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Патент USA US2410377

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2,4i0,377
UNITED STATES PATENT ore-lea
Patented Oct. 29, 1946
2,410,377
BENEFICIATION OF IRON ORES
Robert B. Booth, Springdale, and Earl C. Herken
ho?, Stamford, Conn., assignors to American
Cyanamid Company, New York, N. Y., a cor
poration of Maine
No Drawing. Application June 18, 1943,
Serial No. 491,384
6 Claims. (Cl. 209—166)
1
2
enough, This obviates the necessity of extremely
This invention relates to an improved method.
of bene?ciating iron ore by froth ?otation.
The problem of iron ore bene?ciation has been
accurate pH control and permits a material sav
ing in operating supervision. Although the pH
a serious one because of the low unit value of the
and the nature of the particular acid is not c'rit-'
product and the fact that, while it is not di?icult
ical, there will be optimum conditions for each
particular acid. Another factor which has not as
yet been fully explained is the fact that it is not
to ?oat various iron minerals, the procedures em- I
ployed have resulted in insu?icient recovery of
concentrates suf?ciently rich in iron ore to be
necessary that the actual froth ?otation. take
commercially usable.
place in a circuit which is strongly acid. ‘ On the
According to the present invention we have
found that iron ores can be bene?ciated by the
use of a class of anionic ?otation reagents ob
contrary, if iron ore is conditioned with the hy
drocarbon sulfonates and a suitable acid, the pH
of the flotation circuit may be modi?ed with al
kalies such as soda ash, and, in fact, it is even
possible to ?oat in a weakly, alkaline circuit.’v The
tained from the sulfonation of petroleum hydro
carbons. The cheapest and in many respects
most satisfactory products are the so-called 15 neutralization appears to have but little effect on
the ?otation of the acid conditioned ore. This
green acids which are the water soluble products
permits, with certain ores, operating practically
obtained by the treatment of various petroleum
in a circuit which is not strongly acid,v an im
lubricating oil fractions with sulfuric acid, oleum
portant ‘commercial advantage because ‘strongly
chlorsulfonic acid or other sulfonating agents.
acid circuits require corrosion-proof ?otation ap
paratus, whereas if it is possible to neutralize acid
conditioned ore prior to ?otation only the condi
tioning equipment need be made acid proof, This
the form of hydrocarbon sulfates rather than true
equipment not only represents only a fraction of
sulfonates, that is to say compounds which have
the group SOsH united to a carbon atom. How 25 the total plant, but it is in general of a character
which lends itself readily to economical corrosion
ever, it is customary in the industry to refer to
resistant construction, whereas the ?otation ma
these products as petroleum sulfonates of the
chines themselves are more di?icult to build and
green acid type, and; therefore, throughout the
expensive if they must withstand strongly acid
present speci?cation and claims the term “petro
,
leum sulfonates of the green acid type” will be 30 circuits.
These materials are in the main mixtures of in
determinate composition, and it is probable that ,
a considerable proportion of the green acid is in
used in its common meaning above.
Watér soluble petroleum sulfonates and acid
alone do not appear 'to give optimum results and
'
The _water solublte petroleum sulfonates are
used under de?nite conditions and the present
we have found that conditioning in the presence
of an oil is desirable for best recoveries and
35 grades. It is an advantage of the present inven
tion that the nature of the oil is not particularly
agents generally. According to the present in
critical. Excellent results are obtained with vari
vention the ore must be conditioned with the re
ous hydrocarbon products such as various grades
agent in the presence of a strong acid. The ef
of fuel oil or even crude oil. Since these oils are
fectiveness of the acid treatment is not appar
ently dependent on the nature of the acid anion 40 among the cheapest commercially available ma
terials they may be considered as the preferred
insofar as it does not have a particular depressant
oils to be used in the process of the present in
effect and almost any strong or fairly strong acid
vention. However, other oily materials are ef
may be used, either inorganic or organic. The
fective such as certain fatty acids, mixtures of
limit of effectiveness appears to lie with acids
having an ionization constant of about 10-7. 45 fatty and resin acids such as talloel, esters of
monohydric alcohols and the like. Esters of
Thus carbonic acid gives barely acceptable results
glycerin, while effective, appear to give results
while weaker acids such as boric acid are not sat
which are in most cases inferior to the other oils
isfactory. Sulfuric acid gives excellent results
and, while their use is not critical, for best re
and because of its extremely low cost it is the pre
ferred acid. Certain strongly acid salts appear 50 sults we prefer to use other oils.
