CN101775507B - Extraction method for extracting vanadium pentoxide from low grade oxidized type navajoite - Google Patents
Extraction method for extracting vanadium pentoxide from low grade oxidized type navajoite Download PDFInfo
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- CN101775507B CN101775507B CN2010101146869A CN201010114686A CN101775507B CN 101775507 B CN101775507 B CN 101775507B CN 2010101146869 A CN2010101146869 A CN 2010101146869A CN 201010114686 A CN201010114686 A CN 201010114686A CN 101775507 B CN101775507 B CN 101775507B
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Abstract
The invention provides an extraction method for extracting vanadium pentoxide from low grade oxidized type navajoite. The method is as follows: crushing and grinding raw ores of the oxidized type navajoite, grading the crushed and grinded raw ores into coarse fraction products and fine fraction products; selecting mineral containing vanadium from the coarse fraction products by flotation to obtain vanadium concentrate, combining the fine fraction products with the vanadium concentrate to service as bulk concentrate, and taking the underflow of flotation as final tailings; drying the bulk concentrate, adding CaCO3 into the dried bulk concentrate, evenly mixing the CaCO3 with the bulk concentrate, placing the mixture into a disk granulator for pelletizing, leading particles into a rotary kiln for roasting, discharing and cooling calcined ores, leading the calcined ores into a lattice ball mill for wet grinding, levigating ore pulp, adding sulfuric acid the calcined ore quantity of which is 3%-5% into the ore pulp, performing agitation leach in an agitator bath for 4-6h, keeping the pH value within 2.0-2.5, leading lixivium produced by filtering the ore pulp to the purification procedure, washing leaching residues for three times so as to be prepared into building materials, and performing purification, resin adsorption, resolving, vanadium sinking and roasting on the lixivium to obtain a vanadium pentoxide product. The process of the invention adopts a technique of preparing with low cost, thereby effectivly improving the grade of vanadium raw materials, lowering the production cost and solving the problem of enviromental pollution.
Description
Technical field
The present invention proposes Vanadium Pentoxide in FLAKES dressing and smelting process method from low-grade oxidized form navajoite, relates to grinding grading technique, floatation process and smelting technology.
Background technology
A kind of low-grade oxidized form navajoite is mainly clay matter rock and black siliceous shale, and the main mineral composition of clay matter rock is quartz, opal, illite (hydromuscovite), sepiolite, kaolinite, chlorite etc.; The main mineral composition of black silicious is quartz and opal, contains a small amount of sulfide, carbonate minerals, limonite, feldspar, clay mineral and carbonaceous thing etc.
Top layer, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area belongs to low-grade oxidized form navajoite, raw ore contains Vanadium Pentoxide in FLAKES 0.93%, can be vanadium for the element that reclaims in the ore, essential mineral consists of quartz, mica, opal, illite, kaolin and limonite etc.Vanadium is mainly vanadium (V at a low price
3+, V
4+) the form existence, account for more than 80% of total vanadium, mainly be present in illite, kaolin and the limonite with the isomorphism form.The ore structure is mainly argillaceous texture, micro-scale argillaceous texture, phanerocrystalline-adiagnostic or microlitic structure.The ore structure is mainly microbedding shape and compact mass, local visible lamellar or banded structure.
For low-grade oxidized form navajoite, generally all adopt and traditional extract Vanadium Pentoxide in FLAKES with the salt sodium roasting, this process environments is seriously polluted, and leaching yield is low, and not only contaminate environment has also been wasted China's low grade vanadium resource greatly.
Summary of the invention
The technical problem to be solved in the present invention is, for overcoming defectives such as production cost is too high in the prior art, environmental pollution is serious, propose a kind ofly to extract the Vanadium Pentoxide in FLAKES flotation and metallurgy method from low-grade oxidized form navajoite, it adopts low-cost technique of preparing, effectively improves the grade of vanadium extraction raw material; Adopt the optimization flotation and the smelting technology of tailor-make, compressed the treatment capacity of smelting material, reduced and smelted investment, reduce the unit product production cost, overcome problem of environmental pollution.
