CN101289225A - Novel process for preparing vanadic anhydride from firing residue of vanadium-containing stone coal - Google Patents

Novel process for preparing vanadic anhydride from firing residue of vanadium-containing stone coal Download PDF

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Publication number
CN101289225A
CN101289225A CNA2008100479400A CN200810047940A CN101289225A CN 101289225 A CN101289225 A CN 101289225A CN A2008100479400 A CNA2008100479400 A CN A2008100479400A CN 200810047940 A CN200810047940 A CN 200810047940A CN 101289225 A CN101289225 A CN 101289225A
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leaching
vanadium
scherbinaite
flakes
vanadium pentoxide
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CNA2008100479400A
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杨秋良
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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Abstract

The invention relates to a novel technology for preparing vanadium pentoxide by using stone coal ignited residue containing scherbinaite, which comprises the following steps: the stone coal ignited residue containing scherbinaite is directly filled in a cement leaching tank without being smashed or ball-milled, and then leached by a dilute sodium carbonate solution at normal temperature or by heating at the temperature of 60 DEG C to 100 DEG C; the obtained leach solution is adsorbed by resin and desorbed by saturated sodium chloride; the desorbed solution is dephosphorized and then added with ammonium chloride to precipitate vanadium, so as to obtain ammonium metavanadate, and the ammonium metavanadate is pyrolyzed to obtain the vanadium pentoxide. The invention has the advantages that (1) the nubbly stone coal ignited residue containing the scherbinaite is directly filled in the cement leaching tank for leaching so that the investment of fixed assets is saved and the problem of dust pollution in workshop is solved; (2) energy is saved by utilizing the waste heat of a roasting furnace for heating the leach solution, the leaching speed is quickened, the recovery rate is improved and the grade of vanadium contained in the leach solution is enriched; (3) by adopting the dilute sodium carbonate solution to substitute sulphuric acid for warming leaching, per ton of fine vanadium consumes approximately 2 tons of sodium carbonate only, therefore, production cost is saved compared with leaching per ton by sulphuric acid; (4) the water used for working can be recycled, thus realizing zero release; the leach residue is slightly alkaline and meets the national placement standards of general wastes.

