CN113462894A - Device and method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag - Google Patents

Device and method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag Download PDF

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Publication number
CN113462894A
CN113462894A CN202110619184.XA CN202110619184A CN113462894A CN 113462894 A CN113462894 A CN 113462894A CN 202110619184 A CN202110619184 A CN 202110619184A CN 113462894 A CN113462894 A CN 113462894A
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nickel
water
tank body
cobalt
copper
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李怀明
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Gansu Kangxing Technology Co ltd
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Gansu Kangxing Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04Working-up slag
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0065Leaching or slurrying
    • C22B15/0067Leaching or slurrying with acids or salts thereof
    • C22B15/0071Leaching or slurrying with acids or salts thereof containing sulfur
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0407Leaching processes
    • C22B23/0415Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043Sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08Sulfuric acid, other sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag, which comprises a tank body (1), a transmission mechanism (2), a stirring paddle (3) and a lifting mechanism (4), wherein the stirring paddle (3) is arranged inside the tank body (1), and the transmission mechanism (2) is connected with the stirring paddle (3); one end of the tank body (1) is provided with an overflow port (5), and the other end is provided with a tailing discharge port (6); the lifting mechanism (4) is arranged at one end of the tank body (1); the tank body (1) is provided with a feed inlet (7), a plurality of flue gas inlet openings (8) and a waste gas absorption opening (9). The recovery method comprises the following steps: finely grinding nickel smelting water-quenched slag; adding the levigated water quenching slag and water into a tank body; introducing the smelting industrial waste gas containing sulfur dioxide into the tank body, and starting the stirring paddle to obtain a leaching product containing nickel, copper and cobalt and leached residues. The method can recover valuable metals in the water-quenched slag at lower cost.

Description

Device and method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag
Technical Field
The invention belongs to the technical field of non-ferrous metal smelting, and particularly relates to a device and a method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag.
Background
The water quenching slag is a process waste slag discharged in the nickel smelting process and is FeO & SiO2The granulated slag formed by water quenching of the solution as the main component is discharged 150 ten thousand tons of water quenched slag every year in a certain nickel smelting plant, the annual utilization is about 10 ten thousand tons, the rest is accumulated in an enterprise slag yard, the accumulated storage amount reaches about 3000 ten thousand tons, and the balance is aboutThe ecological environment and the living environment around the enterprise cause serious environmental impact.
The main mineral phases of the water-quenched slag include pyroxene (magnesium-containing), olivine and the like, and in addition, the water-quenched slag contains a large amount of glass phases, and three main structures exist: (1) iron forsterite (Fe, Mg) in columnar distribution2SiO4And fayalite FeSi4A crystalline phase; (2) irregular silicon oxide fill phases between crystalline phases; (3) copper nickel cobalt iron sulfide distributed between the two tissues in a scattered manner. The water quenching slag contains a large amount of iron elements and silicon dioxide, and a small amount of metal elements such as nickel, copper, cobalt, lead, zinc and the like mainly exist in the form of oxides and sulfides. The long-term storage of the water-quenched slag not only causes environmental pollution, but also is huge resource waste, and simultaneously shows that the nickel smelting waste slag has huge development and utilization values.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a device and a method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag, which can fully utilize waste nickel smelting water-quenched slag resources and recover valuable metals in the water-quenched slag at lower cost.
The invention adopts the following technical scheme:
the device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized by comprising a tank body (1), a transmission mechanism (2), a stirring paddle (3) and a lifting mechanism (4), wherein the stirring paddle (3) is arranged inside the tank body (1), and the transmission mechanism (2) is connected with the stirring paddle (3); an overflow port (5) is processed at one end of the tank body (1), and a tailing discharge port (6) is processed at the other end of the tank body (1); the lifting mechanism (4) is arranged at one end of the tank body (1) which is provided with the overflow port (5); the tank body (1) is provided with a feed inlet (7), a plurality of flue gas inlet openings (8) and a waste gas absorption opening (9).
