CN113403486B - Iron removal process of nickel sulfide concentrate leaching solution by goethite method - Google Patents
Iron removal process of nickel sulfide concentrate leaching solution by goethite method Download PDFInfo
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- CN113403486B CN113403486B CN202110681018.2A CN202110681018A CN113403486B CN 113403486 B CN113403486 B CN 113403486B CN 202110681018 A CN202110681018 A CN 202110681018A CN 113403486 B CN113403486 B CN 113403486B
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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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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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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- 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 provides a process for removing iron from nickel sulfide concentrate leaching liquid by a goethite method, wherein the nickel sulfide concentrate leaching liquid contains iron ions, copper ions, nickel ions and cobalt ions, and the process comprises the following steps: adding reduced iron powder into the nickel sulfide concentrate leaching solution to reduce and replace copper ions in the leaching solution, and reducing iron ions in the leaching solution into ferrous ions; oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate; and carrying out solid-liquid separation on the leaching solution after the reaction is completed so as to remove sediment in the leaching solution. The process can efficiently remove iron ions in the nickel sulfide concentrate leaching liquid, solves the problem of influence of iron ions with higher concentration on the nickel recovery process flow and energy consumption, and in addition, iron slag and sponge copper obtained after the reaction can be directly sold, thereby being beneficial to improving the utilization value of raw materials.
Description
Technical Field
The invention belongs to the technical field of nickel sulfide concentrate treatment, and particularly relates to a process for removing iron by a goethite method from a nickel sulfide concentrate leaching solution.
Background
Nickel is an important strategic metal resource, and is widely applied to the fields of aerospace, military and civil industry because of its good extensibility, mechanical properties and chemical stability. In recent years, with the rapid development of the high-nickel ternary lithium battery industry, the market demand of nickel is rapidly increasing. Among nickel mineral resources, the multi-metal nickel sulfide concentrate is one of the most important nickel mineral resources, and has very important position in China and even world nickel resources. Currently, the nickel sulfide concentrate resources in the globally ascertained nickel ore resources account for about 40%. In recent years, ultra-large magma copper-nickel sulfide ore deposits are found in the Hamu region in summer of Qinghai province in China, the amount of 332+333 grade nickel metal is determined to be 106 ten thousand tons (average grade is 0.7%), the amount of 333 grade copper resources is accompanied by 21.77 ten thousand tons (average grade is 0.166%), and the amount of cobalt resources is 3.81 ten thousand tons (average grade is 0.025%), so that the ultra-large magma copper-nickel sulfide ore deposits become second largest nickel ore deposits in China. The discovery of the ultra-large nickel ore effectively relieves the current situation of nickel resource market shortage in China. Along with the progressive development and utilization of the shamu copper-nickel sulfide ore in summer, the development of the green and efficient nickel sulfide concentrate extraction technology has very important significance.
Common treatment methods for nickel ores include a pyrometallurgical process and a hydrometallurgical process, wherein the nickel sulfide concentrate is rich in iron elements, so that the concentration of iron ions in the leaching solution in the wet leaching process is high, the recovery process flow and the energy consumption of nickel are seriously affected, and therefore, a process capable of effectively removing iron from the nickel sulfide concentrate leaching solution needs to be explored.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a process for removing iron by a needle iron ore method from a nickel sulfide concentrate leaching solution, which aims to solve the problem of influence of iron ions with higher concentration in the nickel sulfide concentrate leaching solution on nickel recovery.
In order to achieve the above purpose, the invention provides a process for removing iron from a nickel sulfide concentrate leaching solution by a goethite method, wherein the nickel sulfide concentrate leaching solution contains iron ions, copper ions, nickel ions and cobalt ions, and the process comprises the following steps:
s10, adding reduced iron powder into the nickel sulfide concentrate leaching solution to reduce and replace copper ions in the leaching solution, and reducing iron ions in the leaching solution into ferrous ions;
s20, oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate;
s30, carrying out solid-liquid separation on the leaching solution after the reaction in the step S20 is completed, so as to remove sediment in the leaching solution.
Preferably, in the step S10, the reduced iron powder is added in an amount such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3g/L to 5g/L.
Further preferably, the reduced iron powder is added in such an amount that the concentration of reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L.
Preferably, in the step S10, after the completion of the reduction reaction, the precipitate containing copper ions is removed by solid-liquid separation.
