CN105063351A - Method for selectively separating copper and rhenium from complex molybdenum concentrate - Google Patents
Method for selectively separating copper and rhenium from complex molybdenum concentrate Download PDFInfo
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- CN105063351A CN105063351A CN201510609782.3A CN201510609782A CN105063351A CN 105063351 A CN105063351 A CN 105063351A CN 201510609782 A CN201510609782 A CN 201510609782A CN 105063351 A CN105063351 A CN 105063351A
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Abstract
A method for selectively separating copper and rhenium from complex or low-grade molybdenum concentrate is characterized in that the complex or low-grade molybdenum concentrate containing copper and rhenium is subjected to normal-pressure activation leaching treatment, oxidizing gas is introduced under a mixed acid system, the leaching pH is less than 2, the temperature is 80-100 ℃, the liquid-solid ratio is 2-10: 1, and the leaching time is 0.5-5 h, so that the leaching rate of copper and rhenium can reach more than 95%, the oxidation dissolution rate of molybdenum is lower than 5%, and the grade of the molybdenum concentrate can be improved to more than 47%. And recovering copper, rhenium and molybdenum from the leachate by a step-by-step extraction method to finally produce ammonium rhenate, cathode copper and ammonium molybdate products. The dual targets of improving the molybdenum grade and recovering the copper-rhenium valuable metal are realized.
Description
Technical field
The present invention relates to the field of hydrometallurgy of copper molybdenum rhenium, specifically, relate to a kind of method of selective separation copper rhenium from complicated concentrated molybdenum ore.
Background technology
Molybdenum is a kind of very important rare metal, because it has good heat conduction, conduction, the characteristic such as high temperature resistant, wear-resisting, corrosion-resistant, is widely used in the fields such as iron and steel, chemical industry, electronics, aerospace, biological medicine, agricultural and national defense construction.
Along with molybdenum in China output and consumption increase, the exploitation grade of molybdenum is more and more lower, mineral complexity is more and more higher, since particularly primary molybdenum ore in 2007 is classified as restricted exploitation class Mineral resources by country, the exploitation of low-grade complex association molybdenum ore become focus, there is the ore deposit of the metal associations such as a large amount of molybdenum, copper, rhenium, lead, zinc in recent years, as Tong Mulai ore deposit, Dexing, the plumbous zinc associated minerals of Chi Hong Inner Mongol, Yunnan molybdenum, Chinese gold industry Inner Mongol copper molybdenum rhenium associated minerals, Zhong Lv Peru Toromocho copper-molybdenum etc.For this type of resource, belonged to many metals associations such as molybdenum copper rhenium by the concentrated molybdenum ore of ore dressing output, one is the grade affecting molybdenum in concentrated molybdenum ore, and time for sale in addition, copper rhenium is not only without charge, and even copper is too high can impose a fine in addition.Metals such as selectively removing copper rhenium and do not change the structure of molybdenum glance, thus realize improving molybdenum grade and the double goal reclaiming copper rhenium valuable metal, to Molybdenum Mine, there is good economic benefit.
Summary of the invention
The object of the invention is to, a kind of method of selective separation copper rhenium from complicated concentrated molybdenum ore is provided, realize improving molybdenum grade and the double goal reclaiming the valuable metals such as copper rhenium.The object of the invention is to be achieved through the following technical solutions.
A method for selective separation copper rhenium from complicated concentrated molybdenum ore, its process is followed successively by:
(1) by described concentrated molybdenum ore fine grinding;
(2) the complicated concentrated molybdenum ore after step (1) fine grinding is carried out atmospheric activating leaching, under mixed acid system, pass into oxidizing gas, at leaching pH<2, temperature 70 ~ 100 DEG C, liquid-solid ratio 2 ~ 15:1, under the condition of extraction time 0.5 ~ 6h, selective dissolution chalcopyrite and sulfuration rhenium, obtain the leach liquor of the valuable metal such as cupric, rhenium and contain molybdenum glance leached mud, realize being separated of molybdenum and copper rhenium, copper, rhenium enter leach liquor, and molybdenum is enrichment in leached mud;
(3) leach liquor in step (2) adopts stepwise solvent extraction method to reclaim rhenium, molybdenum and copper, and first adopt exclusive extraction agent extracting copper, strip liquor produces cathode copper by electrodeposition; Liquid Solvent Extraction of Rhenium after extraction copper, rehenic acid ammonium is produced in back extraction; Raffinate extraction molybdenum after extraction rhenium, ammonium molybdate is produced in back extraction;
(4) leached mud in step (2) becomes the higher concentrated molybdenum ore of purity after washing, and molybdenum grade is greater than 47%, for selling or producing molybdenum product.