The device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized in that the tank body (1) is obliquely arranged, and one end of the tank body (1) provided with the tailing discharge port (6) is higher than one end of the tank body (1) provided with the overflow port (5). The included angle between the bottom surface of the tank body (1) and the horizontal plane is 14-18 degrees.
The device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized in that the stirring paddle (3) is a spiral stirring paddle; the lifting mechanism (4) is a spiral lifting mechanism; an exhaust gas absorption cover is arranged above the exhaust gas absorption opening (9).
The recovery method based on the device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized by comprising the following steps of:
step (I): finely grinding the nickel smelting water-quenched slag to obtain finely ground water-quenched slag;
step (II): adding the levigated water quenching slag and water into a tank body; the mass ratio of the water-quenched slag after grinding to water is 1: (4-6);
step (three): introducing smelting industrial waste gas containing sulfur dioxide into the tank body through a plurality of flue gas inlets, and starting a stirring paddle to obtain a leaching product containing nickel, copper and cobalt and leached residues; leaching products containing nickel, copper and cobalt overflow through the overflow port, and residues after leaching are discharged through a tailing discharge port; the mass ratio of the flow of the smelting industrial waste gas containing sulfur dioxide to the water quenching slag is (2-3): 1, the concentration of sulfur dioxide in the smelting industrial waste gas containing sulfur dioxide is 8-10%, and the temperature of the smelting industrial waste gas containing sulfur dioxide is 120-220 ℃.
The recovery method of the device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized in that the content of the water-quenched slag with the granularity of less than 3mm after being ground in the step (I) is more than or equal to 80 percent.
The recovery method of the device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized in that the rotating speed of the stirring paddle in the step (III) is 3r/min-10 r/min.
The invention has the beneficial technical effects that: by adopting the device and the method, on the basis of fully utilizing the industrial flue gas, the sulfur dioxide-containing industrial flue gas is utilized for quick leaching without adding new acid liquid, the nickel, copper and cobalt elements in the nickel smelting water-quenched slag are efficiently and comprehensively recovered, and the aim of comprehensively utilizing industrial solid waste resources is fulfilled.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
Detailed Description
Referring to fig. 1, the device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag comprises a tank body 1, a transmission mechanism 2, a stirring paddle 3 and a lifting mechanism 4, wherein the stirring paddle 3 is arranged inside the tank body 1, the stirring paddle 3 is a spiral stirring paddle, the diameter of the stirring paddle 3 is 1000mm-2400mm, and the length of the stirring paddle 3 is 8000mm-14000 mm; the transmission mechanism 2 is connected with the stirring paddle 3; an overflow port 5 is processed at one end of the tank body 1, and a tailing discharge port 6 is processed at the other end of the tank body 1; the tank body 1 is obliquely arranged, and one end of the tank body 1, which is provided with a tailing discharge opening 6, is higher than one end of the tank body 1, which is provided with an overflow opening 5. The lifting mechanism 4 is arranged at one end of the tank body 1 where the overflow port 5 is processed, and the lifting mechanism 4 is a spiral lifting mechanism. The tank body 1 is provided with a feed inlet 7, a plurality of flue gas inlet openings 8 and a waste gas absorption opening 9, and a waste gas absorption cover is arranged above the waste gas absorption opening 9.
The working principle of the device is as follows: uniformly feeding the levigated water quenching slag into a tank body through a feeder, adding water into the tank body, introducing industrial high-temperature waste flue gas containing sulfur dioxide from a flue gas inlet, and carrying out acid leaching reaction under the action of spiral stirring, wherein the leaching solution is a product, and the leaching slag is a tailing. The flue gas inlet ports are distributed along the two sides of the tank body in a staggered mode, the distance between the flue gas inlet ports and the tank bottom is 100mm, the number of the inlet points is 5-6, the distance between the inlet points is 1000mm, the inlet amount is increased along with the depth of ore pulp, and the inlet amount is controlled by a valve. The inlet nozzle extends into the middle of the rotating blade, and the extending length of the inlet nozzle is 200 mm. The production capacity of the device is 4.0-7.0t/h, the specification and the model of the device can be increased according to the increase of unit production capacity, the groove body of the device needs anticorrosion treatment, and the stirring paddle and the blades need anticorrosion wear-resistant materials.