invention is limited to their use under such con
ditions and does not cover the use of these re
to have some effect and may be used, although in .
which is a further practical advantage as no new
operating technique need to be learned. It is de
sirable to condition the ore with the ?otation re
agents at high solids, for example from 50-70%
which is standard practice in many ?otation op
acid with the Water soluble petroleum sulfonates
affects the surface of the particles has not as yet
been fully determined and the present invention
is not intended vto be limited to any particular
theory of action. It is important to note that a
valuable practical advantage of the present in—
vention lies in the fact that the pH of the circuit
is not critical so long as the acid used is strong
Conditioning and ?otation procedure is not
materially changed by the present invention,
most cases they are de?nitely inferior to the use
of the acids themselves.
The mechanism whereby the presence of an
erations, particularly those involving reagents
containing relatively insoluble oils such as fuel
60
oil. Thus, the procedure is standard in the ?ota
tion of phosphate rock with fatty acids and
fuel oil. Well known conditioning equipment
2,410,377
,
3
.
4
.
may, therefore, be used and special apparatus is
in the fact that it is not peculiarly’ susceptible to
unnecessary except to the extent that the condi
tioning apparatus at least must be corrosion proof.
It is an advantage of the processof the present
invention that it is not highly sensitive to slimes.
temperature and can be operated with very cold
water. This is of real practical advantage be
cause much of the low grade iron ore for which
the present invention is suitable lies in the north
ern part of the United States where low water
temperatures are the rule at the beginning and
end of the short mining season.
The process of the present invention may be
10 used with water soluble petroleum sulfonates as
In common with almost all froth ?otation opera
tions slimes are a detriment. but in the process
of the present invention desliming need not be
carried to completion, and relatively simple and
hence economical desliming operations are quite
suitable.v It is not necessary to deslime to the
completeness which is required with froth ?ota
tion operations using cationic reagents.
the only reagent except for the conditioning acid
and oil. It is also possible to associate these re
agents with other ?otation reagents. For ex
The
action of the slime appears to be av normal or’
ample, mixtures of the water-soluble petroleum
usual one, that is to say the presence of small 15 sulfonates with oil-soluble petroleum sulfonates,
- amounts of slime increase the amount of reagent
such as the so-called mahogany soaps, give ex
, needed for best results, .and when the amount of
V cellent results.
The use of oil soluble petroleum
the slime becomes large the grade of concentrate
sulfonates is not claimed per se in the present
suffers. While the exact behaviour of slime in
invention, but forms the subject matter of our
the present process is not completely known, it is 20 co-pending application, Serial No. 481,906, filed
reasonable to assume that it is substantially
April 5, 1943.
j
. similar to the action in other froth ?otation
The invention will be described in greater de
, procedures.
tail in conjunction with the following speci?c ex
The lack of sensitiveness to small
amples. In the examples the froth ?otation pro
amounts of slime is of considerable practical
value, as the feed preparation need not he so 25 cedure was standardized. All ?otation was ef
.closely controlled and the cost of desliming equip~
fected in Fagergren ?otation machines operating
.ment may be reduced.
at normal speeds and with normal air intake.
It is an important advantage of the process of
Flotation time was chosen in each case to obtain
the present invention that it is applicable to prac
good results. In every case the conditioning of
ticallyall of the ordinary occurring iron minerals 30 the ore with water soluble petroleum sulfonate
and is not restricted to certain particular .ores.
and acid was effected at high solids, usually about
As in the case of most froth ?otation operations,
60-65%.
however, results will differ with different ores.
The petroleum sulfonates of the present in
It is an advantage, however, that concentrates of
vention include the products of reaction of sul
acceptable grade may be produced from low grade
furic acid or oleum with various petroleum lubri
ore having iron contents of the order of 12 or
cating oil fractions. They do not, however, in
13%. It is also an advantage that the process
clude reaction products of the acid with deriva
is so highly selective that in many casesconcen
tives such as cracking still gases containing ethyl
trates of satisfactory grade are obtainable in a
ene, propylene and similar molecular gaseous
rougher operation- However, with many ores, 40 ole?nes, or light unre?ned fuel stocks, such as
kerosene fractions.
and particularly with many low grade ores, clean
ing is advantageous, and in common with froth
Example 1
?otation experience on other ores the precise
?ow sheet for best results will vary somewhat
from ore to ore and should be chosen in accord
4.5
ancewith best ore dressing practice. The lack
of criticalness of the present process, however,
makes the choice of plant and procedure simple
A low gradeMinnesota iron ore, a reject from
an iron bene?ciation operation, containing iron
largely in the form of hematite with,a small
amount of limonite, having a gangue high in
quarts and containing about 15% Fe was de~
slimed in the conventional manner, and condi
and no .operating 'di?iculties are encountered.