Technical scheme of the present invention is that described from low-grade oxidized form navajoite extraction Vanadium Pentoxide in FLAKES flotation and metallurgy method, the major ingredient weight part of low-grade oxidized form navajoite raw ore consists of: V
2O
50.91%-0.95%, TC1.8%-2.2%, SiO
272%-74%, Al
2O
38.5%-10%, S 0.2%-0.4%, surplus is other natural Symbiont; It is characterized in that this method may further comprise the steps:
1) be 10mm-15mm with low-grade oxidized form navajoite crushing raw ore to particle diameter, ball milling accounts for mineral aggregate gross weight 40%-70% to fineness for the mineral aggregate weight of-0.074mm again, classification acquisitions+a mm coarse fraction product and-a mm fine fraction product, 0.030≤a≤0.040; A=0.037mm for example;
2) above-mentioned coarse fraction product again ball milling to 0.074mm mineral aggregate weight account for this ball milling mineral aggregate gross weight 40%-70% again, behind mineral aggregate interpolation 100g-1000g gangue inhibitor per ton and 100g-1000g vanadium minerals collecting agent, obtain vanadium concentrate and true tailings by one thick one single-minded flotation of sweeping;
3) the vanadium concentrate with classification gained fine fraction product and flotation acquisition is mixed into collective concentrate;
4) collective concentrate is sent into the drum dried kiln, utilized rotary kiln exhaust gas in dryer cylinder, to be dried to and contain moisture 6%-7%, get dry back collective concentrate;
5) add 3-5 weight part CaCO by collective concentrate after the 100 weight part dryings
3Consumption, collective concentrate adds CaCO after drying
3, make particle diameter 10mm-12mm particulate material behind the mixing, send into rotary kiln baking, kiln hood negative pressure 80Pa-120Pa, kiln tail negative pressure 160Pa-200Pa; 880 ℃-920 ℃ of high temperature section maturing temperatures, roasting time 2.0 hours-2.5 hours; Coming out of the stove after the roasting is cooled to normal temperature, sends into the ball mill wet-milling, pulp granularity-200 purpose material weight part be not less than the ore pulp total weight parts 60%, the ore grinding ore pulp of mass concentration 50%;
6) the ore grinding ore pulp is adjusted mass concentration to 40%, add the sulfuric acid of roasted ore amount 3%～5% more by weight at this ore grinding ore pulp, agitation leach is 4 hours-6 hours in steel basin, keeps ph2.0-2.5, and slurry filtration produces leach liquor and leached mud; The promptly dry back of roasted ore amount collective concentrate amount; Sulfuric acid concentration 98%;
Leached mud can be done building materials after three washings;
7) leach liquor adds oxidant hydrogen peroxide, adds leach liquor 0.8-1.2% parts by volume hydrogen peroxide, adds soda ash again and regulates pH7～7.5, removes SiO
2, Al
2O
3, Fe gets scavenging solution;
8) scavenging solution advances 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
9) with enrichment the saturated resin of Vanadium Pentoxide in FLAKES resolve with sulphuric acid soln, every liter of solution contains the desorbed solution of Vanadium Pentoxide in FLAKES 50g-100g; Used sulphuric acid soln concentration is every liter of sulphuric acid soln sulfur acid 180g-220g;
10) precipitation: desorbed solution oxidizer hydrogen peroxide, per 100 parts by volume add leach liquor 1.8-2.2 parts by volume hydrogen peroxide, regulate pH2-2.5 with ammoniacal liquor again; Heat to 90 ℃-95 ℃, kept 2 hours-3 hours, the tetravalence vanadium in the desorbed solution is oxidized to the pentavalent vanadium, get throw out;
11) red vanadium calcining: throw out 500 ℃-550 ℃ calcinings 2.5 hours-3.0 hours, is got powdery V
2O
5Product.
Described gangue inhibitor is water glass and Tai-Ace S 150, and the weight ratio consumption of water glass and Tai-Ace S 150 is 1-4: 1.
Described vanadium minerals collecting agent is made up of cation-collecting agent and negatively charged ion collecting agent; Cation-collecting agent is amino dodecane or stearylamine or mixed amine, and consumption is that mineral aggregate per ton adds cation-collecting agent 50g-500g; The negatively charged ion collecting agent is oleic acid or oxidized paraffin wax soap, and consumption is that mineral aggregate per ton adds negatively charged ion collecting agent 50g～500g.
Technical solution of the present invention mainly comprises two stage grinding classification, flotation and smelting, and mechanism is described as follows.
