CN101798113B - Metallurgical method for extracting vanadium pentexide from low-grade stone coal vanadium ores - Google Patents

Metallurgical method for extracting vanadium pentexide from low-grade stone coal vanadium ores Download PDF

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CN101798113B
CN101798113B CN2010101146873A CN201010114687A CN101798113B CN 101798113 B CN101798113 B CN 101798113B CN 2010101146873 A CN2010101146873 A CN 2010101146873A CN 201010114687 A CN201010114687 A CN 201010114687A CN 101798113 B CN101798113 B CN 101798113B
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vanadium
concentrate
adds
ore
flotation
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CN101798113A (en
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连民杰
魏党生
马毅敏
吴海国
寇晓航
叶从新
杨建强
刘景槐
卢东方
姚金江
李婕
张丽敏
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SINOSTEEL MINING CO Ltd
SINOSTEEL MINING DEVELOPMENT Co Ltd
Hunan Research Institute of Non Ferrous Metals
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SINOSTEEL MINING CO Ltd
SINOSTEEL MINING DEVELOPMENT Co Ltd
Hunan Research Institute of Non Ferrous Metals
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Abstract

The invention provides a metallurgical method for extracting vanadium pentexide from low-grade stone coal vanadium ores. The method comprises the following steps of: breaking and grinding the stone coal vanadium ores, grading the stone coal vanadium ore particles to a coarse particle grade and a fine particle grade, grinding and grading the coarse particles to the coarse particle grade, adding kerosene and terpenic oil(C10H17OH) into the obtained products at the coarse particle grade for flotation decarburization to obtain the charcoal concentrate, and adding a gangue inhibitor and a vanadium mineral collector into the obtained products at the coarse particle grade to obtain the vanadium concentrate; using the products at the fine particle grade obtained in two gradations, the flotation charcoal concentrate and the vanadium concentrate as the mixed concentrate, and the floated underflow as tailings; adding CaO into the mixed concentrate, performing granulation, baking and wet-grinding of the mixture, adding sulfuric acid into the mixture for leaching, performing purification, resin adsorption and analysis of the leaching solution, performing vanadium deposition and calcining of the product of the vanadium deposition to obtain V2O5, and washing the leaching mud which can be used as a building additive. In the method, the ore dressing of vanadium-enriched minerals and the pollution-free smelting process are combined, so that the smelting processing capacity is lowered, the smelting investment and the production cost are lowered, the V2O5 yield of the metallurgical method reaches 74.23 percent; and the production cost is reasonable, and the metallurgical method is environmentally-friendly.

Description

A kind of from low-grade stone coal navajoite extraction Vanadium Pentoxide in FLAKES flotation and metallurgy method
Technical field
The present invention extracts the Vanadium Pentoxide in FLAKES dressing and smelting process from the low-grade stone coal navajoite, relates to grinding grading technique, floatation process and smelting technology.
Background technology
Bone coal navajoite is a kind of low-grade oxidized form navajoite, is mainly clay matter rock and danks, and the main mineral composition of clay matter rock is quartz, opal, illite (hydromuscovite), sepiolite, kaolinite, chlorite etc.; The main mineral composition of black carbonaceous is quartz, opal and carbonaceous thing, contains a small amount of sulfide, carbonate minerals, limonite, feldspar, clay mineral etc.
Deep, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area belongs to the low-grade stone coal navajoite, raw ore Vanadium Pentoxide in FLAKES about 0.74%, can be vanadium for the element that reclaims in the ore, essential mineral consists of quartz, mica, carbonaceous thing, 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.Structure of ores is mainly microbedding shape and compact mass, local visible lamellar or banded structure.
