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Hydrometallurgy 64 (2002) 219 – 229

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Sulfuric acid leaching of Kab Amiri niobium–tantalum


bearing minerals, Central Eastern Desert, Egypt
Omneya M. El-Hussaini*, Mohamed A. Mahdy
Nuclear Materials Authority, P.O. Box 530, El Maadi, Cairo, Egypt
Received 2 June 2001; received in revised form 15 April 2002; accepted 17 April 2002

Abstract

The ore under study was obtained from the Kab Amiri area located close to the northern boundary of the Central Eastern
Desert. The ore is constituted of different kinds of refractory minerals. These are mainly represented by the niobium – tantalum
rare earth-bearing minerals namely euxinite, samarsakite and fergusonite, beside the uranium refractory minerals davidite and
zircon. Increasing demand for niobium, tantalum, titanium, uranium, thorium and rare earth elements has stressed the
importance of developing methods for their recovery and processing into marketable form. In the present work, Kab Amiri ore
was subjected to direct agitation leaching with sulfuric acid. Variables such as acid concentration, temperature, time, ore to acid
ratio and oxidant effect were studied. When finely ground ore ( 74 Am) was reacted upon for 2 h with a mixture of sulfuric
acid (10.8 M) and nitric acid (5.3 M) in the ore to acid weight ratio of 1:3 at 200 jC, almost complete recovery of both niobium
and tantalum was achieved while the leaching extents of thorium and total rare earths were 86% and 70%, respectively. On the
other hand, the recovery of both uranium and titanium did not exceed 60% due to their presence in the refractory mineral
davidite. D 2002 Elsevier Science B.V. All rights reserved.

Keywords: Leaching; Sulfuric acid; Refractory minerals; Niobium – tantalum ores

1. Introduction increased demand has firmed prices for tantalum raw


materials, which in turn has encouraged new produc-
Niobium and tantalum elements occur in a great tion from small operations in Africa, Brazil and
variety of ores. Their commercial value in the metal- Thailand. On the other hand, prices have been
lurgical, nuclear and space industries, etc. make their reported to be as low as $53 per kilogram of niobium
recovery desirable in relatively concentrated form. in ingot form to as high as $222 per kilogram of
The total production of tantalum from raw materials niobium in special shapes.
as reported by the Tantalum – Niobium International The chemical study of niobium and tantalum
Study Center (T.I.C) (Linden, 1999) exceeded 5 elements shows that there are large numbers of
million tonnes Ta2O5 during 1999, while the total procedures for their ore decomposition. All niobium
supply of niobium from raw materials is now running minerals can be readily decomposed with hydrofluoric
at approximately 150 –160 million tonnes Nb2O5. The acid with almost complete dissolution. This method is
widely used for the dissolution of columbite– tantalite
minerals (Gupta and Suri, 1994a). Alkali fusion in
*
Corresponding author. Fax: +20-2-758-5832. combination with acid leaching is one of the first

0304-386X/02/$ - see front matter D 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 3 0 4 - 3 8 6 X ( 0 2 ) 0 0 0 4 5 - 2
220 O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229

methods that was adopted on an industrial scale to and other associated metal values include euxinite,
achieve simultaneous breakdown of columbite –tanta- samarsakite and fergusonite. These minerals can be
lite and upgrading niobium and tantalum values (El- processed by the following: chlorination (Gupta and
Hussaini, 1996; Eckert, 1995). Some minerals have Suri, 1994b), alkali fusion followed by acid leaching
been considered for the recovery of niobium, tantalum (Foos, 1960), fusion with ammonium fluoride and

Fig. 1. Separation of niobium – tantalum minerals by physical methods.


O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229 221

Table 1 zircon (Zr,U,Th,Hf)SiO4, euxinite (Y,Er,La,Ce,U,Th)


