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Патент USA US2405581

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Patented Aug. 13, 1946
2,405,581
UNITED STATES PATENT OFFICE
2,405,581
FLOTATION OF SULPHIDE ORES
Cornelius H. Keller, San- Francisco, Calif., as
signorto The Dow Chemical Company, Midland,
Mich., a corporation of Michigan
N0 Drawing. Application October 1-7, 1944,
Serial No. 559,117
11 Claims. (Cl. 209-166)
This invention relates to the concentration of
ores, minerals and the like by ?otation, andv has
for its broad object the provision of certain im
provements in the process’.
7 weight of the organic acid halide was added very
slowly under» continued trituration.
The mass,
at ?rst milky, assumed a canary yellow color
which gradually changed to a deep orange. This
'
reaction was accompanied by a rise in tempera
ture‘. This ceased when the orange color ap
In the froth ?otation of ores, an ore pulp is
?rst prepared by wet grinding to a suitable‘ size
then added. Upon agitating and aerating the
peared, showing that the reaction was completed.
The product consists of organic sulphur com
pounds of undetermined composition.
mixture, the metalliferous values in the ore
collect as a froth which can be readily over
?owed or skimmed 01f and the metal values
To illustrate some of the advantages to be
gained by the use of the crude reaction product
collecting agents as compared to the principal
with or without a suitable pH’ modi?er. A suit
able frothing agent and a ?otation agent are
therein recovered.
and bestv known collecting agent, namely
'
Flotation agents, as, a broad class, are well
known. Generally within the broad class‘ sub
classi?cation is possible into several groups, each
of which will di?er from another in its ?otation
elfect. The present invention is concernedwith
a group of agents which are not only good col
lectors, but are also highly selective in their
x-anthate, the following examples are set forth:
As a general procedure the sample of ore was
ground wet in a ball mill with a suitable pI-I
modi?er. When su?iciently ground, the pulp was
. transferred to either a Fagergren or a Denver
Sub A ?otation machine and the ?otation re
agent and frother were added. The pulp was
action, enabling sulphide copper minerals, sul
then subjected to agitation and aeration and the
phide zinc minerals and others to be ?oated
froth concentrate was removed.
selectively from sulphide iron minerals. The
The designation “R. P.” is employed in the
new agents are obtainedas the reaction product
following tables to indicate the reaction product.
of a carbocyclic acid halide, a monohydric ali 25 To illustrate the present invention, charges
phatic alcohol and’ an alkali thiocyanate', the
of copperv ore from Utah were prepared and
chemical constitution of which’ is‘ not fully known.
treated, comparison being made between the
These possess numerous advantages. For ex
ample, they are soluble to a useful extent in var
various chemical ?otation reagents contemplated
ious organic solvents, such‘ as am'yl alcohol and 30 by this invention and potassium ethyl Xanthate
as collector:
cresylic acid, thereby enabling the agent to’ be
fed as a liquid.
Further, these agents can be
Tabulation #1-C'opper ore from Utah
incorporated and utilized with other agents such
as xanthates.
When treated with an alkali hy
droxide, these agents “are converted into water
_
_
soluble salts which can be fed as Water solutions. “
The materials of the present invention are
Lbs/ton
or other carbocyclic acid'halide upon an alcoholic
solution or suspensionof an alkali thiocyan‘a‘te
monohydric alcohol can be used and I have. suc
per cent
pcopper
copper
per cent
in con
centrate
40
K ethyl xanthate ______ ._
NaONS
NaCNS-N. amylalcohol
.
, benzoylchloride R.,P_._
NaCN S~N, butylalcohol
, benzoylchloride R. P":
45
cessfully employed ethyl, isopropyl, secondary
butyl, N-amyl, N-butyl, octyl and‘a‘ mixture‘ of
amyl alcohols (sold, under the trade-name
“Pentasol”) and diethylcarbinol. '
0. 1
12. 2
0. 1
0. 05
19.12
0.1L
88.8
14. 08 '
0. 09
ethylalcohol
I benzoylchloride R. P._~_
such as potassium thiocyanate, ammonium thic
cyanate, sodium thiocyanate. Any aliphatic
Tailings recovery
er Cent
Jconveniently prepared by the“ interaction of any
carbocyclic acid halide such as benz'oyl chloride,
benzoyl bromide, furoyl chloride, furoyl bromide,
Copper
Gigi?
Flotation reagent used
NaCN S-N. amylalcohol
‘ iuroylchlorideR. P__-__
NaONS¢N.'butyla1cohol-
__iuroylch1oride R. P. .._
NH4ON-S-N. butylalco
‘
, i '
90.0
_
0.1
’ _
‘
0. 1
r
‘
92. 2
‘
14. 8
OJ 092
91. 3
0.1
90.3
.