Further, described complicated concentrated molybdenum ore, be rhenium-containing, many metals of copper, Low Grade Molybdenum Concentrates, molybdenum grade is 5 ~ 45%.
Further, oxidizing gas described in step (2) is one or more in chlorine, oxygen, air.
Further, in step (2), mixed acid system is two kinds and above formation in sulfuric acid, nitric acid, hydrochloric acid, organic acid.
Further, pH<2 is leached described in step (2).
Further, described in step (2), extraction temperature is 80 ~ 100 DEG C.
Further, leaching liquid-solid ratio described in step (2) is 2 ~ 10:1.
Further, described in step (2), extraction time is 0.5 ~ 5h.
Further, in step (2), the leaching yield of copper is more than 95%, and the leaching yield of rhenium is more than 95%.
Further, the molybdenum degree of oxidation in step (2) is lower, and oxidation dissolution rate is below 5%.In slag molybdenum still with molybdenum glance form exist and structure do not change, become the qualified concentrated molybdenum ore that purity is higher after washing, molybdenum content more than 47%.
Further, in step (3), the extraction agent of molybdenum rhenium is tertiary amine extractant, and load organic phase adopts ammoniacal liquor back extraction, and strip liquor is for the production of rehenic acid ammonium and ammonium molybdate.
Further, in step (3), the extraction agent of copper comprises: hydroxyl-ketoxime extraction agent, quinoline extraction agent, tertiary amines extraction agent etc., load organic phase is after washing-back extraction, and strip liquor is for the production of cathode copper.
The per-cent related in the present invention, ratio, unless otherwise indicated, be weight ratio.
Method of the present invention, by adopting atmospheric activating leaching-out technique, the chalcopyrite in selective dissolution concentrated molybdenum ore and sulfuration rhenium, achieves effectively being separated of molybdenum and copper rhenium, has both reclaimed the valuable metal such as copper, rhenium, improved again the grade of concentrated molybdenum ore.Leached mud becomes the higher qualified concentrated molybdenum ore of purity after washing, and molybdenum grade can reach more than 47%.Leach liquor contains the valuable metal such as copper, rhenium, adopts extraction process to realize copper, rhenium and molybdenum stepwise solvent extraction, produces cathode copper, rehenic acid ammonium and ammonium molybdate qualified product after back extraction.Method technical process of the present invention is simple, and production operation is convenient, is easy to realize industrialization.
Embodiment
A method for selective separation copper rhenium from complicated concentrated molybdenum ore, its process is followed successively by: (1) is by described complicated concentrated molybdenum ore fine grinding; (2) by the complicated concentrated molybdenum ore after fine grinding mixed acid system and pass into oxidizing gas condition under, carry out atmospheric activating leaching, control leach pH<2, temperature is 80 ~ 100 DEG C, and liquid-solid ratio is 2 ~ 10:1, and extraction time is 0.5 ~ 5h.Obtain the leach liquor of the valuable metal such as cupric, rhenium and contain molybdenum glance leached mud, analyzing each constituent content in slag and calculate leaching yield.(3) leach liquor adopts stepwise solvent extraction method to reclaim rhenium, molybdenum and copper, first extracting copper, and strip liquor produces cathode copper by electrodeposition; Liquid Solvent Extraction of Rhenium after extraction copper, rehenic acid ammonium is produced in back extraction; Raffinate extraction molybdenum after extraction rhenium, ammonium molybdate is produced in back extraction; (4) after leached mud washing for selling or producing molybdenum product.
Be further described technique of the present invention with following nonlimiting examples, to contribute to understanding the present invention and advantage thereof, and not as limiting the scope of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
Get the complicated concentrated molybdenum ore of 200g, containing molybdenum 39%, copper 5%, rhenium 400g/t.Test conditions: 95 DEG C, liquid-solid ratio 5:1, pH value 1.5, extraction time 4h, oxygen flow 15m
3/ h.
Test-results: copper, rhenium, molybdenum leaching rate: 95.6%, 95.02%, 4.1%.Leached mud main component: molybdenum 47%, copper 0.21%, rhenium 24g/t.Leach liquor composition: Cu7.82g/L, Mo3.31g/L, Re0.068g/L.
