CN112280979A - Method for enriching precious metals from multi-metal alloy material - Google Patents

Method for enriching precious metals from multi-metal alloy material Download PDF

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Publication number
CN112280979A
CN112280979A CN202011298115.5A CN202011298115A CN112280979A CN 112280979 A CN112280979 A CN 112280979A CN 202011298115 A CN202011298115 A CN 202011298115A CN 112280979 A CN112280979 A CN 112280979A
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leaching
filtering
pressure
alloy material
nickel
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CN202011298115.5A
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马磊
周通
丁才生
李金良
李全
闫刚刚
李改变
杜建喜
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08Sulfuric acid, other sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet 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
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • 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

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for enriching precious metals from a multi-metal alloy material, which comprises the following steps: dissolving the multi-metal alloy material and the pre-slurrying solution, adding sulfuric acid for leaching, reacting for 3-4h, controlling the end point pH value to be 0.5, and then feeding into a pressure kettle for pressure oxygen leaching. In the reaction process, the temperature and pressure of the kettle are controlled, after reaction is carried out for 5-7 hours, the elements such as nickel, copper and the like in the multi-metal alloy material are completely leached, and the noble metals such as platinum, palladium, gold, silver and the like are inhibited in slag. And after pressure leaching, performing liquid-solid separation on the ore pulp by a thickener, filtering the supernatant by a filter press, taking the filtrate containing the elements such as nickel, copper and the like as a nickel supplementing raw material of an electrolytic system for producing electrolytic nickel, and enriching the precious metals by using the filter residue containing the precious metal elements. And filtering the underflow by a filter press, taking the filtrate as a pulping front liquid for pulping, and enriching the filter residue with noble metal elements. The method has the advantages of short flow, simple subsequent impurity removal means and high precious metal enrichment multiple.

