CN103526019A - Method for comprehensively recovering vanadium, selenium and silver from polymetallic associated vanadium ore - Google Patents
Method for comprehensively recovering vanadium, selenium and silver from polymetallic associated vanadium ore Download PDFInfo
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- CN103526019A CN103526019A CN201310515704.8A CN201310515704A CN103526019A CN 103526019 A CN103526019 A CN 103526019A CN 201310515704 A CN201310515704 A CN 201310515704A CN 103526019 A CN103526019 A CN 103526019A
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Abstract
The method comprises the steps of crushing vanadium ores in a dry mode, finely grinding the crushed vanadium ores to be smaller than 0.154mm, adding a certain amount of concentrated sulfuric acid, uniformly mixing the crushed vanadium ores and the concentrated sulfuric acid, curing the mixture at the temperature of 150-300 ℃ for 1-8 hours, adding water and an oxidant, stirring and leaching, leaching vanadium and selenium into leaching liquid, retaining silver in leaching slag, reducing and precipitating the leaching liquid to obtain crude selenium, continuously recovering the vanadium from the leaching liquid after selenium precipitation through extraction or ion exchange, and recovering the silver from the leaching slag containing silver by adopting a conventional process. The process improves mineral leaching activity by sulfuric acid aging, thereby improving leaching speed. The method has the advantages of short flow, simple operation, low energy consumption, high metal recovery rate, low production cost and the like, and achieves the aim of comprehensively recovering the silver-vanadium polymetallic ore in a clean, energy-saving and environment-friendly manner.
Description
Technical field
The invention belongs to non-ferrous metallurgy technology field, relate to a kind of method that comprehensively reclaims vanadium selenium silver from many metals association navajoite.
Background technology
Vanadium, selenium all belong to important strategy metal.Selenium is a kind of typical light-sensitive semiconductor material, its chemical property between metal and nonmetal between, be typical semi-metal, be widely used in the industrial sectors such as chemical industry, metallurgy, building materials, electronics, and there is important pharmaceutical use.Vanadium is a kind of important high temperature resistant non-ferrous metal, can be used as the alloying element of High Strength Structural Steel, tool steel, forged steel, rail steel etc., and meanwhile, the oxide compound of vanadium is also indispensable catalyzer in chemical industry.The compound of vanadium and vanadium is also used in electronic industry, aerospace industry, ceramic industry.
Selenium (Se) is the element of tellurian a kind of rareness, is dispersion state in the earth's crust, and its Clark value in the earth's crust is only 0.05 * 10
-6, its abundance estimates to be about 10 of the earth's crust by weight
-7%, accounts for the 70th of chemical element, therefore at the nature extremely difficult industrial concentration that forms conventionally.There is the distribution of selenium all over the world.The reserves of having verified at present selenium are 9.1 ten thousand tons, and reserves basis is 13.1 ten thousand tons, but distributed pole is inhomogeneous, and its Central America is maximum, accounts for 52.7%, is secondly Asia, Africa, respectively accounts for 15.4%, and Europe and Oceania account for respectively 12.2% and 4.4%.China is one of the world main selenium host country of the resources, though selenium is contained, accounts for the more than 1/3 of global selenium resource, possesses industrial reserves and occupies the 4th, the world, is only second to Canada, the U.S. and Belgium.In explored selenium reserves, magmatic Ni-Cu sulfide deposit accounts for the over half of selenium total reserves.
At present, the main raw material that extracts selenium is that the anode sludge of electrolytical refined copper is, the waste material of the residual mud of the flue dust of lead blast furnace, vitriol works, fume from steel making, lead and zinc concentrate calcination fume, pyrite roasting slag and mercury, gold production, from these raw materials, extracting selenium, is generally to process by methods such as sulfuric acid oxidation roasting, oxidizing roasting, alkali roastings.
