CN107326179B - Method for recovering polymetallic from complex antimony-containing gold ore - Google Patents

Method for recovering polymetallic from complex antimony-containing gold ore Download PDF

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CN107326179B
CN107326179B CN201710369538.3A CN201710369538A CN107326179B CN 107326179 B CN107326179 B CN 107326179B CN 201710369538 A CN201710369538 A CN 201710369538A CN 107326179 B CN107326179 B CN 107326179B
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leaching
antimony
gold
filtrate
temperature
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CN107326179A (en
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鲁兴武
朱来东
余江鸿
李俞良
陈一博
程亮
易超
马爱军
陈文波
张恩玉
曹桂银
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Northwest Research Institute of Mining and Metallurgy
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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
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • 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
    • 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
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • 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
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/02—Obtaining antimony
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
    • 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

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

Abstract

The invention discloses a method for recovering polymetallic from complex antimony-containing gold ore, which comprises the steps of dissolving antimony-containing gold concentrate or tailings by using sodium sulfide and caustic soda flakes, introducing steam and oxygen into a leaching tank to dissolve antimony in the ore into leaching solution, filtering, performing electrodeposition on the leaching solution in an electrolysis process, separating antimony out in a cathode plate to obtain crude antimony recovered antimony, performing low-temperature crystallization on the solution after antimony recovery to remove sodium sulfide in a regeneration process to obtain sodium sulfide nonahydrate crystals, refining leaching residues by ball milling, oxidizing and leaching by using high-temperature air, obtaining gold-loaded carbon from the leaching solution by using a carbon slurry method, wherein the total recovery rate of antimony and gold is more than 95%. The whole technological process has strong reliability, no secondary pollution, reduced production cost and environment-friendly and clean production.

