SELECTED PAPERS
3. ROLE OF TEST WORK IN PROCESS ENGINEERING 1. Ore preparation test work
The main objective in ore preparation is to liberate the target uranium minerals so they become available for lixiviation. Sometimes ore preparation includes physical separation and removal of gangue minerals in order to reduce reagent consumption rates in the leaching stage.
FIG. 2. Role of test work on process design risk.
Ore preparation is heavily influenced by the mineralogy of the ore to be treated and the nature of the uranium minerals within the ore. Mineralogy provides the engineer with an understanding of what process steps can be employed to recover the uranium from its ores. This includes information about:
— Particle size distribution at which minerals are liberated;
— Extent of locking, i.e. grain size of uranium within the host mineral;
— Potential for upgrade and rejection of reagent consuming gangue.
3.1.1. Comminution
Ore preparation involves breaking the ore from the ‘run of mine’ (ROM) material to a size that allows the lixiviant to get into contact with the target uranium mineral, a process also known as liberation.
Key to the appropriate design of the comminution circuit is the determination of the energy required to break the rock to the target size. A series of standard laboratory scale tests to determine different breakage indices are widely used in the industry for this purpose. These include Crushing index (Ci), Bond Ball Work index (BWi), Bond Rod work index (RWi) and Semi-Autogenous Grinding (SAG) Mill Comminution (SMC) test. A complete comminution characterization requires approximately 200 kg of sample in the form of either rock chips or PQ core (85 mm diameter).
The comminution characteristics of the ore can be used to accurately predict the overall specific energy (kWh/t) requirements of circuits containing Autogenous and (SAG) Mills, Ball Mills, Rod Mills, Crushers and High Pressure Grinding Rolls (HPGRs).
Other specific equipment may require particular vendor test work in order to determine their specific energy requirements.
An example of comminution equipment is shown in Fig. 3.
TABLE 1. TEST WORK AND PROJECT DEVELOPMENT STAGES
• Mineralogy of metallurgical domains
Pre-feasibility 0 – 30 +25, –15
• Comminution test work (laboratory scale)
• Laboratory scale test work of one or more potential extraction methods (batch and batch lock cycle) and all critical process unit operations
• Variability comminution test work
• Preliminary work on uranium recovery
• Batch test work on composite
• Pilot plant
• Residue geochemical test work
• Geotechnical test work on tailings
• Demonstration plant (recommended for novel processes)
3.1.2. Comminution challenges of case study 2
Case Study 2 required the pre-crushed feed ore (44 mm) to be further reduced to a target P80
size of 810 micron at a rate of approximately 450 tph. Table 2 shows the comminution characteristics of this ore determined by test work.
FIG. 3. Example of Comminution Equipment (SAG Mill, courtesy of Orway Mineral Consultants Pty).
TABLE 2. SUMMARY OF COMMINUTION TEST WORK RESULTS – CASE STUDY 2
Parameter Unit Value Notes
Unconfined Compressive Strength (UCS) MPa N/A
Abrasion index (Ai) 0.142 Abrasiveness similar to
quartz
Crush work index (CWi) kWh/t 15.0 Medium to soft material Bond rod work index (RWi) kWh/t 22.5 Above average
competency
Bond ball work index (BWi) kWh/t 14.7 Average competency ore SAG mill comminution (SMC) –
parameter A*b 29.0 Medium to hard ore
SAG mill comminution (SMC) –
parameter ta 0.27 Medium to hard ore
Ore Specific Gravity (SG) 2.65
3.1.3. Comminution energy requirements of case study 2
Test work information was then employed to model a comminution circuit designed to achieve the required treatment rate and target P80. The process of circuit selection considered the circuit energy efficiency, product size, size distribution, mill water requirements and operability. The circuit selected for this case study was a partial secondary crushing and a single stage SAG mill.
Table 3 shows the specific energy requirements for the selected circuit.
