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Патент USA US3097172

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United States Patent O??ce
3,097,162
Patented July 9, 1963
2
1
been removed. More ‘speci?cally, it is an object of this
invention to provide a ?oatation method by means of
METHOD FOR CONCEN'I‘RATING ALUMINUM
which the aluminum silicates and zircon in such beach
SILICATES AND ZRCON FROM BEACH SAND
sand concentrates can be separated from the quartz. It
Robert E. Baarson, La Grange, and Charles W. Jonaitis, 5 is still another object of this invention to provide a method
Chicago, 'Ill., assignors to Armour and Company, Chi
“(for carrying out the bulk separation of aluminum silicates
cago, 111., a corporation of Delaware
in reject sands concentrates from the quartz and zircon
No Drawing. Filed Dec. 2, 1960, Ser. No. 73,231
therein, and ‘further, to provide a method for separating
2 Claims. (Cl. 209-466)
the zircon from the quartz without the need for additional
This invention relates to a method for concentrating 10 quantities of collecting agent. Further objects and ad
vantages wi‘ll appear as the speci?cation proceeds.
aluminum silicates and zircon in sand deposits which are
In practicing the present invention, the beach sand frac
usually known as beach sands. More particularly, this
tion from which the titanium oxide minerals have been
invention relates to a method for making a bulk separa
separated is vformed into a ?oatation feed. The particles
tion of the non-‘conductive and non-magnetic minerals
15 of this fraction, as received, range ‘from about —30 to
in beach sands from the quartz.
+200 mesh. ‘To the ?otation feed is added an amine col~
Beach sands of the type which the present invention
lector, and a depressant selected from the group consisting
is concerned may be found along the sea shore, but are also
of dextrins, gums and starches. The aqueous feed is ad
found in large inland deposits in Florida and elsewhere.
justed to an alkaline pH, and a frother, such as pine oil
These sand beds or deposits are composed principally of
quartz, while containing a small proportion of valuable 20 or cresy‘lic acid, is introduced into the ‘feed. Amine col
lectors impart some frothing in themselves and for this
minerals, among them being titanium oxide minerals like
reason the use of a frothing agent in the process is
i'lmenite and rutile, in addition to the heavy minerals
optional and may be omitted. Employing standard ?ota
'such as kyanite~'sillimanite, zircon, s'tauro'lite ‘and dumo-r
tion procedures, an aluminum silicates concentrate is ob
-tierite. Usually the content of quartz in these sands will
be at least 90°, while the content of the various heavy 25 tained in the under?ow while a combined zircon and
quartz product is recovered in the over?ow.
minerals may range irom a trace to upwards of 4%.
The over?ow'product may then be re-pulped and worked
The most valuable .product at present in beach sands is
into a ?otation feed to which is added ‘a depressant in the
the titanium oxide minerals. These-and other conductive
form of a ?uorine containing acid. The pH of this feed
and magnet-responsive heavy minerals are recovered from
beach sand deposits by complicated and expensive pro 30 is adjusted to below ‘about 6.0, preferably about 3.0. A
frother, as in the initial ?otation operation, may be added.
cedures. For example, the steps in one of these processes
It is generally unnecessary to introduce further quantities
involves passing the beach sands through a series of spiral
of the amine collector. Again employing conventional
concentrators to make a rough separation of the titanium
?otation techniques, a zircon concentrate is obtained in
oxide and other heavy minerals from the quartz. F ollow
ing the rough separation, there are cleaner and recleaner 35 the over?ow leaving a tailing consisting primarily of
quartz.
spiral circuits to upgrade the ‘concentrate, and a large
Any amine collector can be employed. Preferably,
amount of the middling material is recycled through these
however, the amine ?oatation agent is a primary amine
circuits to increase recovery. The titanium minerals in
containing a hydrophobic group of from 6 to 22 carbon
the heavy mineral concentrate are then further separated
and concentrated by electrostatic and magnetic separators. 40 atoms. Mixed amines like primary, tallow and soya
amines are suitable. Both mono‘ and polyamines may be
The electrostatic separation removes the ilmenite and
used. Very satisfactory results are obtained when the
rutil-e while induced roll magnets are employed to remove
snazrsz
The resultant non—conductive, non-magnetic reject frac
amine ?otation {agent is used in the ‘form of a water-soluble
salt thereof, such as an amine acetate or hydrochloride
The problem involved in using such non-conductive
being preferred.