Description

Method for recovering polymetallic from complex antimony-containing gold ore
Technical Field
The invention belongs to the field of hydrometallurgy, and particularly relates to a comprehensive utilization technology for efficiently recovering multiple metals from complex antimony-containing gold ores.
Background
At present, China has a large amount of antimony-containing gold ores, but in the production process of gold smelting enterprises, antimony is a harmful element, and the element affects the product quality, the leaching index and the recovery rate of precious metals Au and Ag. Along with the shortage of high-quality gold ore resources and the low industrial market, the efficient extraction of complex refractory gold ores becomes the key for increasing profits in the gold smelting processing industry at present. The existing comprehensive utilization process of the antimony-containing gold ore has certain process or environmental-protection defects no matter the fire method or the wet method or the combination of the fire method and the wet method.
The method has the advantages of high-efficiency comprehensive utilization of valuable metals in the antimony-containing gold ores. Related researchers put forward some processing methods, and a patent "a process for separating antimony and gold while smelting antimony" (CN 104152721B) treats materials as high-antimony concentrate, has relatively high grade and almost only two elements of antimony and gold, needs a pyrogenic process, and has high energy consumption; the patent "a new technology of recovering antimony in antimony-containing gold concentrate" (CN 104831315A), only recovered antimony, and adopt cyanidation technology to extract noble metal, apt to produce the secondary pollution, the antimony sulfide value produced in the waste water treatment process is not high; therefore, there is a need to develop an environmentally friendly method for efficient separation and integrated recovery of antimony-containing gold concentrates.
Disclosure of Invention
The invention aims to provide a method for recovering polymetallic from complex antimony-containing gold ores, which has the characteristics of effective systematic recovery of valuable metals in complex materials, clean and environment-friendly process, easy realization of industrial production and the like.
The invention is realized by the following scheme, which comprises the following steps: a method for recovering polymetallic from complex gold-bearing antimony ores, comprising the steps of:
1) leaching: leaching the antimony-containing gold ore powder with an alkali solution, and dissolving the antimony-containing gold ore powder with the alkali solutionThe concentration of the liquid or the circulating alkali liquor is 10-35%, steam is introduced to heat and control the temperature to 70-90 ℃, the leaching reaction time is 1-3 hours, the mass ratio of the alkali liquor to the antimony-containing gold concentrate ore powder is 0.5-3, oxygen or air is introduced in the leaching process, and the flow of the oxygen or the air is 0.5-2m3The leaching is carried out and then the filtration is carried out, the filtrate is sent to the accumulation process, and the filter residue is sent to the gold extraction process;
2) electrodeposition: step 1), heating the filtrate obtained by leaching to 40-50 ℃, transferring the filtrate into an electrolytic bath for electrodeposition, separating out antimony on a cathode steel plate, and sending waste electrolyte generated by electrodeposition to a crystallization process;
3) gold extraction: ball milling and refining the filter residue obtained in the step 1), wherein the grinding fineness is-325 meshes and accounts for 85-95%, delivering the filter residue to a leaching tank for leaching, and controlling the air flow amount to be 0.06-0.2m3The temperature is 30-50 ℃, the time is 6-10d, the gold-loaded carbon is obtained by filtering after leaching, the filtrate after filtering is processed by a carbon slurry method, and the leached residue is temporarily stored as tailings;
4) and (3) crystallization: crystallizing the waste electrolyte obtained in the step 2) at low temperature, controlling the temperature to be 15-18 ℃ to obtain sodium sulfide nonahydrate, and returning the mother liquor to the leaching process.
It is preferable that: the gold leaching reagent for leaching in the leaching tank in the step 3) is a mixture of thiourea and a cicada agent, the mass concentration of the gold leaching agent is 5-25%, and the weight percentage of thiourea is as follows: the mass ratio of the cicada slough agent is 0.3-0.9: 1.
The invention has the beneficial effects that: by utilizing the selective leaching and high-efficiency enrichment process, valuable metals (antimony, gold) and sulfur (sodium sulfide nonahydrate) in the antimony-containing gold concentrate are efficiently recovered and comprehensively utilized, the economic benefit of enterprises is reflected, the environmental protection problem is solved, the reliability of the whole process is high, secondary pollution is avoided, the production cost is reduced, and the environment-friendly clean production is realized.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention is illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
The invention contains Sb20-50%, Au30-200g/t, S20-30%.
Example 1
The antimony-containing gold concentrate comprises Sb23.5%, Au65g/t and S21.5%.
And taking 2t of antimony-containing gold concentrate.
