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Патент USA US2403640

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July 9,1946.
' '.
Filed April 15, 1942
I e ANGUE —<#
- John R,.Cunn_|'nghc|m '
Patented July '9, 1946
I 2,403,640
John R. Cunningham, Larkspur, Calii’., assignor,
by mesne assignmen
Corporation, San Fr ts, to California Research
ancisco, Calif., a corpora
tion of Delaware
Application April 15, 1942, Serial No. 439,068
1 ‘Claim. (Cl.
This invention relates to the separation of co
‘Other objects achieved by. this invention will be '
apparent from the following description and the
baltite from minerals containing it.
Cobaltite, a mineral of the approximate _com-'
appended claim.
position CoAs'S, is an available cobalt mineral
I have found that cobaltite can be readily and
eiliciently‘separated i'rom pyrite or pyrrhotite,‘ or
from both if present together, by subjecting the
from which the pure'metal or its compounds can
‘,be economically produced, provided, however, the
cobaltite can‘ be separated'in concentrated form
mineral mixture to treatment with lime, and
thereafter subjecting the mixture to ?otation in a
system of pH not greater than about 7 in the pres
from other minerals associated therewith. ‘Among -
the minerals frequently associated with cobaltite
are pyrite and pyrrhotite.
Chalcopyrite is also 10
ence of a xanthate collector and a depressant for
the cobaltite, and ?oating the pyrite and/or pyr
Separationof minerals by ?otation methods » rhotite
away from the cobaltite in this system of.
has advanced to the point where almost any min
controlled pH with the aid of the said ?otation
eral or group ofminerals can be separated from ‘ ’
any other mineral or group of minerals of dis
Without embarking upon any detailed scenti?c
tinctly different ?oatability and ?otation char
explanation of the phenomena involved, or in any
acteristics. The di?iculty arises in separating
' ‘minerals of very similar ?oatability and ?otation _ ,way limiting the invention to a theory, I believe
frequently found in association with cobaltite.
that the delicate separation of cobaltite from
In the instant case, cobaltite is found associ 20 pyrite and/0r pyrrhotite thus e?ected is due in
large part to pre-liming the mineral mixture,
ated with gangue (earthy matter of little or no
which depresses the cobaltite more effectively and
mineral value), pyrite and pyrrhotite and, fre
more durably than it depresses the pyrite and
quently, with chalcopyrite. The separation of the
pyrrhotite, so that when the system‘ is subse
group cobaltite-pyrite-pyrrhotite from both the‘
quently neutralized ‘or acidi?ed,‘ the cobaltite is
gang‘ue and the chalcopyrite is easy and straight
still depressed but the pyrite and pyrrhotite are
forward. The gangue canbe'separated by ?oat
not depressed orare not as fully depressed as the
ing the minerals in an acid or neutral circuit, em- ;
cobaltite. Upon ?otation treatment in a system
ploying the usual ?otation agents for ?otation of
pH not greater than about 7 in the presence
; sul?de minerals, whereby the cobaltite-pyrite
pyrrhotite are ?oated and the gangueis rejected. 30 of a xanthate collector (a known class of collectors
suitable for use with sul?de minerals) and a
depressant for the cobaltite (of which many well- '
Also, chalcopyrite can be readily separated by
?oating it in a basic circuit. _The' separation of
known examples are available as hereinafter de
scribed), the cobaltite is still, substantially non
ever, a problem of wholly different magnitude.
