CN111549219A - Method for comprehensively treating and recycling valuable substances from nickel ore - Google Patents
Method for comprehensively treating and recycling valuable substances from nickel ore Download PDFInfo
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- CN111549219A CN111549219A CN202010292699.9A CN202010292699A CN111549219A CN 111549219 A CN111549219 A CN 111549219A CN 202010292699 A CN202010292699 A CN 202010292699A CN 111549219 A CN111549219 A CN 111549219A
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction 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
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
-
- 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
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- 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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- 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 relates to a method for comprehensively treating and recycling valuable substances from nickel ores, which is characterized by comprising the following steps of: 1) crushing and screening nickel-containing ores; 2) leaching with a sulfuric acid solution with a mass concentration of 10-50 wt% according to an acid-mineral ratio of 0.5-1.1: 1; 3) adding hydrogen peroxide according to the mass ratio of hydrogen peroxide to leachate = 0.05-0.1: 1, stirring and heating to 50-80 ℃, then dropwise adding light-burned magnesium powder slurry with the magnesium oxide content of 75-90% and the activity of 50-90 as a purifying agent, and purifying and removing iron; 4) adding active magnesium oxide with the magnesium oxide content of 90-98% and the activity of 100-180% to carry out nickel extraction, and obtaining a nickel hydroxide product and a filtrate; 5) evaporating and concentrating the filtrate, and then carrying out spray drying to obtain a magnesium sulfate product, wherein the generated water is recycled. Reasonable process, simple flow, high production efficiency, lower cost, high comprehensive treatment recovery rate and zero emission.
Description
Technical Field
The invention relates to a method for comprehensively treating and recycling valuable substances from nickel ores, and belongs to the technical field of nickel ore treatment and separation.
Background
The content of magnesium in the nickel-containing ore is generally 10-20 times of the content of nickel. In the traditional wet nickel smelting process, limonite type laterite-nickel ore is generally leached by concentrated acid, then the acid in the feed liquid is neutralized by using a silicon-magnesium-nickel ore pulp, solid-liquid separation is carried out to obtain leachate and solid slag, the solid slag is difficult to recycle and only needs to be stockpiled, and the solid slag is dangerous solid waste slag containing nickel, so the stockpiling can cause environmental pollution. In addition, after the leachate is subjected to alkali neutralization, purification and nickel extraction by using calcium and sodium, magnesium-containing wastewater with large quantity, low concentration and large amount of impurity elements is generated, the components in the magnesium-containing wastewater are complex, the treatment cost is high, and the magnesium-containing wastewater is generally discharged as wastewater, so that the environment is seriously polluted. Therefore, there is a need for improvements in the prior art.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for comprehensively treating nickel ore to recover valuable substances, which can not only obtain a nickel smelting raw material, namely high-grade nickel hydroxide, but also solve the problems of low magnesium ion content and high impurity content in wastewater, thereby solving the problems of high cost and large investment in the traditional magnesium sulfate recovery treatment.
The invention is realized by the following technical scheme: a method for recovering valuable substances through comprehensive treatment of nickel ores is characterized by comprising the following steps:
1) crushing and screening the nickel-containing ore until the granularity is 0.6-2.4 mm to obtain ore sand;
2) leaching the ore sand in the step 1) by using a sulfuric acid solution with the mass concentration of 10-50 wt% according to an acid-ore ratio of 0.5-1.1: 1, and performing solid-liquid separation to obtain a leaching solution and a solid;
3) adding hydrogen peroxide into the leachate obtained in the step (2) according to the mass ratio of 0.05-0.1: 1, stirring, heating to 50-80 ℃, carrying out oxidation treatment on ferrous ions, dropwise adding light-burned magnesium powder slurry with the magnesium oxide content of 75-90% and the activity of 50-90 as a purifying agent, adjusting the pH value, purifying and deironing until the pH value is 2.5-4.0, and carrying out solid-liquid separation to obtain solid and liquid;
4) adding active magnesium oxide with the magnesium oxide content of 90-98% and the activity of 100-180% into the liquid separated in the step 3) as a nickel extracting agent, extracting nickel until the pH value is 8-11, and filtering to obtain a nickel hydroxide product and a filtrate;
5) evaporating and concentrating the filtrate obtained in the step 4), and then performing spray drying to obtain a magnesium sulfate product, wherein water generated by evaporation is recycled as process return water.
