CN111304439A - Method for recovering valuable metals from submarine manganese ore resources - Google Patents

Method for recovering valuable metals from submarine manganese ore resources Download PDF

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Publication number
CN111304439A
CN111304439A CN202010242056.3A CN202010242056A CN111304439A CN 111304439 A CN111304439 A CN 111304439A CN 202010242056 A CN202010242056 A CN 202010242056A CN 111304439 A CN111304439 A CN 111304439A
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China
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leaching
manganese
adopting
reducing agent
ore
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CN202010242056.3A
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Inventor
蒋训雄
汪胜东
李达
冯林永
赵峰
蒋伟
张登高
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BGRIMM Technology Group Co Ltd
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BGRIMM Technology Group Co Ltd
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Priority to CN202010242056.3A priority Critical patent/CN111304439A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0065Leaching or slurrying
    • C22B15/0067Leaching or slurrying with acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0084Treating solutions
    • C22B15/0089Treating solutions by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0407Leaching processes
    • C22B23/0415Leaching processes with acids or salt solutions except ammonium salts solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3844Phosphonic acid, e.g. H2P(O)(OH)2
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846Phosphoric acid, e.g. (O)P(OH)3
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00Obtaining manganese
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

A method for recovering valuable metals from submarine manganese ore resources belongs to the field of comprehensive recovery of submarine mineral resources. The method comprises the following steps: step (1): grinding the seafloor manganese ore to be below 200 meshes, and leaching the ground seafloor manganese ore by adopting a carbon-based reducing agent weak acid leaching system to obtain a leaching solution and leaching slag; step (2): removing impurities from the leachate obtained in the step (1) by adopting an iron vitriol method; and (3): precipitating the impurity-removed solution obtained in the step (2) by adopting a sulfide precipitation process to obtain an enriched sulfide and a manganese-rich solution; and (4): carrying out oxygen pressure leaching on the enriched sulfide in the step (3), and separating leached liquid through an extraction-back extraction process to prepare a related product; and (5): and (4) preparing electrolytic manganese or manganese dioxide from the manganese-rich solution obtained in the step (3) by adopting an electrolytic deposition process. The invention can realize the recovery of valuable metal elements in the iron by a full wet method, can reduce or inhibit the leaching rate of iron and reduce the subsequent iron removal cost.