For the low-grade stone coal navajoite, adopt the prior art method to extract Vanadium Pentoxide in FLAKES, because the production cost height, enterprise can't reach the purpose of profit, has not only wasted resource, also causes serious environmental to pollute
Summary of the invention
The technical problem to be solved in the present invention is, too high for overcoming in the prior art production cost, defective such as environmental pollution is serious proposes a kind ofly to extract the Vanadium Pentoxide in FLAKES flotation and metallurgy method from the low-grade stone coal navajoite, it adopts low-cost technique of preparing, effectively improves the grade of smelting the 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 is that the weight part major ingredient of low-grade stone coal navajoite raw ore has: V from low-grade stone coal navajoite extraction Vanadium Pentoxide in FLAKES flotation and metallurgy method 2O 50.70%-0.80%, TC 9.5%-10.5%, SiO 265%-70%, Al 2O 36.5%-7.0%, S 1.7%-2.0%, surplus is other natural Symbiont; It is characterized in that this method may further comprise the steps:
1) be 10mm-15mm with low-grade stone coal navajoite crushing raw ore to particle diameter, account for total mineral aggregate weight part 35%-55% with ball milling to fineness for the mineral aggregate of-0.074mm again, then classification acquisition+a mm coarse fraction product and-a mm fine fraction product, 0.030≤a≤0.040;
2) gained coarse fraction product again ore grinding to fineness account for total mineral aggregate weight part 50～85% for the mineral aggregate of-0.074mm, classification acquisitions+b mm coarse fraction product and-b mm fine fraction product then, 0.020≤b≤0.028;
3) above-mentioned classification gained+b mm coarse fraction product adds kerosene and pine camphor oil (C 10H 17OH) after, obtain the carbon ore deposit and take off the charcoal mine tailing by twice flotation; Coarse fraction product per ton adds kerosene 30g～500g, adds pine camphor oil (C 10H 17OH) 50g～600g;
4) after gained takes off charcoal mine tailing interpolation gangue inhibitor and contains the vanadium minerals collecting agent, obtain vanadium concentrate and true tailings by one thick one single-minded flotation of sweeping;
Described gangue inhibitor is water glass and Tai-Ace S 150, and the charcoal mine tailing that takes off per ton adds water glass 100g～1000g, adds Tai-Ace S 150 50g～500g; Containing the vanadium minerals collecting agent is amino dodecane and oleic acid, and the charcoal mine tailing that takes off per ton adds amino dodecane 20g～200g, oleic acid 100g～1000g;
5) the carbon ore deposit and the vanadium concentrate of the above-mentioned twice fractionated fine fraction product of merging, flotation acquisition obtain collective concentrate;
6) collective concentrate is sent into the drum dried kiln, utilizes rotary kiln exhaust gas to be dried in dryer cylinder and contains moisture 2%-4%, gets dry back collective concentrate;
7) collective concentrate adds 3-5 weight part CaO after per 100 weight part dryings, makes particle diameter 10mm-12mm particulate material with the disk pelletizing machine behind the mixing, sends into rotary kiln baking, kiln hood negative pressure 90Pa-110Pa, kiln tail negative pressure 170Pa-190Pa; 900 ℃-920 ℃ of high temperature section maturing temperatures, roasting time 2.0 hours-2.5 hours; After roasting was finished, the ball mill wet-milling was sent in the cooling of coming out of the stove again, pulp granularity-200 purpose material be total ore pulp weight 60%, the ore grinding ore pulp of weight ratio concentration 50%;
8) the ore grinding ore pulp is adjusted weight ratio concentration to 40%, adds the sulfuric acid of roasted ore amount 3%～5% by weight, and agitation leach is 3 hours-6 hours in steel basin, keeps pH2.0-2.5, and slurry filtration produces leach liquor and leached mud; Do building materials after three washings of leached mud; The promptly dry back of roasted ore amount collective concentrate amount, sulfuric acid concentration 98%;
9) leach liquor adds oxidant hydrogen peroxide, and the leach liquor of per 100 parts by volume adds the hydrogen peroxide of 0.8-1.2 parts by volume, adds soda ash again and regulates pH7-7.5, removes SiO 2, Al 2O 3, Fe, scavenging solution;
10) scavenging solution enters 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
11) 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;
12) precipitation: the oxidizer hydrogen peroxide is oxidized to the pentavalent vanadium with the tetravalence vanadium in the desorbed solution, and the desorbed solution of per 100 parts by volume adds the hydrogen peroxide of 1.8-2.2 parts by volume, regulates pH2-2.5 with ammoniacal liquor again; Heat to 90 ℃-95 ℃, kept this temperature 2 hours-3 hours, get throw out;
13) red vanadium calcining: throw out was calcined 2.5 hours-3 hours down at 500 ℃-550 ℃, got powdery V 2O 5Product.
