Industrial & Engineering Chemistry Research Volume 38 Issue 11 1999 (Doi 10.1021/ie990156b) Vegliò, F. Passariello, B. Abbruzzese, C. - Iron Removal Process For High-Purity Silica Sands Productio
Industrial & Engineering Chemistry Research Volume 38 Issue 11 1999 (Doi 10.1021/ie990156b) Vegliò, F. Passariello, B. Abbruzzese, C. - Iron Removal Process For High-Purity Silica Sands Productio
In this article, a leaching study, carried out on a quartz sample to obtain high-purity silica
sands, has been presented. A leaching process by using oxalic acid to remove low iron content
from the ore under study and to obtain a material suitable for fiber optic production has been
evaluated. A characterization study has been carried out to establish the location of the iron
impurities on the ore: 77 g/t was the maximum iron contamination, whereas, a final iron content
<10 g/t (as Fe) has to be achieved for the application considered. The effect of the grinding
process on the iron extraction yield has been established; the maximum iron extraction yield
obtained with the ore as-is was about 45-50%, whereas extraction yields greater than 80-90%
can be obtained after grinding the ore in different experimental conditions. An empirical model
was evaluated to correlate the iron extraction yield obtained after 3 h of leaching at 80 C, with
3 g/L of oxalic acid and 10% (w/v) of ore concentration, as a function of the average particle
diameter of the ore after grinding. An iron extraction yield of about 98-100% can be obtained
with an average particle diameter of about 20 m. A schematic flowsheet of the process has
been proposed considering the obtained experimental results and the results obtained in the
literature for the waste treatment aspects. The experimental results have shown the technical
feasibility of this process for the production of high-purity silica sands.
Table 1. Chemical Composition of the Florinas Sample FL for Different Granulometric Classes
sample (m) as-is ore +500 +250-500 +180-250 +125-180 +90-125 +53-90 -53
abundance (%) 100 3.7 37.8 36.3 15.2 5.3 1.4 0.3
SiO2 99.10 98.0 98.3 99.2 99.0 98.5 97.5 94.2
Al2O3 0.40 0.76 0.57 0.14 0.21 0.35 0.77 2.27
Fe2O3a 110 130 90 81 107 186 341 -
K2O 0.33 0.63 0.47 0.13 0.19 0.40 0.81 1.87
Na2O 0.13 0.085 0.11 0.105 0.08 0.067 0.12 0.21
CaO 0.18 0.27 0.15 0.39 0.34 0.26 0.26 0.34
MgO 0.0042 <0.0002 <0.0002 <0.0002 0.0012 0.0056 0.0028 0.043
sum 100.14 99.75 99.60 99.97 99.82 99.58 99.46 98.93
a Composition in g/t.
this quartz ore from an initial Fe2O3 value of 110 g/t to 2.3. Analytical Measurements. A Perkin-Elmer
a final iron content of <10 g/t for optical fiber applica- 6500 ICP (Inductively Coupled Plasma) instrument was
tions. A further target value is <1 g/t for silicon used to determine iron, aluminum, etc., in the liquid
production. samples taken during the leaching and the mineral
The leaching operation, performed with oxalic acid as characterization studies.
the leaching agent, has been carried out in a lab-scale Solid samples, after filtration and washing, were
slurry reactors. With this objective various preliminary brought into solution by treating 0.5 g with HF and
experiments were conducted to ascertain the main HClO4 at high temperature. The process was taken to
operating conditions that must be adopted in the leach- dryness and the residue was then redissolved in 20 mL
ing treatment. For these reasons, chemical and miner- 1:1 HCl, warmed, and brought to volume. A comparison
alogical characterization of FL, preliminary tests to between the iron extraction yield calculated from the
ascertain the reproducibility of the leaching conditions, measures in solution + material balance, and the metal
and leaching tests to assess the effect of the grinding extraction yield calculated from the leach residues
process (ore size distribution) on the iron extraction demonstrates a substantial accord of the experimental
yield (IEY) and on the aluminum extraction yield results in terms of iron extraction yield. When the iron
(AlEY), have been performed. Very low levels of iron extraction yield is approximately 100%, the measures
in the solid residues can be given as <5 g/t for the iron
must be reached in the ore after leaching to permit its
content in the quartz sand.
use for fiber optic applications.
3. Results
2. Materials and Methods
The main objective of the characterization study was
2.1. Ore. The silica sand (noted as FL) comes from to ascertain the iron-bearing minerals in the Santa
the Florinas quarry located in the north of Sardinia, Florinas ore tested by flotation (referred to as FL as-
Italy. Table 1 shows the chemical analysis of the ore in is). On the other hand, the main objective of the leaching
the different size fractions. study was to ascertain the main operating conditions
2.1.1. Grinding Process and Particle-Size Analysis. in lab-scale tests, for iron removal, with particular
The FL material was adopting various particle-size reference to the particle-size factor, which is of funda-
distributions. The FL was ground under different mental importance regarding the type of reactor to be
experimental conditions; dry grinding in an agate adopted in the design and construction of the pilot
laboratory mill was carried out for different periods of leaching unit. (This task is in progress and it is not
treatment to obtain different size fractions for the lab- considered in this phase of the experiment.)
scale leaching studies. Particle size analysis was per- 3.1. Characterization of the FL Ore. The results
formed using Tyler sieves and a Helas laser granulom- of particle-size distribution of Florinas FL are reported
eter. in Table 1. The sample exhibits a modal distribution,
with maximum abundance of particle-size classes be-
2.1.2. X-ray Diffraction and Scanning Electron Mi- tween 500 and 125 m.
croscopy Analysis. The apparatus used was a Siemens
The results of quantitative analysis of the Florinas
D-500 Diffractometer. Operating conditions were: 40 FL sample, for different size classes, are reported in
kV, 40 mA, slit 1, monochromator with curved graphite Table 1. The diffractometric spectra (data not shown)
crystal. Scanning electron microscopy (SEM) analyses of the Florinas FL sample shows that quartz is the main
have been performed by a Philips model 505 coupled component with small quantities of plagioclase and
with microanalysis (energy dispersive system, EDS). k-feldspar. Figure 1 shows a particle of quartz covered
2.2. Leaching Tests. The leaching tests were carried by small feldspar particles as an example. The micro-
out in a column and a stirred reactor. Column leaching analysis carried out by SEM showed that the main iron
tests were conducted percolating the leaching agent impurities are located on the feldspar particles (white
through a packed-bed column by using FL as-is ore. small particles in Figure 1).
Further leaching tests were conducted in a 2-L reactor 3.2. Leaching Tests. 3.2.1. Column Leaching Tests.
with thermostat. Various amounts of mineral (FL as-is Column leaching tests were performed to verify the
or FL ground to various sizes) were treated with 500 possible application of this kind of reactor to reach the
mL of oxalic acid solutions at a temperature of 80 C. targets required for fiber optic production, in terms of
In both cases 0.5-mL samples were taken every so often iron extracted, by using FL as-is ore. Figure 2 shows
and diluted to 2 mL to monitor iron extraction during the iron extraction yield that can be extracted in the
the course of the process. These experimental conditions tested experimental conditions. The maximum yield was
were adopted according to previously reported tests.2,4,5 obtained after 4 h of operation and is about 50%.
Ind. Eng. Chem. Res., Vol. 38, No. 11, 1999 4445
4. Conclusions
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Revised manuscript received June 24, 1999
(9) Panias, D.; Taxiarchou, M.; Douni, I.; Paspaliaris; I., Kon- Accepted July 17, 1999
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Oxalic Acid Solutions. Hydrometallurgy 1996, 42, 257. IE990156B