(1) grind grading.First section grind grading: because the vanadium minerals that contains in the raw ore is mainly mica group, clay mineral etc., it is extremely low that other silicate mineralss such as quartz, garnet contain vanadium, because the difference of grindability, it is easier to be more levigate than not containing vanadium minerals in grinding process to contain vanadium minerals, therefore, can obtain to contain the higher vanadium concentrate of vanadium by grind grading.Regrind: behind first section ore grinding, in the coarse fraction part, it is not enough to contain the vanadium minerals liberation degree, and mill makes and contains vanadium minerals and other gangue mineral fully dissociates once more.
(2) flotation.Adopt water glass or the Tai-Ace S 150 inhibitor as quartz etc., the effect of assisting into reaches and makes the isolating purposes of silicate minerals such as containing vanadium minerals and quartz the cation-collecting agent amino dodecane with negatively charged ion collecting agent oleic acid.
(3) smelt.Collective concentrate enters the dry back of drum dried kiln drying and adds addition of C aCO
3Mixing is to disk pelletizing mechanism grain, particle enters rotary kiln baking, roasted ore is come out of the stove and is cooled off the laggard bulbec grinding machine wet-milling that accords with regular rules, add sulfuric acid agitation leach 4～6h in steel basin that ore pulp adds roasted ore amount 3%～5% behind the ore grinding, keep ph2.0～2.5, slurry filtration produces leach liquor and enters cleaning section, does building materials after three washings of leached mud; Leach liquor through purification, absorption, parsing, precipitation, calcine the product Vanadium Pentoxide in FLAKES.
As known from the above, the present invention is a kind of from low-grade oxidized form navajoite extraction Vanadium Pentoxide in FLAKES flotation and metallurgy method, and it at first adopts the low-cost beneficiation method of special research and development, has improved the grade of metallurgical vanadium extraction raw material; Then adopt the optimization flotation and the smelting technology of tailor-make, compressed the treatment capacity of smelting material, reduced and smelted investment, reduce the unit product production cost, overcome problem of environmental pollution.
Description of drawings
Fig. 1 is ore grinding-classification-floatation process principle flow chart of a kind of low-grade oxidized form navajoite embodiment of the present invention;
Fig. 2 is the smelting principle flow chart of a kind of low-grade oxidized form navajoite flotation concentrate embodiment of the present invention.
Embodiment
Raw ore is that ore deposit, top layer, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area belongs to low-grade oxidized form navajoite, and callable valuable mineral is mainly Vanadium Pentoxide in FLAKES in the ore.Pentoxide content is 0.93% in the ore, and the direct vanadium extraction production cost of raw ore is high, and enterprise is difficult to profit.The present invention is directed to this ore deposit and adopt the beneficiation enrichment vanadium, smelt the technology that reclaims vanadium again.
Raw material: ore deposit, top layer, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area, its main chemical is (%):
| V 2O 5 | TC | SiO 2 | Al 2O 3 | S |
| 0.93 | 2.00 | 72.41 | 9.27 | 0.27 |
Technical process:
1) be 10mm-15mm with low-grade oxidized form navajoite crushing raw ore to particle diameter, ball milling accounts for mineral aggregate gross weight 50%-60% to fineness for the mineral aggregate weight of-0.074mm again, classification acquisitions+0.037mm coarse fraction product and-0.037mm fine fraction product;
2) above-mentioned coarse fraction product again ball milling to-0.074mm mineral aggregate weight account for this ball milling mineral aggregate gross weight 40%-70% again, behind mineral aggregate interpolation water glass 250g per ton, Tai-Ace S 150 200g and oleic acid 100-150g, amino dodecane 200g-300g, obtain vanadium concentrate and true tailings by one thick one single-minded flotation of sweeping;
3) the vanadium concentrate with classification gained fine fraction product and flotation acquisition is mixed into collective concentrate;
4) collective concentrate is sent into the drum dried kiln, utilized rotary kiln exhaust gas in dryer cylinder, to be dried to and contain moisture 6%-7%, get dry back collective concentrate;
