CN111621650B - Method for extracting metallic nickel from laterite-nickel ore - Google Patents
Method for extracting metallic nickel from laterite-nickel ore Download PDFInfo
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- CN111621650B CN111621650B CN202010533112.9A CN202010533112A CN111621650B CN 111621650 B CN111621650 B CN 111621650B CN 202010533112 A CN202010533112 A CN 202010533112A CN 111621650 B CN111621650 B CN 111621650B
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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
- C22B23/02—Obtaining nickel or cobalt by dry processes
- C22B23/023—Obtaining nickel or cobalt by dry processes with formation of ferro-nickel or ferro-cobalt
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
Abstract
The invention discloses a method for extracting metallic nickel from laterite-nickel ore, which comprises the following steps: carrying out reduction smelting treatment on the laterite-nickel ore to obtain a nickel-iron alloy; using zinc and/or magnesium metal melt as an extraction medium, melting the extraction medium, mixing the extraction medium with the nickel-iron alloy, and extracting the nickel-iron alloy to obtain low-melting-point eutectic and extraction residues; the mass ratio of the nickel-iron alloy to the extraction medium is (2: 1) - (1: 4), the extraction treatment temperature is 900-1100 ℃, and the extraction treatment time is 2-5 h; and carrying out vacuum distillation treatment on the low-melting-point eutectic to obtain a condensed extraction medium and a distillation product metallic nickel. The method for extracting metallic nickel from the laterite-nickel ore firstly uses the melt of zinc and magnesium monobasic or dibasic metal as an extraction medium, forms a eutectic with low melting point with nickel in the nickel-iron alloy at high temperature, and then carries out vacuum distillation on the eutectic to separate the extraction medium and the metallic nickel by utilizing the difference of saturated vapor pressure of different metals.
Description
Technical Field
The invention belongs to the field of metallurgy, and particularly relates to a method for extracting metallic nickel from laterite-nickel ore.
Background
In recent years, the stainless steel and new energy industries in China are rapidly increased, and the demand for nickel is greatly increased. For a long time, 60 percent of global nickel resource supply is sourced from nickel sulfide ores, but with the continuous increase of nickel demand and the gradual exhaustion of nickel sulfide resources, the laterite nickel ores accounting for 70 percent of nickel resource reserves become important nickel development resources.
Limonite type laterite-nickel ore has the characteristics of high iron content, low nickel content, low silicon magnesium content and high cobalt content, and is generally treated by a wet process. The wet process mainly obtains nickel leachate through high-pressure acid leaching, and then adopts technologies such as sulfide precipitation, solvent extraction and the like to separate nickel to produce electrolytic nickel, nickel oxide or nickel matte. The garnierite type laterite nickel ore has high content of silicon and magnesium, low content of iron and cobalt and high content of nickel, and is usually treated by adopting a pyrogenic process. The pyrogenic process is mainly used for producing the ferronickel alloy by rotary kiln reduction-electric furnace smelting and is used for manufacturing products such as stainless steel, alloy steel and the like, and the final product of the pyrogenic process is a ferronickel intermediate product and has the problem of high energy consumption. In addition, the traditional pyrometallurgical process mainly uses carbon as a reducing agent, so that a large amount of carbon emission cannot be avoided, and the development of the pyrometallurgical process is further limited by the current strict environmental protection management and control situation. For example, chinese patent CN201710527995.0 discloses a method for treating laterite-nickel ore, which comprises contacting laterite-nickel ore with carbon monoxide in a multistage fluidized reactor and reacting to obtain a first mixed gas containing carbon monoxide, carbon dioxide and nickel carbonyl and a residue; cooling and separating the first mixed gas to obtain liquid nickel carbonyl and a second mixed gas; decomposing liquid nickel carbonyl to obtain carbon monoxide and metallic nickel. The method takes carbon monoxide as a reducing agent, and inevitably generates large amount of emission of carbon gas.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing the method for extracting the metallic nickel from the laterite-nickel ore, which has the advantages of short process flow, low energy consumption, no carbon emission, cleaner and more environment-friendly treatment process.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for extracting metallic nickel from laterite-nickel ore comprises the following steps:
(1) carrying out reduction smelting treatment on the laterite-nickel ore to obtain a nickel-iron alloy;
(2) using zinc and/or magnesium metal melt as an extraction medium, melting the extraction medium, mixing the extraction medium with the nickel-iron alloy, and extracting the nickel-iron alloy to obtain low-melting-point eutectic and extraction residues; the mass ratio of the nickel-iron alloy to the extraction medium is (2: 1) - (1: 4), the extraction treatment temperature is 900-1100 ℃, and the extraction treatment time is 2-5 h;
(3) and carrying out vacuum distillation treatment on the low-melting-point eutectic to obtain a condensed extraction medium melt and a distillation product metallic nickel.
