at the same time,
approximately 91% of Mg, 90% of Ca and >99% of Sr are rejected.
These data are extremely encouraging and validate the use of modern
membrane technology to pre-treat CVS brines. Additional test work
is ongoing to further refine and optimize the use of membranes
prior to continuous testing in a full pilot plant configuration,
including evaluation of variable pressure across the membranes and
the use of anti-scalants in the process. The next stages of work
are being completed by TBT and their partner, GE Water &
Process Technologies.
In a parallel phase of pre-treatment test work (performed by SGS
Canada), the lab treated CVS brine (actual raw brine sample from
CV-1) with additions of caustic soda (NaOH) and soda-ash (Na2CO3)
to determine whether direct chemical precipitation could be used to
remove divalent contaminants. This work successfully demonstrated
that >99% of Ca, Mg and Sr could be removed through careful pH
control with negligible loss of lithium through co-precipitation.
Subsequent work was completed using a High Density Sludge (HDS)
circuit that allowed semi-continuous operation over 3 ½ days to
investigate whether the solids produced by the direct chemical
precipitation could be aggregated and thickened (using a
flocculant), and then removed from the brine flow. This phase of
work also showed excellent results, and resulted in a steady-state
process that produced brines with Ca levels reduced to 2 mg/L, and
Mg and Sr both <1 mg/L, also confirming very low lithium
losses. While it is unlikely that direct chemical
precipitation would be used in isolation to remove divalent
impurities from the CVS brine (owing to relatively high reagent
costs), it is likely that some form of this unit operation will be
used after the membrane step to polish the permeate and raise its
pH to target levels prior to feeding the lithium solvent extraction
circuit.
Solvent Extraction
The primary aim of the solvent extraction (LiSX™) part of the
process, which forms the core of TBT’s and Pure Energy’s modern
approach to the CVS brines, is to selectively extract lithium from
the pre-treated brine and at the same time, effectively concentrate
the lithium into the high purity stream exiting the SX stage. This
solvent extraction step is composed of three parts: (1)
introduction of the pre-treated brine to fresh barren solvent; (2)
scrubbing the loaded solvent with a weak acid solution to clean the
solvent of any low concentrations of co-extracted cations; and (3)
stripping the lithium from the clean, purified solvent to produce a
high purity lithium sulphate solution and generate a clean unloaded
solvent that can be recycled back to the start of the SX loop.
All of the SX test work was completed by TBT at their test
facility in Katzrin, Israel, and was performed in a mixture of 40
mm and 100 mm diameter, 7 m tall Bateman Pulsed Columns. The
initial work looked at optimizing the extraction of Li into TBT’s
proprietary solvent by adjusting the pH of the brine entering the
column, and adjusting the ratio of solvent to brine contact in the
pulsed column. The tests demonstrated that optimal mass transfer of
lithium from brine into solvent was achieved by adding 1.35 g/L of
NaOH (on dry basis) to the input brine, and with the extraction
column working in an ‘organic continuous’ mode i.e. discrete
droplets of brine pulsing down through a continuous solvent matrix.
Operation under these conditions resulted in theoretical maximum
extraction of Li into the solvent (Li concentration of 1,750 mg/L
in the solvent), plus a raffinate (the ‘waste’ brine) containing Li
at concentrations below the available method detection limits
(<3 mg/L); hence lithium was concentrated by a factor of 9
during the initial extraction process.
Scrubbing of the loaded solvent was tested using a weak acid
solution (0.6% H2SO4) in an ‘aqueous continuous’ mode (discrete
droplets of loaded solvent pulsing upwards through a continuous
matrix of aqueous scrub solution). The resulting scrubbed solvent
contained effectively only lithium, with all other potential
contaminants (Na, K, B etc.) present at concentrations below method
detection levels (<3 mg/L).
