You are on page 1of 9

Minerals Engineering, Vol. 3, No. 5, pp. 473-481, 1990 0892-6875/90 $3.

00 + 00
Printed in Great Britain © 1990 Pergamon Press pic

BATCH FLOTATION TESTS BY FATTY ACID ON A PHOSPHATE-IRON OXIDE-


SILICATE REGOLITH ORE SAMPLE FROM SOKLI, FINLAND

WANG Q U N a n d K . HEISKANEN

Lab. of Mineral and Particle Technology, Helsinki University of Technology,


SF-02150 Espoo, Finland
(Received 18 September 1989: accepted 20 November 1989)

ABSTRACT

Batch flotation tests were conducted on a phosphate-iron oxide-silicate regolith


sample using fatty acid as collector. Sodium silicate and other potential
depressants were tested. Sodium silicate is a selective depressant in the
flotation o f apatite from silicate and iron oxide minerals. But there are still
difficulties in obtaining low iron-containing apatite concentrate.

Keywords
Apatite flotation; iron oxide; silicate; fatty acid; sodium silicate; depressants

INTRODUCTION

Beneficiation of phosphate ores is one of the important research subjects in mineral


processing in the world. Because of the large occurrence and many problems in separation,
most of the attention has been put on the separation of apatite from silicate and/or
carbonate minerals, and much progress has been made in the last decade [1].

Magnetite is one of the often associated minerals in the endogenic phosphate ores [2]. The
separation of magnetite from apatite is normally not difficult by magnetic separation [3,4],
but the presence of hematite or other non-magnetic iron oxide minerals, e.g., limonite,
goethite, and siderite, which might be the oxidation or weathering products of magnetite,
could cause difficulties in obtaining low Fe-containing apatite concentrate. In this case, tall
oil flotation [3,4] and magnetizing roasting [5] have been employed. Another case related to
the separation of apatite and iron oxides is the Swedish phosphate-containing hematite ores
[61.
Sokli carbonatite complex is located in north-east Finland. Its economic mineral occurrences
can be divided into two main types on the basis of their mode of occurrence. Phosphorus
ores occur in the weathered upper part of the complex and pyrochlore and apatite-magnetite
occurrences in the deeper parts of the massif. Apatite-francolite regolith is a major part of
the phosphorus ores. It is a loose, light to dark brown material. Its mineralogical and
chemical compositions vary. The main residual primary minerals and secondary minerals are
fluorapatite, magnetite, amphiboles, micas, francolite and goethite [7,8], so the separation
of phosphate, iron oxides and silicates is required.

Batch flotation tests, after desliming and magnetic separation, were conducted in the
laboratory on a Sokli regolith sample, with fatty acid as collector.
473
474 WANGQuN and K. HEISKANE~

EXPERIMENTS

Material

A so-called "Sokli A" phosphate regolith ore sample was obtained from Kemira Oy, Finland.
In the sample, the main minerals could be liberated easily at a coarse size, but the optical
microscopic examination of powder thin slidesshowed that the surfaces of a certain amount
of apatite particles were contaminated by iron oxide. A n X R F analysis for a sample of
"Sokli A" is shown in Table I. From the data it can be seen that the sample is a rich
phosphate ore, containing iron oxides and silicatesas main gangue minerals.

T A B L E 1 X R F analysis of Sokli A sample


Elements NeD MgO AI203 SiO2 P205 K20 (tO TI V Cr

Assay,% 0.42 2.78 2.95 7.26 23.1 0.126 30.0 0.524 0.020 0.011

Elements Mn Fe Zn Sr Zr Nb Ba La ~ C

Assay,% 0.576 16.1 0.069 0.309 0.081 0.212 0.176 0.093 0.195 0.36

Reagents

Industrial grade sodium silicate (liquid) with nominal concentration of 35-45% was used in
the tests and a concentration of 40% was used in the calculation of the dosages. An
industrial grade distilled tall oil type collector "Fatty Acid" from a Finnish forest industry
company Enso-Gutzeit Oy was used. Dowfroth 250 was used as the frother and the dosage
was fixed at 39 g/t. The above three reagents were added into the flotation cell in their
original liquid state. Other reagents used in the tests were all analytical grade chemicals. The
dosages of the reagents were based on the sample weight before grinding. NaOH and H~SO4
were used to regulate and control the pulp pH. The pH just before flotation was taken as
the flotation pH.

Methods

The sample was dried and then crushed to -4 m m by a laboratory cone crusher. The
crushing product was divided into I kg samples by riffling for batch flotation tests.The
sample was ground, deslimed, and magnetite removed before flotation according to the
procedure shown in Figure I.