Embodiment 2
Get the complicated concentrated molybdenum ore of 200g, containing molybdenum 40%, copper 3%, rhenium 300g/t.Test conditions: 90 DEG C, liquid-solid ratio 4:1, pH value 1, extraction time 3h, oxygen flow 20m
3/ h.
Test-results: copper, rhenium, molybdenum leaching rate: 96.8%, 95.2%, 4.9%.Leached mud main component: molybdenum 48%, copper 0.11%, rhenium 20g/t.Leach liquor composition: Cu7.6g/L, Mo6.1g/L, Re0.071g/L.
Embodiment 3
Get the complicated concentrated molybdenum ore of 200g, containing molybdenum 35%, copper 7%, rhenium 350g/t.Test conditions: 80 DEG C, liquid-solid ratio 6:1, pH value 1, extraction time 5h, oxygen flow 20m
3/ h.
Test-results: copper, rhenium, molybdenum leaching rate: 93.3%, 95.1%, 4.5%.Leached mud main component: molybdenum 45%, copper 0.25%, rhenium 21g/t.Leach liquor composition: Cu11.3g/L, Mo4.1g/L, Re0.078g/L.
Claims (9)
1. the method for selective separation copper rhenium from complicated concentrated molybdenum ore, is characterized in that, comprise the following steps:
(1) by described concentrated molybdenum ore fine grinding;
(2) the complicated concentrated molybdenum ore after step (1) fine grinding is carried out atmospheric activating leaching, under mixed acid system, pass into oxidizing gas to leach, selective dissolution chalcopyrite and sulfuration rhenium, obtain the leach liquor of the valuable metal such as cupric, rhenium and contain molybdenum glance leached mud, realize being separated of molybdenum and copper rhenium, copper, rhenium enter leach liquor, and molybdenum is enrichment in leached mud;
(3) leach liquor in step (2) adopts stepwise solvent extraction method to reclaim rhenium, molybdenum and copper, and first adopt exclusive extraction agent extracting copper, strip liquor produces cathode copper by electrodeposition; Liquid Solvent Extraction of Rhenium after extraction copper, rehenic acid ammonium is produced in back extraction; Raffinate extraction molybdenum after extraction rhenium, ammonium molybdate is produced in back extraction;
(4) leached mud in step (2) becomes the higher concentrated molybdenum ore of purity after washing, and molybdenum grade is greater than 47%, for selling or producing molybdenum product.
2. method according to claim 1, is characterized in that, described complicated concentrated molybdenum ore, and be rhenium-containing, many metals of copper, Low Grade Molybdenum Concentrates, molybdenum grade is 5 ~ 45%.
3. method according to claim 1, is characterized in that, oxidizing gas described in step (2) is one or more in chlorine, oxygen, air.
4. method according to claim 1, is characterized in that, in step (2), mixed acid system is two kinds and above formation in sulfuric acid, nitric acid, hydrochloric acid, organic acid.
5. method according to claim 1, is characterized in that, in step (2), leaching condition is that pH<2, extraction temperature is 80 ~ 100 DEG C, and leaching liquid-solid ratio is 2 ~ 10:1, and extraction time is 0.5 ~ 5h.
6. method according to claim 1, is characterized in that, in step (2), the leaching yield of copper is more than 95%, and the leaching yield of rhenium is more than 95%.
7. method according to claim 1, is characterized in that, the molybdenum degree of oxidation in step (2) is lower, and oxidation dissolution rate is below 5%.In slag, molybdenum still exists with molybdenum glance form, and structure does not change, and becomes the qualified concentrated molybdenum ore that purity is higher, molybdenum content more than 47% after washing.
8. method according to claim 1, is characterized in that, in step (3), the extraction agent of molybdenum rhenium is tertiary amine extractant, and load organic phase adopts ammoniacal liquor back extraction, and strip liquor is for the production of rehenic acid ammonium and ammonium molybdate.
9. method according to claim 1, is characterized in that, in step (3), the extraction agent of copper is selected from hydroxyl-ketoxime extraction agent, quinoline extraction agent, tertiary amines extraction agent, and load organic phase is after washing-back extraction, and strip liquor is for the production of cathode copper.
