CN114015896B - Method for extracting metallic nickel from nickel-iron alloy - Google Patents
Method for extracting metallic nickel from nickel-iron alloy Download PDFInfo
- Publication number
- CN114015896B CN114015896B CN202111215607.8A CN202111215607A CN114015896B CN 114015896 B CN114015896 B CN 114015896B CN 202111215607 A CN202111215607 A CN 202111215607A CN 114015896 B CN114015896 B CN 114015896B
- Authority
- CN
- China
- Prior art keywords
- nickel
- ferronickel
- iron alloy
- water leaching
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/06—Sulfating roasting
-
- 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
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for extracting metallic nickel from nickel-iron alloy: mixing nickel-iron alloy powder with Na 2 SO 4 Uniformly mixing, placing the mixture into a heating furnace, introducing sulfur dioxide and oxygen to maintain the sulfating atmosphere in the heating furnace, and preserving the temperature for 0.5-4 h at 600-800 ℃; soaking the roasting product in water to obtain water leaching slag and water leaching liquid; and adding a nickel precipitating agent into the water leaching solution for reaction, and filtering to obtain a nickel-containing solid product and filtrate. The invention adds Na into the ferronickel powder 2 SO 4 After that, na 2 SO 4 Will be associated with NiSO formed during sulfation 4 Forming a binary eutectic phase, thereby preventing dense NiSO 4 The formation of the layer promotes the continuous occurrence of the sulfation reaction, and effectively improves the nickel conversion rate of the large-granularity ferronickel particles; in addition, na 2 SO 4 Can also destroy the NiFe which is an adverse product generated in the sulfation roasting process 2 O 4 (nickel ferrite) to promote the sulfation reaction to proceed smoothly.
Description
Technical Field
The invention belongs to the field of nonferrous metallurgy, and particularly relates to a method for extracting metallic nickel from nickel-iron alloy.
Background
Nickel is a silvery white metal with good ductility, magnetism and corrosion resistance, and is known as a "vitamin in the iron and steel industry". Nickel is an important strategic metal that is widely used in the fields of stainless steel, batteries, electroplating, alloys, and the like. At present, nickel resources are mainly obtained from nickel sulfide ores and nickel oxide ores (namely laterite nickel ores) in crust resources, wherein the laterite nickel ores account for about 72 percent. The laterite nickel ore in China is imported from Indonesia and Philippines, and the external dependency is over 80%.
At present, the pyrometallurgy process of laterite-nickel ore mainly comprises a dry pre-reduction-electric furnace smelting method, a direct reduction magnetic separation method, a sintering-blast furnace method and the like, and different grades of ferronickel are produced.
In the patent document with the publication number of CN112941314A, ferric hydroxide is obtained by acid-dissolving nickel-iron alloy, replacing sponge nickel, removing iron by oxidation and washing slag; and (3) acid-dissolving sponge nickel, removing impurities, and evaporating and crystallizing to obtain the battery grade nickel sulfate. The method has the advantages of low energy consumption, low cost and simple process, and can realize the efficient recycling of the ferronickel, but has the problems of high acid consumption, long flow, need of adding iron powder additionally and the like.
In the patent document with the publication number of CN113044821A, after the ferronickel alloy is dissolved by using acid liquor, ferric phosphate is prepared by adding an oxidant into a phosphorus source or a phosphorus source and the action of a precipitation auxiliary agent, further the ferric phosphate can be used as a precursor of lithium iron phosphate to prepare a lithium iron phosphate anode material, and after impurity removal, a nickel-containing solution with lower impurity content can be obtained from the solution after precipitation. The method has the advantages of simple operation, short process flow, low equipment requirement, suitability for industrial production and application, but large acid consumption, more generated wastewater and overlong reaction time.
