AU2017369155B2 - Wet metallurgy method for nickel oxide ore - Google Patents
Wet metallurgy method for nickel oxide ore Download PDFInfo
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- AU2017369155B2 AU2017369155B2 AU2017369155A AU2017369155A AU2017369155B2 AU 2017369155 B2 AU2017369155 B2 AU 2017369155B2 AU 2017369155 A AU2017369155 A AU 2017369155A AU 2017369155 A AU2017369155 A AU 2017369155A AU 2017369155 B2 AU2017369155 B2 AU 2017369155B2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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Abstract
The present invention improves the nickel recovery rate in a dezincing step for removing zinc contained in a nickel oxide ore in wet metallurgy that uses high pressure acid leaching of the ore. A wet metallurgy method comprising: a leaching step S1 for acid leaching of nickel oxide ore under high pressure to obtain a leachate; a neutralization step S3 for removing a neutralization precipitate generated by adding a neutralizing agent to said leachate and obtaining a post-neutralization solution; a dezincing step S4 for removing zinc precipitate generated by blowing hydrogen sulfide gas into said post-neutralization solution to obtain a post-dezincing solution; and a nickel recovery step S5 for adding a sulfiding agent to said post-dezincing solution and recovering the nickel as a sulfide. When the hydrogen sulfide gas is blown in, said post-neutralization solution is successively passed through multiple reaction tanks that are connected in series while the volume of hydrogen sulfide gas blown into the second reaction tank from the top and subsequent reaction tanks is adjusted to 50% to 90% of the total volume of hydrogen sulfide gas blown into all of the reaction tanks.
Description
Technical Field
[0001]
The present invention relates to a hydrometallurgical
method in which nickel oxide ore is subjected to high
pressure acid leaching, and more particularly relates to a
hydrometallurgical method capable of increasing a nickel
recovery rate.
Background Art
[0002]
As one of hydrometallurgical method methods of nickel
oxide ore, a high pressure acid leach (HPAL) process using
sulfuric acid is known. This process is different from a
conventional pyrometallurgical process generally used as a
smelting method for nickel oxide ore in that nickel oxide
ore is processed under wet conditions throughout the
process without performing an oxide ore reduction step and
drying step at high temperature, and is therefore
advantageous in terms of energy and cost. Further, the
HPAL process allows to obtain a nickel- and cobalt
containing sulfide (hereinafter also referred to as a
nickel/cobalt mixed sulfide) which is concentrated to a
nickel grade of about 50 to 60% by mass, and therefore high
purity nickel can easily be obtained by refining.
[0003]
When nickel oxide ore as a raw material is subjected to
high pressure acid leaching to recover nickel as a product,
the nickel oxide ore is generally often processed through
the following steps (a) to (d):
(a) a leaching and solid-liquid separation step in
which water is added to crushed nickel oxide ore to obtain
a slurry, sulfuric acid is then added to the slurry, the
mixture is placed in a reaction container such as an
autoclave and maintained at a temperature of about 240 to
2800C under high pressure to leach valuables such as nickel
and cobalt contained in the nickel oxide ore, and the
slurry is taken out of the reaction container after
leaching and subjected to solid-liquid separation in a
sedimentation tank to separate a leachate containing nickel
and cobalt from a leach residue;
(b) a neutralization step in which the leachate is
adjusted to a predetermined pH by adding a neutralizer to
precipitate an impurity such as iron to obtain a
neutralized slurry, a coagulant is added to the neutralized
slurry containing a neutralized precipitate of the impurity
to separate the neutralized precipitate by solid-liquid
separation so as to obtain a post-neutralization solution
containing nickel and cobalt;
(c) a dezincification step in which a sulfurizing agent is added to the post-neutralization solution while the amount of the sulfurizing agent added is controlled to be in an appropriate range to remove only zinc and copper as sulfides without sulfurizing nickel and cobalt contained as valuables in the post-neutralization solution, the thus obtained sulfide precipitate (also referred to as zinc precipitate) is separated by solid-liquid separation to obtain a post-dezincification solution; and
(d) a nickel recovery step in which a sulfurizing agent
is added to the post-dezincification solution to generate a
nickel/cobalt mixed sulfide, and the mixed sulfide is
separated and recovered.