Preferably, the step S20 specifically includes: heating the reduced leaching solution to a preset temperature, and introducing oxygen into the leaching solution to oxidize ferrous ions in the leaching solution into ferric ions, so that the ferric ions are hydrolyzed to generate goethite type precipitate.
Preferably, the preset temperature is 70-100 ℃, the gas flow of oxygen gas is 0.8-1.2L/min, and the reaction time is 300-500 min.
Further preferably, the preset temperature is 80 ℃, the gas flow rate of introducing oxygen into the leaching solution is 1L/min, and the reaction time is 480min.
Preferably, in the step S20, the pH during the reaction is controlled to 3 to 4.
According to the iron removal process of the nickel sulfide concentrate leaching solution by the goethite method, copper ions and iron ions in the nickel sulfide concentrate leaching solution are reduced by adding the iron powder, the copper ions in the leaching solution can be reduced and replaced by the iron powder on one hand, and the iron ions in the leaching solution can be reduced to ferrous ions on the other hand; then the micro-bubble oxidation method is adopted to generate goethite type sediment for iron removal. The process can efficiently remove iron ions in the nickel sulfide concentrate leaching liquid, solves the problem of influence of iron ions with higher concentration on the recovery process flow and energy consumption of nickel, and also avoids the great loss of nickel and cobalt in the iron removal process, thereby influencing the recovery and utilization of the nickel and cobalt. In addition, the iron slag obtained after the reaction is finished can be directly used as iron ore for sale, copper ions in the leaching solution are replaced in a sponge copper form, and the iron slag can be directly used for sale, so that the utilization value of raw materials is improved.
Drawings
Fig. 1 is a flow chart of a process for removing iron by a goethite method from a nickel sulfide concentrate leaching solution provided by an embodiment of the invention;
FIG. 2 is a graph showing the relationship between the amount of iron powder added and the concentration of copper ions in the leachate during the reduction and replacement of copper ions by reduced iron powder in example 2 of the present invention;
FIG. 3 is a graph showing the relationship between pH and the ion removal rate of metal ions in the leachate during the reaction of generating goethite type precipitate by the microbubble oxidation method in example 3 of the present invention.
FIG. 4 is an X-ray diffraction (XRD) pattern of iron slag in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are merely exemplary and the invention is not limited to these embodiments.
It should be noted here that, in order to avoid obscuring the present invention due to unnecessary details, only structures and/or processing steps closely related to the solution according to the present invention are shown in the drawings, while other details not greatly related to the present invention are omitted.
The embodiment of the invention provides a process for removing iron from nickel sulfide concentrate leaching liquid by a goethite method, wherein the nickel sulfide concentrate leaching liquid contains iron ions, copper ions, nickel ions and cobalt ions, and referring to fig. 1, the process comprises the following steps:
step S10: adding reduced iron powder into the nickel sulfide concentrate leaching solution to reduce and replace copper ions in the leaching solution, and reducing iron ions in the leaching solution into ferrous ions.
Preferably, the addition amount of the reduced iron powder is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3g/L to 5g/L.
Further preferably, the reduced iron powder is added in such an amount that the concentration of reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L.
Preferably, after the completion of the reduction reaction, the precipitate containing copper ions is removed by solid-liquid separation.
The reduced iron powder reduces copper ions in the leaching solution to enable the copper ions to be replaced in a sponge copper form, and then the sponge copper precipitate is filtered to achieve the purpose of removing the copper ions in the leaching solution; in addition, the reduced iron powder also plays a role in reducing iron ions in the leachate into ferrous ions.
And S20, oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate.
Specifically, the step S20 includes: heating the reduced leaching solution to a preset temperature, and introducing oxygen into the leaching solution to oxidize ferrous ions in the leaching solution into ferric ions, so that the ferric ions are hydrolyzed to generate goethite type precipitate.
Goethite is one of the main minerals of hydrous oxides, commonly known as alpha iron oxide monohydrate, having a composition of alpha-Fe 2 O 3 ·H 2 O or alpha-FeOOH has high iron content in precipitate and less adsorption to other metal ions in solution, so that the recovery rate of metal iron is high by adopting a goethite method.