The loaded and scrubbed solvent was stripped of its lithium
using sulphuric acid in ‘aqueous continuous’ mode. The acidic strip
solution is the spent electrolyte generated during the subsequent
electrolytic stage (see below), and therefore requires little or no
additional reagents. Following stripping, a lithium sulphate
solution is formed with effectively-neutral pH (7.7) and at a
concentration close to saturation. At the end of the three-step
LiSX™ process, the SX product going into electrolysis had a purity
greater than 99.9%, and had concentrated Li by a factor of
approximately 38 times. Lithium measured in residual solutions
throughout the SX circuit was below detection levels, indicating
that Li conservation through this stage approached 100%.
Electrolysis
The electrolysis stage (LiEL™)of the process is designed to
convert a high purity lithium sulphate solution into a high purity
lithium hydroxide solution. The reason for doing this is partly
based on Pure Energy’s strategic view on demand vs. supply dynamics
for lithium hydroxide monohydrate in the coming decades, and also
on Pure Energy’s conditional supply contract with Tesla, which
envisages delivery of battery-grade lithium hydroxide monohydrate
to supply the Gigafactory.
The electrolysis testing work was completed by a sub-contractor
to TBT, and was performed using TBT’s novel two compartment
electrochemical cell process (see Figure 2 below). The first phase
of the testing evaluated potential membranes suitable for a mixed
sulphate/hydroxide environment, and a very specialized candidate
membrane was shown to exhibit superior performance. The selected
membrane was formulated to limit hydroxide transport, while still
allowing lithium to migrate through it. The second phase of testing
looked at optimizing current efficiency in the cell while varying
the concentration of lithium hydroxide in the catholyte. The
results from this stage of the test revealed that the optimal
current efficiency of 80% was reached in the cell with a solution
of 3-3.5M lithium hydroxide concentration. Above these
concentrations, the current efficiency started to drop to
unsatisfactory levels. The team also determined that constant
operating temperatures in the cell of approximately 60°C resulted
in the best efficiencies (note that the cell was effectively
self-heating due to the currents used during electrolysis and the
internal resistance). After testing in the cell in batch and
continuous modes, TBT found that steady state operation could be
readily achieved, producing 3M LiOH solution at the cathode, and
the required sulphuric acid solution, suitable for recycling back
to act as the stripping agent for the SX phase.
To view Figure 2, please visit:
http://orders.newsfilecorp.com/files/4131/24048_figure2-resize.jpg
Figure 2 - Conceptual Diagram of
Electrochemical Cell Used during Testing
An intermediate purification step between the SX stripping and
the electrolysis was also contemplated during the mini-pilot
testing work. The team recognized that ion exchange (IX) may be
required to remove any divalent and monovalent
cations that are collected and concentrated by the solvent
exchange process. While the concentrations of these
contaminants are not expected to be high, appropriate test work has
been performed in a dedicated testing facility in Plainfield, IL,
to evaluate IX as a means of purifying the SX strip solution should
it be required. To test the feasibility of this interim step, a
synthetic solution was prepared and several types of resins were
evaluated. The results demonstrated that the effluent from the SX
step, treated with a specific IX resin, meets or exceeds the
purity specifications for the electrolysis step. These
initial performances are promising, and suggest that if the
full-scale pilot plant is run with natural brine from the CVS
Project, it will be feasible to include an IX step to ensure that
the lithium sulphate solution entering the electrochemical cell
will be of the highest purity.
Evaporation and Crystallization
The final stage of the process was to concentrate the 3M lithium
hydroxide solution produced by the electrolytic step using
evaporation until it reached saturation, producing Lithium
Hydroxide Monohydrate crystals from the solution. The crystals were
separated and washed using a centrifuge process and then dried in
an inert atmosphere to avoid carbonation. This test work was
performed by a sub-contractor to TBT at a dedicated testing
facility in Plainfield, IL. The crystallization test work commenced
with a synthetic lithium hydroxide solution having an inferior
composition to that produced by the electrolysis test work. The
work was conducted at bench scale, and high quality Lithium
Hydroxide Monohydrate, complying with battery-grade criteria
(crystal shape, particle size and purity) was produced.
