CN102127657B - Comprehensive recovery method for extracting ferrovanadium from stone coal acid immersion liquid - Google Patents
Comprehensive recovery method for extracting ferrovanadium from stone coal acid immersion liquid Download PDFInfo
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- CN102127657B CN102127657B CN2011100677865A CN201110067786A CN102127657B CN 102127657 B CN102127657 B CN 102127657B CN 2011100677865 A CN2011100677865 A CN 2011100677865A CN 201110067786 A CN201110067786 A CN 201110067786A CN 102127657 B CN102127657 B CN 102127657B
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- jarosite
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/20—Recycling
Abstract
The invention relates to a comprehensive recovery method for extracting ferrovanadium from stone coal acid leaching liquid. The process mainly comprises the following steps of: crystallizing a stone coal sulfuric acid leaching liquid into ammonium aluminum alum sulfate and adding a pH value regulator to the crystallized liquid at a room temperature; oxidizing, precipitating and separating out crystallized liquid into a mixture containing ammonium jarosite and ammoniojarosite, leaching the vanadium-contained mixture separated from the precipitate in alkaline to obtain alkaline leaching liquid and alkaline leaching slag; adding sulphuric acid to the alkaline leaching liquid to acidify and precipitate vanadium pentoxide, calcining, washing and drying the vanadium pentoxide to obtain a refined vanadium product, calcining the alkaline leaching slag to obtain ferric oxide or adding sulphuric acid to dissolve, concentrate and crystallize to obtain polymerase ferric sulfate; and transforming the ammonium aluminum alum sulfate and regenerating vanadium precipitation mother liquor alkali, and the like. The invention has the advantages of good product quality, less reagent amount, low production cost, environmental protection, and the like.
Description
Technical field
The present invention relates to a kind of bone coal pickling liquor vanadium extraction iron comprehensive recovering process.
Background technology
Bone coal is the metallurgical mineral wealth of a kind of important vanadium, and the technology that extracting vanadium from stone coal is commonly used is that sulfuric acid leaches.The technology of from the bone coal acid dip solution, extracting vanadium at present has:
1) bone coal sulphuric leachate → reduction → extraction → back extraction → oxidation → ammonium salt precipitation → calcine smart vanadium;
2) bone coal sulphuric leachate → ammonium salt remove aluminium → selective oxidation deironing → vanadium oxidation → IX → desorb → ammonium salt precipitation → calcine smart vanadium;
Or bone coal sulphuric leachate → ammonium salt removes in aluminium → selective oxidation deironing → vanadium oxidation → IX → desorb → acid and precipitation → ammonium salt wash sodium → calcine smart vanadium;
3) bone coal sulphuric leachate → ammonium salt soaks → ammonium salt precipitation → calcining except that aluminium → oxidation precipitation iron cpd → alkali;
Or bone coal sulphuric leachate → ammonium salt remove aluminium → oxidation precipitation iron cpd → alkali and soak → purification and impurity removal → ammonium salt precipitation → calcine smart vanadium.
For fear of the interference of Fe (III) to the vanadium extraction, must add reductive agent before the extraction of bone coal sulphuric leachate Fe (III) is reduced into Fe (II), meanwhile, the high price vanadium in the solution also is reduced.So, leach liquor is first reduction extraction, back back extraction oxidation, and technical process is long, and the reagent consumption is big, and production cost is high, and liquid is if recycle after the vanadium extraction, and vitriol accumulates in a large number, and soltion viscosity is big, extraction phase-splitting difficulty, directly the discharge-ring environment pollution is big.The IX of bone coal sulphuric leachate deironing rear oxidation, because the organic matter of the many reductibilities of bone coal acidleach process gets into solution, not only vanadium oxidising process oxygenant consumption is big, and oxidation is not thorough, influences the exchange capacity of resin.Though the heavy ferrovanadium compound sedimentation effect of bone coal sulphuric leachate oxidation is pretty good, what obtain is the ironic hydroxide gelatinous precipitate, liquid-solid separation difficulty, and impurity is carried secretly many.In addition, no matter be that which kind of technology precipitation process all can produce ammonia nitrogen waste water, and the iron in the bone coal sulphuric leachate can't fully utilize.