TABLE 3. SPECIFIC ENERGY REQUIREMENT – CASE STUDY 2
Parameter Unit Value
New feed rate tph 450
Feed size, f80 mm 44
Product size, p80 µm 810
Pebble recycle % feed 25
Crusher feed, f80 mm 40
Crusher product, p80 mm 11
Power utilization
Sag milling specific energy kWh/t 12.2
Specific recycle crushing energy kWh/t 0.20
Total grinding specific energy kWh/t 12.4
Grinding circuit efficiency, fsag 1.47
Database information and simulation models are employed to interpret test work data for the specific energy requirements and determine the size of the equipment needed. Table 4 shows the recommended size of the comminution equipment for Case Study 2.
3.2. Leaching test work
3.2.1. Chemistry
The two main lixiviants used in uranium leaching are sulphuric acid (major) and sodium carbonate/bicarbonate (lesser). Sulphuric acid leaching is preferred due to higher recoveries and faster kinetics; however, it is non-selective and in ores with high acid consuming gangue minerals use of sulphuric acid results in higher comparative reagent consumption.
Acid leaching of hexavalent uranium (e.g. Autunite) is shown in the following:
Ca(UO ) (PO ) . 11H O + 7H SO → 2H UO (SO ) + CaSO + 2H PO + 11H O Ferric is typically employed to oxidize insoluble tetravalent uranium:
𝑈𝑂 + 𝐹𝑒 (𝑆𝑂 ) + 2𝐻 𝑆𝑂 → 𝐻 𝑈𝑂 (𝑆𝑂 ) + 2𝐹𝑒𝑆𝑂
The alkaline leach of hexavalent uranium (e.g. Carnotite) is shown in the following:
𝐾 (𝑈𝑂 ) (𝑉𝑂 ) . 3𝐻 𝑂 + 6𝐶𝑂 → 2𝑈𝑂 (𝐶𝑂 ) + 2𝐾 + 2𝑉𝑂 + 4𝑂𝐻 + 𝐻 𝑂 Any tetravalent uranium present in the alkaline leach with the hexavalent form requires an oxidant which can be oxygen, air or hydrogen peroxide.
The reagent consumption for uranium recovery is often less than 5% of the total, with gangue minerals consuming the balance of the reagents.
TABLE 4. COMMINUTION EQUIPMENT SELECTION – CASE STUDY 2
Criteria Units
Primary crusher
Crusher type Jaw
Model CJ615 or equivalent
Installed motor kW 200
Secondary crusher
Crusher type Cone
Model CH660 EC or equivalent
Installed motor kW 290
SAG mill
Diameter – inside shell m 8.53
EGL m 4.80
Imperial ft × ft 28.0 × 15.7
Shaft power MW 5.4
Motor power MW 6.5
Recycle crusher
Crusher type Cone
Model CH440 MF or equivalent
Installed motor kW 190
3.2.2. Leach regimes
The leach regime is selected to suit both the uranium and gangue mineralogy. Leach test work is required to identify the extraction of uranium and gangue elements and to determine reagent consumption.
The main performance indicators to be derived from test work are:
— Extent of uranium extraction;
— Reagent consumption;
— Extent of gangue mineral dissolution;
— Optimum operating conditions.
Table 5 summarizes the leach regimes most commonly used in the recovery of uranium. Figure 4 shows an example of an in-situ leach operation and Figure 5 shows the view inside a pressure leach autoclave.
FIG. 4. Uranium in situ leach operation (Beverley, South Australia, courtesy P. Woods, IAEA).
FIG. 5. View inside a pressure leach autoclave (courtesy Hydromet Pty Ltd).
3.2.3. Leach test work for case study 1
A continuous agitated acid leach pilot campaign on uranium ore was conducted for over 900 hours to provide a design basis for the hydrometallurgical plant of case study 1.
Prior to the continuous pilot plant campaigns, batch test work was conducted to confirm the optimum process conditions relating to:
— Grind size;
— Temperature;
— Slurry SG.
This work provided information regarding:
— Acid consumption rate;
— Oxidant requirements;
— Residence time.