The recovery method of the device for recovering nickel, copper and cobalt from the nickel smelting water-quenched slag comprises the following steps:
step (I): finely grinding the nickel smelting water-quenched slag to obtain finely ground water-quenched slag; the nickel smelting water-quenched slag comprises the following components in percentage by mass: 1.5 to 14 percent of MgO, 0.8 to 5.0 percent of CaO, 0.15 to 0.5 percent of Ni, 0.2 to 0.3 percent of Cu, 0.06 to 0.3 percent of Co0.06 to 0.3 percent of Fe 30 to 45 percent of S, 0.5 to 1.2 percent of S and the balance of SiO2And compounds corresponding to the above metals. The nickel smelting water-quenched slag mainly comprises iron element and silicon dioxide, wherein the mass percentage of the iron element can reach 30-45%, and SiO2The mass percentage of the components can reach 30-42 percent. The content of the ground water-quenched slag with the granularity less than 3mm is more than or equal to 80 percent.
Step (II): uniformly feeding the levigated water-quenched slag into the tank body 1 through a feeder, and adding water into the tank body 1, wherein the mass ratio of the levigated water-quenched slag to the water is 1: (4-6).
Step (three): introducing the sulfur dioxide-containing high-temperature smelting industrial waste gas into the tank body 1 through a plurality of flue gas addition ports 8, wherein the mass ratio of the introduction flow of the sulfur dioxide-containing high-temperature smelting industrial waste gas to the water quenching slag is (2-3): 1, the concentration of sulfur dioxide in the smelting industrial waste gas containing sulfur dioxide is 8-10%, the temperature of the smelting industrial waste gas containing sulfur dioxide is 120-220 ℃, and the temperature of the solution is ensured to be 40-90 ℃; starting the stirring paddle 3, wherein the rotating speed of the stirring paddle 3 is 3r/min-10r/min, and under the stirring of the stirring paddle, nickel, copper and cobalt in the water-quenched slag enter a solution in the form of sulfate ions to obtain a leaching product containing nickel, copper and cobalt and leached residues; the leached product containing nickel, copper and cobalt overflows through an overflow port 5, after the leached product is evaporated and crystallized, the leached product contains 4.0 to 8.0 percent of nickel, 2.0 to 5.0 percent of copper and 1.0 to 3.0 percent of cobalt, and is sent to a smelting system (a fire method or a wet method) to be treated and recycled with valuable metals of nickel, copper and cobalt; the leached residue is conveyed to a tailing discharge port 6 by a screw to be discharged, and is leached tailings. And the waste gas at the overflow part of the liquid level of the leaching tank is pumped out through a waste gas absorption port and enters an industrial tail gas absorption system for treatment.
The principle of the recovery method of the invention: grinding the water quenched slag evenly and feeding the water quenched slag into a device, adding water to form ore pulp, introducing high-temperature industrial waste gas containing sulfur dioxide into the ore pulp, wherein SO in the waste gas2Reacting with water and oxygen in the ore pulp to produce sulfuric acid, reacting sulfide or oxide containing nickel, copper and cobalt in the water-quenched slag with the sulfuric acid, and recovering the nickel, copper and cobalt in the form of sulfate entering the solution.
The main chemical reaction equation is:
2H2O+2SO2+O2→2H2SO4
2Ni3S2+2H2SO4+9O2→6NiSO4+2H2O
2Cu2S+2H2SO4+5O2→4CuSO4+2H2O
CoS+H2SO4+O2→CoSO4+H2O
NiO+H2SO4→NiSO4+H2O
CuO+H2SO4→CuSO4+H2O
CoO+H2SO4→CoSO4+H2O
example 1
Finely grinding the nickel smelting water-quenched slag, wherein the content of the finely ground water-quenched slag with the granularity of less than 3mm is 82 percent; the nickel smelting water-quenched slag comprises the following components in percentage by mass: 0.16% of Ni, 0.22% of Cu and 0.086% of Co.
