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Патент USA US2105807

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2,105,807
Patented Jan. 18, 1938
UNITED STATES PATENT OFFICE
2.105.807
DIITERENTIAL CONCENTRATION OI." NON
~
METALLIC MINERALS
Arthur Crago, Mulberry, Fla., aalignor to Phos
phate Recovery Corporatiom-New York, N. Y.,
a corporation of Delaware
I
No Drawing. Application February 15, 1933,
Serial No. 656,887
5 Claims.
-
(Cl. 209-167)
The present invention relates in general to a
concentration of non-metallic minerals from
their ores, and more particularly to a process
of differential concentration applicable to ores
' of the class consisting of phosphate-calcite-silica
ores, ?uorspar-calcite-silica ores, and ?uorspar
barite-silica ores.
In accordance with the invention, a pulp of
the ore to undergo treatment is agitated in the
9 presence of a fraction of one per cent of a free
fatty acid and a fraction of one per cent of a
substantially insoluble and unsaponi?able 011,
without added agents capable of substantially
affecting its pH value, the desired concentrate
5 being subsequently separated by froth ?otation
or other manner known in the art.
By this
procedure omitting the use of alkali or other
pH-affecting substance, it has been found possi
ble to differentially concentrate one non-metallic
‘0 mineral with- respect to both another non-metal
lic mineral and siliceous gangue. Either phos
phate or ?uorspar can thus be separated from
both calcite and silica; and ?uorspar can be
separated from both barite and calcite. It has
35 also been found possible to separate calcite from
silica by the process of the present invention.
In order that the best results may be obtained
agitation being conducted in a subaeration-?o
tation laboratory testing machine, and the slimes
removed by decantation. The deslimed pulp was
thickened to contain 72% solids, and then there
was added during further agitation- 0.28 pound
of a solution of ?sh-oil fatty acids in an equal
weight of fuel oil, enough more fuel oil to make
a total of one pound of fuel oil, and 0.14 pound of
a frothing agent consisting of three parts of
10
crude rosin residue dissolved in one part of ker
osene oil, all per ton of dry material present.
The pulp showed a pH value of 7.4.
After three minutes agitation the thick pulp
was then diluted and agitated in the machine 15
for the production of a froth over a period of
three minutes, a rougher ?oat concentrate being
separated. The tailing was discarded and the
rougher concentrate cleaned four times by re
agitation without added agents. The tailing 20
from each cleaning was assayed separately, but
constituted a middling which, in commercial
operations, could be returned to the ?otation
cells for additional recovery of values therefrom.
The results are shown in the foliowingtable:
‘
Percent
Percent
Percent
CaF:
sic,
Percent :égoF’
02.0 0.
ered"'
______ _
by the process of the present invention, it has
been found advisable to limit rather narrowly
30 the size of the ore particles subjected to the con
centrating operation, as well as to largely de
Feed __________ -_
100. 0
52. 76
9. 11
37. 37
Finished cone. __
32. 3
98. 38
0. l8
0. 88
4th midd ...... __
2. 4
94. 48
0. 16
slime the ore pulp prior to its admixture with
3rd m1dd__-____._
1st and 2d mldd-
3. 5
l6. 4
87. 54
51. 60
0. 00
0. 51
12.24
47. 48
'5; 7
16.
the reagents.
Tails __________ -.
Slimes ________ --
35.
10. 4
10.02
34. 64
23. 42
7. 45
65. 57
55. 29
6. 8
6. 8
In preparing the ore for treatment by the
35 process of the present invention, it is ordinarily
?rst subjected to a preliminary grinding opera
tion and is thereafter screened or classi?ed to
remove all particles other than those desired.
The undersize may then he deslimed and the
40 oversize reground, deslimed, and added to the
deslimed undersize; or the oversize may be re
ground, added to the undeslimed undersize, and
the whole then deslimed.
The procedures herein described in detail are
45 ?otation procedures, but in many cases parallel
results may be obtained by effecting the concen
trating operation on a shaking table, the concen
trate coming off at the side of the table as if it
were the lighter material and the tailing at the
50 end as if it were the heavier material.
Other features and advantages will appear in
connection with the examples described below.
Ground crude ?uorspar ore from Hillside
Fiuorspar Mines, Rosiclare, Illinois, with a
55 gangue principally of calcium carbonate, but
containing some silica, was screened through 35
mesh‘, the oversize being ground to pass 35-mesh
and added to the undersize; The resulting mix
ture was agitated in a relatively large amount of
69 water to facilitate removal of the slimes, the
5.05 \
30
60. 4
4. 3
35
Other fatty acids, such as oleic acid, have also
been found useful as reagents.
