CN105063351B - 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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- CN105063351B CN105063351B CN201510609782.3A CN201510609782A CN105063351B CN 105063351 B CN105063351 B CN 105063351B CN 201510609782 A CN201510609782 A CN 201510609782A CN 105063351 B CN105063351 B CN 105063351B
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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, it is related to one kind selectivity from complicated molybdenum concntrate
The method for separating copper rhenium.
Background technology
Molybdenum is a kind of very important rare metal, has good heat conduction because of it, conduction, high temperature resistant, wear-resisting, corrosion-resistant
Etc. characteristic, it is widely used in the fields such as steel, chemical industry, electronics, Aero-Space, biological medicine, agricultural and national defense construction.
With molybdenum in China yield and consumption figure increase, the exploitation grade of molybdenum is more and more lower, and mineral complexity is more next
It is higher, since particularly 2007 primary molybdenum ores are classified as restricted exploitation class mineral resources by country, low-grade complex association molybdenum
The exploitation of ore deposit turn into focus, and the ore deposit of the metal association such as a large amount of molybdenums, copper, rhenium, lead, zinc, such as Dexing copper-molybdenum are occurred in that in recent years
Rhenium ore deposit, Yunnan Chi Hong Inner Mongols molybdenum lead zinc associated minerals, Chinese gold industry Inner Mongol copper-molybdenum rhenium associated minerals, Zhong Lv Peru Toromocho copper-molybdenums
Ore deposit etc..For such resource, many metal associations such as molybdenum copper rhenium are belonged to by the molybdenum concntrate of ore dressing output, one is influenceed in molybdenum concntrate
The grade of molybdenum, copper rhenium is not only without charge when for sale in addition, or even copper it is too high also have can impose a fine.The gold such as selectively removing copper rhenium
Belong to without changing the structure of molybdenite, so that the double goal for improving molybdenum grade and reclaiming copper rhenium valuable metal is realized, to molybdenum ore
Mountain has preferable economic benefit.
The content of the invention
It is an object of the present invention to provide a kind of method of the Selective Separation copper rhenium from complicated molybdenum concntrate, realizes and improves
Molybdenum grade and the double goal for reclaiming the valuable metals such as copper rhenium.The purpose of the present invention is achieved through the following technical solutions.
A kind of method of the Selective Separation copper rhenium from complicated molybdenum concntrate, its process is followed successively by：
(1) by the molybdenum concntrate fine grinding；
(2) the complicated molybdenum concntrate after step (1) fine grinding is subjected to atmospheric activating leaching, under mixed acid system, is passed through oxidation
Property gas, leach pH<2,70~100 DEG C of temperature, liquid-solid ratio 2~15:Under conditions of 1,0.5~6h of extraction time, selectivity
Chalcopyrite and sulfuration rhenium are dissolved, the leachate and leached mud containing molybdenite of the valuable metals such as cupric, rhenium is obtained, realizes molybdenum and copper rhenium
Separation, copper, rhenium enter leachate, and molybdenum is enriched with leached mud；
(3) leachate in step (2) reclaims rhenium, molybdenum and copper using fractional extraction method, is extracted first using exclusive extractant
Copper is taken, strip liquor produces tough cathode by electrodeposition；Extract liquid extraction rhenium after copper, back extraction production rehenic acid ammonium；Extract the raffinate extraction after rhenium
Take molybdenum, back extraction production ammonium molybdate；
(4) the scrubbed rear molybdenum concntrate higher as purity of leached mud in step (2), molybdenum grade is more than 47%, is used for
Sale or production molybdenum product.
Further, the complicated molybdenum concntrate, is many metals, the Low Grade Molybdenum Concentrates of rhenium-containing, copper, molybdenum grade is 5~
45%.
Further, oxidizing gas described in step (2) is the one or more in chlorine, oxygen, air.
Further, mixed acid system is two kinds and above composition in sulfuric acid, nitric acid, hydrochloric acid, organic acid in step (2).
Further, pH is leached described in step (2)<2.
Further, extraction temperature described in step (2) is 80~100 DEG C.
Further, it is 2~10 that liquid-solid ratio is leached described in step (2):1.
Further, extraction time described in step (2) is 0.5~5h.
Further, the leaching rate of copper is more than 95% in step (2), and the leaching rate of rhenium is more than 95%.