Uniformly feeding the ground water-quenched slag into the tank body through a feeder, wherein the feeding amount is 4.0t/h, and adding water into the tank body to control the liquid-solid ratio to be 4: 1.
To the groove body at a distance of 9.6m3Introducing 8-10% sulfur dioxide smelting industrial waste gas at a flow rate of/h, and carrying out acid leaching reaction to obtain a leaching product containing nickel, copper and cobalt and leached residues; after evaporation and crystallization of the leached product, 4.16% of nickel, 4.14% of copper and 1.21% of cobalt are contained, the recovery rate of nickel is 37.2%, the recovery rate of copper is 26.7% and the recovery rate of cobalt is 19.3%. The product is sent to a pyrometallurgical system for further recovering valuable metals of nickel, copper and cobalt.
Example 2
Finely grinding the nickel smelting water-quenched slag, wherein the content of the finely ground water-quenched slag with the granularity less than 3mm is 83%; the nickel smelting water-quenched slag comprises the following components in percentage by mass: 0.31% of Ni, 0.24% of Cu and 0.20% of Co.
Uniformly feeding the ground water-quenched slag into the tank body through a feeder, wherein the feeding amount is 6.0t/h, and adding water into the tank body to control the liquid-solid ratio to be 4: 1.
To the groove body at a distance of 14.22m3Introducing 8-10% sulfur dioxide smelting industrial waste gas at a flow rate of/h, and carrying out acid leaching reaction to obtain a leaching product containing nickel, copper and cobalt and leached residues; after evaporation and crystallization of the leached product, 5.13% of nickel, 3.34% of copper and 1.94% of cobalt are contained, the recovery rate of nickel is 41.4%, the recovery rate of copper is 34.6% and the recovery rate of cobalt is 24.2%. The product is sent to a pyrometallurgical system for further recovering valuable metals of nickel, copper and cobalt.
Example 3
Finely grinding the nickel smelting water-quenched slag, wherein the content of the grinded water-quenched slag with the granularity less than 3mm is 84%; the nickel smelting water-quenched slag comprises the following components in percentage by mass: 0.43% of Ni, 0.25% of Cu and 0.22% of Co.
Uniformly feeding the ground water-quenched slag into the tank body through a feeder, wherein the feeding amount is 6.5t/h, and adding water into the tank body to control the liquid-solid ratio to be 4: 1.
To the groove body at a distance of 14.4m3Introducing 8-10% sulfur dioxide smelting industrial waste gas at a flow rate of/h, and carrying out acid leaching reaction to obtain a leaching product containing nickel, copper and cobalt and leached residues; after the leached product is evaporated and crystallized, 6.48 percent of nickel, 3.17 percent of copper and 2.30 percent of cobalt are contained, the recovery rate of nickel is 43.3 percent, the recovery rate of copper is 35.4 percent and the recovery rate of cobalt is 28.8 percent. The product is sent to a pyrometallurgical system for further recovering valuable metals of nickel, copper and cobalt.
Example 4
Finely grinding the nickel smelting water-quenched slag, wherein the content of the finely ground water-quenched slag with the granularity less than 3mm is 87%; the nickel smelting water-quenched slag comprises the following components in percentage by mass: 0.60% of Ni, 0.30% of Cu and 0.28% of Co.
Uniformly feeding the ground water-quenched slag into the tank body through a feeder, wherein the feeding amount is 7.0t/h, and adding water into the tank body to control the liquid-solid ratio to be 4: 1.