The process of the present invention may be 50 tioned at 60-65% solids with various combina
tions of water soluble petroleum sulfonates with
carried out'in any suitable ?otation machine.
and without sulfuric acid.
Where high outputs are needed, particularly with
The conditioned ore
was then diluted to ?otation density, about 22%
solids, and subjected to froth ?otation with a
single cleaning, except in certain cases where
relatively coarse .ore, we have found that the
use of highly developed ?otation machines of the
mechanical type such as Fagergren ?otation ma 55 no sulfuric acid was used and the rougher con
chines are desirable, but the invention is not lim
centrate was obviously too small to be worth
ited thereto.
cleaning. The metallurgical results appear in
Another advantage of the present invention lies
the following table:
Sulfonate used
Lbs/ton
Concentrate,
percent Fe '
pH of
F no l
S ulfuric
‘
acid
'
Assay
2. 18
None
None
62. 55
19. 70
6. 5
2.18
2. l8
2. l8
2. 18
2. 18
2. 18
2. l8
3. 27
3. 27
2. l8
None
0. 94
0. 51
None
1. 22
None
1. 22
3. 59
3. 59
3. 59
1. 63
None
1. (i3
None
None
1. 63
1. 63
None
1. 63
None
61. 97
60. 35
60. 33
55. 08
49. 95
55. 08
57. 53
59. 05
56. 83
46. 10
43. 00
40. D1
92. 28
16. 76
23. 78
58. 28
78. 42
79. 61
83. 68
18. 63
2. 5
6. 5
2. 5
6. (i
6. 6
2. 8
2. 8
2. 6
2. 4
6. 5
_ _ _ _ . _ _ _ -_
2.18
3. 59
1. 63
'60. 57
79. 56
2. 7
(111 Pout _______________________ _.
2. l4
5. 07
‘1. 63
60. 00
63. 54
2. 6
Source
N ame
L. Sonneborn Sons Inc ________ __
D
Do l _ _ _ _ _ . _
Lbs/ton
1 Contained about 88% sulfonic acids, 10% sulfuric acid, and traces of oil.
oil
D‘15 t n'b u tunings
tion
‘2,410,377
5
6
It will be apparent that both acid and fuel oil
are necessary for good'results and that water 501
uble petroleum sulfonates from a wide variety
‘1:1 mixture of'SP-702 andSonesal was used.
The amount of sulfuric acid in every case was 1.63
lbs. per ton. In all cases a rougher concentrate
was removed and cleaned once. The different
tests were made with different oils. The metal
of sources give satisfactory results.
Example 2
lurgical results appear in the following table:
The ore of Example 1 was treated as there de
scribed, except that no fuel oil was used. A
sample of green acids was used as the ?otation
Addition reagent
reagent in the proportion of 2.18 lbs. per ton 10
and the amount of acid varied. two tests being
C°ncentr%.te’
pe/rcent
e
Type
Lbs/ton Assay Distribution
made with no acid but with alkali. The metallur
gical results appear in the following table:
Concentrate per
Lbs.lton
-
5. 45
2. 72
1. 63
O. 54
None
None
None
15
Rougher
Ash
Assay
bution
Distri-
tailliiig
P
None
None
None
None
None
0. 54
3. 60
60. 92
61. 38
61. 97
61. 38
62. 55
61. 62
61. 82
47. 47
40. 02
43. 00
56. 37
19.70
30. 93
10. 88
2. 1
2. 4
2. 6
3.0
6. 5
8. 5
10. 1
Soda
H2804
’
cent Fe
None _____________________________________ . _
Oleic acid
Coconut 011.
Crude oil __________ __
Chlorinated kerosene .