0.15
13.04 '
’
v
0; 15"
_
>
18. 96
.
0. 13
87. 6
hol iuroylchloride R.
P}
0. 15
en
zoylbromide-R. PM‘...
8. 28
‘
0.1
0.095
91. 5
- 010627
90.0
.
10.12? ‘5
A typical example of the preparation of these
materials follows: V8 mol. weight of a suitable
alkali thiocyanate was triturated in a mortar
with 1/; mol. weight of the selected: alcohol.
When these were ground and. mixed, 1/5 mol.-v 55
. LEGEND.-——R. P. stands for Reaction Product.
1 Emulsol used as a frother only with this reagent; cresylic acid
being‘ used in another tests.
Comparing the results: secured, it is" to be
2,405,581
noted that the copper recovery is generally in
creased when the reaction product is employed
instead of potassium ethyl xanthate.
To compare the value of the reaction product
collecting agent with xanthates, a sulphide cop 5
Illustrating the greater selectivity of water sol
uble alkali metal salts of the reaction products
over xanthes, a sulphide copper from Utah was
prepared for ?otation and tested with the £01
lowing results:
Tabulation #4.--C'opper ore from Utah
r
Flotation reagfent used I
Lba/ton
P
t a.“
a
2 .6,8
mm8”02 1mwe25 4 40tm
0_. Q0 2
Ethyl xanthate_._-___-_______.
....1
Cmocvm petnpr.Gtym-i aturnmomwith
TD3 %?rD
t
e
M
u
b
‘
1
m
r
Y24638
9
8
e
0
a
r
n
.15 692
n
m
m
n
i
.
m
0
w
.
H
m
$
l
w
m
ea5.n4“1a
681021 M70169
8
I
..
23 1
6
l
l Cresylic acid used as a frother.
per ore from Arizona was used.
The selectivity with respect to iron is quite
The results are
shown in the following table
'
pronounced on this ore.
-
’
Tabulation #2.—Copper ore from Arizona
Concentrate
Flotation reagent used 1
LbsL/ton
Tailings
per cent
Per cent
copper
Per cent
iron
copper
Copper re
covery per
cent in con
centrate
Iron recovery
per cent LD.
concentrate
ethyl mutilate..-“
amyl xauthate. ___-__--_..._.___
R. P. ?otation reagents were prepared from alcohol, benzoylchlorlde and NsONS.- Only the alcohol is
indicated in tabulation.
1 Fuel oil mix employed as a frother in each case.
The reaction product enables several per cent
To illustrate the compatibility of the reaction
products with xanthates and the greater selec
potassium ethyl xanthate or potassium amyl 45 tivity obtained by the addition of the reaction
more copper to be recovered than does either the
puri?ed ester or even a larger quantity of either
xanthate.
To demonstrate the collecting effectiveness and
products of this invention to xanthates, different
percentages of the reaction products were added
to xanthate in various stages of its preparation.
selectiveness of the reaction‘ products dissolved
in cresylic acid or amylalcohol as compared to
xanthate, a sulphide copper ore from Arizona 50‘ Also, a water soluble alkali salt of the reaction
was prepared for flotation and treated , witl- the
product was mixed with xanthate in different
following results:
Tabulation #3.—C'opper ore from Arizona
Concentrate
Flotation reagent used 1
Lbs/ton
0 0 3%H%
3
3 5i
Per cent
Per cent
copper
'
11011
MBil 419670-
R. P. ?otation reagents were prepared from an alcohol, benzoylchloride and NaCNS; only the alcohol is
indicated in the tabulation. R‘ P.'s were used in form of 33.3% R. P. to 66.7% cresylic acid and 1-1 B. P. in
pentasol and freed from the alkali halide by ?ltration.
1 Oresylic acid fuel oil mix used as (rather.
An increased copper recovery and a concentrate containing less iron shows the greater se-- lectivity of the “R, P.” flotation agents.
' proportions. All of these preparations were used
» on a Utah sulphide copper ore as shown in the
: 75 subioined tabulation, '
'
-
'
5,405,581
B
Tabulation-#5.-—Copper ore from. Utah. v
Concentrate
T _1
Copper‘ Iron
Flotationreagentsnsed-
. a‘ '
0.02lb./ton ofore with
mgs
cresylic acid as a
frothcr
Per
cent
copper
Per
re‘
_
Flotation reagent
re“
°°verry °°V§§Y
pert
pet in
. initiate
hates
> Reva.
cent tailings
- Lbs/ton
5 t in
cent 0553M ccglcem 0003mm
“on
trate
Pb
Zn
Fe
Pb
Zn
Fe
trate
Pot. salt isopropyl re
10
(a) K. salt isopropyl R.