Sokli A sample 1 kg
I
Rod mill grinding
I
Deslimin~
I*
Magnetic separation
I
Desliming

-I I+
Slime Flotation feed Magnetic product
Fig.1 The flotation feed sample preparation procedure
Batch flotation tests by fatty acid 475

The samples, of 1 kg, with solid concentration 50%, were ground in a laboratory rod mill.
The grinding time was fixed at 6 rain. 1 ml liquid sodium silicate (35-45%) was added into
the mill in grinding.

The grinding products were deslimed by decantation in a flotation cell (3.0 litre) after
agitation and 7 minutes sedimentation. Wet sieving in an ultrasonic bath showed that the
slime was 94% -38 pro. Magnetite particles in the samples were removed in the flotation
machine using a weak electromagnetic device made by the laboratory.

The X R F analysis and the SiOz, PzO5 and Fe distributions of the Sokli A sample, slime,
magnetic product, and the flotation feed are shown in Table 2. The size distribution of
flotation feed is shown in Figure 2. The -38 /~m slime fraction in the flotation feed is
10.6%.

TABLE 2 Assays and distributions in flotation feed preparation products


Elements % Distribution %

Products Wt% I~ AI203 S i O 2 P205 C~O Fe SiO2 P205 Fe

Slime 26.3 7.22 6.37 15.94 17.1 23.3 22.3 47.3 21.0 34.3
Magnetic 9.9 2.35 1.69 4.57 11.5 14.6 44.8 5.1 5.3 26.0
Flot. feed 63.7 2.62 2.80 6.62 24.9 31.3 10.7 47.6 73.8 39.9
Sokli A* 99.9 3.80 3.63 8.87 21.5 28.4 17.1 100.0 100.1 100.2

* Calculated results from slime, magnetic product, and flotation feed.

I00

,2 8o

> 60
09
40

20

0
i0 ~ 10 2 10 3

Size, micron
Fig.2 Size distribution of the flotation feed

Flotation tests were conducted in a Denver flotation machine with a 3 litre cell. The
conditioning times for modifying reagents and for collector were all 5 minutes and for
frother 1 minute. Flotation times were controlled according to the foam layer condition.

The flotation concentrates were analyzed by XRF. The flotation recovery was calculated
based on the sum of the weights of the concentrate and tailings and the flotation feed
analysis is listed in Table 2.
476 WANG QUN and K. HEISKANEN

RESULTS

Fatty acid flotation without dispersant and depressant

The results of the flotation without any dispersant and depressant in different pH media and
using different collector dosages are shown in Figures 3 and 4. It can be seen that in
moderate alkaline pH and with relatively high collector dosage there is some selectivity
between apatite and silicates and iron oxides. The floatability of apatite is higher than that
of iron oxides and silicates.

I00
[] P205
80 • SiO2
[] Fe
60 pH 9
~4
CD
> 40
o
o
20

l l i I "' " l l

0 200 400 600 800 i000 1200 1400


F a t t y Acid, g/t
Fig.3 Recoveries of P205, Fe and SiO 2 in flotation with different "Fatty Acid" dosage

i00

o~O 80

0) 60
-4
©
> 40
o
O
W m P205
20 • SiO2
"Fatty Acid" 850 g/t [] Fe
0 I ! | I " I ' I g
I

5 6 7 8 9 i0 ii 12
pH
Fig.4 Recoveries of P2Os, Fe and SiO 2 at different pH

The effect of sodium silicate

Sodium silicateis used as a depressant of silicateand iron oxide minerals. From Figure 5 it
can be seen that at p H 9 the use of sodium silicatesignificantly improved the flotation
selectivity. When the dosage of sodium silicate increased from 0 to 2500 g/t. the SiO 2 and
Fe recoveries decreased from 70% to 40% while the P2Os recovery was little affected, but
Batch flotation tests by fatty acid 477

further higher sodium silicate dosage also depressed apatite. The effect can also be seen
from the change in the flotation concentrate quality (Fig. 6). The effect of sodium silicate
at pH 11 was not selective (Fig. 7).

One test was conducted at pH 9.0 with one cleaner stage of flotation with sodium silicate
2650 g/t and "Fatty Acid" 1280 g/t. In the cleaning stage no more chemical except for a
drop of frother was added. A cleaner concentrate with 2.92% SiO2, 35.1% P205 and 4.13%
Fe, and with P recovery 65.3% was obtained.

I00

80

.~ 60

8 40

20

0
0 1000 2000 3000 4000
Sodium silicate, g/t
Fig.5 E f f e c t o f s o d i u m silicate dosage o n t h e r e c o v e r i e s o f P 2 0 s,
F e a n d SiO2in flotation a t p H 9

Si20, Fe P205

I
g

. i !!