25
It will be apparent that optimum results are
58. 28
0.78
0.55
56. 72
61.62
90. 39
43. 39
_
0. 76
53. 57
92. 69
-
0.76
59. 52
81. 04
Talloel _ _ _ _ _ _ _ _ _ _ _ _ _ _
_ _ _ _ _ ._
0. 82
57. 18
91. 50
Cottonseed oil
Nabhthenic acid
n-Heptaldehyde
Fuel oil No. 2 _
_____ __
_____ __
___ __
-____
0. 27
0. 77
0. 75
0. 61
59. 87
54. 85
56. 25
57.07
50.09
75. 51
70. 15
84. 88
_____
l. 00
60. 45
75.04
Saponi?ed talloeL. __
_____
Barrett No. 4 ___________________ __
0. 82
0. 76
51. 00
50.88
84. 17
71. 80
Methyl ester of talloel.
20
55. O8
.
_
None _____________________________________ ..
61. 97
43. 00
Crude oil . _ _ _ _ _ _ _ _ l _ _ _ _
_ _ _ __
0.76
59. 63
.94. 07
Lubricating oil (IO-W)
Methvi ester of talluel---
_____
_
0. 80
0.78
60. 68
59. 05
_
.
0.76
0.84
59. 75
60. 45
“Bunker C" fuel 0il.__
Chlorinated kerosene“
75. 75
89.85
93. 29
86.70
Coconut oil _______ __
_
0. 55
obtainable at a pH of about 3 and that when no
n-Heptaldehydc. _
_
O. 71
60. 33
80. 34
Naphthenic acid. _
_
0. 77 ~
. 50.30
61. 38
92. 74
63. 60
acid is used the results drop off sharply.
Example 3
Lauryl mercaptan
22° Bé. fl1e101l-Fuel oil No 2___
_
_
_
0. 69
0. 51
l. 22
60. 45
60. 33
58. 23
77. 28
92. 28
83. 73
Talloel _________________________ _ _
0. 82
54. 50
91. 81
Talloel1 _____________________ __
0. 82
65. 78
93. 60
The ore and procedure were the same as in
Example 1, except for the pulp density in con
ditioning. Two densities were used, 65% solids
and 22% solids. In each case the amount of
green acids was 2.18 lbs. per ton. ‘0.51 lb. per ton
of 22° Bé. fuel oil was used with 1.63 lbs. per
ton of sulfuric acid. The results ‘appear in the
following table:
Concentrate,
- -
per cent Fe
.
Assa
-
per cent solids
Assay
Distri-
y
Pulp density
Ta?mg
.Condi
bution
cent
p erFe
pH
92. 28
30. 65
l. 05
7. 45
2. 5
2. 5
tion-
Flota
-
65
22
22
22
mg
1 Tim this test 2.18 lbs. of a 1:1 mixture of SP-702 and green acid was
use
.
The procedure of Example 1 was followed. ex
cept no cleaning was conducted, using 0.51 lb. of
22° Bé. fuel oil in all tests, unless otherwise noted,
and varying the acid used. The water soluble
40 petroleum sulfonate Was Sonesal (green acids).
The metallurgical results appear in the following
table:
tlon
. .
.
Acidic
material
used
60. 33
50. 71
lowing table:
Concentrate
H28 04
None
1. 63
1. 63
Hydrochloric acid ______ ..
assay.t
93. 84
94. 50
94. 44
2.
2.
3.
4. 30
5. 45
2. 72
53. 8O
54. 73
50.18
90. 72
61. 80
91. 62
3.
7.
2.
.
2. 30
48. 20
92. 89
2.
Phosphoric acid
Sulfnrous acid.
2. 70
4. 00
50.65
55. 20
90. 66
96. 49
2.
3.
53. 95
Neal] 2
0
Assay
Hydrofluorsilicic ac d
1. 63
93. 68
2.
45. 86
79. 41
5.
49. 48
89. 70
2.
Saturated
49. 71
64. 54
6.
1.34
41. 38
94. 82
3.
13. 07
12. 78
12. 72
49. 95
55. O8
57. 07
23. 78
58. 28
84. 88
1. 63
1. 22
12. 62
57. 53
78. 42
1. 63
1. 83
12. 59
58. 23
74. 06
. . . . . . ..
B23 .................. . .
Hydrobromic acid (1.03
21%;‘
1. 22
N011!)