Below the present invention made further specify.
Gained vanadium concentrate can be the higher-grade vanadium concentrate of vanadiumcontent 1.0%-1.5%.
Technical solution of the present invention mainly comprises two stage grinding classification, flotation and smelting, and the mechanism in per stage 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 fine fraction product of vanadium by grind grading; The classification of regrinding: behind first section ore grinding, in the coarse fraction part, it is not enough to contain the vanadium minerals liberation degree, mill makes and contains vanadium minerals and other gangue mineral fully dissociates once more, therefore fine mineral removes this parts of fine mud by classification owing to bigger to next step flotation influence, helps the enforcement of floatation process.
(2) floatation process:
A. charcoal floatation process: adopt and add kerosene and pine camphor oil (C 10H 17OH) etc. to the collecting agent and the pore forming material of charcoal flotation, remove and contain the charcoal mineral, help next step and contain the vanadium minerals flotation;
B. contain the vanadium minerals floatation process: adopt water glass and 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 negatively charged ion collecting agent oleic acid with the cation-collecting agent amino dodecane.
(3) smelting technology: collective concentrate enters the dry back of drum dried kiln drying and adds addition of C aO mixing at 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, ore pulp adds sulfuric acid agitation leach 3～6h in steel basin of roasted ore amount 3%～5%, keep pH2.0～2.5, slurry filtration produces leach liquor and enters cleaning section, does the building materials raw material 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 stone coal type 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 stone coal navajoite of the present invention embodiment.
Fig. 2 is that calcification granulation roasting-low acidleach of a kind of low-grade stone coal navajoite of the present invention flotation concentrate embodiment goes out basic flowsheet of coal preparation.
Embodiment
Ore deposit, deep, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area belongs to low-grade stone coal type navajoite, and callable valuable element is mainly Vanadium Pentoxide in FLAKES in the ore.Pentoxide content is 0.74% 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, deep, Sinosteel Corporation Hunan phoenix mining industry company limited Tang Tuo mining area, its main chemical is (weight %):
V 2O 5 TC SiO 2 Al 2O 3 S
0.74 10.14 67.97 6.75 1.85
The inventive method comprises:
1) the low-grade stone coal navajoite being milled to fineness is that 0.074mm accounts for 35～55%, classification acquisition+0.037mm and-two products of 0.037mm;
2) above-mentioned+0.037mm product once more ore grinding account for 50～85% to fineness for-0.074mm, classification acquisitions+0.023mm and-two products of 0.023mm;
3) above-mentioned+0.023mm coarse fraction product adds kerosene and pine camphor oil (C 10H 17OH), amount ranges is: coarse fraction product per ton adds kerosene 20g～200g, pine camphor oil 50g～500g, adopts the two-stage flotation decarburization, obtains carbon ore deposit and decarburization product;
4) above-mentioned flotation decarburization mine tailing adopts water glass and Tai-Ace S 150 as gangue inhibitor, and amino dodecane and oleic acid are as collecting agent, and flotation obtains vanadium concentrate and true tailings; Decarburization mine tailing per ton adds water glass 300g～700g, adds Tai-Ace S 150 100g～400g; Containing the vanadium minerals collecting agent is amino dodecane and oleic acid, and the charcoal mine tailing that takes off per ton adds amino dodecane 50g～150g, oleic acid 300g～800g;
5) twice fractionated fine fraction product, the carbon ore deposit that flotation obtains and the merging of vanadium concentrate obtain collective concentrate and go into the vanadium extraction operation;