In the patent document with publication number CN112626356A, nickel-iron alloy and magnesium metal with proper granularity are heated to 750-880 ℃ in inert atmosphere and are kept for 2-5 hours; continuously raising the temperature to 900-1200 ℃, vacuumizing to realize vacuum distillation of the magnesium melt in a boiling state, and preserving the heat for 5-10 hours; after the distillation is finished, the materials are cooled to room temperature and winnowing is carried out, thus obtaining the separated flaky metallic nickel and porous metallic iron alloy. The method has high safety and operability and short process flow, and can realize the high-efficiency separation of nickel and iron in the nickel-iron alloy; but has the problems of long time consumption, high requirement on vacuum equipment and the like.
In the patent document with the publication number of CN112941313A, crude nickel-iron alloy is subjected to crushing grinding, pressurized ammonia leaching, filtering and evaporative crystallization, a sulfuric acid system is adopted in the pressurized ammonia leaching, and high-value class I nickel sulfate hexahydrate and high-grade saleable fine iron powder can be directly obtained after ammonia leaching and ammonia evaporation. The technical condition of the method is easy to control, and no waste water and waste residue are generated; but has higher requirements on the compression resistance and corrosion resistance of equipment.
In the patent document with publication number CN113265532A, the crude ferronickel alloy is subjected to oxidizing roasting and spray granulation, and then the ferronickel oxide powder is subjected to spray granulation; alkali dissolution and ammonia leaching of the nickel iron oxide powder to obtain iron slag and leaching liquid; extracting the leaching solution, and taking the raffinate to remove oil to obtain the nickel ammonia solution. The method reduces the energy consumption of high-pressure leaching, and simultaneously the obtained nickel-ammonia solution is directly used for synthesizing ternary precursors, so that the ammonium source which needs to be introduced in the synthesis process is reduced; but the energy consumption is still higher and the flow is longer.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects in the prior art, and provides a method for extracting metal nickel from ferronickel, which has the advantages of simple process, low energy consumption and low equipment requirement.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for extracting metallic nickel from nickel-iron alloy, comprising the following steps:
(1) Mixing nickel-iron alloy powder with Na 2 SO 4 Uniformly mixing, placing the mixture into a heating furnace, introducing sulfur dioxide and oxygen to maintain the sulfating atmosphere in the heating furnace, and preserving the temperature for 0.5-4 h at 600-800 ℃;
(2) Soaking the roasting product obtained in the step (1) in water to obtain water leaching slag and water leaching liquid; the main component of the water leaching slag is Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 ；
(3) Adding a nickel precipitating agent into the water leaching solution for reaction, and filtering to obtain a nickel-containing solid product and filtrate, wherein the nickel-containing solid product is Ni (OH) 2 Or NiCO 3 The filtrate is Na 2 SO 4 A solution.
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, in step (1), the Na 2 SO 4 The addition amount is 20-100% of the weight of the ferronickel powder. Na (Na) 2 SO 4 The addition amount is less than the range, na 2 SO 4 The effect on improving the nickel conversion rate is not obvious.
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, in the step (1), the volume ratio of sulfur dioxide to oxygen is 0.5:1-2:1. Only if the sulfur potential and the oxygen potential in a specific range are ensured, the sulfation reaction can be efficiently carried out; if the amounts are outside this range, the sulfation reaction proceeds slowly. The source of sulfur dioxide may be pure sulfur dioxideGas or tail gas of smeltery containing sulfur dioxide (SO in tail gas) 2 About 10% in concentration), the source of oxygen can be industrial oxygen or air, and the total amount of mixed gas is introduced in the whole sulfating process to ensure that enough sulfur dioxide and oxygen are provided to completely convert the raw material ferronickel alloy into target product (NiSO) 4 And Fe (Fe) 2 O 3 )。
In the method for extracting the metallic nickel from the nickel-iron alloy, preferably, in the step (2), the solid-liquid mass ratio in the water leaching process is 1:5-1:20, the water leaching temperature is 30-80 ℃, and the water leaching time is 0.5-2 h.
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, in the step (3), the nickel precipitating agent is NaOH or Na 2 CO 3 。
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, in the step (3), the final pH value of the reaction is 7 to 9.