The specific reaction process of deironing by goethite method comprises oxidation reaction and hydrolysis reaction:
oxidation reaction:
4Fe 2+ +O 2 +4H + →4Fe 3+ +2H 2 O
hydrolysis reaction:
Fe 3+ +H 2 O→FeOH 2+ +H +
FeOH 2+ +H 2 O→FeOOH+2H +
oxygen first reacts Fe with 2+ Oxidation to Fe 3+ ，Fe 3+ Through hydrolysis to form simple hydrolysate FeOH 2+ The hydrolysate is further hydrolyzed and nucleated to form FeOOH microcrystal, and the FeOOH microcrystal is aggregated and grown to form goethite type solid sediment alpha-FeOOH, wherein Fe 2+ Oxidation and Fe 3+ The hydrolysis reactions occur sequentially in a compositional cascade.
The oxidation reaction is carried out by oxygen, the oxidation process involves physical processes such as gas-liquid diffusion, mass transfer and the like, the speed is slower, and Fe 3+ Is extremely unstable in solution, and therefore Fe 3+ Formation of FeOH by hydrolysis 2+ Is fast. But if it doesFe in solution 3+ The content is too high>1 g/L), fe is liable to be caused 3+ Fe (OH) formation 3 Colloidal precipitation, thus, in the process of iron removal by the goethite method, the key is to control Fe 2+ Is a reaction product of the oxidation rate of the catalyst.
Preferably, the preset temperature is 70-100 ℃, the gas flow of oxygen gas is 0.8-1.2L/min, and the reaction time is 300-500 min.
Further preferably, the preset temperature is 80 ℃, the gas flow rate of introducing oxygen into the leaching solution is 1L/min, and the reaction time is 480min.
Iron is removed by adopting a goethite method, and Fe in leaching liquid 3+ The concentration of (2) has a large influence on iron removal, and thus, fe is controlled 2+ The oxidation speed of (2) is the key of iron removal by goethite method, and the invention adopts a microbubble oxidation method to oxidize Fe 2+ Controlling the flow rate of the introduced oxygen to control Fe 2+ To solve the problem of difficult iron removal control in goethite method.
Preferably, the pH during the reaction is controlled to 3-4.
Fe in the process of deironing by goethite method 2+ Oxidation rate of ions and [ H ] + ] 0.25 Inversely proportional, as the pH increases, the Fe in solution 2+ The oxidation speed of Fe is accelerated 3+ The number of ion hydrolysis precipitation is increased, and the iron removal efficiency is obviously improved; however, if the pH is too high, fe is formed by oxidation reaction 3+ Ion concentration of more than 1g/L, easy Fe generation 3+ Fast precipitation and formation of Fe (OH) 3 The colloid causes a great deal of nickel and cobalt to be adsorbed, and the loss rate of nickel and cobalt is dramatically increased.
And step S30, carrying out solid-liquid separation on the leaching solution after the reaction in the step S20 is completed, so as to remove the precipitate in the leaching solution.
Specifically, the leaching solution after the completion of the reaction in step S20 is filtered to remove the precipitate in the leaching solution.
The above-described process for removing iron from a nickel sulfide concentrate leachate by the goethite method will be described below with reference to specific examples, which are understood by those skilled in the art to be specific examples of the above-described process for removing iron from a nickel sulfide concentrate leachate by the goethite method of the present invention, and are not intended to be limiting in all respects.
Example 1: preparation of nickel sulfide concentrate leaching solution
The nickel sulfide concentrate of the embodiment of the invention is provided by Qinghai yellow river mining company, and the main components and phase analysis of the nickel sulfide concentrate are shown in tables 1 and 2.
Table 1: main metal component of nickel sulfide concentrate
Table 2: full element semi-quantitative analysis (XRF) of nickel sulfide concentrate
Treating the nickel sulfide concentrate by adopting an superfine grinding-oxygen pressure leaching process to obtain a nickel sulfide concentrate leaching solution:
step one, size mixing: mixing the nickel sulfide concentrate with water to form nickel sulfide concentrate slurry with the concentration of 25%.
Step two, fine grinding: placing the nickel sulfide concentrate slurry into a ball mill for ball milling to form superfine milled nickel sulfide concentrate; wherein the ball milling time is 6min, and the mass ratio of ore materials with the granularity of the superfine mill nickel sulfide concentrate below 400 meshes is more than 90 percent.
Step three, leaching: placing the superfine grinding nickel sulfide concentrate into a reaction furnace, adding sulfuric acid solution with the concentration of 50g/L as leaching solution, and introducing oxygen with the pressure of 1.4Mpa into the sulfuric acid solution to leach metal elements in the superfine grinding nickel sulfide concentrate; wherein the solid-to-liquid ratio of the superfine grinding nickel sulfide concentrate to the sulfuric acid solution is 200g/L, the leaching temperature is 110 ℃, and the leaching time is 300min.