[0004]
For example, Patent Literature 1 discloses a
hydrometallurgical method based on the above-described high
pressure acid leaching, which includes a leaching step in
which nickel oxide ore is subjected to leaching using
sulfuric acid and then to solid-liquid separation to obtain
a leachate; a neutralization step in which a neutralizer is
added to the leachate to generate a neutralized precipitate
containing an impurity, and the neutralized precipitate is
removed to obtain a post-neutralization solution; a
dezincification step in which hydrogen sulfide gas is added
to the post-neutralization solution to generate zinc
sulfide, and the zinc sulfide is removed to obtain a mother liquor for nickel recovery; and a nickel recovery step in which hydrogen sulfide gas is added to the mother liquor to recover nickel and cobalt as a mixed sulfide.
[0005]
In the method disclosed in Patent Literature 1, a leach
residue is appropriately added to the leachate and the pH
of the post-neutralization solution is adjusted to 3.0 to
3.5 in the neutralization step, and further a sulfurization
reaction is performed in the dezincification step in a
state where suspended solids including the neutralized
precipitate and the leach residue remain in the post
neutralization solution so that the turbidity of the post
neutralization solution is 100 to 400 NTU (Nephelometric
Turbidity Unit). The thus obtained slurry containing a
sulfide precipitate is subjected to solid-liquid separation
in a filtration step in the dezincification step to obtain
the sulfide precipitate and a final solution containing
nickel and cobalt.
Citation List
Patent Literature
[00061
Patent Literature 1: JP 2010-37626 A
Summary of Invention
[00071
In the above-described HPAL process using nickel oxide
ore as a raw material, conditions for generating a sulfide
precipitate of zinc in the dezincification step approximate
to conditions for generating a sulfide precipitate of
nickel, and therefore there is often a case where nickel
loss occurs due to coprecipitation of zinc and nickel in
the zinc precipitate. The recovery rate of nickel has a
great impact on the economic efficiency of the process, and
therefore it is desirable to reduce nickel loss as much as
possible.
[0008]
In light of the above circumstances, the present
invention seeks to provide a hydrometallurgical method for
nickel oxide ore based on high pressure acid leaching which
is capable of increasing the recovery rate of nickel by
reducing the amount of nickel coprecipitated with
impurities such as zinc and copper when zinc contained in
the nickel oxide ore is removed.
[00091
The present inventors have found that the recovery rate
of nickel can be increased by providing two or more
reaction tanks connected in series for the dezincification
reaction, and by adjusting the distribution ratio of hydrogen sulfide gas blown into the reaction tanks when a dezincification reaction (sulfurization reaction) is performed by sulfurization by adding a sulfurizing agent to a post-neutralization solution obtained by neutralizing a leachate obtained by subjecting nickel oxide ore to high pressure acid leaching.
[0010]
More specifically, the present invention is directed to
a hydrometallurgical method for nickel oxide ore,
including: a leaching step in which nickel oxide ore is
subjected to acid leaching under high pressure, and a leach
residue is then removed to obtain a leachate; a
neutralization step in which a neutralizer is added to the
leachate to generate a neutralized precipitate, and the
neutralized precipitate is removed to obtain a post
neutralization solution; a dezincification step in which
hydrogen sulfide gas is blown into the post-neutralization
solution to generate a zinc precipitate, and the zinc
precipitate is removed to obtain a post-dezincification
solution; and a nickel recovery step in which a sulfurizing
agent is added to the post-dezincification solution to
recover nickel as a sulfide, wherein in the dezincification
step, the hydrogen sulfide gas is blown into two or more
reaction tanks connected in series to allow the post
neutralization solution to flow therethrough in order in such a manner that an amount of the hydrogen sulfide gas blown into the second and following reaction tanks from top is adjusted to 50% or more but 90% or less of a total amount of the hydrogen sulfide gas blown into all the reaction tanks.