The nickel-containing ore in the step 1) is high-magnesium low-iron nickel ore obtained by conventional beneficiation of laterite nickel ore.
The crushing in the step 1) is dry crushing, so that the water consumption of a system is reduced, and the concentration of magnesium ions is improved.
The leaching in the step 2) is one or more of conventional heap leaching, soaking leaching and agitation leaching.
The solid-liquid separation in the step 2) and the step 3) is realized by adopting one or more of a thickener, a box type filter, a vacuum filter, a belt filter, a vertical filter press and a countercurrent washing device.
The sulfuric acid in the step 2) is a byproduct sulfuric acid of a non-ferrous metal smelting plant.
The hydrogen peroxide in the step 3) is used as an oxidant and is used for oxidizing ferrous ions, and the reaction mechanism is as follows: 2FeSO4+H2O2+2H2SO4→2Fe2(SO4)3+2H2O。
The light-burned magnesium powder in the step 3) is used as a purifying agent for adjusting the pH value, purifying and removing iron, and the reaction mechanism is as follows:
MgO+H2SO4→MgSO4+H2O
the active magnesium oxide in the step 4) is used as a nickel extracting agent to replace calcium agents and sodium agents in the traditional process, and nickel ions are recovered from the leaching solution, so that the concentration of magnesium ions in the solution is improved, the introduction of other impurity ions is avoided, and the grade of nickel hydroxide is improved.
The evaporation and concentration in the step 5) are evaporation completed by adopting a conventional multi-effect evaporation or MVR evaporator, and the problems that after nickel in the traditional nickel-containing ore is recovered, magnesium-containing waste water needs to be discharged to pollute the environment, or the treatment investment needs to be increased for environmental protection and the treatment difficulty is increased are solved.
The spray drying in the step 5) is completed by adopting a conventional pressure type or centrifugal spray drying tower or a fluidized bed granulation dryer, a heat source is natural gas or high-temperature waste heat flue gas, the hot air temperature is 200-400 ℃, and compared with the traditional cooling crystallization process, the spray drying has the characteristics of simple flow, low cost and high production efficiency.
The magnesium sulfate product of the step 5) comprises MgSO4·H20. Anhydrous MgSO (MgSO)4The bulk density is 0.2-1.2, the fertilizer can be used for crop planting, can be used as a feed additive for livestock and aquaculture, and can be used as a leaching agent for livestock and aquacultureThe rare earth can also be used as an industrial product in industries such as leather making, explosive, paper making, porcelain, dye printing and the like.
The filtrate obtained in the step 4) and the evaporated concentrated solution obtained in the step 5) can be prepared singly or in a mixed manner according to factors such as customer requirements and transportation requirements, and a 10-30% magnesium sulfate solution is provided for users, so that the magnesium sulfate solution can be used in industries such as agriculture, animal husbandry, fishery, rare earth mining, papermaking and printing and dyeing.
The invention has the advantages and effects that:
the invention takes the high-magnesium low-iron garnierite as the raw material, and the garnierite is treated by the process steps, thereby not only improving the magnesium ion content of the solution, but also using light-burned magnesium powder as a purifying agent and active magnesium oxide as a nickel extracting agent, effectively reducing the impurity content, reducing the impurity removal cost, creating favorable conditions for magnesium sulfate recovery, and recovering the magnesium sulfate by evaporation concentration and spray drying treatment without discharging waste water outwards.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
TABLE 1 elemental grades of nickel-containing ores
1) Carrying out dry crushing and screening on the nickel-containing ore until the particle size is 0.6-2.4 mm, and obtaining ore sand;
2) stirring and leaching the ore sand in the step 1) for 3 hours by using a sulfuric acid solution with the mass concentration of 35 wt% according to the acid-ore ratio of 0.85:1, and performing solid-liquid separation by using a thickener to obtain a leaching solution and a solid; the obtained solid contains 0.15% of nickel and 0.0093% of cobalt, and the components in the leaching solution are shown in a table 2:
TABLE 2 leachate Components g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 4.38 | 12.56 | 52.47 | 0.02 | 0.38 | 0.35 | 0.95 | 0.09 | 0.45 | 0.5 |
3) Adding hydrogen peroxide into the leachate obtained in the step (2) according to the mass ratio of 0.09:1, stirring and heating to 70 ℃, carrying out ferrous ion oxidation treatment, dropwise adding light-burned magnesium powder slurry with 75% of magnesium oxide content and 90% of activity as a purifying agent, adjusting the pH value, purifying and deironing until the pH value is 3.5, and carrying out solid-liquid separation by using a belt filter to obtain solid and liquid; the liquid composition obtained is shown in Table 3:
TABLE 3 purified liquid fraction g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 3.98 | 0.0013 | 54.15 | 0.02 | 0.17 | 0.09 | 0.1 | 0.0075 | 0.42 | 3.45 |
4) Adding active magnesium oxide with the magnesium oxide content of 95% and the activity of 150 as a nickel extracting agent into the liquid separated in the step 3), extracting nickel until the pH value is 9, filtering to obtain a nickel hydroxide product and a filtrate, wherein the components of the filtrate are shown in a table 4;
TABLE 4 composition of the solution after nickel extraction in g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 0.0009 | 0.0008 | 53.04 | 0.0009 | 0.0075 | 0.0053 | 0.014 | 0.0003 | 0.42 | 9.3 |
5) Evaporating and concentrating the filtrate obtained in the step 4) by an MVR evaporator, and then performing spray drying by a centrifugal spray drying tower, wherein the heat source is high-temperature waste heat flue gas, the temperature of hot air is 230 ℃, a magnesium sulfate product is obtained, the magnesium sulfate component is shown in a table 5, and water generated by evaporation is recycled as process return water.