Further, the molybdenum degree of oxidation in step (2) is relatively low, and oxidation dissolution rate is below 5%.Molybdenum is still with brightness molybdenum in slag
Ore deposit form is present and structure does not change, turns into the higher qualified molybdenum concntrate of purity, molybdenum content more than 47% after washing.
Further, the extractant of molybdenum-rhenium is tertiary amine extractant in step (3), and load organic phase is stripped using ammoniacal liquor, instead
Extraction liquid is used to produce rehenic acid ammonium and ammonium molybdate.
Further, the extractant of copper includes in step (3)：Hydroxyl-ketoxime extractant, quinoline extractant, tertiary amine kind of extractants
Deng, load organic phase it is scrubbed-back extraction after, strip liquor is used to produce tough cathode.
The percentage that is related in the present invention, ratio, are weight ratio unless otherwise indicated.
The method of the present invention is by using atmospheric activating leaching-out technique, chalcopyrite and vulcanization in selective dissolution molybdenum concntrate
Rhenium, realizes efficiently separating for molybdenum and copper rhenium, has both reclaimed the valuable metals such as copper, rhenium, the grade of molybdenum concntrate is improved again.Leach
As the qualified molybdenum concntrate that purity is higher after slag is scrubbed, molybdenum grade is up to more than 47%.Leachate contains the valuable gold such as copper, rhenium
Category, copper, rhenium and molybdenum fractional extraction are realized using extraction, and tough cathode, rehenic acid ammonium and the qualified production of ammonium molybdate are produced after back extraction
Product.The method technological process of the present invention is simple, and production operation is convenient, it is easy to accomplish industrialization.
Embodiment
A kind of method of the Selective Separation copper rhenium from complicated molybdenum concntrate, its process is followed successively by：(1) by the complicated molybdenum essence
Ore deposit fine grinding；(2) by after fine grinding complicated molybdenum concntrate is in mixed acid system and is passed through under conditions of oxidizing gas, carry out atmospheric activating
Leach, pH is leached in control<2, temperature is 80~100 DEG C, and liquid-solid ratio is 2~10:1, extraction time is 0.5~5h.Acquisition cupric,
Each element cubage leaching rate in the leachate and leached mud containing molybdenite of the valuable metals such as rhenium, analysis slag.(3) leachate is adopted
Rhenium, molybdenum and copper, first extracting copper are reclaimed with fractional extraction method, strip liquor produces tough cathode by electrodeposition；Extract liquid extraction rhenium after copper,
Back extraction production rehenic acid ammonium；Extract the raffinate extraction molybdenum after rhenium, back extraction production ammonium molybdate；(4) leached mud washing after be used for sell or
Produce molybdenum product.
With following nonlimiting examples to the present invention technique be further described, with contribute to understand the present invention and
Its advantage, and not as limiting the scope of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
The complicated molybdenum concntrates of 200g are taken, containing molybdenum 39%, copper 5%, rhenium 400g/t.Experimental condition：95 DEG C, liquid-solid ratio 5:1, pH value
1.5, extraction time 4h, oxygen flow 15m3/h。
Result of the test：Copper, rhenium, molybdenum leaching rate：95.6%th, 95.02%, 4.1%.Leached mud main component：Molybdenum 47%, copper
0.21%th, rhenium 24g/t.Ammonium acetate：Cu7.82g/L、Mo3.31g/L、Re0.068g/L.
Embodiment 2
The complicated molybdenum concntrates of 200g are taken, containing molybdenum 40%, copper 3%, rhenium 300g/t.Experimental condition：90 DEG C, liquid-solid ratio 4:1, pH value
1, extraction time 3h, oxygen flow 20m3/h。
Result of the test：Copper, rhenium, molybdenum leaching rate：96.8%th, 95.2%, 4.9%.Leached mud main component：Molybdenum 48%, copper
0.11%th, rhenium 20g/t.Ammonium acetate：Cu7.6g/L、Mo6.1g/L、Re0.071g/L.
Embodiment 3
The complicated molybdenum concntrates of 200g are taken, containing molybdenum 35%, copper 7%, rhenium 350g/t.Experimental condition：80 DEG C, liquid-solid ratio 6:1, pH value
1, extraction time 5h, oxygen flow 20m3/h。
Result of the test：Copper, rhenium, molybdenum leaching rate：93.3%th, 95.1%, 4.5%.Leached mud main component：Molybdenum 45%, copper
0.25%th, rhenium 21g/t.Ammonium acetate：Cu11.3g/L、Mo4.1g/L、Re0.078g/L.