Advantageous Effects of Invention
[0011]
According to the present invention, it is possible to
reduce the amount of nickel coprecipitated with impurities
such as zinc and copper when zinc contained in nickel oxide
ore is removed, thereby increasing the recovery rate of
nickel.
Brief Description of Drawings
[0012]
FIG. 1 is a process flow chart showing a
hydrometallurgical method for nickel oxide ore according to
an embodiment of the present invention.
FIG. 2 is a graph obtained by plotting a relationship
between the particle diameter of each of samples of zinc
sulfide obtained in Examples and the blowing ratio of
hydrogen sulfide gas during generation of the zinc sulfide.
FIG. 3 is a graph obtained by plotting a relationship
between the Ni grade of each of samples of zinc sulfide obtained in Examples and the blowing ratio of hydrogen sulfide gas during generation of the zinc sulfide.
FIG. 4 is a graph obtained by plotting a relationship
between the Ni grade and the particle diameter of each of
samples of zinc sulfide obtained in Examples.
Description of Embodiments
[0013]
Hereinbelow, a hydrometallurgical method for nickel
oxide ore according to an embodiment of the present
invention will be described. As shown in FIG. 1, the
hydrometallurgical method starts from a leaching step Si in
which nickel oxide ore as a raw material is crushed into
small pieces by a crushing means such as a crusher, and
water is added thereto to obtain a slurry. Then, sulfuric
acid is added to the slurry, and the mixture is placed in a
pressure vessel such as an autoclave and subjected to
sulfuric acid leaching under high temperature and pressure
at, for example, 240 to 2800C to leach nickel and cobalt as
valuables.
[0014]
Then, in a solid-liquid separation step S2, a slurry
obtained by the above-described sulfuric acid leaching is
subjected to multistep washing, and then a leach residue is
removed from the slurry by solid-liquid separation to obtain a leachate containing nickel, cobalt, and impurity elements. Then, in a neutralization step S3, an alkali such as calcium hydroxide or calcium carbonate is added as a neutralizer to the leachate to adjust the pH of the leachate to precipitate the impurity elements as a neutralized precipitate. Then, a flocculant (coagulant) is added to a slurry containing the neutralized precipitate, and the slurry is subjected to solid-liquid separation to remove the neutralized precipitate to obtain a post neutralization solution containing nickel and cobalt. It is to be noted that if necessary, the neutralized precipitate obtained in the neutralization step S3 may be returned to the solid-liquid separation step S2. As shown by a dotted line in FIG. 1, at least part of the leach residue obtained in the solid-liquid separation step S2 may be added to the leachate in the neutralization step S3.
[0015]
Then, in a dezincification step S4, hydrogen sulfide
gas is blown as a sulfurizing agent into the post
neutralization solution to generate a zinc-containing
sulfide precipitate (zinc sulfide), and a slurry containing
the sulfide precipitate is subjected to solid-liquid
separation to remove the zinc sulfide to obtain a post
dezincification solution. Finally, in a nickel recovery
step S5, a sulfurizing agent such as hydrogen sulfide gas is added to the post-dezincification solution to generate a nickel/cobalt mixed sulfide containing nickel and cobalt, and a slurry containing the nickel/cobalt mixed sulfide is subjected to sold-liquid separation to recover the nickel/cobalt mixed sulfide and to obtain a post sulfurization solution (barren solution). As shown in FIG.
1, if necessary, the barren solution may be returned to the
solid-liquid separation step S2.