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, the filtrate in step (3) is evaporated and crystallized or frozen and crystallized to obtain Na 2 SO 4 。
The above method for extracting metallic nickel from nickel-iron alloy, preferably, the Na 2 SO 4 Returning to the step (1) to be mixed with the ferronickel powder as an additive.
In the above method for extracting metallic nickel from nickel-iron alloy, preferably, in the step (1), the particle size of the nickel-iron alloy powder is not more than 0.5mm.
In the method for extracting the metallic nickel from the ferronickel alloy, preferably, in the step (2), the water leaching slag is returned to the step (1) for sulfatizing roasting again, so that a higher nickel leaching rate is ensured.
The invention mainly generates the following chemical reactions in the sulfating roasting process:
Fe(s)+O 2 (g)→Fe 2 O 3 (s)；
Ni(s)+O 2 (g)→NiO(s)；
SO 2 (g)+O 2 (g)→SO 3 (g)；
NiO(s)+SO 3 (g)→NiSO 4 (s)。
the invention innovatively introduces Na in the sulfating roasting process 2 SO 4 ，Na 2 SO 4 Will be associated with NiSO formed during sulfation 4 Forming a binary eutectic phase, thereby preventing dense NiSO 4 Layer formation promotes continuous sulfation reaction, effectively improves nickel conversion rate in large-particle-size nickel-iron alloy particles, and in addition, na 2 SO 4 Can also destroy the NiFe which is an adverse product generated in the sulfation roasting process 2 O 4 (nickel ferrite) promotes the sulfation reaction to proceed smoothly, and the reaction equation is as follows:
NiFe 2 O 4 +Na 2 SO 4 ＝Na 2 Fe 2 O 4 +NiSO 4 。
the invention combines nickel-iron alloy powder with proper granularity with Na 2 SO 4 After mixing evenly, sulfating roasting is carried out, and SO in the mixed gas is reasonably controlled 2 With O 2 The proportion ensures that nickel element in the ferronickel alloy selectively generates water-soluble sulfate and iron element selectively generates oxide. Due to NiSO 4 And Na (Na) 2 SO 4 Is easy to dissolve in water, fe 2 O 3 Insoluble in water, and can be used for preparing NiSO by water leaching and filtering 4 、Na 2 SO 4 Solution and Fe 2 O 3 Separating and then in NiSO 4 、Na 2 SO 4 Adding NaOH or Na into the solution 2 CO 3 Depositing nickel and filtering to obtain Ni (OH) product 2 Or NiCO 3 And Na (methyl acetate) 2 SO 4 A solution; na (Na) 2 SO 4 The solution is evaporated and crystallized or frozen and crystallized to obtain Na 2 SO 4 ，Na 2 SO 4 Returning to the previous step as an additive for the sulfatizing roasting process.
Compared with the prior art, the invention has the advantages that:
(1) The invention adds Na into the ferronickel powder 2 SO 4 After that, na 2 SO 4 Will be associated with NiSO formed during sulfation 4 Forming a binary eutectic phase, thereby preventing densificationNiSO 4 The formation of the layer promotes the continuous occurrence of the sulfation reaction, and effectively improves the nickel conversion rate of the large-granularity ferronickel particles; in addition, na 2 SO 4 Can also destroy the NiFe which is an adverse product generated in the sulfation roasting process 2 O 4 (nickel ferrite) to promote the sulfation reaction to proceed smoothly.
(2) The invention uses nickel-iron alloy powder and Na 2 SO 4 After mixing evenly, sulfating roasting is carried out, and SO in the mixed gas is reasonably controlled 2 With O 2 The ratio of the nickel to the iron is such that the nickel element in the nickel-iron alloy selectively generates water-soluble sulfate and the iron element selectively generates oxide to separate metallic nickel from the nickel-iron alloy.
(3) The mixed gas in the sulfating roasting process can contain SO in a smelting plant 2 Exhaust gas as SO in mixed gas 2 Solves the air pollution problem of related smeltery, changes waste into valuable and changes SO-containing materials 2 The waste gas is utilized in a high-value way, so that the cost for extracting nickel from the nickel-iron alloy can be effectively reduced; o (O) 2 Can be replaced by air, and the cost can be further reduced.