Vanadium resource on earth distribution range is wider, vanadium deposit type is mainly divided into Magmatic vanadium titano-magnetite and appositional pattern navajoite, explored vanadium resource reserves have 98% symbiosis in vanadium titano-magnetite in the world, the reserves of vanadium titano-magnetite are very large in the world, are mainly distributed in the C.I.S., the U.S., South Africa, China, Norway, Sweden, Holland, Canada and Australian.By the end of the year 2010, vanadium resource reserves are verified (with V by China
2o
5meter) 21% of 4290 Wan Dun，Zhan world total reservess.China's vanadium resource is mainly composed and is stored in Magmatic vanadium titano-magnetite and appositional pattern shale navajoite.In vanadium titano-magnetite, vanadium resource accounts for 53% of total reserves, concentrates and is distributed in Panxi, Sichuan and area, Chengde.In appositional pattern shale navajoite, vanadium resource accounts for 47% of total reserves, is mainly distributed in the ground such as Shaanxi, Hunan, Hubei, Anhui, Zhejiang, Jiangxi, Guizhou.
20 century 70s have been found many metals of selenium vanadium silver accompanying mineral deposit mid-term in In Yichang Area, Hubei Province.This association navajoite is one to be rich in the shale type sedimentary deposit of selenium, silver, vanadium, 2339.8 ten thousand tons of vanadium silver ore amounts, wherein V
2o
521.8 ten thousand tons, Ag1863.40 ton, Se926.49 ton, silver, selenium reserves reach large ore deposit, and vanadium is medium-scale, belongs to the multi-metal complex navajoite of vanadium silver selenium association.Vanadium in ore is mainly contained in containing in vanadium hydromica, has no the independent mineral of vanadium.Selenium is mainly composed in silver minerals such as having aguilarite, brightness silver-acanthite, naumannite and rich selenium sulphur germanium silver ore.Argentiferous, vanadium minerals dispersion and disseminated grain size are fine, and directly the difficulty of sorting output vanadium concentrate and silver preparation concentrate or silver-colored selenium concentrate is large, and the rate of recovery is low and concentration ratio is little.Therefore, from comprehensive recovery angle, consider, be applicable to directly smelting, or ore beneficiation remove calcium magnesium after the silver-colored vanadium selenium of output collective concentrate smelt again.For comprehensive research of reclaiming selenium in this association navajoite, there is no report both at home and abroad, although the recovery technology of association selenium is more ripe in other ore deposit, but be mainly that the method for volatilizing by pyrogenic process makes selenium enter flue gas with the form volatilization of tin anhydride, then by smoke absorption and sulphur dioxide reduction, reclaim and obtain thick selenium, as reclaimed in copper flue gas during smelting in selenium, ANODE SLIME TREATMENT flue gas, reclaim selenium.But for many metals of selenium vanadium silver associated minerals, because vanadium, silver-colored grade are low, adopt high-temperature roasting energy consumption high, the rate of recovery of selenium is lower, unreasonable economically; And in production process, be easy to produce containing SeO
2have poison gas, toxic gas is easy to reveal, and has dust from flying, environmental pollution is serious.
Summary of the invention
The object of the invention is, navajoite for many metals associations such as silver-colored selenium, the slaking of a kind of employing sulfuric acid is provided, Oxidation Leaching technique is the comprehensive selenium that reclaims from many metals association navajoite, silver, the method of vanadium, specifically by many metals association navajoite dry-type pulverizing, be finely ground to and be less than 0.154mm, then add a certain amount of vitriol oil to mix, slaking 1～8h at the temperature of 150～300 ℃, then add water and oxygenant to carry out agitation leach, vanadium and selenium are entered in leach liquor by leaching, silver is stayed in leached mud, leach liquor adopts precipitate reduction to go out thick selenium, after heavy selenium, liquid continues to reclaim vanadium by extraction or ion-exchange, the leached mud of argentiferous adopts traditional wet method silver leaching process to reclaim silver.