the staurolite and dumortierite.
tions from this operation contain minerals which are in 4.5 salt. Amine-nitrile blends sold under the trademark
Armo?ote, land amines alone, taken up in a frother such as
themselves valuable. The composition of these tractions
pine oil or an ‘alcohol such as isopropanol, are also
is roughly 40 to 50% aluminum silicates, also referred
effective.
to as the kyanite-sillimanite fraction, 20% to 30% zircon,
To achieve theoutstanding results of the present inven
and 25 to 40% quartz. Heretofore, there has been no
practical and commercially feasible way of recovering 50 tion it is only necessary to add small quantities of the
collecting agent to the ore. Usually, from about 0.1
these valuable-minerals from the reject beach sand concen
to about 4.0 pounds of the agent per ton of ore will be
trates. It is with these fractions that the present invention
satisfactory, with ‘from 0.3 to about 1.0 pound per ton
is principally concerned.
non-magnetic ores to obtain an aluminum silicates and 55
The pH of the aqueous feed formed [from the starting
beach sand fraction may be controlled by the addition of
minor amounts of such inorganic alkaline reagents as
recoveries has heretofore received little attention. The
sodium or potassium hydroxide. A pH of from 7.5 to i12
industry has: [always realized that this discarded material
may be used but a range of 8 to 10 is preferred. The im
contains valuable heavy minerals but no commercially
feasible method has up to now been devised to obtain the 60 portant point is to ‘have a su?icient amount of the alka
line reagent present to maintain the pH of the alkaline
minerals in proper grade and recovery. Applicants have
side.
solved the problem and have provided through this inven
The depressant employed in bringing about a separa
tion a ?otation method which enables the bulk concen
tion of the aluminum silicates from the zircon and quartz
tration of the valuable aluminum silicate and zircon frac-..
may, as indicated, be selected from the group consisting
tions from the non-conductive, non-magnetic fraction of
of dextrins, gums and starches. These agents have the
beach sand concentrates.
effect of depressing the aluminum silicate fraction of
It is therefore a general object of this invention to
the beach sand permitting the zircon and quartz ?otation
provide a method for concentrating the aluminum silicates
to be recovered in the over?ow.
and zircon minerals in beach sands, and speci?cally, to
The ?uorine containing acid employed to effect a sepa
provide a ?otation method for accomplishing the concen 70
ration between the zircon and quartz is preferably hy
tration of aluminum silicates ‘and zircon from beach sand
dro?uoric acid, although other ?uorine containing acids
concentrates from which the titanium oxide minerals have
zircon product of high ‘grade in economically practical
3,097,162
3
4
can be substituted as well as mixtures of hydro?uoric
Metallurgical Results
acid and other ?uorine containing acids.
The pulp density in the conditioning and ?otation circuits may be varied widely. In the conditioning circuit
the solids may be as low as 25%.
weight, weight, Percent percent percent
grams 136mmt heavyl grade recovery
Product
However, 60 to 85%
5
mmem s
solids is preferred and 70% solids is considered an opti
.
.
.
mum condition.
.
.
.
A1
In the ?otation circuit the solids may
t7
1
run as high as 40% and as low as 15 0.
‘
ummum
s'li ate
l c
S_
A 25% pup
density, however, is especially e?ective for ?otation.
Quartz con "i
'Ihe ?otation operations described above can be ‘carried 10
COmPOSlte ---- --
232
it?
3538
-
146
29 2
10'87 """""""" "
52%~
it’?
50° ---------------------------------- -
out in the usual type of ?otation cells provided with means
for supplying an to the lower portion of the cells. It 1s
signi?cant that the method of this invention permits a
EXAMPLE H
clean separation to be made between all of the aluminum
Preparation of ore ____________ ___ ____ __ As received.
silicates from the zircon and quartz on the one hand 15 Flotation machine ___________________ __ Fagergren.
and the zircon from the quartz on the other. The sepaWater _____________________________ __ Dlstilled.
rate mineral concentrates can be further upgraded by
Temperature ________________________ _- 25° C.
Reagents and Conditions
Conditions
Reagents, pounds per ton
Point of addition
Time
Float Percent
cond.