1) Leaching: leaching the antimony-containing gold concentrate ore powder by using 10% alkali solution (prepared by mixing sodium sulfide and caustic soda flakes), introducing steam, heating to control the temperature to be 75 ℃, performing leaching reaction for 1h, wherein the mass ratio of the alkali solution to the antimony-containing gold concentrate ore powder is 0.5, introducing oxygen or air in the leaching process, and the flow of the oxygen or air is 0.5m3The leaching is carried out and then the filtration is carried out, the filtrate is sent to the accumulation process, and the filter residue is sent to the gold extraction process;
2) electrodeposition: heating the filtrate obtained in the step 1) to about 40 ℃, transferring the filtrate into an electrolytic bath for electrodeposition, separating out antimony on a cathode steel plate, and sending waste electrolyte generated by electrodeposition to a crystallization process;
3) gold extraction: ball-milling and refining the filter residue obtained in the step 1), wherein the grinding fineness is-325 meshes and accounts for 85%, then feeding the filter residue into a leaching tank for leaching, and controlling the air flow to be 0.06m3At the temperature of 30 ℃ for 6d, leaching, filtering, obtaining gold-loaded carbon by a carbon slurry method from a filtered solution, and temporarily storing leaching residues as tailings;
4) and (3) crystallization: crystallizing the waste electrolyte obtained in the step 2) at a low temperature, controlling the temperature to be 15 ℃ to obtain sodium sulfide nonahydrate, and returning the mother liquor to the leaching process.
Wherein the mass concentration of the gold leaching agent for leaching in the leaching tank in the step 3) is 5 percent, and the mass concentration of thiourea is as follows: the mass ratio of the cicada slough agent is 0.3: 1.
The calculated overall yield was: 95.7 percent of antimony, 95.2 percent of gold and 81.7 percent of sulfur.
Example 2
The antimony-containing gold concentrate comprises Sb35.5%, Au35g/t and S28.5%.
And taking 2t of antimony-containing gold concentrate.
1) Leaching: leaching the antimony-containing gold concentrate ore powder by using 35% sodium hydroxide solution, introducing steam, heating to control the temperature to be 90 ℃, leaching for 2.5h, wherein the mass ratio of the alkali solution to the antimony-containing gold concentrate ore powder is 2, and introducing oxygen or air in the leaching process, wherein the flow of the oxygen or air is 1.5m3Min, filtering after leaching, and delivering filtrate to electrodepositionSequentially, the filter residue is sent to a gold extraction process;
2) electrodeposition: heating the filtrate obtained in the step 1) to about 50 ℃, transferring the filtrate into an electrolytic bath for electrodeposition, separating out antimony on a cathode steel plate, and sending waste electrolyte generated by electrodeposition to a crystallization process;
3) gold extraction: ball-milling and refining the filter residue obtained in the step 1), wherein the milling fineness is-325 meshes and accounts for 90%, then feeding the filter residue into a leaching tank for leaching, and controlling the air flow to be 0.1m3At the temperature of 40 ℃ for 8d, leaching, filtering, obtaining gold-loaded carbon by a carbon slurry method from a filtered solution, and temporarily storing leaching residues as tailings;
4) and (3) crystallization: crystallizing the waste electrolyte obtained in the step 2) at a low temperature, controlling the temperature to be 18 ℃ to obtain sodium sulfide nonahydrate, and returning the mother liquor to the leaching process.
Wherein the mass concentration of the gold leaching agent for leaching in the leaching tank in the step 3) is 15 percent, and the mass concentration of thiourea is as follows: the mass ratio of the cicada slough to the cicada slough is 0.6: 1.
The calculated overall yield was: 94.2 percent of antimony, 96.5 percent of gold and 76.6 percent of sulfur.
Example 3
The antimony-containing gold concentrate comprises Sb42.6%, Au185g/t and S16.5%.
And taking 2t of antimony-containing gold concentrate.
1) Leaching: leaching the antimony-containing gold concentrate ore powder by using 20% circulating alkali liquor, introducing steam, heating to control the temperature to be 70 ℃, leaching for 3 hours, wherein the mass ratio of the alkali liquor to the antimony-containing gold concentrate ore powder is 3, and oxygen or air is introduced in the leaching process, wherein the flow of the oxygen or air is 2m3The leaching is carried out and then the filtration is carried out, the filtrate is sent to the accumulation process, and the filter residue is sent to the gold extraction process;
2) electrodeposition: heating the filtrate obtained in the step 1) to about 45 ℃, transferring the filtrate into an electrolytic bath for electrodeposition, separating out antimony on a cathode steel plate, and sending waste electrolyte generated by electrodeposition to a crystallization process;
3) gold extraction: ball-milling and refining the filter residue obtained in the step 1), wherein the milling fineness is-325 meshes and accounts for 95%, then feeding the filter residue into a leaching tank for leaching, and controlling the air flow to be 0.2m3At the temperature of 50 ℃ for 10d, leaching and filtering, wherein gold-loaded carbon is obtained from a filtered solution by a carbon slurry method, and leaching residues are temporarily stored as tailings;
4) and (3) crystallization: crystallizing the waste electrolyte obtained in the step 2) at a low temperature, controlling the temperature to be 18 ℃ to obtain sodium sulfide nonahydrate, and returning the mother liquor to the leaching process.
Wherein the mass concentration of the gold leaching agent for leaching in the leaching tank in the step 3) is 25 percent, and the mass concentration of thiourea is as follows: the mass ratio of the cicada slough agent is 0.9: 1.
The calculated overall yield was: 97.5 percent of antimony, 95.5 percent of gold and 85.5 percent of sulfur.