[0016]
In the embodiment of the hydrometallurgical method
according to the present invention, zinc is selectively
precipitated and settled as a sulfide in the
dezincification step S4 so as to be separated from nickel
and cobalt. At this time, two or more reaction tanks for
blowing hydrogen sulfide gas into the post-neutralization
solution are provided to perform a sulfurization reaction,
and are connected in series so that the post-neutralization
solution obtained in the neutralization step flows
therethrough in order. Further, the ratio of the amount of
hydrogen sulfide gas blown into the second and following
reaction tanks from the top out of the reaction tanks
connected in series to the amount of hydrogen sulfide gas
blown into all the reaction tanks (hereinafter also
referred to as "blowing ratio") is adjusted to be in an
appropriate range. This makes it possible to reduce the amount of nickel coprecipitated with impurities such as zinc and copper, thereby increasing the recovery rate of nickel.
[0017]
More specifically, in the dezincification step S4, when
n-number of reaction tanks for performing a dezincification
reaction are provided in the order of a No. 1 reaction tank,
a No. 2 reaction tank, a No. 3 reaction tank, ... and a No.
n reaction tank from the top so that the post
neutralization solution flows therethrough in this order,
the ratio of the amount of hydrogen sulfide gas blown into
(n-1)-number of reaction tanks including the No. 2 and
following reaction tanks to the amount of hydrogen sulfide
gas blown into all the reaction tanks from the No. 1
reaction tank to the No. n reaction tank (i.e., blowing
ratio) is adjusted to 50% to 90%. This makes it possible
to reduce the amount of nickel coprecipitated with
impurities such as zinc and copper.
[0018]
Further, when the blowing ratio is set to such a high
value, particles of the sulfide precipitate can grow to
have a large particle size. As a result, solid-liquid
separability in the dezincification step can also be
improved. In the dezincification step, fine particles of
the sulfide precipitate are likely to be formed. Therefore, when a slurry containing such fine particles is subjected to solid-liquid separation using a filtration device such as a filter press, a filter cloth is quickly clogged so that the volume of a liquid that can pass through the filter cloth reduces. In order to recover the filter cloth, the filter cloth needs to be frequently backwashed or replaced, which may reduce production efficiency. However, when the blowing ratio is set to such a high value as described above, particles of the sulfide precipitate have a large diameter so that filterability improves.
[0019]
As described above, in order to improve not only the
recovery rate of nickel but also solid-liquid separability,
the blowing ratio is preferably adjusted to 60% to 90%,
more preferably 60% to 85%. This makes it possible to
increase the particle diameter of particles of zinc sulfide
(also referred to as "zinc sulfide precipitate") to be
finally generated which allows to prevent the clogging of a
filter cloth of a subsequent filtration device, such as a
filter press. As a result, the ability of the filtration
device to allow a liquid to pass through it improves, which
makes it possible to improve productivity. The reason why
such an increase in blowing ratio allows particles of the
zinc sulfide precipitate to grow to have a large particle
diameter is because when the blowing ratio increases, the number of fine particles of sulfides of impurities including zinc which are generated in an early stage of a sulfurization reaction in the No. 1 reaction tank decreases, and particles of the sulfides grow using these small number of fine particles as nuclei (also referred to as "seeds") in the No. 2 and following reaction tanks.
[0020]
When the blowing ratio is less than 60%, the ratio of
hydrogen sulfide gas blown into the No. 1 reaction tank is
relatively high. In this case, fine particles of zinc
sulfide as nuclei are excessively generated in the No.1
reaction tank, and particles of sulfides grow using these
large number of fine particles as nuclei in the No. 2 and
following reaction tanks, which makes it difficult to
obtain particles of zinc sulfide having a large particle
diameter. On the other hand, when the blowing ratio
exceeds 90%, generation of fine particles of zinc sulfide
as nuclei is suppressed in the No. 1 reaction tank, which
leads to a shortage of seeds. In this case, there is a
fear that particle grow is insufficient in the No. 2 and
following reaction tanks. That is, when more than 10% but
less than 40% of hydrogen sulfide gas supplied to all the
reaction tanks is blown into the No. 1 reaction tank, seeds
can be stably generated. More specifically, the blowing
ratio may be appropriately adjusted so that the particles grow to the extent that a filter cloth is not easily clogged in subsequent filtration treatment.