Summary of the invention
The object of the present invention is to provide and can avoid ammonia nitrogen waste water to produce, efficient recovery iron improves the comprehensive utilization of resources rate, protection environment, a kind of bone coal pickling liquor vanadium extraction iron comprehensive recovering process that reduces production costs.
Technical scheme of the present invention may further comprise the steps: the mode through crystalline sulfuric acid aluminium ammonium alum in containing scherbinaite coal sulphuric leachate is removed aluminium; Liquid after the crystallization that obtains is added pH value regulator regulator solution acidity to 1.0~3.5, cross and to filter liquid after the acid adjustment; Liquid adds the crystal seed oxidation and separates out and contain vanadium jarosite and ammonium jarosite deposition after the acid adjustment, and mistake filters liquid after the jarosite that contains vanadium and ammonium jarosite precipitation mixture and the precipitation; Contain the vanadium jarosite and ammonium jarosite precipitation mixture alkali soaks filtration, the alkali immersion liquid and the ferruginous alkali that must contain vanadium soak slag, and the alkali immersion liquid of gained adds the sulfuric acid acidation precipitation, red vanadium and deposition vanadium mother liquid; Red vanadium calcining after scouring obtains smart vanadium except that sodium, filtration, oven dry; Alkali soaks slag and adds sulfuric acid dissolution and produce bodied ferric sulfate, or with alkali soak slag calcine red stone; Described crystal seed is meant one or more in yellow modumite, jarosite, the ammonium jarosite.
It is in the bone coal sulphuric leachate, to form 1~3 of Tai-Ace S 150 ammonium alum crystal chemistry reaction stoichiometric number by the aluminium in the bone coal sulphuric leachate extraordinarily to go into (NH that described crystalline sulfuric acid aluminium ammonium alum removes aluminium
4)
2SO
4, NH
4Cl, NH
4NO
3, NH
3H
2Among the O one or more make aluminium in the solution with NH
4Al (SO
4)
212H
2The crystallization of O form is separated out.
Described pH value regulator is meant CaCO
3, CaO, Ca (OH)
2, in the ammoniacal liquor, volatile salt, bicarbonate of ammonia one or more.
Described oxidation is separated out and is meant and after acid adjustment, adds H in the liquid
2O
2, NaClO
3And the peroxosulphuric ammonium in one or more; Make the oxidation of divalent in the solution become ferric iron, and simultaneously trivalent vanadium and tetravalence vanadium are oxidized to the pentavalent vanadium.The present invention makes iron separate out with jarosite and ammonium jarosite through adding crystal seed, and the vanadium in the while inducing solution is separated out with yellow crystalline precipitate.
Described alkali soaks and is meant in jarosite that contains vanadium and ammonium jarosite precipitation mixture and adds NaOH, KOH, Na
2CO
3, NaHCO
3, K
2CO
3, KHCO
3In one or more agitation leach precipitation mixtures in vanadium.
Thereby adding the sulfuric acid acidation precipitation through alkali immersion liquid in the technology of the present invention makes the vanadium in the solution separate out with red vanadium form deposition.
Described calcining is meant that the red vanadium that deposition is separated out removes wherein free-water and combination water through 250~550 ℃ of pyroprocessing.
Thereby add water washing through the present invention and remove the impurity of calcining the solubilities such as sodium that are mingled with in the Vanadium Pentoxide in FLAKES that obtains except that sodium.
The described bodied ferric sulfate of producing is meant and soaks the alkali that obtains and soak slag containing vanadium jarosite and ammonium jarosite precipitation mixture alkali, adds the sulphuric acid soln dissolving, concentrates, and crystallization gets ferric polysulfate solid.
Described calcining is meant that containing vanadium jarosite and ammonium jarosite precipitation mixture alkali soaks the alkali that obtains and soak slag and remove wherein free-water and combination water through pyroprocessing.