To the groove body at 16.59m3Flow introduction in/hCarrying out acid leaching reaction on smelting industrial waste gas with 8-10% of sulfur dioxide concentration to obtain a leaching product containing nickel, copper and cobalt and leached residues; after evaporation and crystallization of the leached product, the recovery rate of nickel is 7.68 percent, copper is 2.90 percent, cobalt is 2.16 percent, the recovery rate of nickel is 51.3 percent, the recovery rate of copper is 41.4 percent, and the recovery rate of cobalt is 30.8 percent. The product is sent to a pyrometallurgical system for further recovering valuable metals of nickel, copper and cobalt.

Claims (6)

1. The device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag is characterized by comprising a tank body (1), a transmission mechanism (2), a stirring paddle (3) and a lifting mechanism (4), wherein the stirring paddle (3) is arranged inside the tank body (1), and the transmission mechanism (2) is connected with the stirring paddle (3); an overflow port (5) is processed at one end of the tank body (1), and a tailing discharge port (6) is processed at the other end of the tank body (1); the lifting mechanism (4) is arranged at one end of the tank body (1) which is provided with the overflow port (5); the tank body (1) is provided with a feed inlet (7), a plurality of flue gas inlet openings (8) and a waste gas absorption opening (9).
2. The device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag according to claim 1, wherein the trough body (1) is obliquely arranged, and one end of the trough body (1) provided with a tailing discharge opening (6) is higher than one end of the trough body (1) provided with an overflow opening (5); the included angle between the bottom surface of the tank body (1) and the horizontal plane is 14-18 degrees.
3. The device for recovering nickel, copper and cobalt from nickel smelting water-quenched slag according to claim 1, wherein the stirring paddle (3) is a spiral stirring paddle; the lifting mechanism (4) is a spiral lifting mechanism; an exhaust gas absorption cover is arranged above the exhaust gas absorption opening (9).
4. A method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag based on any one of claims 1 to 3, which comprises the following steps:
step (I): finely grinding the nickel smelting water-quenched slag to obtain finely ground water-quenched slag;
step (II): adding the levigated water quenching slag and water into a tank body; the mass ratio of the water-quenched slag after grinding to water is 1: (4-6);
step (three): introducing smelting industrial waste gas containing sulfur dioxide into the tank body through a plurality of flue gas inlets, and starting a stirring paddle to obtain a leaching product containing nickel, copper and cobalt and leached residues; leaching products containing nickel, copper and cobalt overflow through the overflow port, and residues after leaching are discharged through a tailing discharge port; the mass ratio of the flow of the smelting industrial waste gas containing sulfur dioxide to the water quenching slag is (2-3): 1, the concentration of sulfur dioxide in the smelting industrial waste gas containing sulfur dioxide is 8-10%, and the temperature of the smelting industrial waste gas containing sulfur dioxide is 120-220 ℃.
5. The method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag according to claim 4, wherein the content of the water-quenched slag with the granularity of less than 3mm after being ground in the step (one) is more than or equal to 80%.
6. The method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag according to claim 4, wherein the rotation speed of the stirring paddle in the step (III) is 3r/min to 10 r/min.
CN202110619184.XA 2021-06-03 2021-06-03 Device and method for recovering nickel, copper and cobalt from nickel smelting water-quenched slag Withdrawn CN113462894A (en)

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CN109182743A (en) * 2018-10-30 2019-01-11 河钢股份有限公司承德分公司 A kind of hydrometallurgy Leach reaction device and leach the method containing vanadium raw materials
CN109825699A (en) * 2019-01-21 2019-05-31 成都虹波钼业有限责任公司 It is a kind of to contain SO using calcining molybdenum ore concentrate2The method of tail gas leaching nickel cobalt raw material
CN111575491A (en) * 2020-06-29 2020-08-25 株洲冶炼集团科技开发有限责任公司 Resource comprehensive utilization method for purifying cobalt-nickel slag by zinc hydrometallurgy arsenic salt
CN112143900A (en) * 2020-10-10 2020-12-29 何耀 Red mud leaching slag washing tank and use method thereof
CN112725624A (en) * 2020-12-07 2021-04-30 中南大学 Method for efficiently recycling arsenic-cobalt-nickel-containing slag

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Application publication date: 20211001