[00211
It is to be noted that when three or more reaction
tanks are provided in series, the last reaction tank may
serve as a buffer tank into which a large amount of
hydrogen sulfide gas is not blown. When the last reaction
tank serves as a buffer tank, a reaction time can be
secured by the buffer tank even when the short pass of a
processed liquid occurs in the reaction tanks located
upstream from the last reaction tank, which prevents a
reduction in total reaction efficiency. However, the
number of reaction tanks for dezincification reaction is
preferably 3 or less. This is because when there are a
large number of reaction tanks in which substantially no
sulfurization reaction occurs, problems occur such as waste
of equipment costs and energy costs and redissolution of
the zinc sulfide precipitate due to the oxidation of the
slurry staying in the excess reaction tanks by air
contained in the slurry. Further, zinc sulfide particles
separately prepared or zinc sulfide particles recovered by
solid-liquid separation may be supplied to the No. 1
reaction tank as seeds, which makes it possible to generate
coarser zinc sulfide particles.
[0022]
In the dezincification step S4, a dezincification
reaction is preferably performed at a pH of 2.5 or higher
but 3.5 or lower. If the pH is lower than 2.5, zinc is
insufficiently separated due to redissolution of zinc
sulfide that has once been generated. On the other hand,
if the pH exceeds 3.5, elements, such as iron and nickel,
that should not be removed may also be precipitated, which
increases a precipitate load on a filter cloth or a
filtration device used in subsequent filtration treatment.
Particularly, in the case of iron, a large amount of fine
precipitate is generated, which promotes the clogging of a
filter cloth. Therefore, in order to achieve a sufficient
flow rate of the filter cloth, the filter cloth needs to be
frequently backwashed, which may reduce production
efficiency.
[0023]
It is to be noted that in the dezincification reaction,
an acid is generated after the reaction as shown in the
following formula 1. Therefore, the dezincification
reaction is preferably performed while the pH is maintained
at 2.7 or higher but 3.0 or lower so that the pH falls
within the above range even when an acid is generated.
[Formula 1]
ZnSO 4 +H 2 S-ZnS+H 2 SO 4
Examples
[00241
Nickel oxide ore was subjected to hydrometallurgical
leaching at high temperature and pressure in accordance
with a process flow chart shown in FIG. 1 to recover nickel
in the form of a sulfide. More specifically, nickel oxide
ore including laterite ore, saprolite ore, and limonite ore
and sulfuric acid were placed in an autoclave as a pressure
vessel and heated to a temperature of 240 to 2600C by a
steam heater to perform leaching under high pressure, and
then the obtained leach slurry was subjected to solid
liquid separation to remove a leach residue to obtain a
leachate. Calcium hydroxide was added as a neutralizer to
the leachate to adjust the pH of the leachate to 3.0 to 3.5
to generate a neutralized precipitate. Then, an anionic
flocculant was added to remove the neutralized precipitate
by solid-liquid separation to obtain a post-neutralization
solution.
[0025]
Then, three reaction tanks (No. 1 reaction tank, No. 2
reaction tank, No. 3 reaction tank) were prepared which
were connected in series and each of which had an almost
cylindrical shape having a diameter of 7.7 m and a height
of 12 m (capacity: 460 M 3 ). The post-neutralization
solution was continuously supplied to the first No. 1
reaction tank at a flow rate of 1200 to 1450 m 3 /hr so as to flow through the No. 1 reaction tank, the No. 2 reaction tank, and the No. 3 reaction tank in this order. Further, hydrogen sulfide gas was blown into each of these three reaction tanks to sulfurize zinc contained in the post neutralization solution to generate zinc sulfide. At this time, the ratio of the amount of hydrogen sulfide gas blown into the No. 2 reaction tank and the No. 3 reaction tank to the amount of hydrogen sulfide gas blown into all the three reaction tanks, that is, the blowing ratio was changed little by little from 5.1% to 86.3%.