P.,
%; pentasol
xanthate, 40%...“
(D) K. salt lsopropyl R.
..
0. 10
90. 5
25. 0
Pot. salt 2d butyl r
action product.
18. 6
12.1
0.12.
89. 2
22.9
Pot. salt pentasol ie
action product _____ __
20. 0
13.2
0. 12
89. 5
22. 2 15
Ethyl xanthate.
0 _______ __
(d) K.saltisopropylR. ,
P., 60%; pentasol
780.4
7.8
4.3 _____________ ._
10.1 85.5 13.2. 9.5
6.7 82.5
,
0.04
Do
Do ...... _-
0.04
0.15
14.9
R, 60%; pentasol
xanthate, 40%"--.
Do
20. 6
P., 60%; pentasol
‘ xanthate, 40.%__.-_
(c) K. salt isopropyl R.
action product _____ __
0.15.
0.04
_
0.15
_
, 0.04
_
0.1.5
81.2
8.0
4.7 _____________ __
8.2 86.6 12.5 10.6
82.1
8.1
8.7
87.7
92.1 11.6
5.4 82.8
I
4.6..
13.7
8.1v
4.786.61615
1\I111ereo A___Ethyl Xanthate.
_
,
0.034 91.4 11.0- 7,4
0.154 5.7 86.6 15.8
MinerecA ____ __
_
0.34
xanthate, 40%_____
18. 4
15.5
0. 10
91. 6
30.1
P., 100
_________ __
22.4
13. 7
0.12
89.1
21.2
Pentasol xanthate, 100%_
16. 8
21. 1
0.12
89. 9
43. 8
20. 6
13. 9
0.12
89. 3
24- 7
19.4
16. 6
0.12
89.2
30.7
I claim:
1. The improvement in the concentration of
ores by ?otationwhich comprises subjecting a
18.4
18.8
0.12
89. 4
37. 3
25 operation in the presence of an effective quantity
K. salt isopropyl R.
K. salt isopropyl R. P.,
80%; ethyl xanthate,
20% _________________ __
action product _____ __
60%; ethyl xanthate,
K. salt isopropyl R. P.,
11.8
8.1
4.8 87.0 13.4
sulphide ore in the form of a pulp to a ?otation
40%; ethyl xanthate,
60% _________________ __
0.154
20
K. salt isopropyl R. P.,
40% ................. __
92.5
Pot. salt pentas
K. salt isopropyl R. P.,
of a froth ?otation agent comprising a reaction
product of an aliphatic monohydric alcohol, an
Ethyl xanthate, 100%".
15.8
19.9
0.11
90. 2
46. 4
alkali thiocyanate and a carbocyclic acid halide.
K. salt isopropyl R. P.,
100% ________________ __
23. 6
15. 0
0. 13
88. 4
23. 3
2. The improvement in the concentration of
30 ores by ?otation which comprises subjecting a
LEGEND:
.
sulphide ore in the form of a pulp to a ?otation
(a) Wet K. salt of isopropyl R. P. mixed with commercial pentasol
operation in the presence of an effective quantity
xanthate dried.
of a froth ?otation agent comprising a reaction
(b) Wet K. salt of isopropyl R. P. mixed with pentasol xanthate
ingredients dried.
product of an aliphatic monohydric alcohol, an
(c) Isopropyl reaction product mixed with pentasol, CS2 and 35
alkali thiocyanate and benzoylchloride.
enough KOH to form double salt and dried.
(d)hDtry K. salt of isopropyl R. I’. mixed with commercial pcntasol
3. The improvement in the concentration of
xant a e.
ores by ?otation which comprises subjecting a
sulphide ore in the form of a pulp to a ?otation
To show the selective action of the reagents of
this invention upon sulphide lead and sulphide 40 operation in the presence of an effective quantity
of a froth ?otation agent comprising a reaction
zinc minerals over sulphide iron mineral as com
product of an aliphatic monohydric alcohol, an
pared with xanthates, a series of tests were made
alkali thiocyanate and furoylchloride.
on a lead-zinc ore from Idaho.