0. 61
lbs/ton fuel oil) ...... ._
'
It will be apparent that there is an optimum
amount of fuel oil, which for this particular ore
and petroleum sulfonate was about 0.6 pound.
Example 5
.
Carbonic acid.
.
pH
bution
51. 70
53. 10
53. 92
Chlorine . _ . . .
_
Assay
is r1
1. 63
1. 63
1. 63
Hydro?uoric acid__ __
Sulfuric acid. __
per cent Fe
per cen
Lbs/ton
50 Nitric acid ....... ._
.
Fuel
per cent Fe
Tailing
Example 4
The procedure of Example 1 was followed using
2.18 lbs..pe_r ton of a water soluble petroleum sul
fonate, SP-702, with varying amounts of fuel
oil. The metallurgical results appear in the fol~
Feed
Concentrate,
D‘ t '
Type
Lbs‘lton
.
Example 6
v
Ore of Example 1 was conditioned at high solids
with 2.18 lbs. per ton of water soluble petroleum
sulfonate, using SP-702 for the ?rst 13 tests and
Sonesal (green acids) for all the remainder but
the last test. In the last test 2.18 lbs/ton of a
60 Weak oil re?nery acid 1-.
5. 23
51. 58
91. 20
Formic acid ____________ __
3. 27
46. 91
96.02
3.
Acetic acid"
____ . .
2. 72
50.18
95. 27
4.
Acrylic acid.
Oxalic acid..
.... ..
______ ._
3. 60
2. 72
43. 30
51. 23
96. 12.
81. 31
3.
2.
Lactic acid. .
______ _.
3. 27
43. 88
96. 17
3.
Tartaric acid
Citric acid__ _
____ _ _
.... _ _
3.27
2. 72
51.11
53. 92
95. 85
93. 99
3.
3.
Maleic anhydride ______ __
Tricarballylic acid _____ __
Benzoic acid ___________ __
3. 27
3. 60
3. 27
44. 58
45. 74
29. 53
95. 54
94.76
87. 57
2.
3.
3.
Phthalic acid __________ _ _
2.
3. 82
44. 22
S9. 81
3.
ton fuel oil) __________ __
2. 73
35. 83
91. 57
3.
p.'l‘oluene sulfonic acid. _
Phenol (1.03 lbs/ton fuel
2.18
50.06
95. 89
oil) __________________ . .
4. 36
47.06
61. 94
Salicylic acid (1.03 lbs./
3.
'
7.
l Contained about 48% H2804.
It will be apparent that all of the stronger acids
work satisfactorily and good results are obtained
2,410,377
7
down to acids having an ionization constant of
10*". It should be noted that the somewhat lower
grade of concentrate is due to the fact that in
the above example there was no cleaning, the
data being on rougher ?otation alone.
It will be noted that .the presence of slime're
quired an increase in ‘the amounts of reagents
for best results, the increase in the amount ‘of
fuel oil needed being particularly striking with
For this 5 the undeslimed ore. _ At the same time it will be
particular ore cleaning is of importance to obtain
concentrates of commercial grade.
noted that excellent grades were obtainable with
good recovery for partially deslimed ore as well
Example 7
as for completelydeslimed ore, the latter show
ing only a slight improvement in grade but per
The procedure of Example 1 was followed, but 10 mitting the use of materially reduced amounts
acid salts instead of free acids were used. The
of reagent. In common with usual ?otation prac
metallurgical results appear in the following tatice, operation on completely undeslimed ore was
ble:
much less economical.
Green acids
Acidic Salt used
LbsJton
used
220 Bé.
lbs/ton
fuel 011
3. 27
2.18
Type
Lbs/ton
Potassium bisulfate...
Sodium chlorosulfonate._
10.9
5.45
concenmgg’ per cent
Rto‘ighsr
al 111,,
Assay
1.00
0. 52
PH
Distribution
55.90
59.87
85.
79.39
Example 8
2.2
2.6
ExampZe 9
A sample of the ore of Example 1 wasdivided
In order to determine the effects of the re
into three parts. One portion was not deslimed 25 agents of the present invention on various iron
at all. A second portion was partially deslimed,
minerals present in ores, the pure minerals were
“using ordinary desliming procedures, and the
ground to -—100 mesh, +325 mesh and deslimed
prior to ?otation. They were conditioned with
green acids, fuel oil, and sulfuric acid (in each
other Was deslimed completely. In each case the
ore was conditioned at high solids with green
acids, sulfuric acid, and 22° Be. fuel oil, optimum
proportions being used for each product. The
at» case there was a blank with no acid, except in the
case of goethite), and were ?oated in a labora
tory Fager'gren flotation machine. As the miner
completely deslimed material was cleaned once
als are pure, the ef?ciency of ?otation is meas
ured by the percent of material ?oated. The re
sults appear in the following table:
. and the partially deslimed and undeslimed ma
terial was cleaned twice.