(4) In the process of the invention, byproduct Na is present 2 SO 4 Can be used as an additive for sulfating roasting of nickel-iron alloy to obviously improve the nickel extraction rate and redundant Na 2 SO 4 Can be sold. Compared with the prior art, the invention has the advantages of renewable additive, high nickel extraction rate and the like.
(5) The water leaching slag produced after water leaching is Fe 2 O 3 Can be used as ideal iron-making raw material.
In conclusion, the method has the advantages of short process flow, low energy consumption, low cost, easily-controlled technical conditions and high nickel extraction rate, and can realize the efficient separation of nickel and iron in the nickel-iron alloy, thereby meeting the strong requirements of new energy battery markets in the future on nickel. The process has no waste water, waste gas and solid waste, and has the advantages of environmental protection, environmental protection and the like.
Drawings
FIG. 1 is a flow chart of the process of the invention for extracting metallic nickel from nickel-iron alloy.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings and preferred embodiments in order to facilitate an understanding of the invention, but the scope of the invention is not limited to the following specific embodiments.
Unless defined otherwise, all technical and scientific terms 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 be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of the nickel-iron alloy powder obtained in the step (1) is mixed with 10g of Na 2 SO 4 Mixing, placing in a heating furnace, and continuously introducing pure SO 2 The flow rates of the gas and the industrial oxygen are respectively 200ml/min and 400ml/min, the sulfating atmosphere is maintained, the temperature is heated to 700 ℃, the temperature is kept for 1h, and the sample is taken out after being naturally cooled to 50 ℃ in a furnace.
(3) Leaching the roasting product obtained in the step (2) with water at a solid-liquid mass ratio of 1:5, a leaching temperature of 50 ℃ and a leaching time of 0.5h, filtering to obtain leaching residues and leaching liquid, wherein the leaching residues mainly comprise Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 。
(4) Is immersed in waterAdding NaOH solution into the solution to precipitate nickel, wherein the pH value of the reaction end point is 8, and filtering to obtain a solid product Ni (OH) after the nickel precipitation is finished 2 And Na (Na) 2 SO 4 Solution, na 2 SO 4 The solution is evaporated and crystallized to obtain Na 2 SO 4 Can return to the step (2) for reuse.
Analysis and detection are carried out on the sample obtained in the embodiment, and the detection result shows that the leaching rate of Ni element is 93%, and the Fe content of the water leaching slag is 62.6%.
Example 2:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of the ferronickel powder obtained in step (1) and 4g of Na 2 SO 4 Mixing, placing into a heating furnace, and introducing simulated smelting plant SO-containing material 2 Tail gas of (SO in tail gas) 2 10% in concentration) and air at flow rates of 1500ml/min and 1000ml/min, respectively, maintaining sulfating atmosphere, heating to 600deg.C, maintaining the temperature for 2 hr, and taking out after naturally cooling the sample in the furnace to 50deg.C.
(3) Soaking the roasted product obtained in the step (2) in water at a solid-liquid mass ratio of 1:5, a soaking temperature of 30 ℃ and a soaking time of 1h, filtering to obtain water leaching slag and water leaching liquid, wherein the water leaching slag mainly comprises Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 。
(4) Adding Na into the water extract 2 CO 3 The pH of the reaction end point is 9, and the solid product NiCO is obtained after filtration 3 And Na (Na) 2 SO 4 Solution, na 2 SO 4 Evaporating and crystallizing the solution to obtain Na 2 SO 4 . And analyzing and detecting the sample, wherein the detection result shows that the Ni leaching rate is 81.1%, and the Fe content of the water leaching slag is 59.3%.
Example 3:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of the ferronickel powder obtained in step (1) was mixed with 20g of Na 2 SO 4 Mixing, placing in a heating furnace, introducing pure SO 2 The flow rates of the gas and the air are respectively 200ml/min and 1000ml/min, the sulfating atmosphere is maintained, and the mixture is heated to 600 ℃ and kept for 4 hours; and taking out the sample after the sample is naturally cooled to 50 ℃ in the furnace.