0 I000 2000 3000 4000


S o d i u m silicate, g/t
Fig.6 E f ~ c t o f s o d i u m silicate dosage on the concentrate grades of P2Os,
Fe and SiO2offlotation a t p H 9

The effects of sodium hexametaphosphate ([NaPO3] 6)


The effect of another effective dispersant, sodium hexametaphosphate, was tested and the
result is shown in Figure 8. It can be seen that [NaPO3] 6 can improve the selectivity between
apatite and silicates, but not between apatlte and iron oxides. When the dosage of [NaPO3] 6
is high, apatite, silicates and iron oxides were all totally depressed. The affinity of
polyphosphate ions on the Ca sites might be the reason for the depression of apatite.

] H E 3/~,--~F
478 WANGQUNand K. HEISKANEN

i00
"Fatty Acid" 1280 g/t
pH II
~o 80

.~ 60

~ 40
P205
20 SiO2
[] Fe
0 |

0 i000 2000 3000 4000


Sodium silicate, g/t

Fig.7 E f f e c t o f s o d i u m silicate dosage on t h e r e c o v e r i e s o f P205,


Fe and S i O 2 0 f f l o t a t i o n a t p H II

i00
m P205
80 o SiO2
. m Fe
60

40
o

20

0
0 200 400 600 800 i000 1200
[NaPO3] 6, g/t
Fig.8 Effect of [NaPO3] 6 dosage on the recoveries of P205,
Fe and SiO 2 in flotation at pH 9

The effect of EDTA

One of the possible reasons for the loss of flotation selectivity might be that the Ca** ions
dissolved in the pulp activated the silicate minerals and iron oxide minerals. The effect of
a strong chelator EDTA (ethylene diamine tetraacetic acid) was tested and the result is
shown in Figures 9 and 10. It can be seen from the figures that EDTA did not have a
significant effect on the flotation with the used dosages.

Effects of other depressants

Nine different depressants other than sodium silicate were preliminarily tested. The results
are summarised in Table 3, which shows that K2CrO4, tannic acid, and dextrin can also
selectively depress silicate and iron oxide minerals.
Batch flotation tests by fatty acid 479

i00 ' "


1..
~o 80

® 60
-,--I
@
>
O 40
~J
(1) [] P205
• SiO2
20 I pH 9
[] Fe "Fatty Acid" 1280 g/t
0 , ,
0 i00 200 300
EDTA, g/t

Fig.9 Effect of EDTA dosage on the recoveries of P~.O5, Fe and SiO 2


in flotation at pH 9 and without sodium silicate

I00
B P205
do 80 SiO2
B Fe
(D 60 pH 9
-,-I
0)

20 "Fatty Acid" 1280 g/t


Sodium silicate 2650 g/t
0
0 100 200 300
EDTA, g/t
FIg.10 Effect of EDTA dosage on the recoveries of P205, Fe and SiO2
in flotation at pH 9 and with sodium silicate

TABLE 3 Summary of depressants tests*


Flotation ~ i=lotatlan R~m~yerleR%
Depressant ~ ~ ~/t. % SIO2 P2¢~ Fa SIO2 P'J(~ F~

None 0 8.7 68.5 5.71 28.0 7.34 59.0 77.0 47.1


Oxalic add 1000 6.5 85.2 6.02 27.6 8.48 77.4 94.5 67.5
K2Cr207 200 9.2 26.4 6.16 25.0 9.52 24.7 26.6 23.6
K2CrO4 100 7.0 64.3 4.85 30.3 6.88 47.1 79.4 35.4
Q~C 1000 8.7 49.9 4.83 29.2 5.93 36.4 56.6 27.7
Corn starch 1000 8.9 69.0 5.04 29.3 6.17 52.5 61.1 39.8
BS-N *° 1000 9.1 55.8 5.11 29.0 5.42 43.1 65.1 28.3
Quebracho 1000 9.3 14.3 6.45 22.5 6.35 14.0 13.0 8.5
Oextrln 1000 9.3 84.7 5.96 27.6 6.30 76.2 94.2 65.6
Dextrin 1000 9.2 47.6 4.61 29.3 4.01 33.1 56.0 17.8
Tannlcacid 1000 8.9 49.2 5.18 29.3 4.03 38.6 58.1 18.5
Sodium silicate1060 9.2 34.0 3.92 32.5 2.12 20.2 44.5 9.1

* Flotation after 4 times desllming, "Fatty Acid" 850g/t


**Borresperse N, a Ungnosulphonate mixture.
480 WANG QUN and K. HElSKANEN

DISCUSSION

In phosphate ore processing, Sokli ore is a special case which has the problem of the
separation of apatite and non-magnetic iron oxide minerals, which occur from the
weathering of the deposit that caused the oxidization of magnetite into goethite. Only one
similar case has been found in the literature, which is the Sukulu deposit in Uganda with
the weathered ore mainly being composed of apatite, magnetite, hematite, hydrated iron
oxides, and quartz [3].