?oatable but the pyrite and pyrrhotite are ?otable,
The ?oatabilities and ?otation characteristics of 35 especially
in the presence of an activator.
these three minerals are so. similar that, hereto
mixture consists of cobaltite plus
fore tomy knowledge, they have not been sep
' pyrite and/or pyrrhotite, and no more, only the
arated except by cumbersome and expensive
cobaltite. from the pyrite and pyrrhotite is, how
single ?otation stepv described is necessary, and.
step may be repeated, subjectingthe cobaltite
It is an object achieved by the present inven 40 reject
and the pyrite-pyrrhotite ?oated mixture‘
tion toe?ect a‘ facile, economical separation. of
each to a further similar ?otation treatment.
cobaltite from ores, concentrates and the like‘ con
' However, if, as is usually the case, gangue is
taining it in association’ with pyrite, pyrrhotite,
or other'iron sul?de minerals of similar ?otation
It is a further ‘and particular object achieved
by this invention to separate cobaltite. from ores,
concentrates and the likevcontaining it in associ-'
ation with pyrite or pyrrhotite, or vboth, together '
with chalcopyrite.
present, or if, as is often the case, chalcopyrite
is present, in the mineral mixture, a preferred
modi?cation is employed. A single illustration
with respect ,toja chalcopyrite-gangue-cobaltite
pyrite-pyrrhotite ore will su?ice‘ toillustr'atelthis _
1 preferred modi?cation‘.
In such case the
ore, suitably ,vcomminuted, will
?rst be liined, as by mixing with lime water, mix
8 long enough to clean and brighten the surface -
ing dry lime with the ground ore and. adding
of the sul?de particles. The. pulp, thus adjusted
water, or otherwise making an alkaline pulp con
as to pH. is withdrawn through va conduit 1 and
introduced into a ?otation cell 8 where it is sub
jected to ?otation in the presence of suitable
quantities of a frother, such as pine oil, and a
xanthate collector. such as amyl xanthate, ‘or
pine‘oil as vfrothing agent and potassium ethyl
potassium amyl xanthate, whereby all of the sul
xanthate as collector. The reject of gangue, co
?de minerals, that is. pyrite, pyrrhotite and cobal
baltite, pyrite and pyrrhotite, in pulp condition,
tite. are ?oated and the gangue is rejected. The
is then rendered approximately neutral to acid . reject or tailings of gangue is withdrawn through "
and the mixture'is subjected to ?otation in the
a conduit 9 and suitably disposed of,‘ and the
taining lime. The chalcopyrite is then ?oated.
Any other mineral ?otable in a basic circuit may
likewise be- ?oated. This ?otation step may be
accomplished in the usual way, as by the use of
presence of a xanthate collector to ?oat‘ the co
baltite, pyrite and pyrrhotite away from the
gangue. It will be noted that in this step the
?oated sul?des are withdrawn through a conduit
the cobaltite depressant has not been used. The
next step involves the use of a xanthate collector
and a cobaltite depressant, whereby the cobaltite
pressant for cobaltite, such as mono calcium aryi
reference to a simple cobaltite-pyrite-pyrrhotite
the pyrite and pyrrhotite are ?oated and the co
l0 and introduced tola ?otation cell ll . Suitable
quantities of a frother, such as ‘pine oil, a
' cobaltite is also ?oated. - This is possible because 15
xanthate collector, such as amyl xanthate, a de
sulfonate, and an activator, which may be a heavy
metal salt, such as ferric sulfate, along with suf
is depressed and rejected and only the pyrite and
ficient water to form a suitable pulp, are added
pyrrhotite are ?oated, as described above with 20 and the mixture is subjected to ?otation. whereby
baltite is rejected. If ‘need be, more acid may be
_In the‘more complex separation of cobaltite
added to adjust the pH _of the pulp to 7 or less.
of the pH in this and the following
chalcopyrite, gangue, pyrite and pyrrhotite, as 25 Maintenance
?otation step at 'l or less, preferably from 7 to 4,
just described, the order of steps is highly impor
is especially important because the difference in
tant. It is important that the chalcopyrite be
?oatability. between cobaltite on the one‘ hand
?oated ?rst in a basic circuit and that gangue
and pyrite and pyrrhotite on the other hand is
be subsequently separated. I have found that if
small. By means of careful control‘ of pH' and
the gangue is ?rst separated and the chalcopyrite
proper selection of ?otation agents,- I am'able' suc
from an o're containing it in association with
or other like mineral is then separated, the ?o
tation products and tailings in subsequent sep
aration steps are contaminated with chalcopyrite.