Mineralogical and chemical analysis of Kab Amiri ore material
(Nb,Ta,Ti)(O,OH) and davidite (Fe,La,U,Ca)(Ti,Fe,V,
Gangue Economic Associated Chemical % Cr)(OH,O) minerals. On the other hand, the petro-
mineralsa mineralsb mineralsb analysis
graphic studies of silica veinlets indicate that their
Quartz Euxinite Hematite Nb2O5 16.16 radioactivity is mainly due to the presence of zircon
Alkali Feldspar Samarsakite Ta2O5 12.08
Muscovite Fergusonite TiO2 4.48
mineral (Ammar, 1993).
Phlogopite Daviditea FeOc 23.40
Fluorite Zircona REEd 0.09
ThO2 0.04 2. Methods and material studied
U3 O8 0.23
ZrO2 0.19
LOIe 0.31
The niobium – tantalum raw material under study
a was selected from Kab Amiri. The ore was ground to
From Ammar (1993).
b
The grains were heated at 1000 jC before XRD analysis. 500 Am and physically treated with heavy liquids,
c
Total iron as FeO. as shown in Fig. 1. Grains of buff and black colors
d
Total rare earth elements oxides. were separated from the heavy fractions. They were
e
LOI: loss on Ignition at 900 jC. differentiated as the economic and the associated
minerals, respectively. The mineralogical composition
detected by X-ray diffraction (XRD, using Phillips
bifluoride (Gupta and Suri, 1994c), direct acid dis- PW 223/30) and the chemical analysis of the selected
solution with H2SO4 (Bock, 1979a; Vacariu et al., ore sample ( 74 Am) are given in Table 1.
1999), or combination of H2SO4 and HF (Krismer and In order to study the distribution of minerals in
Hoppe, 1984). different grain sizes, the ore was crushed to 590 Am
The niobium –tantalum rare earth-bearing minerals then the fractions were separated to various sizes
which occur in the form of multiple oxides are from 500 to 74 mesh. The distributions of the
commonly associated with uranium minerals. These economic elements in each size were determined as
minerals are opened by different methods including shown in Table 2. From the obtained data, it is clear
acid leaching, atmospheric alkaline leaching, pressure that the elements are variably distributed among the
alkaline leaching, roasting and chloride roasting fol- separated fractions.
lowed by acid and alkaline leaching (El Shazly and El The agitation leaching process was performed
Hazek, 1970). under different conditions summarized in Table 3, to
Owing to the refractory nature of some uranium achieve the best leaching efficiency of different ele-
minerals such as davidite, more aggressive conditions ments. Direct leaching has been applied to the ore of
are required for leaching than those used in conven- 74 Am size using sulfuric acid (97 – 99%) obtained
tional uranium circuits (Ritcey et al., 1993). from ADWIC. Nitric acid (69 – 72%) obtained from
The present work is concerned with the leaching BDH was used as an oxidant. The leaching tests were
process performed upon Kab Amiri ore. This area is
located near the Qena – Safaga Road, i.e., close to the
northern boundary of the Central Eastern Desert. Two
Table 2
radioactive anomalies were reported in the Kab Amiri Distribution percentage of elements of Kab Amiri ore material in
monsogranite: one in the pegmatites and the other in different grain sizes
the silica veinlets. The pegmatites host rocks are Grain size Weight Distribution (%)
composed of quartz cores surrounded by alkali feld- (Am) (%) Nb2O5 Ta2O5 TiO2 REE2O3 ThO2 U3O8
spar outer zones. Both cores and outer zones are
500 8.2 10.6 7.9 17.5 14.2 10.0 17.5
separated by an incomplete zone of muscovite. The 420 6.6 8.4 6.4 12.6 10.7 7.8 12.5
muscovite zone shows high radioactivity, within 297 6.1 8.9 6.2 13.8 9.1 6.9 9.0
which visible black metallic minerals are detected. 250 10.6 8.7 13.2 13.5 14.6 10.6 13.3
The X-ray diffraction (XRD) results of the black 125 17.2 15.2 19.0 11.0 15.8 17.2 17.5
metallic minerals showed that they are composed of 74 51.3 48.2 47.4 31.7 35.6 47.5 30.1
222 O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229

Table 3
Studied factors affecting the agitation leaching of Kab Amiri ore material using sulfuric acid
Factors Factors’ values Fixed conditions
Temperature Sulfuric acid Time Ore to Oxidant,
(jC) concentration (M) (h) acid ratio HNO3 (M)
Temperature (jC) 33, 56, 65, 94, 135, 174, 200, 315 – 18.0 2 1:2.5 0.0
Sulfuric acid (M) (i) 18.0, 14.4, 10.8 65 – 2 1:2.5 0.0
concentration (ii) 18.0, 15.8, 14.4, 12.2, 10.8, 9.4 200 – 2 1:2.5 0.0
Time (h) 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 7.5 200 10.8 – 1:2.5 0.0
Ore to acid ratio (wt/vol) 1:1.5, 1:2.0, 1:2.5, 1:3.0, 1:5.0 200 10.8 2 – 0.0
Oxidant concentration, 0.0, 2.2, 5.3, 8.4, 9.4, 12.7 200 10.8 2 1:3.0 –
HNO3 (M)