The batch test work culminated with a trade off study that confirmed an economic optimum at a P80 of 710 microns. However, leaching ores with a P80 of 710 microns present particle suspension challenges which cannot be addressed in a batch test.
TABLE 5. URANIUM LEACH REGIMES
Leaching regime Characteristics Main process design inputs from
test work Heap leach
- Mainly used in acid leach;
- Some application on alkaline leach.
- Used for low grade ores;
- It can be dynamic or permanent heap;
- Require a careful environmental review regarding ripios disposal and emergency pond storage capacity;
- May involve the oxidation of sulphide gangue minerals for the
- Low temperature (typically 20 – 40°C, only acid leach).
- Gas exhaust system needed to remove radon for high grade ores;
- Conducted in mechanically agitated tanks or Pachuca tanks;
- Feed to leaching may require thickening to achieve a high pulp density in order to achieve a negative water balance.
- Uranium and gangue extraction extent;
- Acid/alkali and oxidant consumption rates;
- Residence time (6–48 hours);
- Pulp density (typically 35–70%);
- Temperature.
- Lower impurity levels in leach product;
- May involve the oxidation of sulphide gangue minerals for the production of acid.
- Uranium and gangue extraction extent;
The pilot plant was configured to address these above challenges as well as confirm:
— Particle suspension;
— Leach efficiency;
— Reagents consumption rates;
— Materials of construction.
3.2.3.1. Particle suspension
Particle suspension in case study 1 was achieved by increasing the solids content in the slurry above the hinder settling zone at between 68–70% solids w/w using a pitch blade turbine impeller. Test work was conducted using slurries from the pilot plant to determine impeller and tank design parameters. Figure 6 shows a photograph of the agitation test tank and Fig. 7 shows the surface response at slurry densities of 65% (a), 70% (b) and 75% (c).
Agitation test work for case study 1 provided the following information:
— Apparent viscosity: 300–2000 mPa·s;
— Slurry density: 65–70% w/w;
— Specific torque: 37–58 Nm/m3;
— Power/unit value: 0.6–3.7 kW/m3;
— Baffle — aspect ratio: 0.10–0.12.
FIG. 6. Test agitation tank (courtesy of Mixtec Pty).
a) Surface response at 75% solids
b) Surface response at 70% solids c) Surface response at 65% solids
FIG. 7. Surface response during agitation tests — case study 1 (courtesy of Hydromet Pty Ltd).
3.2.3.2. Leaching efficiency
The uranium leach extraction profile of the pilot plant circuit (Fig. 8) for Case Study 1 is shown in Fig. 9.
Leaching pilot plant results provided design criteria for:
— Residence time;
— Uranium extraction;
— Gangue extraction;
— Temperature and pH conditions.
Materials of construction
In addition to leach performance, pilot campaigns are also useful to gain information about materials of construction for equipment exposed to aggressive conditions.
FIG. 8. Atmospheric leach circuit of a pilot plant (courtesy of SGS Pty Ltd).
FIG. 9. Overall leach efficiency profile — case study 1.
Alloys tested during the pilot campaign for case study 1 included stainless steel UNS–S31603 and UNS–S30403 as well as alloys UNS–S32001, UNS–S31803, UNS–S32101 and UNS–
S40977. With the exception of UNS–S40977, all alloys tested were resistant to the test conditions. Figure 10 shows UNS–S40977 alloy with slight but clearly visible etching or other evidence of attack.
a) As retrieved b) After cleaning
FIG. 10. UNS–S40977 coupon from pilot campaign — case study 1.
3.3. Solid–liquid separation test work
Two systems are used for solid–liquid separation of uranium leach residue:
— Thickeners:
• Prior to filtration;
• In lieu of filtration (in a Counter Current Decantation (CCD) arrangement).
— Filtration (with or without thickening):
• Vacuum belt filtration;
• Pressure filtration.
Where slurry viscosities are non-Newtonian resin in pulp has been used for uranium recovery, after resin removal the spent slurry is sent to the tailings facility.