[0026]
Then, a post-sulfurization solution taken out of the
last No. 3 reaction tank was supplied to a Buchner funnel,
in which a filter cloth was placed on a perforated plate
having a plurality of pores and a diameter of 60 cm, and
subjected to solid-liquid separation by vacuum suction on
the filtrate side. In this way, zinc sulfide (zinc sulfide
precipitate) samples 1 to 46 generated at different blowing
ratios were obtained. It is to be noted that blowing of
hydrogen sulfide gas into the No. 2 reaction tank and the
No. 3 reaction tank was performed in such a manner that
most of the hydrogen sulfide gas was blown into the No. 2
reaction tank, that is, the No. 3 reaction tank was used to
react zinc sulfide particles grown in the No. 2 reaction
tank with remaining dissolved hydrogen sulfide gas to finally grow the zinc sulfide particles. More specifically, the amount of hydrogen sulfide gas blown into the No. 3 reaction tank was appropriately increased or decreased without changing the blowing ratio on the basis of the particle diameter of sampled grown zinc sulfide particles.
[0027]
The following Table 1 shows the blowing ratio during
generation of each of the zinc sulfide samples 1 to 46 and
the particle dimeter of each of the zinc sulfide samples 1
to 46 generated at the shown blowing ratio. FIG. 2 shows a
graph obtained by plotting a relationship between the
blowing ratio and the particle dimeter of zinc sulfide.
The particle diameter of zinc sulfide was measured by
observing the sample collected during steady operation with
a microscope and by using a Microtrac. It is to be noted
that the pH and temperature of the slurry in the reaction
tanks during generation of the zinc sulfide samples 1 to 46
were maintained at 2.7 to 2.9 and 60 to 670C, respectively.
The composition of the post-neutralization solution was as
follows: nickel concentration 3.5 to 4.0 g/L, iron
concentration 0.7 to 1.4 g/L, and zinc concentration 60 to
140 mg/L. The zinc concentration of the post
dezincification solution was reduced to about 5 to 12 mg/L.
[0028]
[Table 1]
Blowing Particle Blowing Particle Samples diameter of Samplesratioo) diameter of Zn sulfide (m) Zn sulfide ( m) 1 5.1 8.1 24 60.1 11.4 2 7.6 8.4 25 63.8 18.1 3 11.0 9.1 26 66.4 14.1 4 11.6 6.9 27 66.5 10.7 5 12.9 9.1 28 66.7 17.8 6 13.2 7.2 29 67.3 10.6 7 13.9 7.9 30 67.9 12.5 8 23.7 8.1 31 68.4 15.6 9 23.8 9.9 32 68.6 11.5 10 23.8 7.7 33 69.0 13.6 11 24.1 7.7 34 80.1 14.3 12 24.1 9.3 35 81.0 19.0 13 28.5 6.6 36 81.6 11.0 14 28.6 6.4 37 82.0 10.1 15 28.6 8.3 38 82.2 16.7 16 30.8 7.7 39 83.4 22.6 17 30.8 6.9 40 84.1 16.8 18 48.1 7.7 41 84.5 28.1 19 48.3 7.0 42 84.6 15.0 20 48.8 6.9 43 84.8 30.1 21 49.0 8.2 44 84.9 18.7 22 51.5 7.9 45 86.2 22.0 23 53.5 9.8 46 86.3 16.7
[0029]
As can be seen from the results shown in Table 1 and
FIG. 2, particles of the zinc sulfide samples 24 to 46
obtained by adjusting the ratio of hydrogen sulfide gas
blown into the No. 2 and following reaction tanks to 60% or
higher but 90% or lower were coarse and had a particle
diameter of about 10 pm or more. These zinc sulfide
samples 24 to 46 were prepared by continuously performing smelting over several days (at least 24 hours) per sample at different blowing ratios, but a filtration device to which the slurry taken out of the No. 3 reaction tank was supplied was not clogged. On the other hand, particles of all the zinc sulfide samples 1 to 23 prepared at a blowing ratio of less than 60% were fine and had a particle diameter of less than 10 pm. Each of these zinc sulfide samples 1 to 23 were prepared by continuously performing smelting at different blowing ratios, and as a result, a filtration device was clogged before the elapse of 24 hours.