After the leaching reaction of the superfine grinding nickel sulfide concentrate is finished, filtering the superfine grinding nickel sulfide concentrate to obtain nickel sulfide concentrate leaching solution, wherein the concentration of iron, nickel, cobalt and copper in the nickel sulfide concentrate leaching solution is 31.5g/L (0.563 mol/L), 17.2g/L (0.29 mol/L), 0.61g/L (0.01 mol/L) and 2.94g/L (0.0459 mol/L) respectively.
Example 2: influence of the addition amount of reduced iron powder on the iron removal process
Step one, adding reduced iron powder into the nickel sulfide concentrate leaching solution obtained in the embodiment 1 to reduce copper ions in the leaching solution, so that the copper ions are replaced in a sponge copper form, reducing iron ions in the leaching solution into ferrous ions, and removing sponge copper precipitates through filtration after the reduction reaction is completed.
Oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate: heating the reduced leaching solution to 80 ℃, and introducing oxygen into the leaching solution to oxidize ferrous ions in the leaching solution into ferric ions, so that the ferric ions are hydrolyzed to generate goethite type precipitate, wherein the flow rate of the oxygen introduced into the leaching solution is 1L/min, and the reaction time is 480min.
And thirdly, filtering the leaching solution after the reaction in the step two to remove the precipitate in the leaching solution.
Under the above conditions, the influence of the addition amount of the reduced iron powder on the iron removal process of the nickel sulfide concentrate leaching solution by the goethite method is examined. Fig. 2 is a graph showing the relationship between the addition amount of iron powder and the concentration of copper ions in the process of reducing and replacing copper ions by the reduced iron powder in the leaching solution of nickel sulfide concentrate, and the experimental results obtained under the above conditions are shown in fig. 2.
As can be seen from fig. 2, when the addition amount of the iron powder is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution reaches 3.0g/L or more, the concentration of copper ions in the solution is greatly reduced, so that the addition amount of the iron powder in the solution of the present invention is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is preferably 3.0g/L to 5.0g/L; when the addition amount of the iron powder is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L, the concentration of copper ions in the solution is reduced from 2940mg/L to 3ppm, at this time, theoretically, the copper ions in the leaching solution can be removed completely, the addition amount of the iron powder is continuously increased, and the concentration of the copper ions is basically unchanged, so that the addition amount of the reduced iron powder is selected to be optimal so that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L.
Example 3: influence of pH during the reaction on the iron removal Process
Step one, adding reduced iron powder into the nickel sulfide concentrate leaching solution obtained in the embodiment 1 to reduce copper ions in the leaching solution, so that the copper ions are replaced in a sponge copper form, reducing iron ions in the leaching solution into ferrous ions, and removing sponge copper precipitates through filtration after the reduction reaction is completed; wherein the addition amount of the reduced iron powder is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L.
Oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate: heating the reduced leaching solution to 80 ℃, and introducing oxygen into the leaching solution to oxidize ferrous ions in the leaching solution into ferric ions, so that the ferric ions are hydrolyzed to generate goethite type precipitate; wherein, the gas flow of the oxygen gas introduced into the leaching solution is 1L/min, and the reaction time is 480min.
And thirdly, filtering the leaching solution after the reaction in the step two to remove the precipitate in the leaching solution.
Under the above conditions, the influence of the pH in the reaction process on the iron removal process of the nickel sulfide concentrate leaching solution by the goethite method is examined. FIG. 3 is a graph showing the relationship between pH and the ion removal rate of each metal ion in the leachate during the reaction of forming goethite type precipitate by using the microbubble oxidation method, and the experimental results obtained under the above conditions are shown in FIG. 3.
As can be seen from fig. 3, as the pH of the reaction increases from 1.5 to 3, the removal efficiency of iron ions in the nickel sulfide concentrate leachate increases from 36.5% to 92%, and at this time, the concentration of nickel ions and cobalt ions in the leachate is basically unchanged, and the ion concentration is basically unchangedThe removal rate was close to 0 and remained unchanged. When the pH of the reaction is continuously increased to 5, the removal efficiency of the iron ions is basically kept unchanged, but at the moment, the ion removal rate of the nickel ions and the cobalt ions is sharply increased, and the ion loss rate is sharply increased. This is due to Fe 2+ Oxidation rate of [ H ] + ] 0.25 Inversely proportional, as the pH increases, the Fe in solution 2+ Accelerated ion oxidation, fe 3+ The number of ion hydrolysis precipitation is increased, and the iron removal efficiency is obviously improved; however, when the pH is 5, the oxidation of Fe occurs due to the pH being too high 3+ Ion concentration of greater than 1g/L, resulting in Fe 3+ Fast precipitation and formation of Fe (OH) 3 The colloid adsorbs a large amount of nickel ions and cobalt ions, and the loss rate of the nickel ions and the cobalt ions is increased sharply. Therefore, when the goethite method is adopted for removing iron, the pH value in the reaction process of generating goethite type sediment by the microbubble oxidation method is controlled to be optimal between 3 and 4.