In the above method, preferably, in the step (3), the vacuum degree during the vacuum distillation treatment is 240Pa, the distillation treatment temperature is 1000 Pa and 1300 ℃, and the distillation treatment time is 0.5-2 h.
In the above method, preferably, in the step (1), the specific obtaining process of the nickel-iron alloy includes:
(a) mixing laterite-nickel ore, water and a fluxing agent to obtain a raw material mixture;
(b) granulating and drying the raw material mixture to obtain dry pellets with the particle size of less than 1 cm;
(c) adding the dried pellets into an electric arc furnace, and introducing hydrogen to carry out reduction smelting treatment to obtain a ferronickel melt;
(d) discharging the ferronickel melt into a granulating chamber through a launder, spraying high-pressure nitrogen to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to form ferronickel alloy particles, and settling at the bottom of the granulating chamber to obtain the granulated ferronickel alloy.
The invention adopts hydrogen to reduce and smelt the laterite-nickel ore, nickel and iron are generated in the reduction smelting process to form alloy melt, and other oxides such as SiO2MgO, unreduced FeO and the like form slag, and the ferronickel alloy is directly obtained by separating the slag from the metal melt.
Preferably, in the step (c), the reduction smelting treatment refers to smelting at the temperature of 1400 ℃ and 1650 ℃ for 40-60min, and the introduction amount of hydrogen is 400m in the range of 200-3Hydrogen gas.
The above process, preferably, in the step (d), the pressure of the high-pressure nitrogen gas is 0.2 to 2 MPa.
In the above method, preferably, in the step (a), the flux includes one or more of limestone, quicklime and slaked lime; the mass ratio of the laterite-nickel ore, water and the fluxing agent is (75-90): (5-10): (5-15).
Preferably, in the step (b), the drying temperature is 80-120 ℃ and the drying time is 30-60 min.
In the above method, preferably, the condensed extraction medium melt obtained in the step (3) is subjected to heat preservation, and the heat-preserved extraction medium melt is returned to the step (2).
In the method, the temperature for heat preservation is preferably 800-.
Compared with the prior art, the invention has the advantages that:
(1) the method for extracting metallic nickel from the laterite-nickel ore firstly uses zinc and magnesium monobasic or dibasic metal melt as an extraction medium, forms a low-melting-point eutectic with nickel in the nickel-iron alloy at high temperature, and then separates the extraction medium and the metallic nickel by vacuum distillation of the eutectic by utilizing the difference of saturated vapor pressure of different metals (high vapor pressure of magnesium and zinc and low vapor pressure of nickel), and meanwhile, the metal extraction medium melt can be recycled. The method for extracting the metallic nickel from the laterite-nickel ore is an environment-friendly, green and recyclable metallic nickel extraction method.
(2) The method for extracting metallic nickel from the laterite-nickel ore carries out direct reduction smelting on the laterite-nickel ore to obtain the ferronickel alloy, does not need a pre-reduction roasting process, and has short process flow and low energy consumption.
(3) The method for extracting the metallic nickel from the laterite-nickel ore adopts the hydrogen as the reducing agent in the reduction smelting process, does not generate carbon emission, and has cleaner and more environment-friendly treatment process.
(4) The invention adopts high-pressure nitrogen to cool and granulate the ferronickel melt to obtain the granulated ferronickel alloy, replaces the crushing procedure before the subsequent melt extraction, creates favorable conditions for the subsequent nickel metal extraction, simplifies the process and reduces the energy consumption.