The metallurgical re
sults appear in the following table, in which the
Reagents, lbs/ton >
.
Mineral
H2504
No 2
Green
fuel
acids
weightrgrams
'
Do ___________ __
?oated
Feed Float Tail
o1
Magnetlte _______ __
Per cent
pH
-
8.
0. 75
'1. 0
2. 5
30. 6
27. 1
‘3. 5
None
0. 75
1.0
7. 1
30.5
0. 7
29. 8
88. 6
2.3
0. 75
1. 0
2. a
30.1
24.6
5. 5
s1. 7
0. 75
1. 50
1. 50
1. 50
0. 75
0. 75
3. 00
3. 00
0. 75
0. 75
O. 75
0. 75
1. 0
5. 0
5. 0
5. 0
1. 0
1.0
5. 0
5. O
1. 0
1. 0
l. 0
1. O
6. 9
2. 5
6. 6
2. 2
2. 4
6. 9
2. 9
6. 8
3. 3
6. 6
2.1
6. 4
30. 2
33. 6
32. 7
29. 4
29. 4
29. 9
30. 8
30. 4
31. 3
30. 9
31. 7
31. 3
1. 2
32. 2
14. 8
29. 3
27.1
l. l
20. 1
1. 4
30. 8
20. 3
31. 5
5. 7
29. 0
l. 4
17. 9
0. 1
2. 3
28. 8
10. 7
29. 0
O. 5
10. 6
0. 2
25. 6
4. 0
95. 8
45. 3
99. 7
92. 2
3. 7
65. 3
4. 6
98. 5
65. 7
99. 4
18. 2
Titaniferous mag
name __________ ,_
?rst test is on completely deslimed, the second
on partially deslimed, and the third on unde
slimed ore:
mixtures of water soluble petroleum sulfonates
Assay
Product
K525i]?
’'
Per cent
Lbs/ton used
Fe distri
Per cent Per cent
e
.
Erample 10
An iron ore of Example 1 was conditioned with
bution
msol.
Green
acids
_
100. 00
14. 73
100. 00
_
_
8. 19
18. 33
28. 96
59. 34
16. 1O
73. 82
_
3. 80
6. 62
l. 71
R311. tail ______ _.
69. 68
l. 77
8.37
Head __________ __
Slime __________ __
Clean cone- _ ____
100. 00
3. 42
18. 74
14. 92
'37. 94
58. 75
100. 00
8. 70
73. 78
2nd clean. tail...
1st clean. tail____
1.13
3. 35
30. 02
10. 99
2. 27
2.47
Rgh. tail ______ __
73. 36
2. 60
12. 78
.Hcad __________ __
100. O0
14. 60
100. 00
Clean. 0on0 .... __
2nd clean. tail"1st clean. tail__-_
24. 87
3. 56
5.09
51. 77
16. 08
5. 67
Rgh. tail _____ _.
66. 48
l. 30
HS 0
2 4
oil
____ __
88. 18
2. 72
2. 18
3. 92 ______________ __
1.98 ______________ __
5. 92
Fuel
______________ __
2,410,377
10
chloride. The metallurgical results of the double
and various types‘ of mahogany soaps Or oil sol
uble petroleum sulfonates. Conditioning was at
?oat appear in the following table:
high solids and in every case 1.63 lbs. per ton of
sulfuric acid were used. The amount of green
acids was 1.09 lbs. per ton. In all but one of the
tests there was no additional fuel oil. The ?oats
are rougher ?oats only. The metallurgical re
sults appear in the following table:
22., Be.
Oil soluble sulfonate used
Percent Fe‘
Product
per cent Fe
{gel/oil.
5. ton
Assay
'
tors, Inc.) ________________________ ._
None
59. 05
83.03
0.98 lb./ton Calol sodium sulfonate
(Standard Oil Co. of California)__..