Can with described deposition vanadium mother liquid regenerate alkaline solution.Its operating process comprises: change into 1~3 of sodium hydrogen carbonate solution chemical reaction stoichiometric number by sodium bisulfate in the deposition vanadium mother liquid earlier and extraordinarily go into lime carbonate or Wingdale; Stirring at room 1~4 hour; Cross and filter sodium hydrogen carbonate solution and gypsum; Sodium hydrogen carbonate solution adds 50~100 ℃ of causticizations of lime again and filters to pH13~15, alkaline solution, alkaline solution returns and contains vanadium jarosite alkali and soak operation and recycle.
With the above-mentioned Tai-Ace S 150 ammonium alum that obtains make the transition ammoniumsulphate soln.
Described Tai-Ace S 150 ammonium alum makes the transition and is meant NH
4Al (SO
4)
212H
2After the O crystal is dissolved in water, adds lime and transfer pH to 3.5~8.5, make Al wherein change into Al (OH)
3Filter, gained filtrating is returned the crystallization of bone coal sulphuric leachate and is separated out Tai-Ace S 150 ammonium alum operation and recycle, and filter residue is stored up.
Liquid returns bone coal sulphuric leachate operation and recycles after the described precipitation.
The concrete technological process that the present invention implements is:
Bone coal pickling liquor vanadium extraction iron comprehensive recycling process process mainly may further comprise the steps: with V
2O
5Meter contains the bone coal sulphuric leachate crystalline sulfuric acid aluminium ammonium alum of vanadium 1.5~25g/L; The liquid chamber temperature adds pH value regulator regulator solution acidity after the crystallization; The oxidation of liquid adding crystal seed is separated out and is contained vanadium jarosite and ammonium jarosite precipitation mixture after the acid adjustment, and precipitation mixture alkali is soaked filtration, and the alkali immersion liquid and the ferruginous alkali that must contain vanadium soak slag; The alkali immersion liquid adds the heavy red vanadium of sulfuric acid acidation, red vanadium calcining after washing dry smart vanadium product; Alkali soaks slag and adds sulfuric acid dissolution and produce bodied ferric sulfate, or calcine red stone; The relevant parameter of its technological process is: press aluminium formation Tai-Ace S 150 ammonium alum NH in the bone coal sulphuric leachate
4Al (SO
4)
212H
21~3 extraordinarily ammonium or ammonia of O crystal chemistry reaction stoichiometric number; The liquid chamber temperature adds pH value regulator regulator solution acidity to pH 1.0~3.5 after the crystallization; Liquid becomes ferric iron and trivalent vanadium and tetravalence vanadium to be oxidized to 1~3 oxygenant extraordinarily of pentavalent vanadium chemistry reaction stoichiometric number by oxidation of divalent after the acid adjustment, and adds 45~95 ℃ of crystal seeds and stir 1~3 hour heavy vanadium jarosite and ammonium jarosite mixture of containing; Contain the vanadium precipitation mixture by 1: 1.0~5.0g/ml of solid-to-liquid ratio, add NaOH, KOH, Na
2CO
3, NaHCO
3, K
2CO
3, KHCO
3In one or more, 11~14,25~100 ℃ of control pH values, 0.5~3.5 hour after-filtration of agitation leach; The alkali immersion liquid of gained adds 0.5~2.5,25~100 ℃ of stirrings of sulfuric acid adjust pH and separated out red vanadium in 1~3 hour; 250~550 ℃ of calcinings of red vanadium 1~2 hour, cooling by 1: 1.0~5.0g/ml of solid-to-liquid ratio, adds 25~100 ℃ in water, agitator treating 0.5~3.5 hour, filtering drying gets V
2O
5Product; Alkali soaks the alkali that obtains and soaks slag; 1: 1.0~5.0g/ml adds sulfuric acid dissolution by solid-to-liquid ratio, and control terminal point pH2.0~3.0 are crossed and filtered polymeric ferrous sulphate solution; 85~155 ℃ of normal pressures of polymeric ferrous sulphate solution are concentrated into and contain Fe>15wt%, and crystallisation by cooling gets ferric polysulfate solid; Or alkali is soaked slag got red stone in 1~3 hour through 200~500 ℃ of calcinings.