Fluorspar carrying more than 2% of silica
yields so much ?uosilicic acid as to be useless 40
for. the production of hydro?uoric acid. As a
result of this and other reasons, ?uorspar con
taining upwards of 98% of calcium ?uoride com
mands at least double the price of the spar car
rying only 96% of calcium ?uoride. It has 45
hitherto proved impossible to produce a 98%
?uorspar from the relatively impure material
generally mined. According'to the present in
vention, by a suitable choice of, reagents it has
proved possible to obtain a satisfactory so-called 50
acid spar, as shown by the example given above.
A phosphate ore from North Africa,pknown as
Constantine rock, with a gangue largely of cal
cium carbonate, was raised from uncommercial
grade to commercial grade by ?otation with fuel 55
oil and a soap-forming fatty acid.
The ore was
ground to pass a 35-mesh sieve, and deslimed by
agitation with water and decanting the slimes. '
The wet deslimed material, in a pulp containing
‘72% of solids, was mixed with one pound of fuel 60
2
9,105,807
oil, one pound of crude oleic acid (red oil) and
0.14 pound of the kerosene-rosin solution above
identified. all per ton of. dry material present.
The thick pulp was diluted and agitated in the
Thedetailedresultsandasaayar
‘
arelhcwnln,
the following table:
Per-
?otation machine, and a rougher froth concen
trate was separated. Upon removal of the tall
ing, the rougher concentrate was put back into
.
00.
3.11..
B.P.L. Ins. 004 m
20:;_
the machine and reagitated without added
agents for two minutes, and thereafter a finished
or cleaned concentrate was separated. The re
sults are shown in the following ‘table. in which
the tailing from the cleaning operation is‘desig
nated as a middling.
'
-
'
use 141
11.51 .............. ..
10.67 1.21
00.40 1.00
as“ 11114
sass 1am
sass
an
11.10
11.00
1.s
70.1
a4
1111
1a:
an
a1
40.4
oass- an
0.11:
042
40.0
can an;
7.0a
112.4
41.4
A lot of phosphate ore from Consolidated Inn
ing and melting Co., of Trail, 3. 0., had to be 15
cent
Wt.
B. P. L.
00004
Ins.
'
'
'
mm
recov
cry
ground to pass ZOO-mesh to free the silica gangue.
The ore was then treated to remove part of a
56. I8
26. 8
O. 70
68. 56
17.66
E. 92
14. 8
I. 7
66. 2
40. 6
s. 26 ................ -.
0. 99
l. 42
15.6!
19. 3
72. 0
18.8
1.0
12. 2
82. 9
18. 0
15.4
8S. 1
It was found that better results were some;
times obtained when solid fatty acids of ?sh
oil. dissolved in part of the fuel oil, were sub
stituted for the oleic acid.
By slightly varying conditions, it was found
possible to float limestone away from silica. A
mixture consisting of one part Ocala limestone,
largely calcite, and about three parts of the tail
ings from a mill of the Phosphate Recovery Cor
poration treating Florida pebble phosphate, was
screened through 24-rnesh, and the oversize
ground to the same mesh and added to the under
size. The rmulting material was deslimed by
agitation with water and decantation, and thick
ened to contain 70% solids. The thick pulp was
calcium carbonate gangue, whereupon a phos
phate concentrate was separated. To eifeet these
results the ground ore was deslimed by agitation
with water and decantation. The deslimed ma
terial in the state of a thick pulp was agitated
with 2.5 pounds of fuel oil, 0.84 pound of crude
oleic acid, and 0.28 pound of Tarol No. 2 (a mix
ture of 75% steam distilled pine oil and 25% rosin
oil by volume), all per ton of deslimed solids.
The material thus conditioned was diluted and
frothed to separate a small weight concentrate.
richer in the carbonate and poorer in the phos
phate. The remaining pulp was thickened and 30
agitated with 0.2 pound of caustic soda, 4 pounds
of fuel 011, 0.84 pound of crude oleic acid, and
0.14 pound of the frothing agent above referred
to as Tarol No. 2, all per ton of solids, whereupon
it was diluted, and a phosphate ?oat concentrate
separated.
Thedetailedresultsandassaysareshownin'
the following table:
agitated for three minutes with 2 pounds of fuel
oil and 0.53 pound of crude oleic acid, both per
ton of dry material present, the pH value of the
at?
pulp being 7.8. No bubble-forming‘ agent or
other added ?otation agent was found necessary.
