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A R T I C LE I N FO A B S T R A C T
Keywords: Aluminium hydroxide hydrate membrane technology was recently developed as a novel, simple, and low cost
Tailing gel-based filtration system. Previous work examined the properties of the gel and showed that it has great
Hydrate gel membrane potential to be used as separation means for filtration of suspended solids. In this study, the gel was applied to
Filtration the dewatering of copper mine tailings for the first time. The filtration process efficiency was measured by
Pre-coat
filtration rate, the turbidity of the supernatant liquid, cake thickness and the final cake moisture content. The
Pressure filter
filtration performance was also tested against other filter aids typically used in mining operations. It is evident
that the application of hydrate gel membrane for filtrating copper tailings is encouraging. It was found that the
comparative advantage of the hydrate membrane lies in producing much lower turbidity water than other filter
aids. Although the flux rate of the hydrate gel membrane was a little lower than the three filter aids tested, the
cake moisture and thickness was comparable. Also, the hydrate gel membrane could be easily spread out against
a retaining fabric and worked well at low to no pressure, with optimum flux rates at about 10 psi and acceptable
flux rate at zero pressure. This study suggests that hydrate gel membranes can be applied in the mining industry,
especially where operating and capital costs are a concern and operators are seeking low turbidity water and/or
a cake suitable for stacking or reprocessing. The technology showed great potential to be utilized for filtering
thickener underflow tailings.
⁎
Corresponding author.
E-mail address: m.edraki@cmlr.uq.edu.au (M. Edraki).
https://doi.org/10.1016/j.mineng.2019.02.030
Received 31 January 2018; Received in revised form 16 May 2018; Accepted 13 February 2019
Available online 20 February 2019
0892-6875/ © 2019 Elsevier Ltd. All rights reserved.
D. Liu, et al. Minerals Engineering 135 (2019) 1–8
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
access the feasibility and filterability of tailings using a developed hy- the filterability of tailings using the hydrate gel membrane. Whatman
drate membrane as a precoat filtration medium. Copper tailings from a filter paper 114 with a pore size of about 2–7 µm was also used in the
base metal mine in Queensland, Australia, were tested. Three other tests. The clarity of filtrate produced was measured using a Turbidity
filter aids which are commonly used for filtering tailings were also meter WP81. Tap water was used in all the tests for diluting tailing
selected and compared. This current study provides knowledge to guide slurries.
application of hydrate gel membranes for filtering tailings thickener
underflows. 2.2. Pore size and surface area analysis of hydrate gel membrane
Aerogels were produced for pore size and surface area analysis. A
2. Material and methods
total of 5 mL of different gel samples was washed by absolute ethanol in
a Falcon tube equipped with Taffeta fabric at the bottom for one week.
2.1. Raw materials
After water molecules were replaced with ethanol, the samples were
put inside an automated tousimis Autosamdri®-815, Series B super-
Aluminium hydroxide hydrate membrane was produced by mixing
critical dyer. This equipment replaced the ethanol molecules with su-
aluminium sulphate and sodium bicarbonate (baking soda) solutions
percritical CO2. Because supercritical CO2 behaves like gas, no structure
(1) (Malekizadeh and Schenk, 2017). During the reaction, aluminium
shrinkage due to surface tension of liquids during normal drying oc-
hydroxide hydrate quickly formed leading to a gelatinous precipitate
curred. The equipment was run in manual mode for more than 3 h with
that could be poured onto filter media for filtration purposes. Both
more filling and purging periods in order to obtain integrated aerogel.
aluminium sulphate and sodium bicarbonate are required for hydrate
The filling process was repeated 3 times (each time for 30 min). Four
filter formation, as direct addition of pre-soaked aluminium hydroxide
different gel samples with different pH (0824 (pH = 7.51), 0825
did not result in the formation of coherent gelatinous hydrate. The gel
(pH = 7.01), 0829 (pH = 6.38), 0830 (pH = 5.83)) were produced and
produced is expected to be low cost and not hazardous.
washed for pore size and surface area analyses. The 0824 gel without
Al2(SO4)3 + 6NaHCO3 → 3Na2SO4 + 2Al(OH)3 + 6CO2 (1) any pH adjustment was used for the following tailing dewatering tests.