Description

Contain the scherbinaite coal and burn the novel process that slag prepares Vanadium Pentoxide in FLAKES
Technical field
The present invention relates to rare non-ferrous metal hydrometallurgy industry, specifically relate to a kind of scherbinaite coal that contains and burn the novel process that slag is taked dilute soda solution leaching preparation Vanadium Pentoxide in FLAKES.
Background technology
The burning slag that contains scherbinaite coal calcification baking or blank oxidizing roasting is extracted Vanadium Pentoxide in FLAKES, existing processes is generally dump leaching of dilute sulphuric acid normal temperature or drill traverse and normal temperature and stirs leaching recovery technology down, these technologies are taked the dilute sulphuric acid leaching, poor selectivity, the sulfuric acid consumption is big, and leaching liquid foreign matter content height needs to transfer alkali, resin ion-exchange or solvent extraction pH value need transfer alkali to 2-2.5, the production cost height; Leaching liquid and tail water are for acid and contain a large amount of heavy metal ion and have certain environmental protection hidden danger.
Summary of the invention
Problem to be solved by this invention is to propose a kind of scherbinaite coal that contains at above-mentioned prior art to burn the novel process that slag prepares Vanadium Pentoxide in FLAKES, and its leaching rate of recovery is consistent with the sulfuric acid to leach rate, and production technique is easy to control, low cost, no environmental protection hidden danger.
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: contain the scherbinaite coal and burn the novel process that slag prepares Vanadium Pentoxide in FLAKES, include following step successively:
1) at first choose and contain the scherbinaite coal and burn slag, do not pulverize, ball milling does not directly fill in the cement leaching vat;
2) with 5-10% (mass percentage concentration) dilute soda solution normal temperature leaching 5-15 days, or leaching 2-12 hour of under 60-100 ℃ of temperature, heating;
3) the gained leaching liquid is through D201 or D301 resin absorption, and the saturated sodium-chloride desorb purifies dephosphorization with stripping liquid, adds the ammonium chloride precipitation and gets ammonium meta-vanadate, and pyrolysis obtains Vanadium Pentoxide in FLAKES.
Press such scheme, the described scherbinaite coal burning slag that contains of step 1) is meant at 8-72 hour burning slag of 750 ℃-1050 ℃ insulation roastings.
Press such scheme, the described cement leaching vat of step 1) are volume 10-2000m 3The cement pit of band dodge gate.
Press such scheme, step 2) described heat refer to utilize contain scherbinaite coal roasting waste heat and heat or heat with the boiler steam separately.
Contain scherbinaite coal calcification baking or blank oxidizing roasting and burn the heat new technology theory foundation of leaching preparation Vanadium Pentoxide in FLAKES of slag dilute soda solution:
Contain the vanadium illite, the vanadium in kaolinite, the roscoelite after high temperature and oxygenizement discharge, vanadium under weakly reducing atmosphere under high temperature and oxygenizement with slag in metal oxide effects such as iron generate corresponding vanadium compound.
V 2O 3+FeO+O 2→Fe 2O 3·V 2O 3
Fe 2O 3·V 2O 3+1/2O 2→Fe 2O 3·V 2O 4
Fe 2O 3V 2O 4Fe when temperature keeps more than or equal to 870 ℃ 2O 3V 2O 4Further oxygenolysis becomes liquid Vanadium Pentoxide in FLAKES and Fe 2O 3, be to take block roasting because of containing the scherbinaite coal, at first in roasting process because of the effusion of charcoal and fugitive constituent.Make it contain scherbinaite coal dense structure and become loose, form the microfissure passage.Then in hot environment, it is inconsistent that bulk contains navajoite stone external and internal pressure, causes liquid Vanadium Pentoxide in FLAKES through the microfissure passage, and (high pressure) almost all infiltrates into external surface layer (low pressure) internally, vanadium moved in bulk contain navajoite stone surface and enrichment.Bulk contains the inner dilution of navajoite stone, and liquid Vanadium Pentoxide in FLAKES is through being cooled to solid-state Vanadium Pentoxide in FLAKES, and liquid Vanadium Pentoxide in FLAKES is through being cooled to solid-state Vanadium Pentoxide in FLAKES, thereby helps the leaching of dilute soda solution.
Fe 2O 3·V 2O 4+1/2O 2→Fe 2O 3+V 2O 5
The vanadium pentoxide that is generated when adding a certain amount of lime in roasting process generates corresponding vanadic acid calcium.
V 2O 5+CaO→Ca(VO 3) 2
When the leaching stone coal vanadium-containing of heating with dilute soda solution burns slag, burn Vanadium Pentoxide in FLAKES in the slag and generate vanadic acid sodium with vanadic acid calcium and enter in the leaching liquid and realized separating of vanadium and slag.
V 2O 5+Na 2CO 3＝2NaVO 3+CO 2↑
Ca(VO 3) 2+Na 2CO 3→NaVO 3+CaCO 3↓
Beneficial effect of the present invention is:
1. the present invention does not pulverize containing scherbinaite coal burning slag, and ball milling does not directly advance the leaching vat leaching with block-shape morphology, saves the investment of fixed capital, has solved the dust pollution in workshop again;
2. the present invention utilizes the waste heat of the stoving oven leaching liquid save energy of heating, and accelerates leaching speed, improves the rate of recovery, and pregnant solution water contains the vanadium grade.Leaching need be more than 5 days down because of normal temperature, and 60 ℃ only need 12 hours, and 80 ℃ only need 4 hours, and 100 ℃ need 2 hours, and the leaching of heating can reduce the investment of leaching vat and resin;
3. the present invention substitutes sulfuric acid with the leaching of heating of dilute soda solution, and smart vanadium per ton consumes about 2 tons of soda ash and gets final product, than can save production cost ten thousand yuan of 2-3 of sulfuric acid to leach essence per ton;