Du Rietz [9] discussed the separation of apatite and iron oxides by fatty acid flotation. It
was indicated that apatite may be easily floated from iron oxide minerals by oleate above
pH 8 from the viewpoint of the solubility products of the Ca +* and Fe 3+ fatty acid soaps.
In the case of Sukulu, apatite was successfully floated from iron oxide minerals and silicates
by sodium oleate at pH 10 after desliming and magnetic separation [3].

But from the above tests results for Sokli ore, it can be seen that the floatability of iron
oxide is not far from that of apatite, even in the alkaline pH range and after desliming. The
reasons might be that the surface iron oxide contamination decreased the floatability of
apatite, and Ca ``+ ions dissolved from the apatite surface activated the flotation of silicate
and iron oxide minerals causing the unselective bulk precipitation of calcium fatty acid soap
onto the minerals, the high collector dosage required in the tests implying both of the
reasons. The residual slime in the pulp also caused a decrease in selectivity. Comparing the
results in Figures 5 and 6 and in table 3 for sodium silicate depression, it can be seen that
the desliming degree strongly effected the flotation selectivity.

Sodium silicate is an effective slime dispersant and silicate depressant. It is also used to
improve the flotation of apatite from iron oxide ores [10]. In the above test results, sodium
silicate appears the most selective modificant (see Table 3). The possible mechanism of
selective depression might be that the adsorption of polysilicate polymer onto the
hydroxylated site on the surface of silicate and iron oxide minerals induced the increase in
surface hydrophilicity and slime dispersion. The over dosage also caused the depression of
apatite.

In order to obtain high apatite recovery with high concentrate quality, cleaning and
scavenging are essential. The laboratory batch flotation test with one cleaning stage
increased the P205 content in the concentrate from 32.1% to 35.1%, and decreased the Fe
content from 6.40% to 4.13%. The iron content in the concentrate is still high. It was found
that some Fe-containing phosphate minerals are present in the ore [8]. The floatability of
these minerals is still a question, which might be another factor which caused the high iron
content in concentrate.

Fatty acid collectors are relative cheap reagents, but desliming for fatty acid flotation is
usually required. In the case of the tested sample, About 20% phosphate was lost in slime.
The selective desliming by selective flocculation is worthy of study.

CONCLUSION

Sodium silicate is an effective selective depressant and dispersant in the fatty acid flotation
of apatite from silicates and iron oxide minerals in Sokli phosphate ore. But there are still
difficulties in obtaining low iron-containing apatite concentrate.

The depressive action of sodium hexametaphosphate is not selective between apatite and
iron oxides. EDTA did not have a significant effect on the flotation of the ore under the
dosages used in the tests. Another nine depressants were also tested, and among them
K2CrO4, tannic acid, and dextrin showed promising selective depression.
Batch flotation tests by fatty acid 481

ACKNOWLEDGEMENTS

The authors are thankful to Kemira Oy for the delivery of the tested sample and its
mineralogical information. One of the authors (WQ) would also like to acknowledge the
scholarship provided during the research period by the State Commission of Education of
P. R. China

REFERENCES

. Moudgil B.J. & Somasundaran P., Advances in Mineral Processing (Arbiter Sym.),
p.426, SME/AIME, Littleton (1986).

. Houot R., Inter. J. Miner. Process., 9, 353 (1982).

3. Fleming M.G. & Robinson A.J., IMPC (London), paper VIII-47, IMM (1960).

4. Betz E.W., Mineral processing (Proceedings of 13th IMPC, Warsaw 1979), p. 1846
Elsevier, Amsterdam (I 981 ).

. Cohen E. & Hammoud N.S., Mineral processing (Proceedings of 13th IMPC, Warsaw
1979), p. 1828, Elsevier, Amsterdam (1981).
. Kihlstedt P.G., Progress in Mineral Dressing (Trans. Inter. Miner. Dress. Congr.,
Stockholm), 559, Almqvist & Wiksell, Stockholm (1958).
. Vartiainen H. & Paarma H., Economic Geology, 74, 1296 (1979)

8. Vuotovesi T., X-Ray Diffractometric Analysis of Composition of Three Ore Sample


from Sokli. Research Report (in Finnish), Kemira Oy (1988).
. Du Rietz C., Progress in Minerals Dressing (Trans. Inter. Miner. Dress. Congr.,
Stockholm), 417, Almqvist & Wiksell, Stockholm (1958).
10. Bolin N.J., Scand. J. Metal., 12, 246 (1983).