Nitrogen adsorption, which is widely used for the characterization
When hydrate was produced by mixing aluminium sulphate and
of a range of porous materials, was used for pore size and surface area
sodium bicarbonate solutions, the mixture appeared milky and did not
analysis of different dried aerogel samples. Nitrogen sorption experi-
show any initial signs of gelatinousness (coherence of hydrate mole-
ments were carried out on a Micromeritics TriStar 3020 analyser after
cules). However, as the mixture was positioned on top of a holding
degassing under vacuum on a Micromeritics VacPrep061 at 100 °C for a
mesh, where it was allowed to settle, accumulate and compress, alu-
minimum of 8 h. The test time was roughly 13 h per sample. The spe-
minium hydroxide hydrate molecules then became denser and the ge-
cific surface areas were calculated from the adsorption isotherms via a
latinousness increased. Gelatinousness further increased as the fresh
multi-point Brunauer–Emmett–Teller (BET) model.
hydrate solution was washed to remove excess sodium sulphate pro-
duced by the reaction and the colour changed from milky white to light
2.3. Hydraulic conductivity tests
grey. Older hydrates (e.g. after 3 months of storage at room tempera-
ture) were also more gelatinous compared to freshly produced hydrates
Hydraulic conductivity of the hydrate gel membrane and the three
and were used in this study for filtering tailings.
filter aids was determined using the constant head method (Klute and
The copper-lead-zinc ore tailings were obtained from a base metal
Dirksen, 1986). The columns were wet from the bottom using the
mine site in Queensland Australia. The feed slurry was prepared by
deionized water (percolating solution). The same solution was then
mixing a known quantity of tailing sample with an appropriate amount
applied continuously, while the flow rates were determined using mass
of tap water using a mechanical stirrer to make a solid percentage of
and volume measurements. These flow rates were used to calculate
15 wt% or 40 wt%, which are the typical solid concentrations for tail-
hydraulic conductivity using Darcy’s law. A pre-coated filter cloth with
ings thickener underflow, and was used for filtration tests. The size
a pore size of 100 µm was used with a precoat thickness of 4.1 cm and
distribution of the copper tailings from a discharge point was measured
maintained for all experiments. During preliminary experiments, this
by a Laser Diffraction Malvern Mastersizer (Model No MSX14) and the
gradient was determined to be the minimum gradient to enable flow to
results are shown in Fig. 2. Tailing has > 80% particles smaller than
occur. The column leaching was continued until a stable flow rate and
283 µm and has > 50% particles smaller than 28 µm.
thus hydraulic conductivity were achieved. The final stable hydraulic
Filter aids, Celite 545, Diacel 200, and Harborlite ER 2.2, were
conductivity was determined by at least 10 consecutive stable flow
purchased from Filchem Australia Pty Ltd. Three types of filter cloth
rates, with less than 3% change between consecutive measurements
with a pore size of 5 µm, 25 µm, and 100 µm were selected for testing
(Mace and Amrhein, 2001).
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
Table 1
Porosity and surface area of dried aerogels of different gel samples.
Sample Surface area, Porosity Total Porosity
m2/g < 150 nm porosity > 150 nm
smallest pore size below 20 nm. As the pH of gel samples decreases, the
porosity and surface areas of their corresponding aerogels increase. For
gel 0830, the porosity reached 90% with a surface area of 405 m2/g.
The high porosity and surface area may allow a good water flux rate for
hydrate gel membranes. Hydrate membranes were further applied for
filtering mine tailings in this study. The performance of the hydrate
membrane in filtering copper tailings is discussed below.
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
Table 2
Constant head permeability (hydraulic conductivity) tests of hydrate gel membrane and three filter aids (with deionized water).
Filter aids Hydrate gel membrane Celite Diacel Harborlite
−6 −5 −6
Average hydraulic conductivity K (m/s) 1.49 × 10 1.14 × 10 4.57 × 10 2.72 × 10−6
Median hydraulic conductivity K (m/s) 1.54 × 10−6 1.15 × 10−5 4.60 × 10−6 2.74 × 10−6
25 µm, and the filter paper of 2–7 µm is summarized in Table 3. As were 454, 185, and 280 NTU, respectively. Obviously, despite the rapid
shown in Table. 3, in the presence of the 100 µm filter cloth, without filtration rate, the use of filter aids as precoat failed to remove fine
the precoat of hydrate gel membrane or filter aids, the cake moisture tailing particles, leading to poor separation results. By contrast, al-
content was 15.3% with a cake thickness of 5 mm. However, the tur- though the filtration rate with the gel was reduced, the water clarity
bidity of filtrate was poor with a value of 566 NTU. Because the tailing was greatly improved with the cake moisture content still comparable
was quite fine, a large number of fine tailings particles was likely to the other filter aids.