The present invention and existing compared with techniques have the following advantages and effect:
Advantage of the present invention is in technical process the bone coal sulphuric leachate through crystalline sulfuric acid aluminium ammonium and acid adjustment to certain pH value; After acid adjustment, add certain crystal seed again in the liquid; And oxidation; Iron is separated out with heavy jarosite and ammonium jarosite deposition, and the vanadium in the inducing solution also precipitates and separates out simultaneously, the jarosite of separating out exists its purity height, particle slightly to be easy to liquid-solid the separation with ammonium jarosite with crystalline form; In jarosite and the ammonium jarosite except that containing vanadium other impurity seldom help the separation and the recovery of follow-up vanadium, iron.It is simple that technology of the present invention also has technology, the characteristics of good product quality.And the iron in the precipitation slag that the oxidation precipitation operation in the existing technology obtains is to separate out with the form of ironic hydroxide; Vanadium is then separated out with the form of many ferric vandate; And these compounds all are to separate out with the form of flocks; Wherein being mingled with a large amount of impurity, under boiling state, will not stirred for a long time and could crystallization separate out jarosite and ammonium jarosite deposition because do not add ferric ion in the seed-solution, is exactly floss otherwise precipitate what separate out.In addition, the present invention removes the quality that sodium technology has significantly improved the Vanadium Pentoxide in FLAKES product through adopting acidifying precipitation and calcining, washing.Integral body through technology of the present invention designs again, cooperatively interacting between each step, thereby can effectively avoid ammonia nitrogen sewage, and reduce environmental pollution, also meet the development trend that China's energy-conserving and emission-cutting technology is transformed.
Embodiment
Below in conjunction with embodiment, the present invention is further described, following examples are intended to explain the present invention rather than to further qualification of the present invention.
Embodiment 1
With V
2O
5Meter contains the bone coal acid dip solution 3000ml of vanadium 3.83g/L, adds ammoniacal liquor adjust pH to 3.0 crystalline sulfuric acid aluminium ammonium alum and removes aluminium, becomes ferric iron and trivalent vanadium and tetravalence vanadium to be oxidized to 1.5 VAL-DROP extraordinarily that the pentavalent vanadium chemistry reacts stoichiometric number by oxidation of divalent in the solution; Add yellow modumite and make 85 ℃ of crystal seeds and stir and heavyly contained vanadium jarosite and ammonium jarosite mixture in 1 hour, contain vanadium jarosite and ammonium jarosite mixture by solid-to-liquid ratio 1: 3g/ml, adding NaOH controls pH value 13; 80 ℃, agitation leach 1.5 hours is filtered, filter residue through 350 ℃ of calcinings 2 hours purity is 99.5% iron oxide red; The 85 ℃ of adding sulfuric acid adjust pH 1.5 precipitation filtration washings of filtrating get red vanadium filter cake; 350 ℃ of calcinings of red cake 1.5 hours, the cooling back adds 45 ℃ in water by solid-to-liquid ratio 1: 3g/ml; Agitator treating 1.5 hours, filtering drying gets the V of purity 99.6%
2O
5Product.Liquid and wash water earlier change into 1.5 of sodium hydrogencarbonate chemical reaction stoichiometric number by sodium pyrosulfate in the solution and extraordinarily go into lime carbonate after the precipitation; Stirring at room 2 hours; Cross and filter sodium hydrogen carbonate solution and gypsum, sodium hydrogen carbonate solution adds 90 ℃ of causticizations of lime again and filters the mixing solutions that obtains sodium hydroxide and yellow soda ash to pH13.5.