(min)
pH
Starch
solids
Armac NaOH
3366
T
15‘ rougher -------------- --
9.1 T
7.3
2nd mugh“ ------------- --
213 F _____________ __
Zircon cone _____________ __
3.0
0.8
0
0.12
0.2
11""
Pine
HF
oil
(48%)
0.17
0.17
______ __
(L08
2'54
NOTE.—~1st and 2nd ronghers ?ltered and combined in cell for addition of hydro?uoric
acid (48%) ‘and subsequent ?otation. ‘Starch 3366 obtained from Corn Products. (Un
modi?ed Corn Starch.)
V
gravity separation, electrostatic or magnetic separation,
etc. to give the very high grade required of these minerals. 40
Metallurgical Results
This procedure enables the recovery of 90% or more of
the aluminum silicates and zircon contained 1n the beach
.
.
.
.
.
Product
.
grea‘dgilfst' perlcili‘ltt’ Eggs‘; Pggggt 5,3253%,
W
'
We‘
sand concentrates.
t
minerals
Whereas these materials were treated as a waste prod
uct in normal beach sand operations from which titanium 45 Alclgrlllcinum silicates
oxide minerals were concentrated the method of this illzircon c0110 ___________ __
iii;
iiig
vention now provides a practical and commercially feasible
Quartz C0110 ---------- --
13°
26- 5
means for recovering valuable products from these waste
Composite _____ __
giigi
2%.?)
23:2
9'12 ---------------- -
499 __________________________________ __
materials.
This invention is further described in the following 50
speci?c examples.
EXAMPLE I
EXAMPLE III
Preparation of ore ___________________ _. As received.
Flotation machine ___________________ __ Fagergren.
Preparation of ore ___________________ __ As received.
55 Flotation machine ___________________ __ Fagergren.
Water ______________________________ _. Distilled.
Water _____________________________ __ Distilled.
Temperature ________________________ _. 25° C.
Temperature ________________________ _. 25° C.
Reagents and Conditions
Conditions
Reagents, pounds per ton
Point of addition
Time
00nd.
1
Float Percent
(min) solids
_____________ __
15“ Tougher -------------- -— i
v
2nd rousher ------------- -- {
g
1A
2
pH
Dextrin Armae NaOH
164
T
20
______ __
2% ______ __
Zircon cone __________________ "5/; ""'i% ______ __
Pine
oil
HF
(48%)
i
l
______ __
1
0t 8
.
.
,
2.0
0 1
________________ __
________ __
0 2
______ __
0.04
o. 17
______________ __
0 17
0 O8 _
2‘54
l I-—Initial; F-Final.
N era-1st and 2nd roughers ?ltered and combined in cell for addition of hydro?uoric acid (48%) and sub: sequent ?otation. Dextrln 164 obtained from Corn Products. Armac T is an acetate salt of tallow amine.
3,097,162
5
Reagents and Conditions
Conditions
Point of addition
Time
cond.
Float Percent
(min) solids
_____________ __
1“ mughe’ -------------- -- i
14
Reagents,‘ pounds per ton
20
%
2
______ _.
Zircon conc _____________ __
Dcxtrin Armae
164
T
Pine
oil
HF
(48%)
NaOH
7.8 I____-_
2% ______ __
.-
2nd “ugh”------------- --
pH
Trace
351a.“
2.0
0. 2
0.17
0.2
0‘ 17
q
.
‘race
e. 35
________ l.
E6
0 08
1' 97
No'rE.-1st and 2nd roughers ?ltered and combined in cell for addition of hydro?uoric acid (48%) and sub
sequent ?otatlon. A minute amount of caustic was necessary to raise the pH of the roughers.
Metallurgical Results
trate. Percent Heavy Minerals essentially is the total
heavy mineral grade in each product obtained, with the
Weight, Weight, Percent Percent Percent
grams Percent heavy gTade Temvery
Pmduct
minerals
remainder being quartz. Percent ‘Grade indicates the
grade of the mineral being concentrated, taking into ac
.
count both the quartz and other heavy minerals
as con
20
Alummum silicates
taminants. _Percent Recovery represents that portion of
cone ________________ _.
153
so. 5
97. so
giggltlz‘gggcf_________ __
?ts
28-1
8}: 6%
.
95. 0
63,7
the total mineral appearing in the particular product that
60~ 0
93- 5
is considered to be the cencentrate.
______________ “ 25
comp‘mte ----- --
While in the foregoing speci?cation this invention has
501 ---------------------------------- --
been described in relation to a speci?c embodiment there
of and many details have been set forth for this embodi
merit, it will be apparent to those skilled in the art that the
EXAMPLE IV
preparation of ore ___________________ __ As receivg¢
invention is susceptible to other embodiments and that
Flotation machine ___________________ __ Fagergren
30 many of the details set forth herein can be varied widely
Water _____________________________ __ Distilled.
Without departing from the basic concepts of the inven
Temperature ________________________ __ 25° C.
tion.
Reagents and Conditions
Conditions
Point of addition
Time
cond
Float Percent
(min) solids
Reagents, pounds per ton
pH
Dextrin
164
Duo- NaOH
mac C
Pine
011
HF
(48%)
0.8
2.0
0.1
______ __
_
0.17
...... __
0. 04
0.2
Zircon conc _____________ __
0.17 .
0' 08
2 54
'
Norn-lst and 2nd roughers ?ltered and combined in cell for addition of hydro?uoric acid (48%) and subse
quent ?otation.
Dextrin 164 obtained from Corn Products. Duomac O is a diacetate salt of a coco diamine.
Metallurgical Results
50
minum silicate and zircon from a non-conductive, non
Weight, Weight, Percent Percent Percent
grams percent heavy
grade recovery
Product
We claim:
1. In a process for the concentration of quartz, alu
magnetic fraction of beach sand concentrate, comprising
the steps of ?oating a zircon and quartz fraction from the
minerals
55 aluminum silicates in the sand in an aqueous solution
_ _ _ _ _ __
174
34.
96.23
95
69
-._
192
38.3
91.34
60
S8 5
containing an amine collector and a depressant selected
from the group consisting of dextrins, gums and starches,
Quartz conc .......... ._
135
26. 9
4. 91
________________ __
said aqueous solution being at a pH of from about 7.5 to
Composite _____ __
501
Aluminum silicates
cone . _ _ _ _ _
Zircon cone.
0
__________________________________ __
about 12, and then ?oating the zircon from the quartz
of said zircon-quartz fraction in the presence of a ?uorine
containing acid and at a pH from about 6.0 to about 2.0.
2. In a process for the concentration of quartz, alu
REMARKS
The me in the tests conducted was the resultant non
conductor, non-magnetic product from electrostatic sepa
minum silicate and zircon from a non-conductive, non
magnetic fraction of beach sand concentrate, comprising
the steps of ?oating ‘a zircon ‘and quantz, fraction from
The 65 the aluminum silicates in the sand in an aqueous solution
ration and separation over induced roll magnets.
electrostatic separation removed the ilmenite and rutile
at a pH of about 8.0 containing an amine collector and
while the induced roll magnets removed the staurolite and
a depressant selected from the group consisting of dex
dumortieriite leaving an aluminum silicates-zircon-quartz
trins, gums and starches, said amine collector having at
‘fraction. This fraction had an approximate composition
least one hydrophobic gnoup of from 6 to 22 carbon
of 45% aluminum silicates, 25% zircon, and 30% quartz. 70 atoms, and then ?oating the zircon from the quartz of
Compositions on this and subsequent concentrates were
said zircon-quartz fraction, without adding more of the
obtained by petrographic analysis. Heavy mineral anal
collecting agent in the presence of a ?uorinecontaining
ysis was obtained by heavy media separation.
acid and at a pH of about 3.0.
The analyses indicate an upgrading of minerals in both
the ‘aluminum silicates concentrate and the zircon concen 75
(References on following page)
3,097,162
References Cited in the ?le of this patent
UNITED STATES PATENTS
‘2,177,985
2,205,503
2,341,046
Harris ______________ __ Oct. 31, 1939
Tmtter _____________ __ June 25, 1940
Kirby _______________ __ Oct. 9, 1940
8
2,792,940
2,970,688
Baaa'son ____~_ ________ __ May 21, 1957
Uhland ______________ __ Feb. 7, 1961
OTHER REFERENCES
~
Gaudin: Flotation, page 500 (Sillimanite and Kyan'ite),
Second Edition, McGraw-Hill, 1957.
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