carried out in 100 ml stoppered Pyrex containers. A (Koerner et al., 1963) leaving 30.3% leached species
thermometer was placed through a fitted opening, and in the liquor. On the other hand, overheating causes
the reaction vessel was heated using a hot plate with reduction and dehydration of some rare earth elements
magnetic stirrer. forming insoluble sulfate salts (Vickery, 1961).
The determination of niobium, tantalum, total rare The ability of both titanium and uranium to be
earth elements, titanium, thorium and uranium in leached with concentrated sulfuric acid at various
solution were carried out using a UV –VIS spectro- temperatures is less than 45%, Fig. 2b. This may be
photometer (Shimadzu UV-160A). The values of total attributed to their presence in the refractory minerals
iron and zirconium were obtained by Atomic Absorp- davidite and/or zircon.
tion Spectrophotometer (UNICAM 969).
3.2. Effect of sulfuric acid concentration

3. Results and discussion Two sets of experiments were performed at 65 and


200 jC. The agitation leaching process was carried
Relating to the process of the present work, sulfuric out by mixing sulfuric acid with the ground ore to
acid (considered to be an inexpensive reagent) was 74 Am in ore to acid ratio of 1.0:2.5 for 2 h.
used for leaching the niobium –tantalum rare earth
minerals. The effects of different factors on the 3.2.1. Low temperature
leaching extents of the minerals’ constituents were Fig. 3 reveals that at 65 jC the leaching extents of
studied in detail as follows. the studied elements did not exceed 50% except for
thorium, which reached 63%. At ordinary temperature,
3.1. Effect of temperature thorium may form the readily soluble sulfate salt which
in turn forms the octahydrate [Th(SO4)28H2O] in
Increasing the temperature was found to be effec- excess of sulfuric acid (Mathur and Tandon, 1986).
tive in increasing the leaching extents of the elements It was reported by Bielecki et al. (1991) that at
composing the economic minerals. Above 300 jC, temperatures ranging from 40 to 100 jC, most of
hydrolysis may occur thus the leaching extents de- thorium quantities were dissolved by leaching the ore’s
creased. The results are shown in Fig. 2a and b. This residue with sulfuric acid ranging from 0.5 to 5.0 M.
set of experiments was conducted using concentrated
sulfuric acid (18 M), on the ground ore to 74 Am at 3.2.2. High temperature
an ore to acid ratio of 1.0:2.5 for 2 h. As shown in Fig. 4a and b, the economic elements
Under these conditions, niobium reached its max- were more effectively leached with the lower concen-
imum leaching extent of 73.5% at 200 jC, while most trations of sulfuric acid than the higher, except for
of tantalum may precipitate as tantalum hydroxide titanium, which reached its maximum leaching extents
O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229 223

Fig. 2. (a) Effect of temperature on leaching extent of Nb2O5, Ta2O5, REO and ThO2 upon leaching the ground ore to 74 Am with 18 M
H2SO4 in ore to acid ratio of 1:2.5 for 2 h. (b) Effect of temperature on leaching extent of TiO2 and U3O8 upon leaching the ground ore to
74 Am with 18 M H2SO4 in ore to acid ratio of 1:2.5 for 2 h.

at 15.8 M sulfuric acid. Above 12.2 M, sulfuric acid advantages, the foremost of which is the significant
leaching of thorium and rare earth elements was found reduction in the operating costs.
to be independent of the acid concentration.
At 200 jC, it is preferable to apply the leaching 3.3. Effect of time
process using 10.8 M sulfuric acid. Higher concen-
tration should be avoided due to the fact that concen- The reaction between Kab Amiri ore ground to
trated sulfuric acid is consumed in attacking the 74 Am and sulfuric acid of concentration 10.8 M in
gangue constituents of the ore. ore to acid ratio of 1.0:2.5 was studied at 200 jC,
Lerner (1961) found that sulfuric acid of concen- while varying the leaching time from 0.5 to 7.5 h. The
tration ranging from 9.2 to 13.2 M is sufficient to results in Fig. 5a and b show that most of the elements
decompose the niobium mineralization in niobium- composing the ore reached their highest leaching
containing ores. This leads to numerous processing extents within a few hours. The leaching extents of
224 O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229

Fig. 3. Effect of sulfuric acid concentration on leaching extent of Nb2O5, Ta2O5, REO, ThO2, TiO2 and U3O8 upon leaching the ground ore to
74 Am with H2SO4 in ore to acid ratio of 1:2.5 at 65 jC for 2 h.