6) collective concentrate enters the drum dried kiln, utilizes rotary kiln exhaust gas to be dried to moisture 6～7% in dryer cylinder;
7) dried collective concentrate adds 3%～5% (weight part) addition of C aO, at disk pelletizing mechanism grain particle diameter 10～12mm, enters rotary kiln baking, kiln hood negative pressure 100Pa, kiln tail negative pressure 180Pa behind the mixing; 900～920 ℃ of high temperature section temperature, behind the residence time 2.0～2.5h, the laggard bulbec grinding machine wet-milling that accords with regular rules of cooling of coming out of the stove, pulp granularity-200 order 60%, concentration 50%;
8) the ore grinding ore pulp is adjusted concentration to 40%, adds 98% sulfuric acid agitation leach 3～6h in steel basin of roasted ore amount 3%～5% (weight part), keeps pH2.0～2.5, and slurry filtration produces leach liquor and leached mud; Leach liquor enters cleaning section, does building materials after three washings of leached mud;
9) leach liquor adds oxidant hydrogen peroxide, and the leach liquor of per 100 parts by volume adds the hydrogen peroxide of 1 parts by volume, adds soda ash again and regulates ph7～7.5, removes SiO 2, Al2O 3, Fe gets scavenging solution;
10) scavenging solution advances 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
11) use 200g/LH 2SO 4Solution is resolved vanadium and is reached 50～100g/L;
12) precipitation: the oxidizer hydrogen peroxide is oxidized to the pentavalent vanadium with the tetravalence vanadium in the desorbed solution, and the desorbed solution of per 100 parts by volume adds the hydrogen peroxide of 2 parts by volume, regulates pH2～2.5 with ammoniacal liquor again, heats 90～95 ℃, keeps 2h～3h;
13) red vanadium calcining at 500～550 ℃ of calcining 2.5～3.0h, gets product powdery V 2O 5
Mineral processing index: the total concentrate V of vanadium 2O 51.04%, V 2O 5The rate of recovery 90.51%.
Smelting recovery 82%.
Select smelting total yield 74.23%.

Claims (2)

1. one kind is extracted the Vanadium Pentoxide in FLAKES flotation and metallurgy method from the low-grade stone coal navajoite, and the major ingredient of low-grade stone coal navajoite raw ore is: V 2O 50.70%-0.80%, TC 9.5%-10.5%, SiO 265%-70%, Al 2O 36.5%-7.0%, S 1.7%-2.0%, surplus is other natural Symbiont; It is characterized in that this method may further comprise the steps:
1) be 10mm-15mm with low-grade stone coal navajoite crushing raw ore to particle diameter, being milled to fineness with ball milling again is 35%-55% for the-mineral aggregate of 0.074mm accounts for total mineral aggregate part by weight, then classification acquisition+a mm coarse fraction product and-a mm fine fraction product, 0.030≤a≤0.040;
2) gained coarse fraction product again ore grinding to fineness be 50～85% for the-mineral aggregate of 0.074mm accounts for total mineral aggregate part by weight, classification acquisitions+b mm coarse fraction product and-b mm fine fraction product then, 0.020≤b≤0.028;
3) after above-mentioned classification gained+b mm coarse fraction product adds kerosene and pine camphor oil, obtain the carbon ore deposit and take off the charcoal mine tailing by twice flotation; Coarse fraction product per ton adds kerosene 30g～500g, adds pine camphor oil 50g～600g;
4) after gained takes off charcoal mine tailing interpolation gangue inhibitor and contains the vanadium minerals collecting agent, obtain vanadium concentrate and true tailings by one thick one single-minded flotation of sweeping;
Described gangue inhibitor is water glass and Tai-Ace S 150, and the charcoal mine tailing that takes off per ton adds water glass 100g～1000g, adds Tai-Ace S 150 50g～500g; Containing the vanadium minerals collecting agent is amino dodecane and oleic acid, and the charcoal mine tailing that takes off per ton adds amino dodecane 20g～200g, oleic acid 100g～1000g;