Drawings
Fig. 1 is a process flow chart of the invention in the embodiment 1 for extracting metallic nickel from laterite-nickel ore.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a method for extracting metallic nickel from laterite-nickel ore, the technological process diagram of which is shown in figure 1, and the method comprises the following steps:
s1: taking laterite-nickel ore containing 1.72% of nickel and 18.38% of iron, adding fluxing agent (limestone and quicklime in a mass ratio of 1: 1) to mix for 3min in a mixer with the rotating speed of 17r/min, then adding water, and continuing mixing for 5min to obtain a mixture; wherein the mass ratio of the laterite-nickel ore to the fluxing agent to the water is 75:15: 10;
s2: placing the mixture into a material box of a double-roller briquetting machine, and pressing the mixture into pellets with the particle size of less than 1cm under the pressure of 60MPa, wherein the dropping strength of the pellets is 95 percent, the compressive strength of the pellets is 143N/piece, and the thermal burst index of the pellets is 0.60 percent;
s3: drying the pellets at 105 deg.C for 30 min;
s4: conveying the dried pellets to a smelting furnace, introducing hydrogen for reduction smelting, wherein the temperature range of the smelting furnace is 1550 ℃, and the amount of the introduced hydrogen is 200m under the standard atmospheric pressure3/(ton of laterite nickel ore), the total smelting time is 45min, and ferronickel melt is obtained; tail gas generated in the reduction smelting process is returned to S3 for drying the pellets;
s5: discharging the high-temperature ferronickel melt obtained in the step S4 into a granulating chamber through a launder, spraying nitrogen with the pressure of 0.5MPa to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to generate ferronickel alloy particles, and settling the ferronickel alloy particles at the bottom of the granulating chamber to obtain granulated ferronickel alloy;
s6: adopting metal magnesium as an extraction medium, melting the metal magnesium, mixing the molten metal magnesium with the granulated ferronickel alloy, and extracting the granulated ferronickel alloy to obtain an extracted low-melting-point eutectic and extraction residues; wherein the mass ratio of the granulated ferronickel alloy to the metal magnesium is 1:1, the extraction treatment temperature is 900 ℃, and the extraction treatment time is 2.5 h;
s7: and (3) carrying out vacuum distillation treatment on the eutectic after extraction in the S6 (the vacuum degree is 150Pa, the temperature is 1000 ℃, and the distillation treatment time is 0.5h) to obtain a condensed magnesium melt and a distillation product metallic nickel. And (3) preserving the temperature of the condensed magnesium melt (the temperature of the heat preservation treatment is 800 ℃) to obtain a circulating magnesium melt extraction medium, returning the circulating magnesium melt extraction medium to S6 for multiple times of extraction until the nickel and cobalt in the reaction system are completely extracted, and finally obtaining the metal nickel with the purity of 99.03%, wherein the total recovery rate of nickel is 94.53%.
Example 2:
the method for extracting metallic nickel from the lateritic nickel ore comprises the following steps:
s1: taking laterite-nickel ore containing 1.81% of nickel and 17.69% of iron, adding fluxing agent (limestone and quicklime in a mass ratio of 40: 60) to mix for 3min in a mixer with the rotating speed of 17r/min, then adding water, and continuing mixing for 5min to obtain a mixture; wherein the mass ratio of the laterite-nickel ore to the fluxing agent to the water is 80:10: 10;
s2: putting the mixture into a material box of a double-roller briquetting machine, and pressing the mixture into pellets with the particle size of less than 1cm under the pressure of 60MPa, wherein the dropping strength of the pellets is 92 percent, the compressive strength of the pellets is 135N/piece, and the thermal burst index of the pellets is 0.40 percent;
s3: drying the pellets at 108 ℃ for 36 min;
s4: conveying the dried pellets to a smelting furnace, introducing hydrogen for reduction smelting, wherein the temperature range of the smelting furnace is 1570 ℃, and the amount of introduced hydrogen is 250m under standard atmospheric pressure3/(ton of laterite nickel ore), the total smelting time is 50min, and ferronickel melt is obtained;
s5: discharging the high-temperature ferronickel melt obtained in the step S4 into a granulating chamber through a launder, spraying nitrogen with the pressure of 0.6MPa to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to generate ferronickel alloy particles, and settling the ferronickel alloy particles at the bottom of the granulating chamber to obtain granulated ferronickel alloy;
s6: adopting metal magnesium as an extraction medium, melting the metal magnesium and extracting the granulated ferronickel alloy to obtain an extracted low-melting-point eutectic and extraction residues; wherein the mass ratio of the granulated ferronickel alloy to the metal magnesium is 1: 2, the extraction treatment temperature is 970 ℃, and the extraction treatment time is 3.0 h;
s7: and (3) carrying out vacuum distillation treatment on the eutectic body extracted in the S6 (the vacuum degree is 125Pa, the temperature is 1050 ℃, and the distillation treatment time is 1.0h) to obtain a condensed magnesium melt and a distillation product metallic nickel. And (3) preserving the heat of the condensed magnesium melt (the heat preservation treatment temperature is 850 ℃) to obtain a circulating magnesium melt, returning the circulating magnesium melt to S6 for multiple times of extraction until the nickel and cobalt in the reaction system are completely extracted to obtain the metal nickel with the purity of 99.18%, wherein the total recovery rate of nickel is 95.01%.