The oiled pulp was diluted and frothed in the
?otation machine for one minute, during which
a calcium carbonate ?oat was separated. The
results are shown in the following table:
Percent
wt.
100
22
78
Area
4
O9
$35%? ? $28 ! sway-9 883823 5
0 E
88
ee
C 001
0008' In" reohvery
23. 04
90. 64
B. P. L.
4. 10
86. 6
18. 6
The foregoing procedure raised the B. P. L. con
tent to a grade of commercial utility.
By a somewhat modified procedure ?uorspar
has been separated from barite. A table feed
?uorspar ore carrying calcium carbonate, from d5
Hillside Fluorspar Mines, Rosiclare, 111., was
. The tailings were evidentlymostly silica, which
was the principal ingredient of the phosphate
tailings put into the original mixture.
Another lot of the same Constantine ore was
mixed with an equal weight of deslimed barite
ore from Paga Mining Co., Cartersville, 6a., and
the mixture ground to pass 35-mesl1. The ground
material was deslimed by agitation for a three
around to pass 65-mesh, and deslimed by agita-' minute period with water and decantation until
tion with water and decantatlon. The deslimed all the slimes seemed to have been removed. The
coarse material in a dilute pulp was. agitated results of the desliming operation are shown in
with 1.20 pounds of sodium oleate and 0.1 pound the following table:’
of pine oil, both per ton of solids, and a carbon
ate ?oat concentrate was ?rst removed. The so
dium oleate was of course a’ soap, produced from
fatty acid and alkali. The tailing remaining was
70 thickened and in this state agitatedwith 1 pound
of fuel oil, 0.5 pound of crude oleic acid, and 0.14
pound of the kerosene-rosin solution above iden
tl?ed, all per ton of original solids in the deslimed
pulp, whereupon it was diluted and a phosphate
II ?oat‘concentrate removed.
Pub
Pceantreoovty
cent
.
.
"i- cm s10. 0.00. peso. Cal‘; “04
2am 20.00
10.11
2.41 I 10a
"5132s" an
0am 2010
.
.
Zl'esd.__.--..- 10o.
1a70
21. 4s
Slime...... .. 12.2 14.40 21.00
2114
211.11
us
1.2
1011.
111
110
pulp of deslimed material was thickened
70
3
2,100,001
to 72% solids and‘ agitated with 0.5 pound of fuel
011, 0.19 pound of ?sh-oil fatty acids, and 0.14
pound of the kerosene-rosin solution'above iden
ti?ed, all per ton of ?otation feed, whereupon it
was diluted and a ?uorspar ?oat concentrate
separated. The ?uorspar rougher concentrate
thus obtained was re?oated four times, in each
instance without the addition of further agents,
to yield a ?nished concentrate of over 98% pm'ity,
10 four cleaner tailings constituting middlings be
barite-silica ores, in the presence of a fraction of
one per cent of a free fatty acid and a fracion of
one per cent of a substantially insoluble and un
saponi?able oil, without added alkali or other
agent capable of substantially aifecting its pH
value; and separating by froth ?otation in the
case of a phosphate-calcite-silica ore a concen
ing obtained which, in commercial practice,
trate relatively rich in phosphate and relatively
would be retreated to yield further recoveries.
The ?uorspar ?nished concentrate contained over
poor in calcite-silica, in the case of a ?uorspar~
calcite-silica ore a concentrate relatively rich in
86% of the ?uorspar in the original material.
15 The rougher tailing resulting from the ?rst ?oat
was rethickened, agitated with 0.32 pound of
caustic soda, 2 pounds of fuel oil, 0.45 pound of
' ?sh-oil fatty acid, and 0.14 pound of the kero
sene-rosin solution above identi?ed, all per ton
20 of solids present, whereupon it was diluted and
agitated to yield a barite rougher concentrate, a
?nal tailing being also obtained. The barite
rougher concentrate was re?oated twice without
added agents to yield a ?nished concentrate, as
25 well as two cleaner tallings constituting mid
dlings. The results are shown in the following
table:
30
am
Pay.