This technique, by sulfuric acid slaking, improves leaching of ores active, thereby improves leaching velocity.There is the advantages such as flow process is short, simple to operate, energy consumption is low, metal recovery rate is high, production cost is low, reach the object of silver-colored vanadium multi-metal ore deposit clean energy-saving, eco-friendly comprehensive recovery.
The object of the invention is to be achieved through the following technical solutions.
From many metals association navajoite, a comprehensive method that reclaims vanadium selenium silver, is characterized in that, comprises the following steps:
(1) broken, fine grinding: many metals association navajoite is broken, be finely ground to particle diameter and be less than 0.154mm, filter, be dried to water content and be less than 20%;
(2) sulfuric acid slaking: step (1) fragmentation, fine grinding, filtration, dried many metals association navajoite are mixed and mix post curing thoroughly with the vitriol oil;
(3) Oxidation Leaching: the material after step (2) slaking is added to water and oxygenant mixing, and agitation leach for some time, then solid-liquid separation, obtains containing vanadium, the leach liquor of selenium and the leached mud of argentiferous;
(4) the heavy selenium of reduction: add reductive agent reduction in the leach liquor of step (3) gained, the selenium in solution is reduced into simple substance selenium and separates out, solid-liquid separation obtains thick selenium and contains vanadium solution;
(5) reclaim vanadium: from the vanadium solution that contains of step (4) gained, through extraction or ion-exchange, reclaim vanadium;
(6) reclaim silver: from the argentiferous leached mud of step (3) gained, reclaim silver.
Step (3) obtains refining after thick selenium, step (4) reclaims vanadium and step (5) reclaims the routine techniques that silver adopts those of ordinary skills' grasp, does not repeat them here.
In the present invention unless otherwise indicated beyond, the ratio, the per-cent that relate to are mass ratio.
In some embodiments, in step (2), curing temperature is 150～300 ℃, curing time 1～8h, and the described vitriol oil is more than 90% sulfuric acid of mass concentration, the add-on of the vitriol oil is 20～50% of described many metals association navajoite.
In some embodiments, in step (3), extraction temperature is 50～100 ℃, liquid-solid ratio 8: 1～1: 1, extraction time 1～8h.
In some embodiments, the described oxygenant of step (3) is at least one in sodium chlorate, hydrogen peroxide, chlorine or clorox.
In some embodiments, the oxygenant consumption described in step (3) is 1～10% of vanadium silver selenium polymetallic ore.
In some embodiments, the reductive agent described in step (4) is iron powder or sulfurous gas.
In some embodiments, the reductive agent consumption described in step (4) is 3～12 times of selenium quality in solution.
In some embodiments, in step (4), reduction temperature is 40～90 ℃, recovery time 0.5～6h.
In some embodiments, step (1) is by the fragmentation of many metals association navajoite, fine grinding particle diameter to being less than 0.154mm, and wherein particle diameter is less than accounting for more than 85% of 0.074mm, filters, is dried to water content and be less than 15%.
In some embodiments, in step (3), extraction temperature is 70～90 ℃, and liquid-solid ratio is 2: 1～4: 1, extraction time 2～4h.
The present invention is directed to the navajoite of many metals associations such as silver-colored selenium, the sulfuric acid slaking that adopts, Oxidation Leaching technique is the comprehensive method that reclaims selenium, silver, vanadium from many metals association navajoite, compared with prior art, there is the advantages such as flow process is short, simple to operate, energy consumption is low, metal recovery rate is high, production cost is low, can be with clean energy-saving, comprehensive selenium, silver, the vanadium reclaiming in many metals of the vanadium silver shale ore that contains selenium of eco-friendly mode.
Accompanying drawing explanation
Accompanying drawing is principle process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is made and being further illustrated.