Example 3:
the method for extracting metallic nickel from the lateritic nickel ore comprises the following steps:
s1: taking laterite-nickel ore containing 1.79% of nickel and 18.18% of iron, adding fluxing agent (limestone and quicklime in a mass ratio of 35: 65) to mix for 3min in a mixer with the rotating speed of 17r/min, then adding water, and continuing mixing for 5min to obtain a mixture; wherein the mass ratio of the laterite-nickel ore to the fluxing agent to the water is 80:12: 8;
s2: putting the mixture into a double-roller briquetting machine feed box, and pressing the mixture into pellets under the pressure of 60MPa, wherein the dropping strength of the pellets is 94 percent, the compressive strength of the pellets is 140N/piece, and the thermal burst index of the pellets is 0.50 percent;
s3: drying the pellets at 100 deg.C for 40 min;
s4: conveying the dried pellets to a smelting furnace, introducing hydrogen for reduction smelting, wherein the temperature range of the smelting furnace is 1550 ℃, and the amount of the introduced hydrogen is 300m under the standard atmospheric pressure3/(ton of laterite nickel ore), the total smelting time is 55min, and ferronickel melt is obtained;
s5: discharging the high-temperature ferronickel melt in the S4 into a granulating chamber through a launder, spraying nitrogen with the pressure of 0.6MPa to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to generate ferronickel alloy particles, and settling the ferronickel alloy particles at the bottom of the granulating chamber to obtain granulated ferronickel alloy;
s6: adopting metal magnesium as an extraction medium, melting the metal magnesium and extracting the granulated ferronickel alloy to obtain an extracted low-melting-point eutectic and extraction residues; wherein the mass ratio of the granulated ferronickel alloy to the metal magnesium is 1: 3, the extraction treatment temperature is 1000 ℃, and the extraction treatment time is 3.5 h.
S7: carrying out vacuum distillation treatment on the eutectic after extraction in the S6 (the vacuum degree is 120Pa, the temperature is 1000 ℃, and the distillation treatment time is 1.5h) to obtain a condensed magnesium melt and a distillation product metallic nickel; and (3) separating and preserving the condensed magnesium melt (the heat preservation treatment temperature is 850 ℃) to obtain a circulating magnesium melt, returning the circulating magnesium melt to S6 for multiple times of extraction until the nickel and cobalt in the reaction system are completely extracted to obtain the metal nickel with the purity of 99.30%, wherein the total recovery rate of nickel is 95.79%.
Example 4:
the method for extracting metallic nickel from the lateritic nickel ore comprises the following steps:
s1: mixing 1.86% of nickel-containing laterite-nickel ore and 17.97% of iron-containing laterite-nickel ore with fluxing agents (60: 40 limestone and quicklime in mass ratio) in a mixer at the rotating speed of 17r/min for 5min, then adding water, and continuously mixing for 5min to obtain a mixture; wherein the mass ratio of the laterite-nickel ore to the fluxing agent to the water is 82:8: 10;
s2: placing the mixture into a material box of a double-roller briquetting machine, and pressing the mixture into pellets with the particle size of less than 1cm under the pressure of 60MPa, wherein the dropping strength of the pellets is 94 percent, the compressive strength of the pellets is 136N/piece, and the thermal burst index of the pellets is 0.40 percent;
s3: drying the pellets at 100 deg.C for 50 min;
s4: conveying the dried pellets to a smelting furnace, introducing hydrogen for reduction smelting, wherein the temperature range of the smelting furnace is 1570 ℃, and the amount of introduced hydrogen is 300m under standard atmospheric pressure3And/or (ton of laterite-nickel ore), wherein the total smelting time is 60min, and ferronickel melt is obtained.