passing through the filter cloth, causing the contamination of filtrate Similarly, by using a finer filter cloth of 25 µm, the presence of
water quality and resulting in poor separation of tailings solids and hydrate gel membrane also generated a lowest filtrate turbidity value of
water. 37.4 NTU and similar moisture content with the other precoated filter
By using 1 mm thick gel as a precoat, it was found that the water aids. It is interesting to find that the filtrate turbidity in the presence of
clarity of filtrate after pressure filtration improved significantly with a the hydrate gel membrane using 25 µm cloth (37.4 NTU) increased
turbidity value of only 7.1 NTU. As indicated in Fig. 6 which shows the compared to that using 100 µm cloth (7.1 NTU). As investigated by a
clarity difference of the filtrate filtered in the absence and presence of light microscope, the pore size of the 100 µm cloth was randomly dis-
the hydrate gel membrane, the filtrate water obtained was visibly clear tributed with the biggest size around 100 µm and also much smaller
and transparent after the treatment of the gel. It is also noted that when pores present at the same time. However, 25 µm cloth had an evenly
increasing the hydrate gel membrane thickness from 1 mm to 2 mm, the distributed 25 µm pore size, which may more easily facilitate the pas-
filtrate turbidity and cake moisture content also increased. The increase sing of fine particles and therefore a higher filtrate turbidity.
in filtrate turbidity may have resulted from the partial passing of the The filtration results of 40 wt% tailing using 2–7 µm filter paper as a
fine gel as it was noted that the filtrate colour was milky instead of supporting material are also listed in Table 3. It was shown that the
dark. selection of finer sized filter media improved the overall filtrate tur-
The filtration performance of the hydrate gel membrane was also bidity. The use of hydrate membrane still generated the best filtrate
compared with three filter aids under identical testing conditions. As water clarity.
shown in Table 3, the application of Celite, Diacel and Harbolite as On the other hand, the filtrate volume of 15% of tailings as a
precoat for filtration all resulted in very high turbidity of filtrate. The function of time using different filter medium is shown in Fig. 7. As
filtrate turbidity values in the presence of Celite, Diacel, and Harborlite shown from Fig. 7, the overall filtration rates increased compared to
Fig. 5. Filtrate volume of 40% of tailings as a function of time filtered with and without the hydrate gel membrane and other filter aids in the presence of filter cloth
or paper of (a) 100 µm, (b) 25 µm, and (c) 2–7 µm.
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
Table 3
Filtration performance of 40 wt% tailings, using different size of filter cloth and filter paper under 10 psi pressure.
Filter cloth or No gel 1 mm thick gel 1 mm thick Celite 1 mm thick 1 mm thick Harborlite 2 mm thick Celite 2 mm thick gel
paper 545 Diacel 545
Cake moisture 100 µm 15.3% 22.4% 23.3% 24.7% 24.5% 25.1% 26.2%
25 µm 21.1% 24.1% 22.8% 23.1% 25.7% NT* NT*
2–7 µm 4.8% 26.7% 25.4% 26.7% 26.8% NT* NT*
Filtrate turbidity (NTU) 100 µm 566 7.1 454 183 280 524 71.4
25 µm 1332 37.4 1278 457 837 NT* NT*
2–7 µm 216 8.8 28 17.1 15.9 NT* NT*
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
Fig. 7. Filtrate volume of 15% of tailings as a function of time filtered with and without the hydrate gel membrane and other filter aids in the presence of filter cloth
of (a) 100 µm, (b) 25 µm, and (c) 5 µm.
Table 4
Filtration performance of 15 wt% tailings using different size of filter cloth under 10 psi pressure.
Filter cloth No gel 0.5 mm thick gel 1 mm thick gel 1 mm thick Celite 545 1 mm thick Diacel 1 mm thick Harborlite
Filtrate turbidity (NTU) 100 µm 1145 NT* 12.8 287 632 546
25 µm 1383 489 12.5 1268 1235 1152
5 µm 110 NT* 10.2 NT* NT* NT*
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D. Liu, et al. Minerals Engineering 135 (2019) 1–8
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