Example 4: technological conditions for optimizing iron removal process of nickel sulfide concentrate leaching solution by adopting goethite method
Step one, adding reduced iron powder into the nickel sulfide concentrate leaching solution obtained in the embodiment 1 to reduce copper ions in the leaching solution, so that the copper ions are replaced in a sponge copper form, reducing iron ions in the leaching solution into ferrous ions, and removing sponge copper precipitates through filtration after the reduction reaction is completed; wherein the addition amount of the reduced iron powder is such that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3.88g/L.
Oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate: heating the reduced leaching solution to 80 ℃, and introducing oxygen into the leaching solution to oxidize ferrous ions in the leaching solution into ferric ions, so that the ferric ions are hydrolyzed to generate goethite type precipitate, wherein the gas flow of the oxygen introduced into the leaching solution is 1L/min, the reaction time is 480min, and the pH value in the reaction process is 3.
And thirdly, filtering the leaching solution after the reaction in the step two to remove the precipitate in the leaching solution.
Filtering the leaching solution to obtain iron slag precipitate and nickel sulfide concentrate leaching solution, wherein the content of iron in the nickel sulfide concentrate leaching solution is 0.012g/L.
The XRF total element semi-quantitative analysis of the iron slag obtained by filtering the nickel sulfide concentrate leaching solution is carried out, and the XRF total element semi-quantitative analysis result of the iron slag is shown in table 3.
Table 3: semi-quantitative analysis (XRF) of iron slag
As is clear from table 3, the main elements in the iron slag are Fe (65.7%), O (31.3%), S (1.90%), and other elements are Ni, co, si, al, cl, ca, and the like.
Further, the iron slag was quantitatively analyzed by using an ICP-OES inductively coupled plasma emission spectrometer, and the results of the quantitative analysis of the main metal elements in the iron slag and the analysis of the composition of the leachate are shown in table 4.
Table 4: quantitative analysis (ICP-OES) of main metal elements in iron slag and composition analysis of leaching liquid
As is clear from Table 4, the Fe content in the iron slag can reach 55.9%, and the iron slag can be directly sold as iron ore, and the Ni and Co contents are only 0.23% and 0.03%. The concentration of Fe, ni and Co in the nickel sulfide concentrate leaching solution which is not deironing by adopting the goethite method is 31.5g/L, 17.2g/L and 0.61g/L respectively, and after the nickel sulfide concentrate leaching solution is deironing by adopting the goethite method, the concentration of Fe, ni and Co in the nickel sulfide concentrate leaching solution is 0.012g/L, 16.38g/L and 0.607g/L respectively, at the moment, the removal rate of iron in the nickel sulfide concentrate leaching solution is more than 99 percent, the loss of nickel is less than 3 percent, and the cobalt is almost free.
Fig. 4 shows an X-ray diffraction (XRD) pattern of the iron slag, and it is apparent from fig. 4 that the iron slag obtained by the above-described process is a single-phase α -FeOOH.
According to the iron removal process of the nickel sulfide concentrate leaching solution by the goethite method, copper ions and iron ions in the nickel sulfide concentrate leaching solution are reduced by adding the iron powder, the copper ions in the leaching solution can be reduced and replaced by the iron powder on one hand, and the iron ions in the leaching solution can be reduced to ferrous ions on the other hand; the iron is removed by generating goethite type sediment through a microbubble oxidation method, so that the removal rate of iron in the nickel sulfide concentrate leaching solution can reach more than 99%, the loss of nickel is less than 3%, and cobalt is almost free of loss. Therefore, the process can efficiently remove the iron ions in the nickel sulfide concentrate leaching liquid, solves the influence of the iron ions with higher concentration on the nickel recovery process flow and energy consumption, and also avoids the larger loss of nickel and cobalt in the iron removal process, thereby influencing the recovery and utilization of the nickel and cobalt. In addition, the iron content in the iron slag obtained after the reaction is finished reaches more than 55%, the iron slag can be directly sold as iron ore, copper ions in the leaching solution are replaced in a sponge copper form, and the iron slag can be directly sold, so that the utilization value of raw materials is improved.