Total Lithium Recovery
The process is designed such that the potential for significant
lithium loss from the system is limited to the first half of the
circuit. The likely areas for any potential minor lithium losses
are: in the pre-treatment stage, where a portion of the brine is
rejected by membranes for discharge back to the basin, or by
entrainment with calcium carbonate and magnesium hydroxide during
the polishing step. The process is designed to capture most streams
for recycling back into the process. After the first stage of SX
extraction, all bleeds and washes of solutions from the process are
looped back into the process at various points, and hence, will not
result in any lithium loss from the system. Test work completed
during this mini-pilot program has demonstrated that the only real
loss of lithium from the process is caused by the efficiency of the
membrane at the pre-treatment stage (LiP™). As such, the flowsheet
described above can be expected to recover 85-90% of the lithium
from the raw feed brine. It is possible that recovery can be
improved and such possibility will be investigated during operation
of a full pilot plant. Notwithstanding possible future increases in
efficiency, recovery of 85-90% of the lithium is extremely
encouraging given oft-quoted industry figures of maximum 40-60%
efficiency at all lithium brine plants operating today.
Dr. Ron Molnar, Professional Metallurgical Engineer (Ontario
P.E.# 100111288), is a qualified person as defined by NI 43-101,
and has reviewed and approved the scientific and technical
information that forms the basis for this news release. Dr.
Molnar is independent of the Company.About Pure Energy
Minerals Ltd.
Pure Energy is a lithium resource developer that is driven to
become a low-cost supplier for the burgeoning lithium battery
industry. While the Company is currently focused on the
development of the CVS Lithium Brine Project and the adjoining
Glory Lithium Clay Project in Clayton Valley, Nevada, it is
actively evaluating new lithium targets in North and South
America.
Pure Energy has developed core strengths in innovative
development and processing technologies for lithium brines and
lithium mineral deposits. The Company’s key attributes and
activities include:
- Generating positive results on a large land position with
excellent infrastructure in a first-class mining jurisdiction:
approx. 11,000 acres in four main claim groups in Clayton Valley,
Esmeralda County, Nevada;
- The only lithium brine resource in North America except for its
neighbor, which is the only producing lithium operation in the
United States (Albemarle’s Silver Peak lithium brine mine);
- An inferred mineral resource containing approximately 816,000
metric tonnes of Lithium Carbonate Equivalent (LCE) at an average
grade of approximately 102 mg/L lithium, reported in accordance
with NI 43-101 (see July 2015 Inferred Resource Report);
- An advanced program of testing the efficacy and economics of
modern environmentally-responsible processing technologies to
convert the CVS brines into high purity lithium products for new
energy storage uses; and,
- An active business development program, applying its expertise
to the evaluation of new lithium targets around the world.
On behalf of the Board of Directors, “Patrick Highsmith” Chief
Executive Officer
Forward Looking Statements: The information in this news release
contains forward looking statements that are subject to a number of
known and unknown risks, uncertainties and other factors that may
cause actual results to differ materially from those anticipated in
our forward looking statements. Factors that could cause such
differences include: changes in world commodity markets, equity
markets, costs and supply of materials relevant to the mining
industry, change in government and changes to regulations affecting
the mining industry. Forward-looking statements in this release may
include statements regarding mineral processing, adaptation of test
work to larger scale and/or future operational scales, estimates of
reduced future capital and operating expenses, delivery of a
preliminary economic assessment, future exploration programs,
operation plans, geological interpretations, and mineral tenure
issues. Although we believe the expectations reflected in our
forward looking statements are reasonable, results may vary, and we
cannot guarantee future results, levels of activity, performance or
achievements.
Neither TSX Venture Exchange nor its Regulation Services
Provider (as that term is defined in the policies of TSX Venture
Exchange) accepts responsibility for the adequacy or accuracy of
this release.
CONTACT:
Pure Energy Minerals Limited (www.pureenergyminerals.com)
Email: info@pureenergyminerals.com
Telephone – 604 608 6611
Pure Energy Minerals (TSXV:PE)
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