Claims (6)
1. a kind of method of the Selective Separation copper rhenium from complicated molybdenum concntrate, it is characterised in that comprise the following steps：
(1) by the complicated molybdenum concntrate fine grinding；
(2) the complicated molybdenum concntrate after step (1) fine grinding is subjected to atmospheric activating leaching, under mixed acid system, is passed through oxidisability gas
Body is leached, selective dissolution chalcopyrite and sulfuration rhenium, obtains cupric, the leachate of rhenium and leached mud containing molybdenite, realize molybdenum with
The separation of copper rhenium, copper, rhenium enter leachate, and molybdenum is enriched with leached mud；Mixed acid system is in sulfuric acid, nitric acid, hydrochloric acid, organic acid
Two kinds and the above constitute；Leaching condition is, pH<2, extraction temperature is 80~100 DEG C, and it is 2~10 to leach liquid-solid ratio:1, leach
Time is 0.5~5h；
(3) leachate in step (2) reclaims rhenium, molybdenum and copper using fractional extraction method, first using extractant extracting copper, back extraction
Liquid produces tough cathode by electrodeposition；Extract liquid extraction rhenium after copper, back extraction production rehenic acid ammonium；Extract the raffinate extraction molybdenum after rhenium, back extraction
Produce ammonium molybdate；
(4) the scrubbed rear molybdenum concntrate higher as purity of leached mud in step (2), molybdenum grade is more than 47%, for selling
Or production molybdenum product；
The complicated molybdenum concntrate, is many metals, the Low Grade Molybdenum Concentrates of rhenium-containing, copper, and molybdenum grade is 5~45%.
2. according to the method described in claim 1, it is characterised in that oxidizing gas described in step (2) be chlorine, oxygen,
One or more in air.
3. according to the method described in claim 1, it is characterised in that the leaching rate of copper is more than 95% in step (2), the leaching of rhenium
Extracting rate is more than 95%.
4. according to the method described in claim 1, it is characterised in that the molybdenum degree of oxidation in step (2) is relatively low, oxidation dissolution rate
Below 5%；Molybdenum still exists with molybdenite form in slag, and structure do not change, turns into higher qualified of purity after washing
Molybdenum concntrate, molybdenum content more than 47%.
5. according to the method described in claim 1, it is characterised in that the extractant of molybdenum-rhenium is tertiary amine extractant in step (3), is born
Lotus organic phase is stripped using ammoniacal liquor, and strip liquor is used to produce rehenic acid ammonium and ammonium molybdate.
6. according to the method described in claim 1, it is characterised in that in step (3) extractant of copper be selected from hydroxyl-ketoxime extractant,
Quinoline extractant, tertiary amine kind of extractants, load organic phase is scrubbed-back extraction after, strip liquor is used to produce tough cathode.
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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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| 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 |
| CN105671323B (en) * | 2016-03-07 | 2017-10-17 | 紫金矿业集团股份有限公司 | The method of Recovering Copper rhenium from rich rhenium slag |
| CN105907992B (en) * | 2016-06-28 | 2018-08-31 | 西北有色金属研究院 | A kind of method that pressure oxidation detaches molybdenum, copper and rhenium in Low Grade Molybdenum Concentrates |
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| 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 |
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| 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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| CA2364213A1 (en) * | 2001-12-03 | 2003-06-03 | Cominco Engineering Services Ltd. | Process for the treatment of molybdenum concentrate |
| FI121713B (en) * | 2009-06-26 | 2011-03-15 | Outotec Oyj | Procedure for dissolving calcopyrite concentrate |
| US20060182674A1 (en) * | 2005-02-02 | 2006-08-17 | Javier Jara | Reduction of copper content in the molybdenite concentrate |
| CN102212683A (en) * | 2011-06-15 | 2011-10-12 | 王钧 | Wet metallurgical method with comprehensive reclamation, basically no three wastes and zero discharge |
| CN103526013B (en) * | 2013-10-23 | 2016-01-20 | 北京矿冶研究总院 | Comprehensive recovery method of complex molybdenum sulfide ore |
| CN103924081A (en) * | 2014-04-28 | 2014-07-16 | 北京矿冶研究总院 | Method for recovering molybdenum and rhenium from molybdenum concentrate pressurized leaching solution |
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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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