0.98 lb./ton Calol sodium sulionata..0.84 lb./ton Ultranate N o. 2 (Atlantic
None
0. 54
53. 33
53. 33
90.83
91. 36
Re?ning Co.) _____________________ __
None
58. 35
84. 37
Welght
100. 00
Assay
Distribu
mm
13.40
100. 00
Anionic ?otation tailing. _ __
Secondary slime ____________ __
74. 94
1. 21
1. 54
37. 13
8. 61
3. 35
Cationic ?otation concentrate.
_
Cationic ?otation tailing ____________ __
12. 90
10. 95
38. 77
62. 06
37. 32
50. 72
Example 13
The procedure of Example 1 was followed, using
.
.
Distri
bution
0.98 lb./ton SP-312 (Stanco Distribu-
Perf’ent
Feed _______________________________ . _
10
Concentrate,
‘
15 2.18 lbs. per ton green acids and, 1.63 lbs. per ton
sulfuric acid, except in the case of the sixth test
of the ?rst table. This sixth test was a blank
test and no sulfuric acid was used. The pulp
was then diluted to ?otation density and varying
20
amounts of alkali were used to neutralize partly
or wholly the acidity. Flotation was then ef
fected and the metallurgical results appear in the
following tables, in which the ?rst shows various
Example 11
The procedure of Example 1 was followed but
amounts of soda ash, including the blank test,
the ore was ?rst deslimed, then scrubbed or
and the second table shows the effect of various
polished by agitation in a ?otation cell with the
types ofralkali:
’
7
air shut off at 25% solids, and thenagain de
slimed to remove secondary slimes. Condition
ing was with 1.63 lbs. per ton of sulfuric acid, 1.09
Concentrate,
i‘e per cent R oug h er
lbs. per ton green acids, and 0.51 lb. per ton 22°
gig/Z2111 ——
___-__ - tailing
D
Bé. fuel oil. Two cleaning ?oats were conducted. 30
Assay Distribution
The metallurgical results appear in the following
table:
None
60. 33
92. 28
2. 5
Pmduct
Head __________________ __
Per cent
weight
Per cent
Fe
Per cent
insol.
Per
cent
~ ' -
dtlifglgg
100. 00
100.00
6. 14
2. 40
14. 83
6. 61
Clean. conc ____ __
17. 15
70. 70
Comb. clean. tails_
11. 49
3. 79
Rgh. tail _______________ __
62.82
4.07
Prim. slime
Sec. slime..-
.54
l. 63
2. 18
57 88
57. 53
59. 57
88.25
90. 25
88. 71
2.7
5. 9
7. l
8. 60
3. 60
58.86
61. 82
86. 25
10. 88
10. 1
Alkali. used
Concentrate per
cent Fe
Type
The results should be compared with the com
pletely deslimed ore of Example 8. It will be noted 45
that the grade is slightly higher, the recovery
almost as good, and the amount of reagent halved.
In many cases the saving in reagent obtainable
by scrubbing is commercially worthwhile.
8.0
Lbs/ton Assay
Calcium carbonate _______ __
Hydrated lime ____ __
tilllllilg
9
Distribu-
“on
l. 0
56. 28
87. 64
_
1.0
57. 94
87.06
_.
1. 0
59.00
86. 61
Ammonia ________________ __
0.83
56. 76
87.03
Caustic soda__.-
Rougher
3. 5
6. 8
6. 3
.
8. 6
It will be apparent that there is but little loss
in ef?ciency when the acid conditioned material
50 is neutralized with alkali.
Example 12
The ore of Example 1 was deslimed, condi
tioned at 67% solids with 2.18 lbs. per ton green
Example 14
The effect of the process of the present inven
tion on various iron ores was tested. In each case
acids, 1.63 lbs. per ton sulfuric acid and 0.51 lb.
per ton 22° Be. fuel oil. The conditioned ore was 55 the ore was ground, if necessary, deslimed, con
then diluted to 22% solids and ?oated in a Fager
ditioned at 60-65% solids, diluted to ?otation pulp
gren ?otation machine.
density and ?oated in a Fagergren ?otation ma
The concentrate was
then conditioned at about 6% solids with 2.18 lbs.
chine.