Embodiment 2
With V
2O
5The bone coal acid dip solution 1000ml that meter contains vanadium 9.31g/L presses NH
4Al (SO
4)
212H
2The O crystal is separated out 1.5 times of adding (NH in leach liquor of chemical reaction stoichiometric number
4) SO
4, crystallization removes aluminium, and liquid adds CaCO after the crystallization
3Be neutralized to pH value to 2.0 and filter, filtrating becomes ferric iron and trivalent vanadium and tetravalence vanadium to be oxidized to 1.5 of pentavalent vanadium chemistry reaction stoichiometric number by oxidation of divalent and extraordinarily goes into hydrogen peroxide oxidation, and adding embodiment 1 obtains contains the vanadium jarosite and the ammonium jarosite mixture is done 60 ℃ of agitation leachs of crystal seed 2.0 hours; Deposition is separated out and is contained vanadium jarosite and ammonium jarosite mixture; Contain vanadium jarosite and ammonium jarosite mixture by solid-to-liquid ratio 1: 4.5g/ml, the sodium hydroxide that adding embodiment 1 obtains and the mixing solutions of yellow soda ash, 95 ℃ of agitation leachs were filtered in 1 hour; 65 ℃ of adding sulfuric acid adjust pHs, 2.0 precipitations of filtrating are crossed and are filtered red vanadium filter cake; 500 ℃ of calcinings of red cake 1 hour, the cooling back adds 65 ℃ in water by solid-to-liquid ratio 1: 4g/ml; Agitator treating 1 hour, filtering drying gets the V of purity 99.3%
2O
5Product; Filter residue adds 98% concentrated sulfuric acid dissolution by solid-to-liquid ratio 1: 2g/ml, and control terminal point pH is 2.5, crosses and filters polymeric ferrous sulphate solution, and 90~150 ℃ of normal pressures of polymeric ferrous sulphate solution are concentrated into and contain Fe>15wt%, and crystallisation by cooling gets ferric polysulfate solid.NH
4Al (SO
4)
212H
2After the O crystal is dissolved in water, adds lime and transfer pH to 4.5, stirred 1 hour and filter the ammonium sulfate regeneration soln.
Embodiment 3
With V
2O
5Meter contains the bone coal acid dip solution 500ml of vanadium 20.15g/L, adds the ammonium sulfate regeneration soln that embodiment 2 obtains, and Tai-Ace S 150 ammonium alum NH is separated out in crystallization
4Al (SO
4)
212H
2The O crystal filters, and liquid adds CaCO after the crystallization
3Be neutralized to pH value to 1.8 and filter, filtrating becomes ferric iron and trivalent vanadium and tetravalence vanadium to be oxidized to 1.5 of pentavalent vanadium chemistry reaction stoichiometric number by oxidation of divalent and extraordinarily goes into Sodium Persulfate, and adding embodiment 1 obtains contains the vanadium jarosite and the ammonium jarosite mixture is done 95 ℃ of agitation leachs of crystal seed 1 hour; Deposition is separated out and is contained vanadium jarosite and ammonium jarosite mixture, and precipitation mixture adds Pottasium Hydroxide control pH value 12.5 by solid-to-liquid ratio 1: 2.5g/ml; 55 ℃; Agitation leach 3 hours is filtered, filter residue through 450 ℃ of calcinings 1 hour purity is 99.7% iron oxide red, filtrate 95 ℃ to add 1.3 precipitations of sulfuric acid adjust pH and cross and filter red vanadium filter cake, red cake was calcined 1.5 hours for 400 ℃; The cooling back is by solid-to-liquid ratio 1: 6g/ml; Add 85 ℃ in water, agitator treating 0.5 hour, filtering drying gets the V of purity 99.5%
2O
5Product.
Claims (10)
1. bone coal pickling liquor vanadium extraction iron comprehensive recovering process may further comprise the steps: the mode through crystalline sulfuric acid aluminium ammonium alum in containing scherbinaite coal sulphuric leachate is removed aluminium; Liquid after the crystallization that obtains is added pH value regulator regulator solution acidity to pH1.0~3.5, cross and to filter liquid after the acid adjustment; Liquid adds the crystal seed oxidation and separates out and contain vanadium jarosite and ammonium jarosite deposition after the acid adjustment, and mistake filters liquid after the jarosite that contains vanadium and ammonium jarosite precipitation mixture and the precipitation; Contain the vanadium jarosite and ammonium jarosite precipitation mixture alkali soaks filtration, the alkali immersion liquid and the ferruginous alkali that must contain vanadium soak slag, and the alkali immersion liquid of gained adds the sulfuric acid acidation precipitation, red vanadium and deposition vanadium mother liquid; Red vanadium calcining after scouring obtains smart vanadium except that sodium, filtration, oven dry; Alkali soaks slag and adds sulfuric acid dissolution and produce bodied ferric sulfate, or with alkali soak slag calcine red stone; Described crystal seed is meant one or more in yellow modumite, jarosite, the ammonium jarosite; It is in the bone coal sulphuric leachate, to form 1~3 of Tai-Ace S 150 ammonium alum crystal chemistry reaction stoichiometric number by the aluminium in the bone coal sulphuric leachate extraordinarily to go into (NH that described crystalline sulfuric acid aluminium ammonium alum removes aluminium
4)
2SO
4, NH
4Cl, NH
4NO
3, NH
3H
2Among the O one or more make aluminium in the solution with NH
4Al (SO
4)
212H
2The crystallization of O form is separated out.