[00301
Then, 37 zinc sulfide samples were randomly selected
from the zinc sulfide samples 1 to 46, and their nickel
grades were measured by ICP. The nickel grade of the zinc
sulfide and the blowing ratio are shown in the following
Table 2. FIG. 3 is a graph obtained by plotting a
relationship between the nickel grade and the blowing ratio.
Further, FIG. 4 is a graph obtained by plotting a
relationship between the particle diameter and the nickel
grade of the zinc sulfide.
[0031]
[Table 2]
Samples Blowing ratio (%) Ni grade of Zn sulfide(%) 1 5.1 1.7 2 7.6 1.2 5 12.9 1.7 6 13.2 1.7 7 13.9 1.0 8 23.7 1.2 9 23.8 1.2 10 23.8 1.1 11 24.1 1.3 16 30.8 1.7 17 30.8 1.2 18 48.1 1.0 19 48.3 1.3 20 48.8 1.3 21 49.0 1.4 22 51.5 0.6 23 53.5 0.7 24 60.1 0.7 25 63.8 0.5 26 66.4 0.6 27 66.5 0.8 29 67.3 0.6 30 67.9 0.5 31 68.4 0.6 32 68.6 0.4 33 69.0 0.5 34 80.1 0.4 35 81.0 0.8 36 81.6 0.4 37 82.0 0.7 39 83.4 0.4 41 84.5 0.6 42 84.6 0.4 43 84.8 0.6 44 84.9 0.5 45 86.2 0.7 46 86.3 0.8
[00321
As can be seen from Table 2 and FIG. 3, the nickel
grade of the zinc sulfide can be reduced to 1% or less by
setting the blowing ratio to 50% or more. Further, as can
be seen from FIG. 4, the nickel grade of the zinc sulfide
can be reduced to 1% or less by allowing particles of the
zinc sulfide to have a particle dimeter of about 10 pm or
more, that is, by setting the blowing ratio of hydrogen
sulfide gas to about 60% or more as can be seen from Table
1 and FIG. 2. As described above, when the particle
diameter of the zinc sulfide is 10 pm or more, the effect
of improving filterability can be obtained in addition to
the effect of increasing the recovery rate of nickel.
[0033]
Throughout this specification and the claims which follow,
unless the context requires otherwise, the word "comprise",
and variations such as "comprises" or "comprising", will be
understood to imply the inclusion of a stated integer or
step or group of integers or steps but not the exclusion of
any other integer or step or group of integers or steps.
[0034]
The reference in this specification to any prior
publication (or information derived from it), or to any
matter which is known, is not, and should not be taken as,
an acknowledgement or admission or any form of suggestion that that prior publication (or information derived from it) or known matter forms part of the common general knowledge in the field of endeavour to which this specification relates.
Claims (2)
1. A hydrometallurgical method for nickel oxide ore,
comprising: a leaching step in which nickel oxide ore is
subjected to acid leaching under high pressure, and a leach
residue is then removed to obtain a leachate; a
neutralization step in which a neutralizer is added to the
leachate to generate a neutralized precipitate, and the
neutralized precipitate is removed to obtain a post
neutralization solution; a dezincification step in which
hydrogen sulfide gas is blown into the post-neutralization
solution to generate a zinc precipitate, and the zinc
precipitate is removed to obtain a post-dezincification
solution; and a nickel recovery step in which a sulfurizing
agent is added to the post-dezincification solution to
recover nickel as a sulfide, wherein in the dezincification
step, the hydrogen sulfide gas is blown into two or more
reaction tanks connected in series to allow the post
neutralization solution to flow therethrough in order in
such a manner that an amount of the hydrogen sulfide gas
blown into the second and following reaction tanks from top
is adjusted to 50% or more but 90% or less of a total
amount of the hydrogen sulfide gas blown into all the
reaction tanks.