Many metals association navajoite is broken, be finely ground to and be less than 0.154mm, filter, be dried to water content and be less than 20%; Then the navajoite after filter dehydration is mixed with a certain amount of vitriol oil, the add-on of sulfuric acid is 20～50% of navajoite quality, acid, ore deposit mix thoroughly after at the temperature of 150～300 ℃ slaking 1～8h; In material after slaking, add a certain amount of water and appropriate oxygenant to size mixing, oxygenant is at least one in sodium chlorate, hydrogen peroxide, chlorine or clorox, carry out agitation leach, controlling extraction temperature scope is 50～100 ℃, liquid-solid ratio 8: 1～2: 1, extraction time 1～8h, then solid-liquid separation, obtains containing vanadium, the leach liquor of selenium and the leached mud of argentiferous; Toward adding iron powder or pass into sulfurous gas in leach liquor, carry out precipitate reduction selenium, reduction temperature is 40～90 ℃, recovery time 0.5～6h; Solid-liquid separation obtains thick selenium and containing vanadium solution, the vanadium solution that contains of gained reclaims vanadium through extraction or ion-exchange; Argentiferous leached mud, adopts conventional technique to reclaim silver.
With following indefiniteness embodiment, method of the present invention is further described, to contribute to understanding content of 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
Broken containing the navajoite of selenium silver, be milled to granularity and account for 90% for being less than 0.074mm, by 30% of navajoite quality, adding concentration is 95% sulfuric acid, after mixing thoroughly at 150 ℃ of temperature slaking 1h, then by liquid-solid ratio 2:1, add water and size mixing, and navajoite quality 3% add sodium chlorate.After 90 ℃ of reaction 3h of temperature, carry out solid-liquid separation, V leaching rate 86% now, the leaching yield 84% of selenium.Leach liquor is reduced to heavy selenium, pass into sulfur dioxide gas, gas intake 3Kg/Kg-selenium, filters and obtains selenium powder and containing liquid after vanadium, to containing liquid after vanadium by traditional technology reduce neutralization, extract back extraction, precipitation is calcined and is prepared Vanadium Pentoxide in FLAKES product.And argentiferous leached mud carries out traditional technology Cyanide Leaching, zinc dust precipitation is produced silver products.
Embodiment 2
Broken containing the navajoite of selenium silver, be milled to granularity and account for 75% for being less than 0.074mm, by 25% of navajoite quality, adding concentration is 95% sulfuric acid, after mixing thoroughly at 200 ℃ of temperature slaking 2h, then by liquid-solid ratio 2:1, add water and size mixing, and navajoite quality 3% add chlorine.After 90 ℃ of reaction 3h of temperature, carry out solid-liquid separation, V leaching rate 77% now, the leaching yield 83% of selenium.Leach liquor is reduced to heavy selenium, pass into sulfur dioxide gas, gas intake 5Kg/Kg-selenium, filters and obtains selenium powder and containing liquid after vanadium, to containing liquid after vanadium by traditional technology reduce neutralization, extract back extraction, precipitation is calcined and is prepared Vanadium Pentoxide in FLAKES product.And argentiferous leached mud carries out traditional technology Cyanide Leaching, zinc dust precipitation is produced silver products.
Embodiment 3
Broken containing the navajoite of selenium silver, be milled to granularity and account for 90% for being less than 0.074mm, by 35% of navajoite quality, adding concentration is 98% sulfuric acid, after mixing thoroughly at 200 ℃ of temperature slaking 1h, then by liquid-solid ratio 2:1, add water and size mixing, and navajoite quality 3% add hydrogen peroxide.After 90 ℃ of reaction 3h of temperature, carry out solid-liquid separation, V leaching rate 88% now, the leaching yield 80% of selenium.To leach liquor, add iron powder to reduce heavy selenium, iron powder add-on 8Kg/Kg-selenium, filters and obtains selenium powder and containing liquid after vanadium, to containing liquid after vanadium by traditional technology reduce neutralization, extract back extraction, precipitation is calcined and is prepared Vanadium Pentoxide in FLAKES product.And argentiferous leached mud carries out traditional technology Cyanide Leaching, zinc dust precipitation is produced silver products.