S5: discharging the high-temperature ferronickel melt obtained in the step S4 into a granulating chamber through a launder, spraying nitrogen with the pressure of 0.8MPa to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to generate ferronickel alloy particles, and settling the ferronickel alloy particles at the bottom of the granulating chamber to obtain granulated ferronickel alloy;
s6: adopting metal magnesium as an extraction medium, melting the metal magnesium, mixing the molten metal magnesium with the granulated ferronickel alloy, and extracting the granulated ferronickel alloy to obtain an extracted low-melting-point eutectic and extraction residues; wherein the mass ratio of the granulated ferronickel alloy to the metal magnesium is 1: 3, the extraction treatment temperature is 1000 ℃, and the extraction treatment time is 4.0 h;
s7: carrying out vacuum distillation treatment on the co-melt extracted in the step S6 (the vacuum degree of the distillation treatment is 100Pa, the temperature is 1050 ℃, and the distillation treatment time is 2.0h) to obtain a condensed magnesium melt and a distillation product metallic nickel; and (3) preserving the heat of the condensed magnesium melt (the heat preservation treatment temperature is 850 ℃) to obtain a circulating magnesium melt extraction medium, returning the circulating magnesium melt to S6 for multiple times of extraction until the nickel and cobalt in the reaction system are completely extracted to obtain the metal nickel with the purity of 99.56%, wherein the total recovery rate of nickel is 96.32%.
Claims (7)
1. A method for extracting metallic nickel from laterite-nickel ore is characterized by comprising the following steps:
(1) carrying out reduction smelting treatment on the laterite-nickel ore to obtain a nickel-iron alloy; wherein, the specific obtaining process of the nickel-iron alloy comprises the following steps:
(a) mixing laterite-nickel ore, water and a fluxing agent to obtain a raw material mixture;
(b) granulating and drying the raw material mixture to obtain dry pellets with the particle size of less than 1 cm;
(c) adding the dried pellets into an electric arc furnace, and introducing hydrogen to carry out reduction smelting treatment to obtain a ferronickel melt; the reduction smelting treatment refers to smelting at the temperature of 1400-1650 ℃ for 40-60min, wherein the introduction amount of hydrogen is 400m in a way that 200-400m is introduced into each ton of laterite-nickel ore under standard atmospheric pressure3Hydrogen gas;
(d) discharging the ferronickel melt into a granulating chamber through a launder, spraying high-pressure nitrogen to the ferronickel melt flowing down from the launder, dispersing the ferronickel melt into fine liquid drops in the descending process, cooling and condensing to form ferronickel alloy particles, and settling at the bottom of the granulating chamber to obtain granulated ferronickel alloy;
(2) using zinc and/or magnesium metal melt as an extraction medium, melting the extraction medium, mixing the extraction medium with the nickel-iron alloy, and extracting the nickel-iron alloy to obtain low-melting-point eutectic and extraction residues; the mass ratio of the nickel-iron alloy to the extraction medium is (2: 1) - (1: 4), the extraction treatment temperature is 900-1100 ℃, and the extraction treatment time is 2-5 h;
(3) and carrying out vacuum distillation treatment on the low-melting-point eutectic to obtain a condensed extraction medium and a distillation product metallic nickel.
2. The method as claimed in claim 1, wherein in the step (3), the vacuum distillation process is performed at a vacuum degree of 100-240Pa, a distillation process temperature of 1000-1300 ℃, and a distillation process time of 0.5-2 h.
3. The method of claim 1, wherein in step (d), the pressure of the high pressure nitrogen gas is from 0.2 to 2 MPa.
4. The method of claim 1, wherein in step (a), the flux comprises one or more of limestone, quicklime, slaked lime; the mass ratio of the laterite-nickel ore, water and the fluxing agent is (75-90): (5-10): (5-15).
5. The method of claim 1, wherein in step (b), the drying temperature is 80-120 ℃ and the drying time is 30-60 min.
6. A process according to any one of claims 1 to 5, characterized in that the condensed extraction medium melt obtained in step (3) is subjected to heat preservation and the heat preserved extraction medium melt is returned to step (2).
7. The method of claim 6, wherein the temperature of the incubation is 800-.
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