3.3.1. Thickeners
Thickening test work is used to determine the type of thickener required and to determine the size of the equipment needed. This vendor specific test work aims to determine the following:
— Feedwell solids content and flocculant dose;
— Flocculant type and addition rate;
— Settling rate;
— Underflow solids content;
— Flux (kg/m2/h);
— Overflow suspended solids content;
— Bed residence time required for target underflow solids;
— Yield (Pa).
3.3.2. Filters
Filtration test work is used to determine the type of filter adequate for the required duty and determine the size of the equipment required. These vendor specific tests aim to determine the following:
— Flocculant addition, dose and rate;
— Flux (kg/m2/h);
• Cake formation;
• Cake washing;
• Cake drying;
— Wash efficiency;
— Cycle time;
— Cake thickness (> 7 mm).
An example of the general arrangement of a uranium plant thickener and belt filter is shown in Fig. 11.
FIG. 11. General arrangement of a thickener and vacuum belt filter.
3.3.3. Solid–liquid separation test work in case study 1 3.3.3.1. Thickening
Thickening tests were conducted on uranium leached tailings slurries from the pilot plant campaign. Table 6 shows the test work conducted and the key information from each test used for design.
TABLE 6. THICKENING TEST WORK RESULTS – CASE STUDY 1
Test Key test work information for process engineering Settling
flux vs.
flocculant dose
The settling flux indicated optimum settling performance at feedwell solids concentrations of 7.5% w/w.
Static cylinder test
Underflow solid content vs.
retention time
Settling rates of 19–56 m/h;
Overflow solids of < 100 mg/L;
Ultimate underflow solids densities of 68.6 w/w–70.8% w/w
Overflow solids: < 150 mg/L;
Rise rate: 8 m/h;
Bed solids:
.
Underflow rheology
3.3.3.2. Filtration
Belt filter test work was conducted on slurries from the pilot plant. Key test work results were:
— Cake moisture: 15–20%
— Drying time: 20 seconds
— Filterability: 1500–1600 kg dry solid/h/m2
— Expected wash recovery: > 98%
— Wash ratio: 0.8/ton
3.4. Uranium recovery test work
The following unit operations are employed in recovering uranium from leachates:
— Ion exchange;
• Fixed bed (Fig. 12);
• Carousel (Fig. 13);
• Fluid bed; the fluid bed can be simulated at pilot scale in a cascade set-up (Fig.
14(b)). Commercially, the fluid bed ion exchange systems are constructed in a tower arrangement (Fig. 14(a));
— Solvent extraction;
• Mixer–settler;
• Pulsed columns.
Classical lead–lag column arrangement FIG. 12. Fix bed ion exchange.
FIG. 13. Typical carousel ion exchange flowsheet.
3.4.1. Uranium recovery test work in Case Study 1 3.4.1.1. Ion exchange
The low uranium tenor of the leachate together with its high impurity load predicated the use of a combination of ion exchange and solvent extraction.
The ion exchange circuit was tested at pilot scale with the set-up shown in Fig. 14(b). The high suspended solids in the leachate (around 1000–3000 mg/L) contributed to the selection of a fluid bed system. The resin was eluted with 1.2 molar sulphuric acid.
a) General arrangement of a uranium fluid bed (nimcix).
b) Uranium Pilot Plant Continuous Ion — Simulating Fluid Bed (NIMCIX) (Reproduced with permission from SGS Pty).
FIG. 14. Fluid bed ion exchange.
3.4.1.2. Solvent extraction
The solvent extraction pilot plant had the ion exchange eluate as its PLS. A system consisting of 4 stages of extraction, 2 stages of scrubbing, 3 stages of stripping and one stage of washing was employed.
During piloting, crud formation became pervasive in the extraction circuit and it was discovered to be attributed to suspended solids carried over (Fig. 15). Colloidal silica (Fig. 16) resulted in poor phase separation and a misreport of crud to the entire circuit.
FIG. 15. Crud formation due to suspended solids (Courtesy of Hydromet Pty Ltd).
FIG. 16. Crud formation due to colloidal silica (Courtesy of Hydromet Pty Ltd).