Embodiment 4
Broken containing the navajoite of selenium silver, be milled to granularity and account for 90% for being less than 0.074mm, by 35% of navajoite quality, adding concentration is 98% sulfuric acid, after mixing thoroughly at 250 ℃ of temperature slaking 1h, then by liquid-solid ratio 3:1, add water and size mixing, and navajoite quality 2% add sodium chlorate.After 80 ℃ of reaction 2h of temperature, carry out solid-liquid separation, V leaching rate 90% now, the leaching yield 85% of selenium.To leach liquor, add iron powder to reduce heavy selenium, iron powder add-on 10Kg/Kg-selenium, filters and obtains selenium powder and containing liquid after vanadium, to containing liquid after vanadium by traditional technology reduce neutralization, extract back extraction, precipitation is calcined and is prepared Vanadium Pentoxide in FLAKES product.And argentiferous leached mud carries out traditional technology Cyanide Leaching, zinc dust precipitation is produced silver products.
Embodiment 5
Broken containing the navajoite of selenium silver, be milled to granularity and account for 90% for being less than 0.074mm, by 30% of navajoite quality, adding concentration is 95% sulfuric acid, after mixing thoroughly at 200 ℃ of temperature slaking 2h, then by liquid-solid ratio 3:1, add water and size mixing, and navajoite quality 10% add clorox.After 80 ℃ of reaction 2h of temperature, carry out solid-liquid separation, V leaching rate 89% now, the leaching yield 86% of selenium.Leach liquor is reduced to heavy selenium, pass into sulfur dioxide gas, gas intake 12Kg/Kg-selenium, filters and obtains selenium powder and containing liquid after vanadium, to containing liquid after vanadium by traditional technology reduce neutralization, extract back extraction, precipitation is calcined and is prepared Vanadium Pentoxide in FLAKES product.And argentiferous leached mud carries out traditional technology Cyanide Leaching, zinc dust precipitation is produced silver products.
Claims (10)
1. a comprehensive method that reclaims vanadium selenium silver from many metals association navajoite, is characterized in that, comprises the following steps:
(1) broken, fine grinding: many metals association navajoite is broken, be finely ground to particle diameter and be less than 0.154mm, filter, be dried to water content and be less than 20%;
(2) sulfuric acid slaking: step (1) fragmentation, fine grinding, filtration, dried many metals association navajoite are mixed and mix post curing thoroughly with the vitriol oil;
(3) Oxidation Leaching: the material after step (2) slaking is added to water and oxygenant mixing, and agitation leach for some time, then solid-liquid separation, obtains containing vanadium, the leach liquor of selenium and the leached mud of argentiferous;
(4) the heavy selenium of reduction: add reductive agent reduction in the leach liquor of step (3) gained, the selenium in solution is reduced into simple substance selenium and separates out, solid-liquid separation obtains thick selenium and contains vanadium solution;
(5) reclaim vanadium: from the vanadium solution that contains of step (4) gained, through extraction or ion-exchange, reclaim vanadium;
(6) reclaim silver: from the argentiferous leached mud of step (3) gained, reclaim silver.
2. method according to claim 1, it is characterized in that, in step (2), curing temperature is 150～300 ℃, curing time 1～8h, the described vitriol oil is more than 90% sulfuric acid of mass concentration, and the add-on of the vitriol oil is 20～50% of described many metals association navajoite.
3. method according to claim 1, is characterized in that, in step (3), extraction temperature is 50～100 ℃, liquid-solid ratio 8: 1～1: 1, extraction time 1～8h.
4. method according to claim 1, is characterized in that, the described oxygenant of step (3) is at least one in sodium chlorate, hydrogen peroxide, chlorine or clorox.