Table 5 product magnesium sulfate composition%
| Mg | Fe | Pb | As | Cl- |
| 16.07 | 0.0009 | 0.0004 | 0.0002 | 0.009 |
Example 2
TABLE 1 elemental grades of nickel-containing ores
1) Carrying out dry crushing and screening on the nickel-containing ore until the particle size is 0.6-2.4 mm, and obtaining ore sand;
2) soaking the ore sand obtained in the step 1) for 50 days by using a sulfuric acid solution with the mass concentration of 40 wt% according to the acid-ore ratio of 0.75:1, and performing solid-liquid separation by using a thickener to obtain a leaching solution and a solid; the resulting solids contained 0.20% nickel and 0.001% cobalt, the composition of the leach solution being shown in table 2:
TABLE 2 leachate Components g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 4.57 | 10.76 | 56.24 | 0.02 | 0.36 | 0.31 | 0.88 | 0.087 | 0.4 | 1.0 |
3) Adding hydrogen peroxide into the leachate obtained in the step (2) according to the mass ratio of 0.05:1, stirring and heating to 50 ℃, carrying out oxidation treatment on ferrous ions, dropwise adding light-burned magnesium powder slurry with 75% of magnesium oxide content and 50% of activity as a purifying agent, adjusting the pH value, purifying and deironing until the pH value is 3.3, and carrying out solid-liquid separation to obtain solid and liquid; the components in the resulting liquid are shown in Table 3:
TABLE 3 purified liquid fraction g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 4.11 | 0.002 | 57.28 | 0.019 | 0.13 | 0.08 | 0.079 | 0.0065 | 0.38 | 3.2 |
4) Adding active magnesium oxide with the magnesium oxide content of 90% and the activity of 100 as a nickel extracting agent into the liquid separated in the step 3), extracting nickel until the pH value is 8, filtering to obtain a nickel hydroxide product and a filtrate, wherein the components of the filtrate are shown in a table 4;
TABLE 4 composition of the solution after nickel extraction in g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 0.0008 | 0.0008 | 56.17 | 0.0008 | 0.0064 | 0.0043 | 0.015 | 0.0002 | 0.38 | 9.5 |
5) Evaporating and concentrating the filtrate obtained in the step 4) by an MVR evaporator, and then performing spray drying by a centrifugal spray drying tower, wherein the heat source is high-temperature waste heat flue gas, the hot air temperature is 200 ℃, a magnesium sulfate product is obtained, the magnesium sulfate component is shown in a table 5, and water generated by evaporation is recycled as process return water.