Description

Method for enriching precious metals from multi-metal alloy material
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for enriching precious metals from a multi-metal alloy material.
Background
The multi-metal alloy material is used as an intermediate product in the flotation process, the content of nickel and copper in the raw material reaches 70 percent, and the content of platinum, palladium, gold and silver reaches 500 g/t. After the traditional pyrogenic process is adopted for treatment, metals such as copper, nickel and the like are difficult to remove, and precious metals can enter smoke dust to cause valuable metal loss. Therefore, the direct and effective process technology is adopted to separate nickel and copper from the precious metals, the produced nickel sulfate solution rich in nickel and copper ions is used as a raw material of a nickel electrolysis system to produce electrolytic nickel, and leaching slag rich in the precious metals is used for precious metal extraction, so that the method has great significance for production practice.
Patent document No. 201510032194.8 discloses a method for collecting precious metals from a multi-metal alloy material, which comprises mixing the multi-metal alloy material with ammonium salt, placing the mixture in a high-pressure reaction kettle to perform pressure leaching of main metals copper and nickel, after leaching, filtering and washing to respectively obtain leachate and ammonia leaching residue, wherein the leachate is used as a copper-nickel recovery raw material; adding nitric acid into the ammonia leaching residue to leach in a closed iron reaction kettle, leaching for a period of time, heating, concentrating and evaporating residual nitric acid, stopping heating when the ammonia leaching residue is concentrated to be viscous, simultaneously adding water for dilution, filtering and washing to respectively obtain leachate and acid leaching residue, wherein the leachate contains lead and the like as raw materials for recovering lead, and the slag contains antimony, gold, platinum, palladium and the like; and (3) leaching to remove antimony by adopting pressurized alkali, filtering and washing to obtain an alkali leaching solution and alkali leaching residues, wherein the precious metals enter the residues and are effectively enriched. However, the leaching process in the process is simple, impurities in the materials are all added into the solution, the subsequent impurity removal means is complex, and the ammonia leaching is adopted, so that the problems of long process flow of ammonia recovery process and large equipment investment exist.
The patent document of application No. 201510036256.2 discloses a method for dissolving precious metals in multi-metal alloy by nitric acid, which comprises mixing multi-metal alloy material with nitric acid, leaching in titanium reactor, heating to 85-95 deg.C, keeping for a while, stopping heating when concentrating to viscous state, adding water with weight ratio of 2-6 times of material to dilute, reducing acidity, increasing pH value of terminal point to about 1-3, and facilitating filtration and separation of metals such as main metals lead, nickel and copper and precious metals; filtering and washing to respectively obtain leachate and leaching residue, wherein the leachate contains lead, copper and the like and is used as a raw material for recovering lead and copper, and the leaching residue contains bismuth, antimony, gold, silver, platinum, palladium and the like; and (3) leaching to remove antimony by adopting pressurized alkali, filtering and washing to obtain alkali leaching solution and alkali leaching residue, wherein the precious metal enters the residue, and the precious metal is effectively enriched. However, the process flow is long and the subsequent impurity removal means after nitric acid leaching is very complicated.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for enriching precious metals from a multi-metal alloy material, which has the advantages of short flow, simple subsequent impurity removal means and better environmental protection and economy.
In order to solve the problems, the method for enriching the precious metal from the multi-metal alloy material comprises the following steps:
(1) pulping and dissolving the multi-metal alloy material and the pulping pre-liquid in a pulping tank, and then adding sulfuric acid to carry out leaching operation; the reaction time is 3-4h, and the pH value at the end of leaching is 0.5;
(2) pumping the leaching solution obtained in the step (1) into a pressure kettle for pressure oxygen leaching; the pressure of the pressure kettle is 0.6-0.8MPa, the temperature of the pressure kettle is 120-;
(3) and (3) decompressing and cooling the pressurized leachate obtained in the step (2) through a flash tank, allowing the leachate to enter a thickener for gravity settling, and allowing filter residue obtained after filtering the underflow of the thickener and filter residue obtained after filtering the supernatant to enter a precious metal system for extraction.
Preferably, the step (3) further comprises: and filtering liquid obtained after filtering the underflow of the thickener is used for preparing the liquid before slurrying, and filtering liquid obtained after filtering the supernatant of the thickener is externally attached to a nickel electrolysis system.
Preferably, in the step (1), the sulfuric acid slowly and uniformly enters the slurrying tank within 3 hours for slurry leaching operation, and the reaction is continued for 1 hour after the addition of the sulfuric acid is finished.
Preferably, in the step (2), the reaction temperature is ensured to be between 120 ℃ and 160 ℃ by controlling the pressure of the autoclave.
Compared with the prior art, the invention has the following advantages:
1. in the invention, the leaching agent adopts sulfuric acid and adopts a sulfuric acid leaching (direct slurrying) and pressurized oxygen leaching (one-stage pressurized leaching) process to treat the multi-metal alloy material, so that elements such as nickel, copper and the like in the multi-metal alloy material are completely leached, and precious metals such as platinum, palladium, gold, silver and the like are inhibited in slag.
2. The invention adopts single-tank operation, obtains high nickel-copper leaching rate and enriches noble metals. The invention adopts the original equipment to operate, the process is mature, the post operation is simple, and the post labor intensity is not increased; the method is simple to operate and has good effect in the industrial application process.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a process flow diagram provided in an embodiment of the present invention.
Detailed Description
Example 1
Referring to the flow chart shown in FIG. 1, 1t of polymetallic alloy material and a slurrying front liquid (10-20 g/L of nickel and 5-15g/L of copper; the liquid-solid ratio of the front liquid to the material is 10: 1; the same applies hereinafter) are dissolved in a slurrying tank, 0.86t of sulfuric acid is slowly added into the slurrying tank within 3 hours (the ratio of the sulfuric acid to the material is 0.86: 1; the same applies hereinafter), the reaction is carried out for 1 hour after the addition of the sulfuric acid is finished, and the leaching end point pH value reaches 0.5, and then the pressure leaching process is carried out.
After slurrying and leaching the sulfuric acid, pumping the ore pulp into a pressure kettle through a pressure pump for pressure leaching, wherein the kettle pressure is 0.6MPa, the kettle temperature is 140 ℃, and the reaction time is 5-7h, and then carrying out liquid-solid separation through a thickener.
Filtering the bottom flow of the thickener by a filter press, diluting the filtrate to be used as a pre-slurrying solution for slurrying, and externally attaching filter residues to a precious metal system for extraction. After the supernatant fluid of the thickener is filtered by a filter press, the filtrate contains 100g/L of nickel and 20g/L of copper, and the filtrate is used as an external solution to enter an electrolysis process to produce an electrolytic nickel product. The filtered filter residue is rich in 3000g/t of noble metal, the noble metal enrichment times of the filter residue reach 4-6 times, and the filter residue is used as a raw material to enter a noble metal smelting process.
Example 2
Dissolving 2t of multi-metal alloy material and the liquid before slurrying in a slurrying tank, slowly adding 1.72t of sulfuric acid into the slurrying tank within 3 hours, reacting for 1 hour after the sulfuric acid is added, and returning to the pressure leaching process after the pH value at the leaching end point reaches 0.5.
And (3) after leaching, the ore pulp enters a pressure kettle for pressure leaching, the kettle pressure is 0.6MPa, the kettle temperature is 150 ℃, and after reaction time is 5-7h, liquid-solid separation is carried out by a thickener.
Filtering the bottom flow of the thickener by a filter press, diluting the filtrate to be used as a pre-slurrying solution for slurrying, and externally attaching filter residues to a precious metal system for extraction. After the supernatant of the thickener is filtered by a filter press, the filtrate contains 103.56g/L of nickel and 19.32g/L of copper, and the filtrate is used as an external solution to enter an electrolysis process to produce an electrolytic nickel product. The filtered filter residue is rich in 2800g/t of noble metal and is used as a raw material to enter a noble metal smelting process.
The technical solution provided by the present invention is described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (4)