Description

Method for recovering valuable metals from submarine manganese ore resources
Technical Field
The invention belongs to the field of comprehensive recovery of seabed mineral resources, relates to a method for recovering valuable metals from seabed manganese ore resources, and particularly relates to a method for recovering nonferrous metals from the seabed manganese ore resources by carbon-based reduction and weak acid leaching.
Background
The seabed manganese ore resource is a multi-metal oxidized ore taking iron-manganese oxide as a carrier, and the reserves of the ore on the seabed are extremely rich. With the decrease of the reserves of the land metal mineral resources, the high-quality mineable ores are less and less, the production cost is increased, and the contradiction between supply and demand is increasingly prominent, so that the external dependence of a large amount of metal mineral products in China is increasingly raised, the restriction on the sustainable development of the national economy is increasingly prominent, and the active exploration and development of the deep-sea mineral resources are a main way for solving the contradiction.
Although the reserves of the produced resources of the submarine manganese ore are rich, the submarine manganese ore belongs to complex oxidized ore combined with multiple metals due to different mineralization conditions, and has the remarkable characteristics of high ferromanganese content and low contents of other nickel, cobalt and copper, so that the comprehensive recovery of valuable elements is complex in treatment process. The reduction ammonia leaching process can realize selective leaching separation, and leaching reagents can be recycled, but the problems of ammonia nitrogen wastewater generation and ammonia volatilization are difficult to avoid; the normal-pressure high-acid leaching process is simple, the metal recovery rate is high, but the iron leaching rate is high, so that the filtering is difficult, and a large amount of iron slag generated by the iron removal process becomes hazardous waste; high metal recovery rate can be realized by reducing and leaching sulfur dioxide, but the overall economy of the process is poor due to high cost of the sulfur dioxide; the pyrometallurgical smelting process can realize the enrichment of valuable metals, but the smelted alloy still needs to be separated and extracted by adopting a wet method, and the pyrometallurgical smelting process needs more supporting facilities.
The scholars in China have conducted some researches on reduction leaching of organic matters of manganese oxide ores, and a patent 201810530591.1 discloses a method for treating manganese oxide ores by reduction acidolysis-leaching and iron removal at the same time; patent 201711262557.2 discloses a method for reducing and leaching manganese oxide ore by using cassava starch; patent 201711252556.8 discloses a method for reducing and leaching manganese oxide ore by using cassava dry powder and formaldehyde; patent 201811438137.X discloses a reduction leaching method of galbanum manganese oxide ore; patent 201210042706.5 discloses a reduction leaching method of manganese oxide ore; patent 201510191276.7 discloses a method for producing manganese sulfate by treating manganese oxide ore with carbonaceous reducing agent.
Manganese oxide ore organic matter reduction leaching mainly aims at manganese oxide ore, and seabed manganese ore production resources belong to complex multi-metal iron-manganese oxide ore, and are more complex compared with traditional manganese oxide ore, the difficulty of subsequent solid-liquid separation caused by the fact that a large amount of iron is leached due to the fact that only organic matter reduction leaching is adopted is difficult to avoid, and a large amount of reagent is consumed due to the fact that iron is removed from leaching liquid.
Disclosure of Invention
In order to solve the problem of high iron leaching rate in the traditional manganese oxide ore organic matter reduction leaching and realize the comprehensive utilization of the seabed manganese ore resources, a treatment method for comprehensively recovering the seabed manganese ore resources by a carbon-based reduction weak acid leaching system is provided. In order to achieve the above object, the present invention has the following technical solutions.
A method for recovering valuable metals from submarine manganese ore resources is characterized by comprising the following steps:
step (1): grinding the seafloor manganese ore to be below 200 meshes, and leaching the ground seafloor manganese ore by adopting a carbon-based reducing agent weak acid leaching system to obtain a leaching solution and leaching slag;
step (2): removing impurities from the leachate obtained in the step (1) by adopting an iron vitriol method;
and (3): precipitating the impurity-removed solution obtained in the step (2) by adopting a sulfide precipitation process to obtain an enriched sulfide and a manganese-rich solution;
and (4): carrying out oxygen pressure leaching on the enriched sulfide in the step (3), and separating leached liquid through an extraction-back extraction process to prepare a related product;
and (5): and (4) preparing electrolytic manganese or manganese dioxide from the manganese-rich solution obtained in the step (3) by adopting an electrolytic deposition process.