both titanium and uranium at any time did not exceed maximum leaching. The other leaching conditions
50% for the former and 35% for the latter due to the were kept constant, in which the ground ore 74
refractory nature of davidite. Am was mixed with sulfuric acid of 10.8 M in the ore
to acid ratio of 1:3 and the mixture was heated for 2h
3.4. Effect of ore to acid ratio at 200 jC. The results are shown in Fig. 7.
It was found that the increase in nitric acid con-
A set of experiments was carried out to examine centration above 5.0 M decreases the leaching extents
the effect of ore to acid ratio. The experimental of both niobium and tantalum. This may be due to the
conditions were kept constant as mentioned before formation of protective coating of insoluble niobium
while varying the ore to acid ratio from 1.0:1.5 to and tantalum oxides at higher nitric acid concentration
1.0:5.0. The results are illustrated in Fig. 6a and b. It is (Bock, 1979b). The maximum leaching extent of rare
observed that the leaching extents are high with the earths and thorium was obtained by mixing concen-
exception of uranium and titanium, which are below trated nitric acid of 12.7 M with 10.8 M sulfuric acid,
50%, due to their incorporation in the primary ura- the recovery was 70% and 84%, respectively (Fig. 7).
nium mineral davidite. However, it is possible to say There is the possibility that most of the insoluble rare
that the best leaching extents of most of the elements earth elements and thorium are associated with the
were obtained at ore to acid ratio of about 1:3. refractory minerals, i.e., davidite.
Slight improvement in uranium leaching was
3.5. Effect of oxidant concentration obtained by mixing 9.4 M nitric acid with 10.8 M
sulfuric acid (Fig. 7). This may be attributed to the
These experiments were performed to find the nature of davidite and zircon, which require severe
minimum concentration of nitric acid needed for conditions for complete decomposition such as leach-
O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229 225

Fig. 4. (a) Effect of sulfuric acid concentration on leaching extent of Nb2O5, Ta2O5, REO and ThO2 upon leaching the ground ore to 74 Am
with H2SO4 in ore to acid ratio of 1:2.5 at 200 jC for 2 h. (b) Effect of sulfuric acid concentration on leaching extent of U3O8 and TiO2 upon
leaching the ground ore to 74 Am with H2SO4 in ore to acid ratio of 1:2.5 at 200 jC for 2 h.

ing above atmospheric pressure, or fusion at high trations of 1.88 and 4.68 M, respectively, even in the
temperature. However, the sulfuric acid leaching proc- presence of NaClO3 as oxidant.
ess is commonly applied on the Australian davidite Examining the results in Table 4, it is possible to
concentrates of Radium Hill, at atmospheric pressure say that the decomposition of the refractory niobium –
(George, 1958a). tantalum minerals (euxinite, samarsakite and fergu-
On the other hand, leaching euxinite mineral from sonite) were mainly affected by sulfuric acid concen-
Norway (George, 1958b) under milder conditions tration as well as leaching temperature. Gupta and
than that of Kab Amiri resulted in 12% and 48% Suri (1994c) reported that concentrated sulfuric acid
leaching extent of uranium at sulfuric acid concen- was used for direct leaching of Indian samarsakite
226 O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229

Fig. 5. (a) Effect of agitation time on leaching extent of Nb2O5, Ta2O5, REO and ThO2 upon leaching the ground ore to 74 Am with 10.8 M
H2SO4 in ore to acid ratio of 1:2.5 at 200 jC. (b) Effect of agitation time on leaching extent of U3O8 and TiO2 upon leaching the ground ore to
74 Am with 10.8 M H2SO4 in ore to acid ratio of 1:2.5 at 200 jC.

under nearly similar conditions to those performed 1993). It was reported that (Gshneidner, 1999) the
upon Kab Amiri ore. It was found that both niobium recovery of rare earth elements is applied on indus-
and tantalum remained as insoluble residue, while trial scale, at the expense of uranium and thorium.
thorium, rare earth elements and uranium were trans- Utilizing sulfuric acid on leaching the quartz albite
ferred to the leach liquor. It is worth mentioning that vein dikes and the pegmatite dikes of Bokan Moun-
lower concentrations of sulfuric acid are recommen- tain, Alaska USA, causes the dissolution of more
ded to leach niobium – tantalum minerals (Lerner, than 74% of yttrium, cerium and lanthanum of the
1961). ore.
Increasing the concentration of sulfuric acid, In view of the foregoing results, the optimum
under atmospheric pressure at 200 jC, or mixing conditions for leaching Kab Amiri ore is to mix
with nitric acid has no great influence in improving the ground ore to 74 Am with a mixture of 10.8
the leaching efficiency of both U3O8 and TiO2 (Table M sulfuric acid and 5.3 M nitric acid in a ratio of
4) due to the fact that both elements are incorporated 1:3 for 2 h leaching time at 200 jC. The obtained
in the primary uranium mineral davidite (Ammar, leach liquor contains: 99.50% of Nb2O5, 93.38% of
O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229 227