Product
Percent of
ya
NOOVGI'Y
:tnt
'
85
slimes, of suitably divided particles of an ore of
the class consisting of phosphate-calcite-silica
ores, ?uorspar-calciteesilica ores, and ?uorspar
Cal‘, 010, 00001 1311804 car, B01804
0011100110--.. 20.0 0020
Midd
. 0.4 00.01
Midd . 1.0 0010
10.10
21.40 1000
?uorspar and relatively poor in calcite-silica, and
in the case of a ?uorspar-barite-silica ore a con
3. A process of di?erential concentration which I
comprises agitating a pulp, nearly free from
slimes, of suitably divided particles of an ore of
the class consisting of phosphate-calcite-sillca
ores, ?uorspar-calcite-silica ores, and ?uorspar
barite-silica ores, in the presence of a fraction
of one per cent of a free fatty 0010 and a frac
tion of one per cent of a substantiallynnsoluble
and unsaponl?able oil. without added 'alkali or
other agent capable of substantially affecting its
pH value, the fatty acid being carried in at least
a part of the oil; and separating in the case of
a phosphate-calcite—siiica ore a concentrate rel
100.0
0.00 - 1.00
0.42
21.01
0.00
00.00
0.10
4.04
10.40
02.0
1.0
1.0
0.1
01
01
calcite-silica, in the case of a ?uorspar-calcite
silica ore a concentrate relatively rich in ?uor
spar and relatively poor in calcite-silica, and in
the case of a ?uorspar-barite-silica ore a con
centrate relatively rich in ?uorspar and relatively
poor in barite-silica.
_
MidcL?-
2.0 21.10
1.00
41.01
04.42
22
01
MiddJl-
0.0
4.10
41.00
40.00
1.0
10.0
_ 30001103111105. 04.0 000 14.00
#2__.'- 0.4 000 01.00
01.04
0.02
40.00
0.10
00
01
14.2
0.0
prising agitating a pulp, nearly free from slimes,
of suitably divided particles of a phosphate-cal
cite-silica ore in the presence of, a fraction of
one per cent of a fatty acid soap and a fraction
40
M100.
#1--.-
4.00
.
00 020 00.04
Tall ......... .. 10.0
0.40 0012
000
004
00
00
002
0.00
0.0
0.0
The barite concentrate thus obtained maybe
further treated to raise its grade. It will be noted
45 that 86.1% of the original ?uorspar was re
covered in the form of a concentrate carrying
98.28% of ?uorspar and conforming to the most
exacting commercial demands.
Having thus described certain embodiments
50 of the invention, what is claimed is:
1. A process of differential concentration which
comprises agitating a pulp, nearly free from
of one per cent of a substantially insoluble and
unsaponiflable oil ; separating a ?oat concentrate
relatively rich in calcite and relatively poor in
phosphate-silica: dewatering the remaining pulp;
agitating the dewatered pulp in the presence of a '
fraction of one per cent of a free fatty acid and
a fraction of one per cent‘of a substantially in
slimes, of suitably divided particles of an ore of
the class consisting of phosphate-calcite-silica
ores, ?uorspar-calcite-silica ores, and ?uorspar
barite-silica ores, in the presence of a fraction of
prising agitating a pulp, nearly free from slimes,
of suitably divided particles of a phosphate-cal
one per cent of a free fatty acid and a fraction
of one per cent of a substantially insoluble and
unsaponi?able oil, without added alkali or other
60 agent capable of substantially a?ecting its pH
5. A process of differential concentration com
cite-silicaore in the presence of a fraction of one
per cent of a free fatty acid and a fraction of one
per cent of a substantially insoluble and unsa
poni?able oil, without added alkali or other agent
value; and separating in the case of a phosphate
capable of substantially affecting its pH value:
calcite-silica ore a concentrate relatively rich in
separating a small-weight ?oat concentrate richer
phosphate'and relatively poor in calcite~sllica,
in calcite and poorer in phosphate; dewatering
the remaining pulp; agitating the dewatered pulp
in the case of a ?uorspar-calcite-silica ore a con
centrate'relatively rich in ?uorspar and relatively
poor in calcite-silica, and in the case of a ?uor
spar-barite-silica on a concentrate relatively
rich in ?uorspar and relatively poor in barite
70
4. A process of di?erential concentration com
soluble and unsaponi?able oil, without added
alkali or other agent capable of substantially af
fecting its pH value; and separating a ?oat con
centrate relatively rich in phosphate and rela
tively poor in calcite-silica.
silica.
15
centrate relatively rich in ?uorspar and rela
tively poor in barite-silica.
atively rich in phosphate and relatively poor in
’
r000 ......... .- 100.0 20.10 20.10
10
-
2. A process of differential concentration which
comprises agitating a pulp, nearly free from
in the presence of a fraction of one per cent of
a fatty acid soap and a fraction of one per cent
of a substantially insoluble and unsaponi?able
oil: and separating a ?oat concentrate relatively
rich in phosphate and relatively poor in calcite- 7o
silica.
1
ARTHUR CRAGO.
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