2. method according to claim 1 is characterized in that, described oxidation is separated out and is meant and after acid adjustment, adds H in the liquid
2O
2, NaClO
3And the peroxosulphuric ammonium in one or more.
3. method according to claim 1 is characterized in that, described alkali soaks and is meant in jarosite that contains vanadium and ammonium jarosite precipitation mixture and adds NaOH, KOH, Na
2CO
3, NaHCO
3, K
2CO
3, KHCO
3In one or more agitation leach precipitation mixtures in vanadium.
4. method according to claim 1 is characterized in that, described pH value regulator is meant CaCO
3, CaO, Ca (OH)
2, in the ammoniacal liquor, volatile salt, bicarbonate of ammonia one or more.
5. method according to claim 1 is characterized in that, described calcining is meant that the red vanadium that deposition is separated out removes wherein free-water and combination water through 250~550 ℃ of pyroprocessing.
6. according to each described method of claim 1-5; With described deposition vanadium mother liquid regenerate alkaline solution; Its operating process comprises: change into 1~3 of sodium hydrogen carbonate solution chemical reaction stoichiometric number by sodium bisulfate in the deposition vanadium mother liquid earlier and extraordinarily go into lime carbonate or Wingdale; Stirring at room 1~4 hour is crossed and is filtered sodium hydrogen carbonate solution and gypsum, and sodium hydrogen carbonate solution adds 50~100 ℃ of causticizations of lime to pH13~15 again and filters; Alkaline solution, alkaline solution returns and contains vanadium jarosite alkali and soak operation and recycle.
7. according to each described method of claim 1-5, with the Tai-Ace S 150 ammonium alum that obtains make the transition ammoniumsulphate soln; Described Tai-Ace S 150 ammonium alum makes the transition and is meant NH
4Al (SO
4)
212H
2After the O crystal is dissolved in water, adds lime and transfer pH to 3.5~8.5, make Al wherein change into Al (OH)
3Filter, gained filtrating is returned the crystallization of bone coal sulphuric leachate and is separated out Tai-Ace S 150 ammonium alum operation and recycle, and filter residue is stored up.
8. according to each described method of claim 1-5, liquid returns bone coal sulphuric leachate operation and recycles after the described precipitation.
9. method according to claim 1; It is characterized in that the described bodied ferric sulfate of producing is meant that containing vanadium jarosite and ammonium jarosite precipitation mixture alkali soaks the alkali that obtains and soak slag, 1: 1.0~5.0g/ml adds sulfuric acid dissolution by solid-to-liquid ratio; Control terminal point pH2.0~3.0; Cross and filter polymeric ferrous sulphate solution, 85~155 ℃ of normal pressures of polymeric ferrous sulphate solution are concentrated into and contain Fe>15wt%, and crystallisation by cooling gets ferric polysulfate solid.
10. method according to claim 1 is characterized in that, described calcining is meant that containing vanadium jarosite and ammonium jarosite precipitation mixture alkali soaks the alkali that obtains and soak slag, through 200~500 ℃ of pyroprocessing 1~3 hour, removes wherein free-water and combination water.
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CN112626338B (en) * | 2020-12-16 | 2022-02-25 | 中国科学院过程工程研究所 | Method for recovering vanadium and iron from tetravalent vanadium and divalent iron-containing acid solution |
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