Fig. 6. (a) Effect of ore to acid ratio on leaching extent of Nb2O5, Ta2O5, REO and ThO2 when the ground ore to 74 Am was mixed with 10.8
M H2SO4 at 200 jC for 2 h. (b) Effect of ore to acid ratio on leaching extent of U3O8 and TiO2 upon mixing the ground ore to 74 Am was
mixed with 10.8 M H2SO4 at 200 jC for 2 h.

Ta2O5, 70.00% of REE oxides, 76.32 % of ThO2, acid leaching, but also the associated elements such
48.44% of TiO2 and 44.98 % of U3O8 contents in as rare earth elements, thorium, uranium and tita-
the ore. nium in Kab Amiri ore. All these elements have
great commercial value in metallurgy and nuclear
industries. Thus, the recovery of each element indi-
4. Conclusion vidually from their leach liquor is a most interesting
task.
This work is devoted to the study of the behav- From the present study, it became evident that Kab
ior of not only niobium and tantalum using sulfuric Amiri ore of multi-oxides minerals (euxinite, samar-
228 O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229

Fig. 7. Effect of HNO3 concentration on leaching extent of Nb2O5, Ta2O5, REO, ThO2, TiO2 and U3O8 upon leaching the ground ore to
74 Am with 10.8 M H2SO4 in ore to acid ratio of 1:3 at 200 jC for 2 h.

sakite, fergusonite, davidite and zircon) decomposes with a mixture of sulfuric acid of concen-
in sulfuric acid media. The results obtained from the tration 10.8 M and nitric acid of concentration
laboratory experiments can be summarized as follows: 5.3 M in a ratio of 1:3, and heating for 2 h at
200 jC.
(1) Sulfuric acid leaching of Kab Amiri ore (3) Under the mentioned conditions, almost
material was found effective for the dissolu- complete recovery of both niobium and
tion of the economic elements in the leach tantalum has been achieved while the leaching
liquor—with the added advantages of mini- extents of thorium and total rare earth
mum acid consumption—and convenience for elements were 76% and 70%, respectively.
further extraction procedures. (4) The recovery of both uranium and titanium
(2) The optimum leaching conditions were ob- did not exceed 60% during the leaching
tained by mixing the ground ore to 74 Am process of niobium –tantalum minerals, even

Table 4
Effect of temperature and acids concentrations on leaching extent of the economic elements composing Kab Amiri ore
Temperature Acid concentration (M) Ratio Elements concentration (%)
(jC) H2SO4 HNO3 (wt/vol) Nb2O5 Ta2O5 REEa ThO2 TiO2 U3O8
63 10.8 0.0 1:2.5 28.34 21.19 21.11 31.58 3.57 9.61
14.4 0.0 1:2.5 30.07 18.71 23.33 63.16 2.32 6.11
18.0 0.0 1:2.5 29.21 20.20 48.89 63.16 4.84 6.55
200 10.8 0.0 1:2.5 96.47 86.34 66.67 68.42 45.47 25.76
14.4 0.0 1:2.5 90.28 45.45 61.11 63.16 55.92 13.93
18.0 0.0 1:2.5 73.45 30.30 61.11 63.16 44.73 7.86
200 10.8 0.0 1:3.0 97.77 90.00 72.11 72.11 44.64 17.90
10.8 5.3 1:3.0 99.50 93.38 76.32 76.32 48.44 44.98
10.8 6.4 1:3.0 85.83 84.52 84.21 84.21 44.64 32.31
a
REE calculated as rare earth elements oxides.
O.M. El-Hussaini, M.A. Mahdy / Hydrometallurgy 64 (2002) 219–229 229

in the presence of an oxidant. This is Symposium on Tantalum and Niobium, Germany. Tantalum –
attributed to the fact that they are mainly Niobium International Study Center, Belgium, pp. 51 – 64.
El-Hussaini, O.M., 1996. Extraction of niobium and tantalum ele-
incorporated in the refractory mineral davi- ments from some Egyptian ore materials. PhD Thesis, Faculty
dite. of Science, Cairo University, Egypt.
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