4. the present invention takes the leaching of heating of lower concentration soda ash solution, the leaching liquid meta-alkalescence, and pH value 8-9 is meta-alkalescence also, and the stacking standard that the slag meta-alkalescence meets the general waste of country is soaked in the zero release that can be recycled of heavy metal free ion enrichment, work water.
Embodiment
Below technology of the present invention is described in further detail:
Containing the scherbinaite coal is delivered in the cement leaching vat → piles to heat to flow through D201 or D301 resin absorption → absorption tail water of 60-100 ℃ 2-12 hour → leaching liquid of leaching liquid leaching through the roasting kiln waste heat through 750-1050 ℃ of insulation roasting 8-72 hour burning slag and add leaching agent (soda ash) recirculation leaching → saturated resin after the roasting kiln waste heat is heated and add saturated nacl aqueous solution desorb → stripping liquid purification dephosphorization → add ammonium chloride precipitation and get ammonium meta-vanadate → pyrolysis and get the Vanadium Pentoxide in FLAKES product.Deposition vanadium mother liquid is mended sodium-chlor and is recycled, and tailings adds the fixing a small amount of soluble vanadium of a spot of lime and goes into the stacking of mine tailing storehouse or be sold to the cement mill.
Embodiment 1
1, selects materials and load: select for use 48 hours the scherbinaite coal that contains of 850 ℃ of roastings insulations to burn slag, burn cinder grade 1.448%, sour molten vanadium full-page proof 12.02kg/T, the molten vanadium full-page proof of alkali 12.02kg/T, transformation efficiency 89.01% is not pulverized, not ball milling directly fill in the band dodge gate the cement leaching vat (volume is 1500m 3);
2, leaching: take to contain scherbinaite coal burning slag and 10% soda ash solution by solid-to-liquid ratio normal temperature leaching in 1: 15 days, leaching liquid contains vanadium grade 12.01g/L, with absorption tail water washing 4 times, and with the leaching liquid merging, average liquid hydration vanadium grade 4.98g/L, pH value is 7.5;
3, the wash-out of ion-exchange and Vanadium Pentoxide in FLAKES: adsorbing selected resin is D301, is that Hebi, Henan resin processing plant produces the macroreticular weakly base resin anion(R.A), and loading capacity is the 348kg/T Vanadium Pentoxide in FLAKES.
Leaching liquid is gone out to flow through under enterprising Φ 0.8 * 2mm resin bucket, each resin bucket is filled the exchange column that D301 tree refers to 800kg, control 0.5m 3/ h washes speed, it is 0 that absorption tail water begins, when increasing to 0.4g/L gradually, recoiling to water outlet with clear water does not have muddiness, is added in the resin bucket with deposition vanadium mother liquid preparation saturated nacl aqueous solution, with pump circulation 30 minutes, static immersion was put to treating pond in 2 hours, repeat aforesaid operations 3-4 time with saturated nacl aqueous solution again, wash 2-3 time when water outlet contains the vanadium grade less than 2g/L with deposition vanadium mother liquid, the vanadium removal resin that finishes begins adsorption operation.For the first time the higher-grade of elutriant Vanadium Pentoxide in FLAKES is up to 448g/L, and lowest quality is lower than 2g/L, merges average grade 54.48g/L together, and P content is 0.25g/L.
4, dephosphorization: above-mentioned elutriant is because of phosphorous higher, must purify the quality that dephosphorization could guarantee Vanadium Pentoxide in FLAKES earlier, takes to add earlier 1% ammonium chloride, adds magnesium chloride again, phosphorus generation ammonium magnesium phosphate is precipitated and removes.
5, precipitation: will purify good elutriant supernatant liquor and transfer to the precipitation pond, extraordinarily go into the ammonium chloride precipitation by 2 of pentoxide content, the limit edged stirs, and quiescent setting is after 12 hours, and analytically clear liquid Vanadium Pentoxide in FLAKES grade is reduced to below the 1g/L, it is complete to be considered as precipitation, extract deposition vanadium mother liquid out and add the clear water agitator treating again, quiescent settling 12 hours accesses washings, following throw out is dried product ammonium meta-vanadate packing warehouse-in with drier.
6, the quality of Vanadium Pentoxide in FLAKES: the ammonium meta-vanadate that is produced is through drying, its content is 64.3%, 280 ℃ and takes off ammonium that 500-550 ℃ of calcination got orange Vanadium Pentoxide in FLAKES product in 5 hours, chemical examination by analysis, pentoxide content 98.22%, P 0.015%, S 0.02%, SiO 2: 0.08%, harmful element is lower than national standard, and smart content of vanadium is higher than national standard, meets the specification of quality of metallurgical grade 98.
Embodiment 2
(the leaching vat volume was 2000m in 4 hours with the leaching of 8% (mass percentage concentration) soda ash solution 80 ℃ (containing scherbinaite coal roasting waste heat heats) will to contain scherbinaite coal burning slag 3), its leaching rate of recovery reaches 83%, and all the other are with embodiment 1 (wherein containing scherbinaite coal burning slag is meant at 72 hours burning slag of 750 ℃ of insulation roastings).
Embodiment 3
(the leaching vat volume was 500m in 4 hours with the leaching of 5% (mass percentage concentration) soda ash solution 80 ℃ (containing scherbinaite coal roasting waste heat heats) will to contain scherbinaite coal burning slag 3), to heat to 100 ℃ of leachings 2 hours with steam again, its leaching rate of recovery reaches 85%, and all the other are with embodiment 1 (wherein containing scherbinaite coal burning slag is meant at 8 hours burning slag of 1050 ℃ of insulation roastings).