Cleaning was effected once, except with
the tests marked with an asterisk, where the
per ton of soda ash and 1.63 lbs. per ton of que
bracho. The conditioned ore was then deslimed 60 recleaning was used. In every case the reagent
combination giving best results was employed.
and subjected to cationic ?otation in a Fagergren
?otation cell, using as reagents 0.12 lb. per ton
pine oil and 0.22 lb. per ton laurylamine hydro
The metallurgical results appear in the follow
ing table:
Lbs/ton
Feed
Source of ore
H’s 0‘
Green
acids
22° B6
p Fe
fuel oil
Concentrate,
per cent Fe
?sgg?t
Rougher
tailing
Assay
Distri-
bution
pH
1 2. 72
1. 63
0. 76
Minnesota (a washer reject) _______ __
30. 47
58. 63
92. 66
2.6 _
1. 50
1 1. 63
2.00
1. 63
0. 70
0. 75
New Jersey (a table product)_
Minnesota (classi?er over?ow)
64. 77
13. 72
69. 29
53. 21
95. 87
85.60
2.9
2. 5
1. 96
1. 96
1. 22
_._._do ______________ __
20. 25
60. 18
84. 95
2. 4
3. 10
4. 40
1. 93
2. 20
0.90
0. 77
Minnesota (a taconite
23. 16
52. 06
59.10
65. 25
93.76
73.80
2. 6
5. 7
3. 08
2. 20
l. 55
- 26. 65
48.46
84.44
6.0
1 5. 26
2. 63
2. 47
40. 71
54. 14
94. 84
2. 9
l Cleaned twice.
2,410,377
r
,
12
11
It will be apparent that in the case of all of
the ores commercially useful results were obtained
except with two very refractory Minnesota ores
and a Canadian ore, where the grade was slightly
below the present speci?cations for concentrate.
the pH of the rougher tailing isli‘n, the range of
Zto 6.
'
I
r‘
r
2'. A method of bene?ciating oxidized iron ores
by froth ?otation which comprises conditioning
the ore at high solids with sulfuric acid, and un
sulfonated oil, anda collector for oxidized iron
minerals containing as its major active constitu
to" the e?iciency of the ?otation but because the
ent water soluble petroleum sulfonates of the
ore was highly refractory, containing gangue and
green acid type obtained in the re?ning of pe
iron locked together even in very ?ne sizes.
All of the petroleum sulfonates referred to in 10 troleum lubricating oils, diluting the thus con
ditioned pulp to froth ?otation density, subjecting
the examples under their trade names are typical
it to froth ?otation to produce a concentrate
petroleum sulfonates of the green acid type or,
relatively rich in iron and a tailing relatively poor
In the case of these ores the di?iculty was not due
in the case of Example 10, green acid or mahog
any acid type, as commercially obtained from the
treatment of petroleum lubricating oil fractions
with sulfonating agents, such as sulfuric acid,
oleum, and the like.
in iron, the amount of the sulfuric acid being
sufficient so that in the absence of added alkali,
the pH of the rougher tailings is in the range of
to 6.
'
3. A method according to claim 1 in which th
We claim:
unsulfonated oil is a petroleum hydrocarbon oil.
4. A method according to claim 2 in which the
1. A method of bene?ciating oxidized iron ores 20
unsulfonated oil is a petroleum hydrocarbon oil.
by froth ?otation which comprises conditioning
5. A method according to claim 1 in which the
theore at high solids with an acid substance, the
ore pulp is conditioned at high solids with the
anion of which is a ‘constituent of an acid having
acid, collector and oil, diluted to ?otation pulp
a dissociation constant not less than 10*”, and
density and subjected to froth flotation after sub
which does not adversely affect ?otation, an un
sulfonated oil, and a collector for oxidized iron
stantial neutralization of the acid by means of
minerals containing as its major active constitu
an‘ alkali._
,
6. A method according to claim 2 in which the
ent water soluble petroleum sulfonates of the
green acid type obtained in the re?ning of pe
ore pulp is conditioned at high solids with the
troleum lubricating oils, diluting the thus condi
acidfcollector and oil, diluted to ?otation pulp
tioned pulp to froth ?otation density, subjecting
density and subjected to froth ?otation after sub
it to froth flotation to produce a concentrate rela
stantial neutralization of the acid by means of an
tively rich in iron and a tailing relatively poor
alkali.
in iron, the amount of the acid substance being
ROBERT B. BOOTH.
sufficient so that, in the absence of added alkali,
EARL C. HERKENHOFF.
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