(3) Soaking the roasting product obtained in the step (2) in water at a solid-liquid mass ratio of 1:10, a soaking temperature of 30 ℃ and a soaking time of 1h, filtering to obtain water leaching slag and water leaching liquid, wherein the water leaching slag mainly comprises Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 。
(4) Adding Na into the water extract 2 CO 3 Ending the reaction when the pH of the reaction end point is 8, and filtering to obtain a solid product NiCO 3 And Na (Na) 2 SO 4 A solution. Na (Na) 2 SO 4 The solution is frozen and crystallized to obtain Na 2 SO 4 . And analyzing and detecting the sample, wherein the detection result shows that the Ni leaching rate is 85.4%, and the water leaching slag contains 60.3% of Fe.
Example 4:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of ferronickel powder and 20g of Na 2 SO 4 Mixing, placing in a heating furnace, introducing pure SO 2 The flow rates of the gas and the air are respectively 500ml/min and 5000ml/min, the sulfating atmosphere is maintained, and the temperature is heated to 800 ℃ for protectionAnd (3) heating for 0.5h, and taking out after the sample is naturally cooled to 50 ℃ in a furnace.
(3) Soaking the roasted product in the step (2) for 1h at a solid-liquid mass ratio of 1:10 and a soaking temperature of 80 ℃ to obtain water leaching slag and water leaching liquid, wherein the main component of the water leaching slag is Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 。
(4) Adding Na into the water extract 2 CO 3 Precipitating nickel, wherein the pH value of the reaction end point is 8, and filtering to obtain a solid product NiCO 3 And Na (Na) 2 SO 4 Solution, na 2 SO 4 The solution is frozen and crystallized to obtain Na 2 SO 4 . Analysis and detection were carried out on the sample obtained in this example, and the detection result showed that the Ni leaching rate was 84.9% and that the water leaching residue contained Fe 60.0%.
Example 5:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of ferronickel powder and 6g of Na 2 SO 4 Mixing, placing in a heating furnace, introducing pure SO 2 The flow rates of the gas and the air are 500ml/min and 2500ml/min respectively, the sulfating atmosphere is maintained, the temperature is heated to 800 ℃, the temperature is kept for 1h, and the sample is taken out after being naturally cooled to 50 ℃ in a furnace.
(3) Soaking the roasting product obtained in the step (2) in water at a solid-liquid mass ratio of 1:20, a soaking temperature of 80 ℃ and a soaking time of 1h, filtering to obtain water leaching slag and water leaching liquid, wherein the water leaching slag mainly comprises Fe 2 O 3 Can be used as ideal iron-making raw material; the main component of the water immersion liquid is NiSO 4 With Na and Na 2 SO 4 。
(4) Adding Na into the water extract 2 CO 3 Controlling the pH value of the reaction end point to be 9, and filtering to obtain a solid product NiCO 3 And Na (Na) 2 SO 4 A solution; na (Na) 2 SO 4 The solution is frozen and crystallized to obtain Na 2 SO 4 . And analyzing and detecting the sample, wherein the detection result shows that the Ni leaching rate is 82.6%, and the leaching slag contains 59.7% of Fe.
Example 6:
the invention relates to a method for extracting nickel from nickel-iron alloy, which is shown in figure 1 and comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) 20g of ferronickel powder and 20g of Na 2 SO 4 Mixing, placing in a heating furnace, introducing pure SO 2 The flow rates of the gas and the air are respectively 500ml/min and 5000ml/min, the sulfating atmosphere is maintained, and the temperature is heated to 700 ℃ and kept for 1h; and taking out the sample after the sample is naturally cooled to 50 ℃ in the furnace.