5) add 3-5 weight part CaCO by collective concentrate after the 100 weight part dryings
3Consumption, collective concentrate adds CaCO after drying
3, make particle diameter 10mm-12mm particulate material behind the mixing, send into rotary kiln baking, kiln hood negative pressure 100Pa, kiln tail negative pressure 180Pa; 900 ℃ of high temperature section maturing temperatures, roasting time 2.0-2.5 hour; Coming out of the stove after the roasting is cooled to normal temperature, sends into the ball mill wet-milling, pulp granularity-200 purpose material weight part be not less than the ore pulp total weight parts 60%, the ore grinding ore pulp of mass concentration 50%;
6) the ore grinding ore pulp is adjusted mass concentration to 40%, added the sulfuric acid of roasted ore amount 3%～5% more by weight at this ore grinding ore pulp, in steel basin agitation leach 4-6 hour, keep pH2.0-2.5, slurry filtration produces leach liquor and leached mud; The promptly dry back of roasted ore amount collective concentrate amount rotary kiln baking output inventory, productive rate 94%; Sulfuric acid concentration 98%; Leached mud can be done building materials after three washings;
7) leach liquor adds oxidant hydrogen peroxide, and per 100 parts by volume leach liquors add 1 parts by volume hydrogen peroxide, adds soda ash again and regulates pH7～7.5, removes SiO
2, Al
2O
3, Fe gets scavenging solution;
8) scavenging solution advances 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
9) with enrichment the saturated resin of Vanadium Pentoxide in FLAKES resolve with sulphuric acid soln, every liter of solution contains the desorbed solution of Vanadium Pentoxide in FLAKES 50g-100g; Used sulphuric acid soln concentration is every liter of sulphuric acid soln sulfur acid 180g-220g;
10) precipitation: desorbed solution oxidizer hydrogen peroxide, per 100 parts by volume desorbed solutions add 2 parts by volume hydrogen peroxide, regulate pH2-2.5 with ammoniacal liquor again; Heat to 90 ℃-95 ℃, kept 2 hours-3 hours, the tetravalence vanadium in the desorbed solution is oxidized to the pentavalent vanadium, get throw out;
11) red vanadium calcining: throw out 500 ℃-550 ℃ calcinings 2.5 hours-3.0 hours, is got powdery V
2O
5Product.
Mineral processing index: the total concentrate V of vanadium
2O
51.42%, V
2O
5The rate of recovery 81.96%.
Add CaCO behind the vanadium concentrate drying
3The ore grinding mixing is to the retort furnace roasting, roasted ore add 4% sulfuric acid normal temperature leach must filter after 5 hours leach liquor and leached mud.
Smelt V
2O
5The rate of recovery: 85%.
Select smelting V
2O
5Total recovery: 69.67%.
Claims (3)
1. one kind is extracted the Vanadium Pentoxide in FLAKES flotation and metallurgy method from low-grade oxidized form navajoite, and the major ingredient weight part of low-grade oxidized form navajoite raw ore consists of: V
2O
50.91%-0.95%, TC 1.8%-2.2%, SiO
272%-74%, Al
2O
38.5%-10%, S 0.2%-0.4%, surplus is other natural Symbiont; It is characterized in that this method may further comprise the steps:
1) be 10mm-15mm with low-grade oxidized form navajoite crushing raw ore to particle diameter, ball milling accounts for mineral aggregate gross weight 40%-70% to fineness for the mineral aggregate weight of-0.074mm again, classification acquisitions+a mm coarse fraction product and-a mm fine fraction product, 0.030≤a≤0.040;
2) above-mentioned coarse fraction product again ball milling to-0.074mm mineral aggregate weight account for this ball milling mineral aggregate gross weight 40%-70% again, behind mineral aggregate interpolation 100g-1000g gangue inhibitor per ton and 100g-1000g vanadium minerals collecting agent, obtain vanadium concentrate and true tailings by one thick one single-minded flotation of sweeping;
3) the vanadium concentrate with classification gained fine fraction product and flotation acquisition is mixed into collective concentrate;
4) collective concentrate is sent into the drum dried kiln, utilized rotary kiln exhaust gas in dryer cylinder, to be dried to and contain moisture 2%-4%, get dry back collective concentrate;
5) add 3-5 weight part CaCO by collective concentrate after the 100 weight part dryings
3Consumption, collective concentrate adds CaCO after drying