Claims (2)

1. A method for recovering polymetallic from complex gold ores containing antimony is characterized by comprising the following steps: the method comprises the following steps:
1) leaching: leaching the antimony-containing gold concentrate ore powder by using an alkali solution, wherein the concentration of the alkali solution is 10-35%, introducing steam, heating, controlling the temperature to be 70-90 ℃, and performing leaching reaction for 1-3 hours, the mass ratio of the alkali solution to the antimony-containing gold concentrate ore powder is 0.5-3, introducing oxygen or air in the leaching process, and the flow of the oxygen or air is 0.5-2m3The leaching is carried out and then the filtration is carried out, the filtrate is sent to the accumulation process, and the filter residue is sent to the gold extraction process;
2) electrodeposition: step 1), heating the filtrate obtained by leaching to 40-50 ℃, transferring the filtrate into an electrolytic bath for electrodeposition, separating out antimony on a cathode steel plate, and sending waste electrolyte generated by electrodeposition to a crystallization process;
3) gold extraction: ball milling and refining the filter residue obtained in the step 1), wherein the grinding fineness is-325 meshes and accounts for 85-95%, delivering the filter residue to a leaching tank for leaching, and controlling the air flow amount to be 0.06-0.2m3The temperature is 30-50 ℃, the time is 6-10d, the gold-loaded carbon is obtained by filtering after leaching, the filtrate after filtering is processed by a carbon slurry method, and the leached residue is temporarily stored as tailings;
4) and (3) crystallization: crystallizing the waste electrolyte obtained in the step 2) at low temperature, controlling the temperature to be 15-18 ℃ to obtain sodium sulfide nonahydrate, and returning the mother liquor to the leaching process.
2. The method for recovering polymetallic from complex gold ores containing antimony according to claim 1, wherein: the gold leaching reagent for leaching in the leaching tank in the step 3) is a mixture of thiourea and a cicada agent, the mass concentration of the gold leaching reagent is 5-25%, and the weight ratio of thiourea: the mass ratio of the cicada slough agent is 0.3-0.9: 1.
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CN109881004B (en) * 2019-04-01 2021-01-29 山东恒邦冶炼股份有限公司 Method for reducing gold grade in crude antimony leaching solution
CN111455181A (en) * 2020-04-20 2020-07-28 西部矿业股份有限公司 Efficient and low-cost cleaning process for recovering precious metals from high-sulfur-content hot filter residues
US11319613B2 (en) 2020-08-18 2022-05-03 Enviro Metals, LLC Metal refinement
CN113354164B (en) * 2021-08-10 2021-11-02 北京矿冶研究总院 Comprehensive treatment method of acid wet antimony smelting solution

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CN101338370A (en) * 2008-08-14 2009-01-07 张学贤 Gold-extracting process by thiourea carbon-in-pulp method
CN103276206A (en) * 2013-06-09 2013-09-04 中南大学 Method for leaching gold in alkaline thiourea system efficiently and stably
CN103937977A (en) * 2014-04-28 2014-07-23 新疆星塔矿业有限公司 Comprehensive recovery process of arsenic/antimony-containing gold concentrate
CN104862484A (en) * 2015-05-15 2015-08-26 西北矿冶研究院 Method for extracting antimony from lead anode slime
CN105063354A (en) * 2015-08-18 2015-11-18 北京矿冶研究总院 Cascade recovery method of arsenic-containing and antimony-containing refractory gold ore

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JP2003221628A (en) * 2002-01-31 2003-08-08 Japan Science & Technology Corp Method for extracting gold

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101338370A (en) * 2008-08-14 2009-01-07 张学贤 Gold-extracting process by thiourea carbon-in-pulp method
CN103276206A (en) * 2013-06-09 2013-09-04 中南大学 Method for leaching gold in alkaline thiourea system efficiently and stably
CN103937977A (en) * 2014-04-28 2014-07-23 新疆星塔矿业有限公司 Comprehensive recovery process of arsenic/antimony-containing gold concentrate
CN104862484A (en) * 2015-05-15 2015-08-26 西北矿冶研究院 Method for extracting antimony from lead anode slime
CN105063354A (en) * 2015-08-18 2015-11-18 北京矿冶研究总院 Cascade recovery method of arsenic-containing and antimony-containing refractory gold ore

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