(3) Soaking the roasted product in the step (2) for 0.5h at a solid-liquid mass ratio of 1:20 and a soaking temperature of 80 ℃ to obtain water leaching slag and water leaching liquid, wherein the main components of the water leaching slag are Fe 2 O 3 Can be used as ideal ironmaking raw material, and the main component of the water extract is NiSO 4 With Na and Na 2 SO 4 。
(4) Adding NaOH into the water leaching solution, wherein the pH value of the reaction end point is 9, and filtering to obtain a solid product Ni (OH) 2 And Na (Na) 2 SO 4 Solution, na 2 SO 4 The solution is frozen and crystallized to obtain Na 2 SO 4 。
Analysis and detection were carried out on the sample obtained in this example, and the detection result showed that the Ni leaching rate was 97.5% and the water leaching residue contained Fe63.6%.
Comparative example 1:
the method for extracting nickel from the nickel-iron alloy of the comparative example comprises the following steps:
(1) Crushing and sieving ferronickel (34 wt% of Ni, 55.8wt% of Fe, a small amount of Cu, si and other impurity elements) to obtain ferronickel powder with granularity of 0.1-0.5 mm.
(2) Placing 20g of ferronickel powder into a heating furnace, and introducing pure SO 2 The flow rates of the gas and the air are respectively 500ml/min and 5000ml/min, the sulfating atmosphere is maintained, and the temperature is heated to 700 ℃ and kept for 1h; and taking out the sample after the sample is naturally cooled to 50 ℃ in the furnace.
(3) And (3) leaching the roasted product in the step (2) at a solid-liquid mass ratio of 1:20, a leaching temperature of 80 ℃ and a leaching time of 0.5h, and filtering to obtain leaching residues and leaching liquid.
(4) Adding NaOH into the water leaching solution, ending the reaction when the pH value of the reaction end point is controlled to be 9, and filtering to obtain a solid product Ni (OH) 2 And a filtrate.
Analysis and detection are carried out on the obtained sample, and the detection result shows that the conversion rate of Ni element is only 16.8%, and the content of Fe element in the water leaching slag is 47.5%.
As can be seen from a comparison of the test results of example 6 and comparative example, na is added to the nickel-iron alloy powder according to the present invention 2 SO 4 The continuous occurrence of the sulfation reaction can be promoted, and the nickel conversion rate of the nickel-iron alloy particles can be effectively improved.
Claims (8)
1. A method for extracting metallic nickel from nickel-iron alloy, comprising the steps of:
(1) Mixing nickel-iron alloy powder with Na 2 SO 4 Uniformly mixing, placing the mixture into a heating furnace, introducing sulfur dioxide and oxygen to maintain the sulfating atmosphere in the heating furnace, and preserving the temperature for 0.5-4 h at 600-800 ℃; wherein the volume ratio of sulfur dioxide to oxygen is 0.5:1-2:1; the Na is 2 SO 4 The addition amount is 20-100% of the mass of the ferronickel powder;
(2) Soaking the roasting product obtained in the step (1) in water to obtain water leaching slag and water leaching liquid;
(3) And adding a nickel precipitating agent into the water leaching solution for reaction, and filtering to obtain a nickel-containing solid product and filtrate.
2. The method for extracting metallic nickel from ferronickel alloy according to claim 1, wherein in the step (2), the solid-liquid mass ratio in the water leaching process is 1:5-1:20, the water leaching temperature is 30-80 ℃, and the water leaching time is 0.5-2 h.
3. The method for extracting metallic nickel from ferronickel alloy according to claim 1, wherein in the step (3), the nickel precipitating agent is NaOH or Na 2 CO 3 。
4. The method for extracting metallic nickel from nickel-iron alloy according to claim 1, wherein in step (3), the reaction endpoint pH is 7-9.
5. The method for extracting metallic nickel from nickel-iron alloy according to any of claims 1-4, wherein the filtrate obtained in step (3) is evaporated and crystallized or frozen to obtain Na 2 SO 4 。
6. The method for extracting metallic nickel from nickel-iron alloy according to claim 5, wherein the Na 2 SO 4 Returning to the step (1) to be mixed with the ferronickel powder as an additive.
7. The method for extracting metallic nickel from ferronickel alloy according to any of claims 1-4, wherein in step (1), the particle size of the ferronickel alloy powder is not more than 0.5mm.