5) the carbon ore deposit and the vanadium concentrate of the above-mentioned twice fractionated fine fraction product of merging, flotation acquisition obtain collective concentrate;
6) collective concentrate is sent into the drum dried kiln, utilizes rotary kiln exhaust gas to be dried in dryer cylinder and contains moisture 2%-4%, gets the dry mixed concentrate;
7) collective concentrate adds 3-5 weight part CaO after per 100 weight part dryings, makes particle diameter 10mm-12mm particulate material with the disk pelletizing machine behind the mixing, sends into rotary kiln baking, kiln hood negative pressure 90Pa-110Pa, kiln tail negative pressure 170Pa-190Pa; 900 ℃-920 ℃ of high temperature section maturing temperatures, roasting time 2.0 hours-2.5 hours; After roasting was finished, the ball mill wet-milling was sent in the cooling of coming out of the stove again, pulp granularity-200 purpose material be total ore pulp weight 60%, the ore grinding ore pulp of weight ratio concentration 50%;
8) the ore grinding ore pulp is adjusted weight ratio concentration to 40%, adds the sulfuric acid of roasted ore amount 3%～5% by weight, and agitation leach is 3 hours-6 hours in steel basin, keeps pH2.0-2.5, and slurry filtration produces leach liquor and leached mud; Quantum of output after the collective concentrate amount roasting of the promptly dry back of roasted ore amount, sulfuric acid concentration 98%;
9) leach liquor adds oxidant hydrogen peroxide, and the leach liquor of per 100 parts by volume adds the hydrogen peroxide of 0.8-1.2 parts by volume, adds soda ash again and regulates pH7-7.5, removes SiO 2, Al 2O 3, Fe, scavenging solution;
10) scavenging solution enters 717 ion exchange resin enrichment Vanadium Pentoxide in FLAKESs;
11) 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;
12) precipitation: the oxidizer hydrogen peroxide is oxidized to the pentavalent vanadium with the tetravalence vanadium in the desorbed solution, and the desorbed solution of per 100 parts by volume adds the hydrogen peroxide of 1.8-2.2 parts by volume, regulates pH2-2.5 with ammoniacal liquor again; Heat to 90 ℃-95 ℃, kept this temperature 2 hours-3 hours, get throw out;
13) red vanadium calcining: throw out was calcined 2.5 hours-3 hours down at 500 ℃-550 ℃, got powdery V 2O 5Product.
2. extract the Vanadium Pentoxide in FLAKES flotation and metallurgy method according to claim 1 is described from the low-grade stone coal navajoite, it is characterized in that the higher-grade vanadium concentrate that described vanadium concentrate is vanadiumcontent 1.0%-1.5%.
CN2010101146873A 2010-02-26 2010-02-26 Metallurgical method for extracting vanadium pentexide from low-grade stone coal vanadium ores Expired - Fee Related CN101798113B (en)

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CN102168190A (en) * 2010-12-23 2011-08-31 中南大学 Method for enrichment of vanadium from stone coal mine in a manner of low consumption and high efficiency
CN102167400A (en) * 2011-03-18 2011-08-31 中南大学 Method for preparing vanadium pentoxide from vanadium-containing solution
CN102357420A (en) * 2011-07-14 2012-02-22 酒泉钢铁(集团)有限责任公司 Decarburizing method for high-carbon stone coal navajoite
CN103255287A (en) * 2013-05-03 2013-08-21 湖南省矿产测试利用研究所 Process for extracting vanadium pentoxide from stone coal vanadium ores
CN103706465B (en) * 2013-12-27 2015-07-01 武汉理工大学 Method for selecting preconcentration vanadium from high-calcium type stone coal in flotation mode
CN103752419A (en) * 2014-01-26 2014-04-30 河南天罡实业有限公司 Method for flotation of vanadium pentoxide in fly ash
CN104148161B (en) * 2014-08-06 2016-09-14 昆明理工大学 A kind of bone coal navajoite acidity that reclaims soaks the method for fine beans in slag
CN104386747B (en) * 2014-11-18 2016-03-30 河北钢铁股份有限公司承德分公司 A kind of ion exchange method prepares the method for high purity barium oxide
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
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
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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