2. The hydrometallurgical method for nickel oxide ore
according to claim 1, wherein in the dezincification step, the sulfurizing reaction is performed in a pH range of 2.5 or higher but 3.5 or lower.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016-232416 | 2016-11-30 | ||
| JP2016232416 | 2016-11-30 | ||
| JP2017-002344 | 2017-01-11 | ||
| JP2017002344A JP6350684B2 (en) | 2016-11-30 | 2017-01-11 | Method for hydrometallizing nickel oxide ore |
| PCT/JP2017/041381 WO2018101069A1 (en) | 2016-11-30 | 2017-11-16 | Wet metallurgy method for nickel oxide ore |
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| AU2017369155A1 AU2017369155A1 (en) | 2019-07-11 |
| AU2017369155B2 true AU2017369155B2 (en) | 2022-09-29 |
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| AU2017369155A Active AU2017369155B2 (en) | 2016-11-30 | 2017-11-16 | Wet metallurgy method for nickel oxide ore |
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| EP (1) | EP3550040A4 (en) |
| JP (1) | JP6350684B2 (en) |
| AU (1) | AU2017369155B2 (en) |
| PH (1) | PH12019501187B1 (en) |
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| JP7095606B2 (en) * | 2019-01-17 | 2022-07-05 | 住友金属鉱山株式会社 | Method for producing nickel-cobalt mixed sulfide from nickel oxide ore by hydrometallurgy |
| JP7508977B2 (en) | 2020-09-29 | 2024-07-02 | 住友金属鉱山株式会社 | Dezincification treatment method, nickel oxide ore hydrometallurgy method |
| JP7585921B2 (en) * | 2021-03-24 | 2024-11-19 | 住友金属鉱山株式会社 | Hydrometallurgical process for nickel oxide ore |
| CN116444013B (en) * | 2023-03-31 | 2025-08-26 | 中南大学 | Zinc-iron separation method, application and application of zinc-iron separation device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2049646A (en) * | 1979-05-10 | 1980-12-31 | Inco Ltd | Separation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004305917A (en) * | 2003-04-07 | 2004-11-04 | Sumitomo Metal Mining Co Ltd | Method for removing zinc from nickel sulfate aqueous solution |
| JP5572928B2 (en) * | 2008-07-25 | 2014-08-20 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
| US8911531B2 (en) * | 2009-10-19 | 2014-12-16 | Sumitomo Metal Mining Co., Ltd. | Hydrometallurgical plant of nickel laterite ore and operation method thereof |
| JP6222141B2 (en) * | 2015-03-05 | 2017-11-01 | 住友金属鉱山株式会社 | Method for producing nickel sulfide, method for hydrometallizing nickel oxide ore |
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2017
- 2017-01-11 JP JP2017002344A patent/JP6350684B2/en active Active
- 2017-11-16 AU AU2017369155A patent/AU2017369155B2/en active Active
- 2017-11-16 EP EP17876261.3A patent/EP3550040A4/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2049646A (en) * | 1979-05-10 | 1980-12-31 | Inco Ltd | Separation process |
Also Published As
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|---|---|
| JP2018090889A (en) | 2018-06-14 |
| PH12019501187A1 (en) | 2020-02-24 |
| AU2017369155A1 (en) | 2019-07-11 |
| PH12019501187B1 (en) | 2021-08-11 |
| EP3550040A1 (en) | 2019-10-09 |
| JP6350684B2 (en) | 2018-07-04 |
| EP3550040A4 (en) | 2020-07-29 |
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