3, make particle diameter 10mm-12mm particulate material behind the mixing, send into rotary kiln baking, kiln hood negative pressure 80Pa-120Pa, kiln tail negative pressure 160Pa-200Pa; 880 ℃-920 ℃ of high temperature section maturing temperatures, roasting time 2.0 hours-2.5 hours; Coming out of the stove after the roasting is cooled to normal temperature, sends into the ball mill wet-milling, pulp granularity-200 purpose material weight part be not less than the ore pulp total weight parts 60%, the ore grinding ore pulp of mass concentration 50%;
6) the ore grinding ore pulp is adjusted mass concentration to 40%, add the sulfuric acid of roasted ore amount 3%～5% more by weight at this ore grinding ore pulp, agitation leach is 4 hours-6 hours in steel basin, keeps pH2.0-2.5, and slurry filtration produces leach liquor and leached mud; The promptly dry back of roasted ore amount collective concentrate rotary kiln baking output inventory, productive rate 94%, sulfuric acid concentration 98%;
7) leach liquor adds oxidant hydrogen peroxide, and per 100 parts by volume leach liquors add 0.8-1.2 parts by volume hydrogen peroxide, adds soda ash again and regulates pH7～7.5, removes SiO
2, Al
2O
3, Fe gets scavenging solution;
8) scavenging solution advances 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
9) with enrichment the saturated resin of Vanadium Pentoxide in FLAKES resolve with sulphuric acid soln, every liter of solution contains the desorbed solution of Vanadium Pentoxide in FLAKES 50g-100g; Used sulphuric acid soln concentration is every liter of sulphuric acid soln sulfur acid 180g-220g;
10) precipitation: desorbed solution oxidizer hydrogen peroxide, per 100 parts by volume desorbed solutions add 1.8-2.2 parts by volume hydrogen peroxide, regulate pH2-2.5 with ammoniacal liquor again; Heat to 90 ℃-95 ℃, kept 2 hours-3 hours, the tetravalence vanadium in the desorbed solution is oxidized to the pentavalent vanadium, get throw out;
11) red vanadium calcining: throw out 500 ℃-550 ℃ calcinings 2.5 hours-3.0 hours, is got powdery V
2O
5Product.
2. extract the Vanadium Pentoxide in FLAKES flotation and metallurgy method according to claim 1 is described from low-grade oxidized form navajoite, it is characterized in that described gangue inhibitor is water glass and Tai-Ace S 150, the weight ratio consumption of water glass and Tai-Ace S 150 is 1-4: 1.
3. extract the Vanadium Pentoxide in FLAKES flotation and metallurgy method according to claim 1 is described from low-grade oxidized form navajoite, it is characterized in that described vanadium minerals collecting agent is made up of cation-collecting agent and negatively charged ion collecting agent; Cation-collecting agent is amino dodecane or stearylamine or mixed amine, and consumption is that mineral aggregate per ton adds cation-collecting agent 50g-500g; The negatively charged ion collecting agent is oleic acid or oxidized paraffin wax soap, and consumption is that mineral aggregate per ton adds negatively charged ion collecting agent 50g-500g.
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| CN102586588B (en) * | 2012-03-30 | 2014-05-14 | 彭武星 | Roasting method for refining vanadium pentoxide |
| CN103909057B (en) * | 2014-03-28 | 2015-12-30 | 攀钢集团攀枝花钢钒有限公司 | A kind of method preparing vanadium alloy |
| CN104907163A (en) * | 2015-07-07 | 2015-09-16 | 湖南有色金属研究院 | Mineral separation method of finely disseminated vanadium contained carbonaceous shale |
| CN104941791B (en) * | 2015-07-07 | 2017-06-16 | 湖南有色金属研究院 | A kind of beneficiation method of weathering type bone coal navajoite |
| CN105880007B (en) * | 2016-04-08 | 2018-03-06 | 湖南有色金属研究院 | A kind of separation method of tennantite and galena |
| CN108126828B (en) * | 2017-12-18 | 2019-09-20 | 贵州省贵金属矿产资源综合利用工程技术研究中心有限公司 | A kind of Black Shale-type navajoite vanadium enrichment throws the beneficiation method of tail |
| CN109201311A (en) * | 2018-08-14 | 2019-01-15 | 湖南埃铝环保科技有限公司 | A kind of high-sulphur alumyte desulfuration method |
| WO2021146797A1 (en) * | 2020-01-20 | 2021-07-29 | First Vanadium Corp. | Vanadium extraction from disparate shale ores |
| CN112774854B (en) * | 2021-02-03 | 2022-09-30 | 核工业北京化工冶金研究院 | Method for reducing leaching acid consumption of clay uranium ore |
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| BR0215990A (en) * | 2002-12-17 | 2005-11-01 | Council Scient Ind Res | Process for Nickel Extraction from Low Chromite Ore |
| CN100494420C (en) * | 2007-08-08 | 2009-06-03 | 张美焦 | Pretreatment method for nickel oxide before sintering |
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