8. The method for extracting metallic nickel from ferronickel alloy as claimed in any one of claims 1-4, wherein in step (2), the water leaching residue is returned to step (1) for re-sulfatizing roasting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111215607.8A CN114015896B (en) | 2021-10-19 | 2021-10-19 | Method for extracting metallic nickel from nickel-iron alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111215607.8A CN114015896B (en) | 2021-10-19 | 2021-10-19 | Method for extracting metallic nickel from nickel-iron alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114015896A CN114015896A (en) | 2022-02-08 |
| CN114015896B true CN114015896B (en) | 2023-06-27 |
Family
ID=80056529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111215607.8A Active CN114015896B (en) | 2021-10-19 | 2021-10-19 | Method for extracting metallic nickel from nickel-iron alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114015896B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1098713A (en) * | 1976-02-13 | 1981-04-07 | Theodore C. Frankiewicz | Selective sulfation process for partitioning ferrous and non-ferrous values in an ore |
| CN102268537B (en) * | 2011-08-15 | 2013-05-29 | 广西银亿科技矿冶有限公司 | Method for extracting cobalt and nickel from laterite-nickel ore |
| CN104294034A (en) * | 2013-07-19 | 2015-01-21 | 无锡永发电镀有限公司 | Chloridizing segregation-magnetic separation process for low-grade laterite nickel ore |
| CN206828599U (en) * | 2017-04-27 | 2018-01-02 | 江苏省冶金设计院有限公司 | The system for handling lateritic nickel ore |
-
2021
- 2021-10-19 CN CN202111215607.8A patent/CN114015896B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114015896A (en) | 2022-02-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11459636B2 (en) | Method and system for comprehensive recovery and utilization of copper-nickel sulfide ore | |
| EP3100804B1 (en) | Manufacturing method for nickel powder | |
| CA2856341C (en) | Method for producing high-purity nickel sulfate | |
| CN109110826B (en) | Production method of battery-grade nickel sulfate | |
| KR20090042996A (en) | Production of metallic nickel with low iron content | |
| CN109536732B (en) | Method for preparing ternary precursor material by recycling copper sulfide slag | |
| CN113215398B (en) | Oxygen pressure leaching method of nickel sulfide concentrate | |
| CN109666800A (en) | One kind removing cobalt agent and its application | |
| CN102041388A (en) | Method for recycling metal from waste catalyst containing molybdenum and nickel | |
| CN113621819B (en) | Method for extracting valuable metals from low-grade nickel matte converter slag | |
| CN113265532B (en) | Method for leaching nickel-ammonia solution from nickel-iron alloy by wet method and application | |
| US20240018013A1 (en) | Method for preparing nickel sulfate from ferronickel | |
| CN111647742B (en) | Method for extracting nickel, cobalt and manganese from nickel-cobalt-manganese multi-metal oxide ore by wet process step by step | |
| US11535910B2 (en) | Method for preparing a leach feed matertial | |
| ES2957117A2 (en) | Method for preparing nickel sulfate from nickel-iron-copper alloy | |
| CN111286600A (en) | Method for efficiently recovering zinc and iron from zinc ferrite-containing material | |
| CN114015896B (en) | Method for extracting metallic nickel from nickel-iron alloy | |
| CN111424172A (en) | Wet treatment process of laterite-nickel ore | |
| EP3421626A1 (en) | Method for producing nickel powder | |
| CN110878390A (en) | Method for recovering tungsten from waste hard alloy | |
| CN114614136A (en) | Method for preparing ferric phosphate dihydrate and ternary cathode material from laterite-nickel ore | |
| CN113789441B (en) | Combined leaching process of cobalt-sulfur concentrate and cobalt hydroxide ore | |
| CN117684003A (en) | Method for smelting cobalt nickel hydroxide intermediate product at low cost | |
| CN117613438A (en) | Method for recycling waste ternary lithium ion battery | |
| CN114959252A (en) | Method for producing nickel sulfate by using high-nickel matte |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |