United States Patent 0
CC
1
2,700,606
Patented Jan. 25, 1955
2
2,700,606
It has been found desirable to use an approximately 40%
PRODUCTION OF VANADIUM METAL
Harley A. Wilhelm and John Reed Long, Ames, Iowa,
metric proportions indicated (in addition to the stoichio
or greater, excess of calcium to V205 over the stoichio
metric amount of calcium required to react with the
sulfur present), and best results have been obtained
when the excess is in the range 60—70%.
assignors to the United States of America as repre
reaction is normally carried out in a
sented by the United States Atomic Energy Commission
No Drawing. Application August 1, 1951,
10
Serial No. 239,860
2 Claims. (Cl. 75-84)
The present invention is concerned with a method 15 tained. The reaction 1s initiated by rapidly heating the
bomb to an elevated temperature such as 700° C.
for the production of vanadium metal. More partic
ularly, the present invention is directed to a process for
The process of the present invention may be better
understood by consideration of the examples which
follow.
ployed with impure vanadium pentoxide and which
Example I
will yield ductile massive vanadium metal.
20
Vanadium is one of the most widely distributed ele
A 180-gram quantity of V205
ments occurring in small percentages in granite, sedi
was thoroughly dried and th
mentary rocks, clays and in many iron, lead and copper
veriaed V205 was mixed with
ores. The metal is one of the least volatile metals at the
melting point and has highly desirable characteristics as 25
the reduction of vanadium oxide, which may be em
a structural metal. It is, however, extremely di?icult to
reduce to the pure metallic state from its oxides and
consequently very little of the metal has been obtained.
(bringing the total calcium content of the bomb to 312
g.). The bomb was closed and then heated to about
One method of producing metallic vanadium comprises
700° C. within ?ve minutes. The ?ring of the bomb
the reduction of vanadium pentoxide with calcium metal 30 may be observed as it is characterized by a sudden rise in
in the presence of calcium chloride. This method, how
the temperature of the container. The bomb upon
ever, may only be used with very pure vanadium pent
opening was found to contain a massive regulus of pure
oxide and the product obtained is usually in the form of
vanadium metal weighing 65.4 g. corresponding to a 72%
?nely divided vanadium particles. Other methods have
yield. The slag also contained several smaller pieces of duc
in the past been devised for the production of massive 35 tile vanadium metal (which were recovered from the slag
vanadium metal but these methods require as a starting
by leaching with HCI) su?icient to bring the total amount
material a very pure form of vanadium oxide such as
of metal up to 74.7 g. corresponding to 83% total yield.
chemically pure V205 in order to produce a ductile metal.
The metal recovered was a ductile form having a hard
It is an object of the present invention to provide a
ness of approximately 75 on the Rockwell B scale. The
method for producing ductile, malleable vanadium metal 40 metal is su?iciently malleable that a 90% reduction can
from a vanadium oxide.
,
easily be achieved by cold-rolling.
It is an additional object of the present invention to
The process of the present invention may also be used
provide a method which may be employed with a tech
for the recovery of ductile vanadium metal from technical
nical grade vanadium oxide as the starting material
grade V202 as shown by the following example.
for producing ductile malleable vanadium metal, a sub 45
Example II
stantial portion of which will be in the form of a massive
regulus.
A quantity of air-dried technical grade V205 was
Broadly, the process of the present invention com
treated with hydrogen at an elevated temperature where
prises reacting a mixture of sulfur and vanadium oxide
by substantially all of the vanadium pentoxide was re
with calcium metal whereby the vanadium oxide is re
duced to the V203 form. A ISO-g. quantity of the V203
duced and the resultant product is predominantly a
was mixed with 55 g. of sulfur and 297 g. of metallic
massive (regulus of ductile, malleable vanadium metal.
calcium particles. Five grams of metallic calcium par
The essence of the present invention lies in the employ
ticles was placed in the bottom of a 2.5" bomb con
ment of sulfur as the booster in the reaction mixture.
taining a sintered dolomitic oxide liner and the charge
While the process of the present invention may be
placed on top of the metallic calcium particles.
employed with chemically pure vanadium pentoxide, the 55
great advantage of the present method lies in its ability
quickly heated
started.
to produce massive ductile vanadium metal from the
technical grade vanadium oxides such as technical grade
vanadium pentoxide, sinces the cost of technical grade
vanadium pentoxide is at present about one-seventh of 60 vanadium metal was ductile
the cost of the chemically pure grade vanadium pent
on the Rockwell B scale.
oxide. Technical grade V205 is actually a sodium
vanadate ore concentrate, usually containing about 87
93% V205, 5—6% sodium oxide, and less than 1% of
-
It will be apparent that the above-described embodi
ents of the invention are illustrative ‘and modi?cations
thereof will be apparent to those skilled in the art with
other impurities such as aluminum, iron, calcium, silicon 65 out departing from the spirit of the invention or the
and magnesium. The technical grade V205 is thoroughly
scope of the appended claims.
dried and by the process of our invention is then mixed
What is claimed is:
with ?nely divided metallic calcium and sulfur. The
.
e process of preparing massive ductile vana
sulfur is usually added in an S:V20s ratio of about
dium metal from technical grade vanadium pentoxide
1:8 (in grams). The V205 content of technical grade 70 containing 87—93% of V205, 5-6%
V205 may be considered as 90%, if the actual V205
and less than 1% of other impurities,
content is not known.
ratio is permissible.
Considerable variation in this
forming a reaction
' '
The sulfur acts as a booster, re
acting directly with the calcium. The total heat gen
erated during the reduction of the vanadium oxide may
be considered to be the sum of the heats generated by
the two reactions:
present, and heating the
reaction mixture to approximately 700° C. in a reduc
80 tion bomb.
2. A process as de?ned in claim 1 in which the re
8,700,606
action mixture consists "of 180 parts by weight of said
technicalgrade vanadium pentoxide, 20 .parts by weight
of sulfur, and 312 parts by weight of metallic calcium.
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References Cltedm the ?lelot' thispatent
I
£088,909
UNITED ‘STATES PATENTS
_
Kuzel _____ __v _________ __ Mar. 3, 1914
1,318,709
‘2,421,029
2,561,526
Vautin ______________ __ Oct. 14, 1919
Magram _.___,_ ______ __ May 27, 1947’
McKechnie et al _______ __ July 24, 1951
27,625
Great Britain ,_ _____________ __ of 1896
24,148
Great Britain ______________ __ of 1903
2,576,763
5
Linz ________________ __ Nov. 27, 1951
FOREIGN PATENTS