Table 5 product magnesium sulfate composition%
| Mg | Fe | Pb | As | Cl- |
| 16.25 | 0.0008 | 0.0004 | 0.00015 | 0.01 |
Example 3
TABLE 1 elemental grades of nickel-containing ores
1) Carrying out dry crushing and screening on the nickel-containing ore until the particle size is 0.6-2.4 mm, and obtaining ore sand;
2) heap leaching the ore sand in the step 1) for 30 days by using a sulfuric acid solution with the mass concentration of 50wt% according to the acid-ore ratio of 1.1:1, and performing solid-liquid separation by using a thickener to obtain a leaching solution and a solid; the resulting solids contained 0.20% nickel and 0.001% cobalt, the composition of the leach solution being shown in table 2:
TABLE 2 leachate Components g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 4.81 | 12.08 | 58.45 | 0.018 | 0.31 | 0.34 | 0.79 | 0.082 | 0.46 | 0.37 |
3) Adding hydrogen peroxide into the leachate obtained in the step (2) according to the mass ratio of 0.1:1, stirring and heating to 50 ℃, carrying out oxidation treatment on the dimethyl iron ions, then dropwise adding light-burned magnesium powder slurry with the magnesium oxide content of 90% and the activity of 90% as a purifying agent, adjusting the pH value, purifying and deironing until the pH value is 4.0, and carrying out solid-liquid separation to obtain solid and liquid; the components in the resulting liquid are shown in Table 3:
TABLE 3 purified liquid fraction g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 4.47 | 0.003 | 56.59 | 0.017 | 0.15 | 0.09 | 0.082 | 0.0059 | 0.44 | 3.7 |
4) Adding active magnesium oxide with the magnesium oxide content of 98% and the activity of 180% into the liquid separated in the step 3) as a nickel extracting agent, extracting nickel until the pH value is 11, filtering to obtain a nickel hydroxide product and a filtrate, wherein the components of the filtrate are shown in a table 4;
TABLE 4 composition of the solution after nickel extraction in g/L
| Ni | Fe | Mg | Co | Mn | Al | SiO2 | Cr | Ca | pH |
| 0.0006 | 0.0003 | 55.37 | 0.0005 | 0.0043 | 0.0035 | 0.016 | 0.0003 | 0.42 | 9.8 |
5) Evaporating and concentrating the filtrate obtained in the step 4) by an MVR evaporator, and then performing spray drying by a centrifugal spray drying tower, wherein the heat source is high-temperature waste heat flue gas, the hot air temperature is 400 ℃, a magnesium sulfate product is obtained, the magnesium sulfate component is shown in a table 5, and water generated by evaporation is recycled as process return water.
Table 5 product magnesium sulfate composition%
| Mg | Fe | Pb | As | Cl- |
| 16.51 | 0.0006 | 0.0003 | 0.00011 | 0.008 |
Claims (6)
1. A method for recovering valuable substances through comprehensive treatment of nickel ores is characterized by comprising the following steps:
1) crushing and screening the nickel-containing ore until the granularity is 0.6-2.4 mm to obtain ore sand;
2) leaching the ore sand in the step 1) by using a sulfuric acid solution with the mass concentration of 10-50 wt% according to an acid-ore ratio of 0.5-1.1: 1, and performing solid-liquid separation to obtain a leaching solution and a solid;
3) adding hydrogen peroxide into the leachate obtained in the step (2) according to the mass ratio of hydrogen peroxide to leachate = 0.05-0.1: 1, stirring and heating to 50-80 ℃, carrying out oxidation treatment on ferrous ions, dropwise adding light calcined magnesia powder slurry with 75-90% of magnesium oxide content and 50-90% of activity as a purifying agent, adjusting the pH value, purifying and deironing until the pH value is 2.5-4.0, and carrying out solid-liquid separation to obtain solid and liquid;
4) adding active magnesium oxide with the magnesium oxide content of 90-98% and the activity of 100-180% into the liquid separated in the step 3) as a nickel extracting agent, extracting nickel until the pH value is 8-11, and filtering to obtain a nickel hydroxide product and a filtrate;
5) evaporating and concentrating the filtrate obtained in the step 4), and then performing spray drying to obtain a magnesium sulfate product, wherein water generated by evaporation is recycled as process return water.
2. The method according to the claim 1, characterized in that the nickel-bearing ore of step 1) is high-magnesium low-iron nickel ore obtained from laterite-nickel ore by conventional beneficiation.
3. The method according to claim 1, wherein the crushing in step 1) is dry crushing to reduce water consumption of the system and increase magnesium ion concentration.
4. The method as claimed in claim 1, wherein the leaching of step 2) is one or more of conventional heap leaching, soaking leaching and agitation leaching.
5. The method of claim 1, wherein the solid-liquid separation in step 2) and step 3) is performed by using one or more of a thickener, a box filter, a vacuum filter, a belt filter, a vertical filter press, and a counter-current washing device.
6. The method according to claim 1, wherein the sulfuric acid of step 2) is a by-product sulfuric acid from a nonferrous metal smelting plant.
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