Claims (4)

1, contain the scherbinaite coal and burn the novel process that slag prepares Vanadium Pentoxide in FLAKES, it is characterized in that including following step successively:
1) at first choose and contain the scherbinaite coal and burn slag, do not pulverize, ball milling does not directly fill in the cement leaching vat;
2) with 5-10% (mass percentage concentration) dilute soda solution normal temperature leaching 5-15 days, or leaching 2-12 hour of under 60-100 ℃ of temperature, heating;
3) the gained leaching liquid is through D201 or D301 resin absorption, and the saturated sodium-chloride desorb purifies dephosphorization with stripping liquid, adds the ammonium chloride precipitation and gets ammonium meta-vanadate, and pyrolysis obtains Vanadium Pentoxide in FLAKES.
2, burn the novel process that slag prepares Vanadium Pentoxide in FLAKES by the described scherbinaite coal that contains of claim 1, it is characterized in that the described scherbinaite coal burning slag that contains of step 1) is meant at 8-72 hour burning slag of 750 ℃-1050 ℃ insulation roastings.
3, burn the novel process that slag prepares Vanadium Pentoxide in FLAKES by claim 1 or the 2 described scherbinaite coals that contain, it is characterized in that the described cement leaching vat of step 1) are volume 10-2000m 3The cement pit of band dodge gate.
4, burn the novel process that slag prepares Vanadium Pentoxide in FLAKES by claim 1 or the 2 described scherbinaite coals that contain, it is characterized in that step 2) described heat to refer to utilize contain scherbinaite coal roasting waste heat and heat or heat with the boiler steam separately.
CNA2008100479400A 2008-06-06 2008-06-06 Novel process for preparing vanadic anhydride from firing residue of vanadium-containing stone coal Pending CN101289225A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102172448A (en) * 2011-03-10 2011-09-07 济南大学 Filter material for dephosphorizing wastewater and manufacturing method thereof
CN102534238A (en) * 2012-03-07 2012-07-04 怀化市洪发资源综合利用科技有限公司 Harmless and comprehensive utilization method for vanadium-extraction liquid leached residue
CN103966467A (en) * 2014-03-27 2014-08-06 湖南大学 Chloride-free vanadium extraction process
CN107032400A (en) * 2017-04-27 2017-08-11 攀钢集团研究院有限公司 TiCl4Tailings alkali soak is refined for the method for high-purity vanadium oxide
CN107500354A (en) * 2017-08-17 2017-12-22 芜湖人本合金有限责任公司 A kind of vanadic anhydride and its production method and application

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102172448A (en) * 2011-03-10 2011-09-07 济南大学 Filter material for dephosphorizing wastewater and manufacturing method thereof
CN102534238A (en) * 2012-03-07 2012-07-04 怀化市洪发资源综合利用科技有限公司 Harmless and comprehensive utilization method for vanadium-extraction liquid leached residue
CN103966467A (en) * 2014-03-27 2014-08-06 湖南大学 Chloride-free vanadium extraction process
CN107032400A (en) * 2017-04-27 2017-08-11 攀钢集团研究院有限公司 TiCl4Tailings alkali soak is refined for the method for high-purity vanadium oxide
CN107032400B (en) * 2017-04-27 2019-01-22 攀钢集团研究院有限公司 TiCl4The method that purification tailings alkali is soaked standby high-purity vanadium oxide
CN107500354A (en) * 2017-08-17 2017-12-22 芜湖人本合金有限责任公司 A kind of vanadic anhydride and its production method and application

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Open date: 20081022