The carbon-based reduction weak acid leaching system disclosed by the invention is used for solving the complexity of the submarine manganese ore production resource, the carbon-based reducing agent is adopted, under the condition that the theoretical acid dosage is lower, valuable metal elements are selectively leached, leaching of a small amount of iron is inhibited or reduced, the leachate is subjected to impurity removal, and then the valuable elements in the submarine manganese ore production resource are separated and purified.
The submarine mineral resources comprise submarine ferromanganese oxidized ores such as polymetallic nodules and cobalt-rich crusts, and one or a mixture of more of other common submarine ferromanganese oxidized ores. In the invention, the solution after acid leaching is subjected to iron removal and then is vulcanized and precipitated, and the precipitate is subjected to acid leaching under oxygen pressure and then is extracted, back extracted, separated and purified, and related products are prepared.
Further, the carbon-based reducing agent in the step (1) is carbon-based organic matters such as coke, anthracite, wood chips and the like, wherein the adding amount of the reducing agent is 0.5-5: 1, preferably 1-3: 1, of the molar ratio of the carbon content to the manganese content in the minerals. The reducing leaching temperature is 50-200 deg.C, preferably 90-150 deg.C, and leaching time is 1-6 hr, preferably 2-4 hr. The leaching can be two-stage leaching, wherein the temperature of the first stage leaching is 50-100 ℃, and the leaching time is 0.5-5 hours; the second-stage leaching temperature is 100-.
Further, in the weak acid leaching system in the step (2), the acid dosage is 0.2-3 times of the theoretical acid consumption, the leaching solution-solid ratio is 1-20, the preferable acid dosage is 0.5-1 times of the theoretical acid consumption, and the leaching solution-solid ratio is 2-5.
The invention has the following beneficial technical effects: the carbon-based reducing agent is adopted to leach the submarine manganese ore resource, valuable metal elements in the submarine manganese ore resource can be recovered by a full-wet method, the cost of the carbon-based reducing agent is far lower than that of the traditional sulfur dioxide, and the leaching rate of iron can be reduced or inhibited by adopting a weak acid leaching system, so that solid-liquid separation of ore pulp is facilitated, and the subsequent iron removal cost is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for recovering nonferrous metals by a seabed manganese ore resource carbon-based reduction weak acid leaching system comprises the steps of firstly, grinding the seabed manganese ore to 200 meshes, leaching the seabed manganese ore at a solid-to-solid ratio of 1-20 at a leaching temperature of 50-200 ℃ for 1-6 hours in a one-stage or two-stage leaching mode according to the mole ratio of the carbon content of a reducing agent to the manganese content in the manganese ore of 0.5-5 times and the acid consumption of 0.2-3 times of the theoretical acid consumption, carrying out iron removal and purification on a leaching solution, carrying out vulcanization precipitation on the solution after iron removal, carrying out extraction-back extraction separation on a precipitation slag after oxidation leaching to prepare related products, and carrying out electrolysis on the solution after precipitation to prepare electrolytic manganese or manganese dioxide products.
The process of the present invention is further illustrated by the following non-limiting examples to assist understanding of the contents and advantages of the invention, but is not to be construed as limiting the scope of the invention, which is defined by the claims. Preferred embodiments of the present invention are as follows.
Example 1
100g of undersea manganese ore ground to 200 meshes is taken, 13.3% of saw dust powder is added, the mass of acid ore is 1:2, the liquid-solid ratio is 4:1, the leaching temperature is 99 ℃, the leaching time is 4 hours, the leaching rates of nickel, cobalt and copper are 96.5%, 65%, 88%, the leaching rate of manganese is 40% and the leaching rate of iron is 7%, the leached liquid is subjected to iron removal and then sulfide precipitation, electrolytic manganese is prepared from the precipitated liquid, sulfide precipitation slag is subjected to oxidation leaching, the leachate is subjected to impurity removal by P204, cobalt chloride products are prepared after cobalt extraction-back extraction by P507, and nickel sulfate is prepared from the P507 raffinate.
Example 2
100g of undersea manganese ore ground to 200 meshes is taken, 13.3% of saw dust powder is added, the mass of acid ore is 1:2, the liquid-solid ratio is 4:1, the leaching temperature is 99 ℃, the leaching time is 2 hours, the leaching rates of nickel, cobalt and copper are respectively 94.4%, 58.2%, 77.3%, 28.5% of manganese and 5.2% of iron, the leached liquid is subjected to iron removal and then sulfide precipitation, the precipitated liquid is used for preparing electrolytic manganese, the sulfide precipitation slag is subjected to oxidation leaching, the leachate is subjected to P204 impurity removal, the P507 cobalt-back extraction is used for preparing cobalt chloride products, and the P507 raffinate is used for preparing nickel sulfate.
Example 3
100g of undersea manganese ore ground to 200 meshes is taken, 13.3% of saw dust powder is added, the mass of acid ore is 1:2, the liquid-solid ratio is 4:1, the leaching temperature is 150 ℃, the leaching time is 2 hours, the leaching rates of nickel, cobalt and copper are 81.5%, 90.2%, 51.1%, 76.8% of manganese and 1.2% of iron respectively, the leached liquid is subjected to iron removal and then sulfide precipitation, the precipitated liquid is used for preparing electrolytic manganese, the sulfide precipitation slag is subjected to oxidation leaching, the leachate is subjected to P204 impurity removal, the P507 cobalt-back extraction is used for preparing cobalt chloride products, and the P507 raffinate is used for preparing nickel sulfate.