' cessfully to ?oat the pyrite and pyrrhotite away
from the cobaltite despite this small difference in
?oatability. The cobaltite reject or tailin‘gs is re
35 moved through a conduit l2 and the ?oated pyrite
of steps as described above.
and pyrrhotite are removed through a conduit l3
‘ Of course, if chalcopyrite and gangue are sep
and introduced into a ?otation cell It. Suitable
arated by other means, or if a mineral mixture
quantities of the same reagents as used in cell H,
is_- available which does not contain chalcopyrite
and of-water and/or acid if need be. are intro
or gangue, the procedure of the invention may
40 duced into cell ll and the pyritd-pyrrhotite con- '
This difficulty is avoided by following the order
be suitably modi?ed or simpli?ed.
centrate is subjected therein to a second ?otation
similar to that carried out in cell l I. thus produc
ing a further quantity of cobaltite as reject or
agrammatic drawing representing a process of
tailings and ?oating a purer pyrite-'pyrrhotite
separating cobaltite from an ore containing it in 45 concentrate. The latter concentrate is removed
association with chalcopyrite, gangue, pyrite and
through a conduit I5 and the recovered cobaltite
is removed through a conduit _IB and joined with
Referring to the single ?gure of the drawing.
the ?rst portion of cobaltite concentrate removed
The process of my invention will be more fully
understood by reference to the accompanying di- -
an ore comprising chalcopyrite. pyrite, pyrrhotite.
conduit 12.
cobaltite and gangue, suitably ground and made 50 ‘ through
In the preferred embodiment illustrated by the
into a pulp (about 20-30% solids) and made alka-'
drawing and described above, the’pyrite-pyrrho- '
line with lime solution.v is introduced through a ' tite-cobaltite concentrate resulting fromthe sep
vconduit i into a ?otation cell 2 and is therein
aration of game in ?otation cell 8 is subjected to
subjected to ?otation in the presence of a froth
1a double ?otation as shown, but instead of this,
ing'agent such as pine oil and :a collector such 55 _ a single ?otation step, or three or even more ?o
as potassium ethyl xanthate. The frothing agent
tation steps, may be employed. Thus the cobaltite
and collector may be added separately to the ?o
concentrate may be subjected to further ?ota
tation cell, or maybe incorporated in the ore or ~~
tion to separate any residue of pyrite or pyrrhotite
pulp before it is introduced into the ?otation cell.
therein and the pyrite-pyrrhotite concentrate
Preferably, the frothing
60 my likewise be subjected to further ?otation to‘
pulp in the ?otation cell. ' The ?otation step car-,
ried out in cell 2, and subsequent ?otation steps
hereinafter described, may be carried out in ac-_
cordance with standard procedure, such. for ex
in f‘Principles ofMineral
Dressing" by A. M._G'audin (McGraw-Hill), 1939
, ample,'as that described
edition, pages 402-423. ‘ The chalcopyrlte is float
' ed in cell 2 and is- removed through a conduit 3.
The reject or-tailings. containing the cobaltite.
along with pyrite, pyrrhotite and gangue, is
withdrawn through a conduit 4 and introduced
' into a conditioning vessel 5 to which an acid. such,
for example, as sulfuric acid or hydrochloric acid,
is added through a conduit,‘ in quantity su?ieient
recover any residue of cobaltite therein.‘
The lime used in pretreating the mineral mix
ture. or- in the chalcopyrite separation‘ may be,
pure or impure lime. For. example. it may be a
dolomitic lime. The acid used in the neutraliz
ing or acidifying steps is preferably sulfuric acid.