5. method according to claim 1, is characterized in that, the oxygenant consumption described in step (3) is 1～10% of vanadium silver selenium polymetallic ore.
6. method according to claim 1, is characterized in that, the reductive agent described in step (4) is iron powder or sulfurous gas.
7. method according to claim 1, is characterized in that, the reductive agent consumption described in step (4) is 3～12 times of selenium quality in solution.
8. method according to claim 1, is characterized in that, in step (4), reduction temperature is 40～90 ℃, recovery time 0.5～6h.
9. method according to claim 1, is characterized in that, step (1) is by the fragmentation of many metals association navajoite, fine grinding particle diameter to being less than 0.154mm, and wherein particle diameter is less than accounting for more than 85% of 0.074mm, filters, is dried to water content and be less than 15%.
10. method according to claim 1, is characterized in that, in step (3), extraction temperature is 70～90 ℃, and liquid-solid ratio is 2: 1～4: 1, extraction time 2～4h.
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Cited By (7)
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| CN104946901A (en) * | 2014-03-31 | 2015-09-30 | 尚军刚 | Strong oxidation treatment method of sulfating roasting slag |
| CN104962734A (en) * | 2015-07-14 | 2015-10-07 | 广西大学 | Method for resource utilization of pineapple peel and electrolytic manganese anode slime |
| CN104962745A (en) * | 2015-07-14 | 2015-10-07 | 广西大学 | Method for resource utilization of banana stem and leaf and electrolytic manganese anode slime |
| CN105728199A (en) * | 2016-02-02 | 2016-07-06 | 北京矿冶研究总院 | Method for recovering silver from silver-containing vanadium ore through chemical activation flotation |
| CN104828788B (en) * | 2015-04-24 | 2016-08-17 | 湘潭大学 | A kind of method extracting selenium from hydrargyrum selenic acid mud waste material |
| CN106566925A (en) * | 2016-11-08 | 2017-04-19 | 陕西华源矿业有限责任公司 | Method for achieving acid mixing, curing and leaching of vanadium through stone coal vanadium ore |
| CN107002168A (en) * | 2014-10-22 | 2017-08-01 | 伊那维克澳大利亚有限公司 | A kind of leaching simultaneously in hygrometric state solid and the METAL EXTRACTION method of absorption |
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| CN104946901A (en) * | 2014-03-31 | 2015-09-30 | 尚军刚 | Strong oxidation treatment method of sulfating roasting slag |
| CN104946901B (en) * | 2014-03-31 | 2017-03-15 | 尚军刚 | A kind of sulfating roasting slag Strong oxdiative processing method |
| CN107002168A (en) * | 2014-10-22 | 2017-08-01 | 伊那维克澳大利亚有限公司 | A kind of leaching simultaneously in hygrometric state solid and the METAL EXTRACTION method of absorption |
| CN104828788B (en) * | 2015-04-24 | 2016-08-17 | 湘潭大学 | A kind of method extracting selenium from hydrargyrum selenic acid mud waste material |
| CN104962734A (en) * | 2015-07-14 | 2015-10-07 | 广西大学 | Method for resource utilization of pineapple peel and electrolytic manganese anode slime |
| CN104962745A (en) * | 2015-07-14 | 2015-10-07 | 广西大学 | Method for resource utilization of banana stem and leaf and electrolytic manganese anode slime |
| CN105728199A (en) * | 2016-02-02 | 2016-07-06 | 北京矿冶研究总院 | Method for recovering silver from silver-containing vanadium ore through chemical activation flotation |
| CN105728199B (en) * | 2016-02-02 | 2019-11-12 | 北京矿冶研究总院 | Method for recovering silver from silver-containing vanadium ore through chemical activation flotation |
| CN106566925A (en) * | 2016-11-08 | 2017-04-19 | 陕西华源矿业有限责任公司 | Method for achieving acid mixing, curing and leaching of vanadium through stone coal vanadium ore |
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