1. A method of enriching a precious metal from a multi-metal alloy material, the method comprising:
(1) pulping and dissolving the multi-metal alloy material and the pulping pre-liquid in a pulping tank, and then adding sulfuric acid to carry out leaching operation; the reaction time is 3-4h, and the pH value at the end of leaching is 0.5;
(2) pumping the leaching solution obtained in the step (1) into a pressure kettle for pressure oxygen leaching; the pressure of the pressure kettle is 0.6-0.8MPa, the temperature of the pressure kettle is 120-;
(3) and (3) decompressing and cooling the pressurized leachate obtained in the step (2) through a flash tank, allowing the leachate to enter a thickener for gravity settling, and allowing filter residue obtained after filtering the underflow of the thickener and filter residue obtained after filtering the supernatant to enter a precious metal system for extraction.
2. The method of claim 1, wherein step (3) further comprises: and filtering liquid obtained after filtering the underflow of the thickener is used for preparing the liquid before slurrying, and filtering liquid obtained after filtering the supernatant of the thickener is externally attached to a nickel electrolysis system.
3. The method as claimed in claim 1, wherein in the step (1), the sulfuric acid is slowly and uniformly fed into the slurrying tank for slurry leaching within 3 hours, and the reaction is continued for 1 hour after the addition of the sulfuric acid is finished.
4. The method as claimed in claim 1, wherein in the step (2), the reaction temperature is ensured to be between 120 ℃ and 160 ℃ by controlling the pressure of the autoclave.
CN202011298115.5A 2020-11-19 2020-11-19 Method for enriching precious metals from multi-metal alloy material Pending CN112280979A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3767760A (en) * 1971-12-13 1973-10-23 Falconbridge Nickel Mines Ltd Process for recovery of precious metals from copper containing materials
GB1371086A (en) * 1971-01-22 1974-10-23 Sherritt Gordon Mines Ltd Acid leaching process for treating high grade nickel-copper mattes
CN100999784A (en) * 2006-12-29 2007-07-18 金川集团有限公司 Process of recovering noble metal from hydroxylating metallurgy slag
CN101195857A (en) * 2007-12-20 2008-06-11 金川集团有限公司 Solvent extraction method for acquiring alloy with magnetic separation copper bessemer matte
CN101260463A (en) * 2007-12-20 2008-09-10 金川集团有限公司 Leaching method for alloy material obtained from magnetic copper-nickel concentrate
CN102358919A (en) * 2011-11-02 2012-02-22 长沙矿冶研究院有限责任公司 Method for extracting valuable metal from submarine metallic ore
CN110241310A (en) * 2019-06-18 2019-09-17 深圳市坤鹏冶金工程技术有限公司 A kind of method of high-speed rail high-copper nickel-containing material selectivity oxygen leaching enriching noble metals

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1371086A (en) * 1971-01-22 1974-10-23 Sherritt Gordon Mines Ltd Acid leaching process for treating high grade nickel-copper mattes
US3767760A (en) * 1971-12-13 1973-10-23 Falconbridge Nickel Mines Ltd Process for recovery of precious metals from copper containing materials
CN100999784A (en) * 2006-12-29 2007-07-18 金川集团有限公司 Process of recovering noble metal from hydroxylating metallurgy slag
CN101195857A (en) * 2007-12-20 2008-06-11 金川集团有限公司 Solvent extraction method for acquiring alloy with magnetic separation copper bessemer matte
CN101260463A (en) * 2007-12-20 2008-09-10 金川集团有限公司 Leaching method for alloy material obtained from magnetic copper-nickel concentrate
CN102358919A (en) * 2011-11-02 2012-02-22 长沙矿冶研究院有限责任公司 Method for extracting valuable metal from submarine metallic ore
CN110241310A (en) * 2019-06-18 2019-09-17 深圳市坤鹏冶金工程技术有限公司 A kind of method of high-speed rail high-copper nickel-containing material selectivity oxygen leaching enriching noble metals

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