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Cited By (11)
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| CN105420507A (en) * | 2015-11-30 | 2016-03-23 | 金川集团股份有限公司 | Method for selectively leaching rhenium from copper sulfide arsenic residues under normal pressure |
| CN105671323A (en) * | 2016-03-07 | 2016-06-15 | 紫金矿业集团股份有限公司 | Method for comprehensively recycling copper and rhenium from rhenium-rich residues |
| CN105907992A (en) * | 2016-06-28 | 2016-08-31 | 西北有色金属研究院 | Method for separating molybdenum, copper and rhenium in low-grade molybdenum concentrate through pressurized oxidization |
| CN106868326A (en) * | 2017-03-15 | 2017-06-20 | 辽宁大学 | A kind of method of ionic liquid synergic solvent extraction rhenium |
| CN107419101A (en) * | 2017-07-14 | 2017-12-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| CN112322901A (en) * | 2020-11-04 | 2021-02-05 | 中国地质科学院郑州矿产综合利用研究所 | Method for selectively leaching rhenium from molybdenum concentrate roasting soot |
| CN112760500A (en) * | 2020-12-24 | 2021-05-07 | 中国地质科学院矿产资源研究所 | Method for preparing ammonium rhenate from ion adsorption type molybdenum-rhenium ore |
| CN114164349A (en) * | 2022-02-11 | 2022-03-11 | 矿冶科技集团有限公司 | Method for removing impurities from molybdenum ore with high copper content and performing closed circulation on solution |
| CN115323194A (en) * | 2022-08-16 | 2022-11-11 | 紫金矿业集团股份有限公司 | Process method for treating molybdenite by full wet method under normal pressure condition |
| CN115821081A (en) * | 2022-12-07 | 2023-03-21 | 金川镍钴研究设计院有限责任公司 | Method for separating and enriching rhenium from copper smelting dust collection liquid |
| CN115821081B (en) * | 2022-12-07 | 2024-07-05 | 金川镍钴研究设计院有限责任公司 | Method for separating and enriching rhenium in copper smelting dust collection liquid |
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| CN110592401A (en) * | 2019-10-17 | 2019-12-20 | 西北有色金属研究院 | Method for separating molybdenum and rhenium from rhenium-containing molybdenum concentrate oxidizing solution |
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Cited By (14)
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| CN105420507A (en) * | 2015-11-30 | 2016-03-23 | 金川集团股份有限公司 | Method for selectively leaching rhenium from copper sulfide arsenic residues under normal pressure |
| CN105671323A (en) * | 2016-03-07 | 2016-06-15 | 紫金矿业集团股份有限公司 | Method for comprehensively recycling copper and rhenium from rhenium-rich residues |
| CN105907992A (en) * | 2016-06-28 | 2016-08-31 | 西北有色金属研究院 | Method for separating molybdenum, copper and rhenium in low-grade molybdenum concentrate through pressurized oxidization |
| CN106868326A (en) * | 2017-03-15 | 2017-06-20 | 辽宁大学 | A kind of method of ionic liquid synergic solvent extraction rhenium |
| CN107419101A (en) * | 2017-07-14 | 2017-12-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| CN107419101B (en) * | 2017-07-14 | 2019-01-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| CN112322901A (en) * | 2020-11-04 | 2021-02-05 | 中国地质科学院郑州矿产综合利用研究所 | Method for selectively leaching rhenium from molybdenum concentrate roasting soot |
| CN112760500A (en) * | 2020-12-24 | 2021-05-07 | 中国地质科学院矿产资源研究所 | Method for preparing ammonium rhenate from ion adsorption type molybdenum-rhenium ore |
| CN112760500B (en) * | 2020-12-24 | 2022-07-19 | 中国地质科学院矿产资源研究所 | Method for preparing ammonium rhenate from ion adsorption type molybdenum-rhenium ore |
| CN114164349A (en) * | 2022-02-11 | 2022-03-11 | 矿冶科技集团有限公司 | Method for removing impurities from molybdenum ore with high copper content and performing closed circulation on solution |
| CN115323194A (en) * | 2022-08-16 | 2022-11-11 | 紫金矿业集团股份有限公司 | Process method for treating molybdenite by full wet method under normal pressure condition |
| CN115323194B (en) * | 2022-08-16 | 2023-06-06 | 紫金矿业集团股份有限公司 | Process method for treating molybdenite by full wet method under normal pressure condition |
| CN115821081A (en) * | 2022-12-07 | 2023-03-21 | 金川镍钴研究设计院有限责任公司 | Method for separating and enriching rhenium from copper smelting dust collection liquid |
| CN115821081B (en) * | 2022-12-07 | 2024-07-05 | 金川镍钴研究设计院有限责任公司 | Method for separating and enriching rhenium in copper smelting dust collection liquid |
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