3.5. Product precipitation test work
The loaded strip liquors from solvent extraction or the concentrated eluates from ion exchange report to yellow cake product recovery.
Historically, ammonium based processes have been employed:
2𝑈𝑂 𝑆𝑂 + 6𝑁𝐻 + 3𝐻 𝑂 → (𝑁𝐻 ) 𝑈 𝑂 + 2(𝑁𝐻 ) 𝑆𝑂
The ammonium diuranate (ADU) is sometimes calcined to produce mixed uranium oxide U3O8. Environmental concerns related to the use of ammonium reagents have seen the use of the sodium base processes in more recent years:
2𝑁𝑎 𝑈𝑂 (𝐶𝑂 ) + 6𝑁𝑎𝑂𝐻 + 3𝐻 𝑂 → 𝑁𝑎 𝑈 𝑂 . 6𝐻 𝑂 + 6𝑁𝑎 𝐶𝑂
The sodium diuranate (SDU) is then dissolved in sulphuric acid
𝑁𝑎 𝑈 𝑂 . 6𝐻 𝑂 + 3𝐻 𝑆𝑂 → 2𝑈𝑂 𝑆𝑂 + 𝑁𝑎 𝑆𝑂 + 9𝐻 𝑂
And the resulting uranyl sulphate is converted to uranium tetraoxide:
𝑈𝑂 𝑆𝑂 + 2𝑁𝑎𝑂𝐻 + 𝐻 𝑂 → 𝑈𝑂 . 2𝐻 𝑂 + 𝑁𝑎 𝑆𝑂
The ADU/SDU can then be filtered but is more preferably washed in centrifuges prior to product drying/calcining.
3.5.1. Product specification
Product for sale from a uranium ore processing plant needs to meet the requirements and specifications of the converters. Converters place specifications on at least the following elements:
Cadmium, boron, thorium, iron, vanadium, zirconium, molybdenum, sulphate and phosphate.
3.5.2. Product precipitation test work case study (case study 1)
In case study 1, the loaded strip was sodium uranyl tricarbonate. This was converted to SDU and uranium tetraoxide.
Product precipitation test work is generally conducted on a bench scale because of the limited amount of either strip solution or eluant that can be obtained from a piloting campaign. Test work was conducted to determine:
— Reagent dose and consumption rates;
— Residence time;
— Precipitation and dissolution extent;
— Seed recycle requirements;
— Wash efficiency;
— Product quality.
Figure 17 shows the seeded precipitation profile of the SDU (a), the dissolution profile of SDU in weak acid (b), the uranium tetraoxide precipitation profile (c) and a photograph of the uranium tetraoxide obtained after drying (d).
For the case study 1, the UO4 product typically assayed as shown in Table 7.
a) Batch SDU seeded precipitation profile b) Batch SDU re–dissolution profile
c) Batch uranium tetraoxide precipitation profile
d) Ground UO4 sample after drying
FIG. 17. Product precipitation test work results — case study 1.
TABLE 7. TYPICAL PRODUCT ASSAY — CASE STUDY 1
Element Assay
U 67.0%
K 0.02%
Mn 0.01%
V 0.09%
C <0.01%
Zr 0.02%
Th < 0.001%
Fe < 0.01%
Mo < 0.0001%
P < 0.001%
3.6. Effluent test work
Uranium hydrometallurgical plants are required to dispose of their effluents in a responsible manner. Geochemical tests are performed on batch and pilot test work leach residues to confirm and determine the requirements of the final tailings facility.
The liquid and solid fractions of the effluent are tested to provide the following data:
— Electrical conductivity;
— Redox potential (Eh);
— Elemental assay of both the liquid and solid fractions employing ICP–MS;
— pH;
— Acid potential (AP)/Neutralization potential (NP);
— Net acid generating (NAG) characteristics;
— Kinetic test ASTM D5744–96 to examine the leaching kinetics of critical elements;
— Metals mobility leach tests as in toxicity characteristics leaching procedure (TCLP), both short and long term.