Example 4
100g of undersea manganese ore ground to 200 meshes is taken, 13.3% of saw dust powder is added, the mass of acid ore is 1:2, the liquid-solid ratio is 4:1, the leaching temperature is 150 ℃, the leaching time is 4 hours, the leaching rates of nickel, cobalt and copper are respectively 98.5%, 96.2%, 80.5%, 80.8% and 4.2% of iron, the leached solution is subjected to iron removal and then sulfide precipitation, the precipitated solution is used for preparing electrolytic manganese, the sulfide precipitation slag is subjected to oxidation leaching, the leachate is subjected to P204 impurity removal, the P507 cobalt-back extraction is used for preparing cobalt chloride products, and the P507 raffinate is used for preparing nickel sulfate.
Example 5
100g of undersea manganese ore ground to 200 meshes is taken, 13.3% of saw powder is added, the mass of acid ore is 1:2, the liquid-solid ratio is 4:1, the leaching temperature is 99 ℃, the leaching time is 2 hours, 6.6% of saw powder is added into leaching slag, the acid-ore ratio is 1:4, the liquid-solid ratio is 4:1, the leaching temperature is 150 ℃, the leaching time is 2 hours, the total leaching rates of nickel, cobalt and copper are respectively 98.5%, 97.2%, 80.1%, the leaching rate of manganese is 80.5%, the leaching rate of iron is 9.5%, the leaching solution is subjected to iron removal and then is subjected to sulfide precipitation, electrolytic manganese is prepared from the precipitation solution, the sulfide precipitation slag is subjected to oxidation leaching, the leaching solution is subjected to impurity removal by P204, the P507 cobalt extraction raffinate-back extraction is used for preparing a cobalt chloride product, and the P507 extraction is used.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A method for recovering valuable metals from submarine manganese ore resources is characterized by comprising the following steps:
step (1): grinding the seafloor manganese ore to be below 200 meshes, and leaching the ground seafloor manganese ore by adopting a carbon-based reducing agent weak acid leaching system to obtain a leaching solution and leaching slag;
step (2): removing impurities from the leachate obtained in the step (1) by adopting an iron vitriol method;
and (3): precipitating the impurity-removed solution obtained in the step (2) by adopting a sulfide precipitation process to obtain an enriched sulfide and a manganese-rich solution;
and (4): carrying out oxygen pressure leaching on the enriched sulfide in the step (3), and separating leached liquid through an extraction-back extraction process to prepare a related product;
and (5): and (4) preparing electrolytic manganese or manganese dioxide from the manganese-rich solution obtained in the step (3) by adopting an electrolytic deposition process.
2. The method according to claim 1, wherein the carbon-based reducing agent added in the step (1) is one or more selected from coke, anthracite and wood chips, and the amount of the reducing agent is controlled so that the molar ratio of carbon in the reducing agent to manganese in the seafloor manganese ore resource is 0.5-5: 1.
3. The method of claim 2, wherein the amount of reducing agent is controlled such that the molar ratio of carbon in the reducing agent to manganese in the seafloor manganese ore resource is 1-3: 1.
4. The method as claimed in claim 1 or 2, wherein the leaching temperature in the step (1) is 50-200 ℃ and the leaching time is 1-6 hours.
5. The method as claimed in claim 4, wherein the leaching temperature in the step (1) is 90-150 ℃ and the leaching time is 2-4 hours.
6. The method as claimed in claim 1, wherein the amount of acid used in the weak acid leaching system used in step (1) is 0.2-3 times the theoretical acid consumption, and the leach liquor-to-solid ratio is 1-20.
7. The method as claimed in claim 6, wherein the amount of acid used in the weak acid leaching system used in step (1) is 0.5-1 times the theoretical acid consumption, and the leach liquor-to-solid ratio is 2-5.
8. The method according to claim 1, wherein in the step (1), the carbon-based reduced weak acid leaching system is used, leaching is performed in two stages, the temperature of the first stage leaching is 50-100 ℃, and the leaching time is 0.5-5 hours; the temperature of the second-stage leaching is 100-.
9. The method as claimed in claim 8, wherein the primary leaching temperature is 80-100 ℃ and the leaching time is 2-4 hours; the temperature of the second-stage leaching is 120 ℃ and 180 ℃, and the leaching time is 1-3 hours.
CN202010242056.3A 2020-03-31 2020-03-31 Method for recovering valuable metals from submarine manganese ore resources Pending CN111304439A (en)

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CN111876586A (en) * 2020-07-29 2020-11-03 北京科技大学 Method for comprehensively recovering all elements by roasting and reducing ocean cobalt-rich crusts through biomass

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Publication number Priority date Publication date Assignee Title
CN111876586A (en) * 2020-07-29 2020-11-03 北京科技大学 Method for comprehensively recovering all elements by roasting and reducing ocean cobalt-rich crusts through biomass

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