4. The improvement in the concentration of
The procedure followed consisted in taking off
ores by ?otation which comprises subjecting a
a lead concentrate by means of a small amount of
sulphide ore in the form of a pulp to a ?otation
collecting agent and the usual cresylic acid
operation in the presence of an effective quantity
frother and after conditioning with copper sul
of a froth ?otation agent comprising a reaction
phate and additional collecting agent, a zinc con
product of an aliphatic monohydric alcohol, an,
centrate was taken off. This is shown in Tabu
alkali thiocyanate and benzoylbromide.
lation No. 6, less iron and more lead and zinc 50
v5. The improvement in the concentration of
being recovered with the “R. P.” agent than with
ores by ?otation which comprises subjecting a
the xanthate or Minerec A, a xanthic acid for
sulphide ore in the form of a pulp to a ?otation
mate as made under the Fischer Patent 1,684,536.
operation in the presence of an effective quantity
of a froth ?otation agent comprising a solution
55 of a reaction product of an aliphatic monohydric
Tabulation #6.—Lead-zinc ore from Idaho
alcohol, an alkali .thiocyanate and a carbocyclic
A.
acid halide in an organic liquid.
6. The improvement in the concentration of
ores by ?otation which comprises subjecting a
Assays. per cent Assays, per cent
20%; ethyl xanthate,
80
_________________ __
17. 2
21. 4
0. 12
89. 3
concentrates
Flotation reagent
43. 7
tailings
6O sulphide ore in the form of a pulp to a ?otation
Lbs/ton
Pb
Zn
Fe
Pb
Zn
Fe
Pot. salt isopropyl re
action product _____ __
0.04
57.6
8.1
4.4 ___-._ _-___ __-__
Do ______________ __
0.15
3.4
42.6
6.4 0.45 046 5.5
action product _____ __
0.04
55.4
8.1
o ______________ __
0.15
2.8
43.6
65
Pot. salt 2d butyl re
4.6 _____________ __
6.2 0.48 0.36 5.5
Pot. salt pentasol re
action product _____ __
sulphide ore in the form of a pulp to a ?otation
operation in the presence of an effective quantity
of a froth ?otation agent comprising an amyl
alcohol solution of a reaction product of an ali
0.04
55.3
8.1
Do _________ __
Ethyl xanthate.
Do _____ __
Mmerec A.___
0.15
0.04
0.15
0.034
2.8
50.2
1.5
52.1
42.0
9.4
40.5
9.6
Ethyl xanthate.
0.154 1.88 44.0
7.8 0.13 0.16 5.05
phatic monohydric alcohol, an alkali thiocyanate
MinerecA ___________ __
0.34
6.3 _____________ __
and a carbocyclic acid halide.
51.6
9.6
4.4 _____________ __
operation in the presence of an effective quantity
of a froth ?otation agent comprising a cresylio
acid solution of a reaction product of an aliphatic
monohydric alcohol, an alkali thiocyanate and a
carbocyclic acid halide.
7. The improvement in the concentration of
ores by ?otation which comprises subjecting a
6.4
6.3
7.4
6.3
0.43 0.29 5.4
________ __ ____ 70
0.15 0.13 5.1
_____________ ._
Pot. salt pentasol re
action product ..... ._
0.154 1.73 45.8
6.8 0.13 0.08
5.3
8. The improvement in the concentration of
75 “ores by ?otation which comprises subjecting a
7
2,405,531
8
sulphide ore in the form of a pulp to a ?otation
operation in the presence of an e?ective quantity
sulphide ore in the form of a pulp to a ?otation op
eration in the presence of an effective quantity of
of a froth ?otation agent comprising a water sol
a froth ?otation agent comprising (1) a reaction
product of an aliphatic monohydrlc alcohol, an
alkali thiocyanate, and a carbocyclic acid halide
and (2) an alkali metal salt of an alkyl sulphur
uble reaction product of an aliphatic monohydric
alcohol, an alkali thiocyanate, a carbocyclic acid
halide and an alkali hydroxide.
9. The improvement in the concentration of
ores by ?otation which comprises subjecting a
sulphide ore in the form of a pulp to a ?otation
operation in the presence of an effective quantity‘ 10
of a froth ?otation agent comprising (1) a reac
tion product of an aliphatic monohydric alcohol,
an alkali thiocyanate, and a carbocyclic acid ha
lide and (2) an alkali metal xanthate of a mono
hydric aliphatic alcohol.
10. The improvement in the concentration of
ores by ?otation which comprises subjecting a
derivative of carbonic acid.
_
11. The improvement in the concentration of
ores by ?otation which comprises subjecting a
sulphide ore in the form of a pulp to a ?otation
operation in the presence of an effective quantity
of a froth ?otation agent comprising (1) a reac
tion product of an aliphatic monohydric alcohol,
an alkali thiocyanate, and a carbocyclic acid ha
15 lide and (2) an alkyl sulphur derivative of car
bonic acid.
.
CORNELIUS I-L KELLER.
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