but other acids capable of producing the’ desired
pH. such ashydrochloric and phosphoric acids, I
may. be used.‘ -
Following are speci?c examples of suitable '
frothing. collecting, activating and 'depressing
agents capable of use in accordance with my-v
invention, these speci?c examples belonging to
rdco811M classes of ?otation
agents; many of
set forth in Gmidin’s "Principles of '
material is preferably held in conditioning vessel
‘ to adjust the pH of the pulp to about 4 to '1. The,
Mineral Dressing,” referred to supra, at the
pages’ indicated below:
Frothing agents (page 363):
LbJton of ore
III. Reflotation of pyrite-pyrrhotite
Pine oil
Frother, such as pine oil ______ -_'
Higher alcohols
Collector, preferably amyl xan
thate __________________ __'___
Fuse] oil
Cresylic acid
0.5 to 0.1
0.1 to 0.25 1
Depressant for cobaltite, such as
Eucalyptus oil
mono calcium aryl sulfonate__ 0.25 to 0.5_
Activator, such as ferric sulfate-_ ’
0.5 to 2
Collectors (page 371) :
_The depressants used in accordance with my in
Amyl xanthate
Butyl xanthate
Propyl xanthate
vention are of the type of non-?oating dispersing
agents. Their function, as stated, is to depress
the cobaltite. They accomplish this result by se
Ethyl xanthate
Sodium and potassium salts of the above 15' lectively wetting the surface of the cobaltite
particles, thereby inhibiting bubble attachment to
and ?otation of the cobaltite particles. The acti
Sulfonated petroleum sludge
vators, which are preferably heavy metal salts,
Activators (pages 395 and 396):
have the effect‘ of promoting the'ac'tion of the
Ferric sulfate
'20 collecting agents. They appear to e?ect this re
Lead, nitrate
sult by preferential adsorption of the heavy metal
Lead chloride
ion, e. g. ferric ion, on the pyrite and pyrrhotite
Copper sulfate
particles, and forming heavy metal xanthate, e. 'g.
Copper chloride
. ferric xan'thate.
Cobaltite depressants (pages 393 and 394) :
25 : I claim:
Mono calcium_aryl sulfonate
Mono sodium aryl sulfonate .
In a method‘ of e?'ecting separation of cobaltite'
Sodium sul?de
Sodium cyanide
from a pulp mixture thereof with chalcopyrite.
gangue', and from iron sul?de minerals of similar
Sodium silicate
?oatability'to the cobaltite: that sequence of steps
which consists in ?rst rendering the pulp mix
ture alkaline with lime; adding av frother and a
may vary considerably. However, in ?oating py
.' collector comprising a xanthate, and subjecting
rite, Pyrrhotitc and cobaltite away ‘ from the
vsaid pulp to a‘ ?rst froth ?otation to ?oat said
gangue, in ?oating‘ pyrite and pyrrhotite away
chalcopyrite from said gangue, iron sul?de min
from cobaltite, and in re?oating the pyrite 35 erals and said cobaltite; then adding. acid to ad
pyrrhotite concentrate, I prefer to use the agents
Just the pH of the reject of gangue, iron sul?de
in the following approximate proportions:
minerals and cobaltite to a value not greater
than about 7 and a collector comprisinga xan
LbJtonof ore
I Ll'lotation of pyrite,- pyrrhotite
thate; then subjecting the pulp thusformed to a
'40 second ‘froth ?otation to‘ ?oat the cobaltite and
and cobaltite away from
iron sul?de minerals from the gangue; then add
Brother», such as pine oil .-__~_____ 0.3 to 0.2
ing to the cobaltite and iron sul?de a depressant
The amounts of such agents that may be used
collector,v preferably
amyl xanthate_.;..-__e ______ __ 0.25 to 0.75
. 45
II. Flotation of pyrite and pyrrho-
tite‘ away from cobaltlte:
Frother, such as pine oil______ -..'
0.5 to 0.1
erals comprising a' heavy metal salt; and subject
ing the pulp thus formed to .a third froth ?ota
tion to ?oat said iron sulfide minerals from said
‘Xanthate collector preferably
cobaltlte in the presence‘of said depressant._
' amyl xanthate_____-_____l__.._
0.25 to 0.5
Depressant for cobaltite. such as
mono calcium aryl sufonate--- 0.25 to 0.5
Activator, such as ferric sulfate-.. '
for the cobaltite a collector comprising 9. mn
thate, and an activator for the iron sul?de min
1 to 2
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