The foregoing is merely exemplary of the application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the application and are intended to be comprehended within the scope of the application.
Claims (5)
1. The process for removing iron from nickel sulfide concentrate leaching liquid by adopting a goethite method is characterized in that the nickel sulfide concentrate leaching liquid contains iron ions, copper ions, nickel ions and cobalt ions, and comprises the following steps:
s10, adding reduced iron powder into the nickel sulfide concentrate leaching solution to reduce and replace copper ions in the leaching solution, and reducing iron ions in the leaching solution into ferrous ions;
s20, oxidizing the nickel sulfide concentrate leaching solution subjected to the reduction treatment by adopting a microbubble oxidation method to generate goethite type precipitate; the step S20 specifically includes: heating the reduced leaching solution to 70-100 ℃, introducing oxygen into the leaching solution at a gas flow rate of 0.8-1.2L/min to oxidize ferrous ions in the leaching solution into ferric ions, hydrolyzing the ferric ions to generate goethite type precipitate, reacting for 300-500 min, and controlling the pH value in the reaction process to 3-4;
s30, carrying out solid-liquid separation on the leaching solution after the reaction in the step S20 is completed, so as to remove sediment in the leaching solution.
2. The process according to claim 1, wherein in the step S10, the reduced iron powder is added in such an amount that the concentration of the reduced iron powder in the nickel sulfide concentrate leaching solution is 3g/L to 5g/L.
3. The process according to claim 2, characterized in that in step S10, the reduced iron powder is added in such an amount that the concentration of reduced iron powder in the nickel sulphide concentrate leaching solution is 3.88g/L.
4. A process according to any one of claims 1 to 3, wherein in step S10, after completion of the reduction reaction, the precipitate containing copper ions is removed by solid-liquid separation.
5. The process according to claim 1, wherein the predetermined temperature is 80 ℃, the flow rate of the oxygen gas introduced into the leachate is 1L/min, and the reaction time is 480min.
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| JP2003277067A (en) * | 2002-03-20 | 2003-10-02 | Sumitomo Metal Mining Co Ltd | Method for manufacturing nickel sulfide with excellent oxidation resistance |
| CN109825700A (en) * | 2019-03-18 | 2019-05-31 | 中国科学院过程工程研究所 | A kind of method of valuable metal in low-temperature atmosphere-pressure selective extraction nickel sulfide concentrate |
| WO2020044849A1 (en) * | 2018-08-30 | 2020-03-05 | 日揮グローバル株式会社 | Method for producing nickel sulfate compound |
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| CN103409622B (en) * | 2013-07-22 | 2016-01-20 | 昆明理工大学科技产业经营管理有限公司 | A kind of method of individual curing high-iron zinc sulfide concentrate |
| CN104017991A (en) * | 2014-06-06 | 2014-09-03 | 郴州市金贵银业股份有限公司 | Process for efficiently and selectively separating copper in lead copper matte |
| CN108570557B (en) * | 2017-03-14 | 2020-01-24 | 湖南埃格环保科技有限公司 | Method for separating iron, chromium, nickel, copper and zinc from high-iron high-chromium electroplating sludge leachate |
| CN111663040A (en) * | 2020-06-22 | 2020-09-15 | 中南大学 | Method for enhancing oxygen oxidation iron removal in solution by using microbubble generator |
| CN111748690B (en) * | 2020-07-30 | 2021-06-22 | 中南大学 | Method for purifying and deironing hydrometallurgy leaching solution based on hydrothermal lattice transformation |
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| JP2003277067A (en) * | 2002-03-20 | 2003-10-02 | Sumitomo Metal Mining Co Ltd | Method for manufacturing nickel sulfide with excellent oxidation resistance |
| WO2020044849A1 (en) * | 2018-08-30 | 2020-03-05 | 日揮グローバル株式会社 | Method for producing nickel sulfate compound |
| CN109825700A (en) * | 2019-03-18 | 2019-05-31 | 中国科学院过程工程研究所 | A kind of method of valuable metal in low-temperature atmosphere-pressure selective extraction nickel sulfide concentrate |
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