CN102424914B - Method for comprehensively recovering aluminum and potassium from vanadium extraction from stone coal - Google Patents
Method for comprehensively recovering aluminum and potassium from vanadium extraction from stone coal Download PDFInfo
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- CN102424914B CN102424914B CN2011103864030A CN201110386403A CN102424914B CN 102424914 B CN102424914 B CN 102424914B CN 2011103864030 A CN2011103864030 A CN 2011103864030A CN 201110386403 A CN201110386403 A CN 201110386403A CN 102424914 B CN102424914 B CN 102424914B
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Abstract
The invention discloses a method for comprehensively recovering aluminum and potassium from vanadium extraction from stone coal. The technical process of the method mainly comprises: crystallizing pentaphyllum potassium aluminum sulfate in sulfuric acid leachate of stone coal; purifying pentaphyllum potassium aluminum sulfate recrystals, or adding water to dissolve the pentaphyllum potassium aluminum sulfate recrystals and adding a potassium-containing pH regulator to precipitate aluminum; filtering to obtain aluminum hydroxide and a potassium sulfate or potassium hydrogen sulfate solution; transforming the potassium sulfate or potassium hydrogen sulfate solution by lime to obtain potassium carbonate or potassium hydroxide; and thus, effectively separating and recovering aluminum and potassium. The method has the advantages that: the aluminum and potassium recovery rates are high; the products are diversified; impurities harmful to the recycling of water from vanadium extraction from stone coal are not introduced in the aluminum and potassium recovery technical process; the reagent consumption is small; the production cost is low; environment pollution is avoided; and the like.
Description
Technical field
The present invention relates to a kind of extracting vanadium from stone coal aluminium, potassium comprehensive recovering process.
Background technology
Bone coal is a kind of containing the vanadium multi-metal mineral wealth, usually contains SiO in bone coal
250%-75%, Al
2O
37%-17%, K
2O2%-5%, V
2O
50.15%-3.5%, containing V
2O
5Be greater than 0.8% bone coal and can be used as the navajoite exploitation.Aluminium in bone coal and potassium are mainly with potash mica (KAl
2(Si
3Al) O10 (OH)
2) and illite (K (Al, V)
2(Si, Al)
4O10 (OH)
2) form exist.The conventional process of extracting vanadium from stone coal is sulfuric acid leaching, and the technique of extracting at present vanadium from the bone coal acid dip solution has:
1) bone coal sulphuric leachate → ammonium salt is except the smart vanadium of aluminium → reduction → extraction → back extraction → oxidation → ammonium salt precipitation → calcine to obtain;
2) bone coal sulphuric leachate → ammonium salt is except the smart vanadium of aluminium → selective oxidation deironing → vanadium oxidation → ion-exchange → desorb → ammonium salt precipitation → calcine to obtain;
3) bone coal sulphuric leachate → ammonium salt is except the smart vanadium of aluminium → soak → purification and impurity removal of oxidation precipitation iron cpd → alkali → ammonium salt precipitation → calcine to obtain.
In the bone coal sulphuric leachate general containing Al up to 8~18g/L, the interference for fear of Al to the process for extracting vanadium process, the bone coal sulphuric leachate usually will add ammonia or ammonium salt to make aluminium in solution with Tai-Ace S 150 ammonium alum (NH before vanadium extraction
4Al (SO
4)
212H
2O) crystalline form is removed.Due to the complicated component of bone coal sulphuric leachate, add the chemical reagent that the process for extracting vanadium process adds, after vanadium extraction, liquid is recycled to the discharge of to a certain degree having to.Therefore, no matter the vanadium that adopts which kind of technique to extract in the bone coal sulphuric leachate all can produce ammonia nitrogen waste water, and the potassium in the bone coal sulphuric leachate does not all obtain effective recycling.
Summary of the invention
The object of the present invention is to provide and can avoid ammonia nitrogen waste water to produce, efficient recovery aluminium and potassium, improve the comprehensive utilization of resources rate, protection of the environment, a kind of extracting vanadium from stone coal aluminium, the potassium comprehensive recovering process that reduce production costs.
Technical scheme of the present invention comprises the following steps: in the bone coal sulphuric leachate, add rich potassium material except aluminium, the aluminium in solution is separated out with Tai-Ace S 150 arcanite (being alum) crystalline form, and guarantee after crystallization in liquid that the concentration of K maintains 0.1-15g/L; Tai-Ace S 150 arcanite recrystallization purification (can obtain high-purity alum); Or reclaim respectively aluminium and potassium after Tai-Ace S 150 arcanite transition, wherein Separation and Recovery obtains can be used as rich potassium material containing potassium solution and returns except the aluminium operation, also can join in Tai-Ace S 150 arcanite transformation process and recycle; Except after liquid vanadium extraction after aluminium, returning to bone coal acidleach operation, recycle.
Describedly add rich potassium material to refer in the bone coal sulphuric leachate and add K except aluminium
2SO
4, KHSO
4, KOH, K
2CO
3, KHCO
3In one or more, make aluminium in solution with Tai-Ace S 150 arcanite (KAl (SO
4)
212H
2O) form crystallization.
It is that Tai-Ace S 150 arcanite crystallisate is added to the water rising temperature for dissolving that described Tai-Ace S 150 arcanite is made the transition, add containing the potassium acidity regulator and make the transition, regulate pH value to 4.0~8.0 aluminium in solution is separated out with aluminum hydroxide precipitation, filter to obtain aluminum hydroxide filter cake and vitriolate of tartar and/or potassium hydrogen sulfate solution.
Described is KOH, K containing the potassium acidity regulator
2CO
3, KHCO
3In one or more.
The described water rising temperature for dissolving that adds refers to first and adds water by 1: 1~10g/ml of solid-to-liquid ratio, and 25~125 ℃ of stirrings make Tai-Ace S 150 arcanite dissolution of crystals.
Described aluminium hydroxide can, through calcining to obtain aluminum oxide, also can add sulfuric acid or dissolving with hydrochloric acid and obtain Tai-Ace S 150 or aluminum chloride.Described vitriolate of tartar and/or potassium hydrogen sulfate solution: can directly return to the bone coal sulphuric leachate and be used as rich potassium material except the aluminium operation; Also directly condensing crystal obtains vitriolate of tartar or sal enixum; Can also be to add calcium carbonate or barium carbonate to stir transition, filter to obtain gypsum or barium sulfate, and salt of wormwood and/or potassium bicarbonate solution.
Described calcining refers to that aluminium hydroxide obtains alumina product in 1-5 hour through 800-1250 ℃ of calcining.
Described vitriolate of tartar and/or potassium hydrogen sulfate solution add calcium carbonate or barium carbonate stirs 0.5-5 times that refers to transition by calcium sulfate or barium sulfate formation chemical reaction stoichiometric number, add calcium carbonate or barium carbonate, 0-100 ℃ is stirred 0.5-5 hour, make vitriolate of tartar or sal enixum in solution change into salt of wormwood or saleratus, filter to obtain calcium sulfate or barium sulfate solid, and salt of wormwood and/or potassium bicarbonate solution.
Described salt of wormwood and/or potassium bicarbonate solution directly return to the bone coal sulphuric leachate and are used as rich potassium material except the aluminium operation; Or return to Tai-Ace S 150 arcanite operation transition as containing the potassium acidity regulator; Or condensing crystal obtains salt of wormwood and/or saleratus, or add lime causticization, filter and to obtain calcium carbonate and alkalescence containing potassium solution.
Described salt of wormwood and/or potassium bicarbonate solution add lime causticization and refer to that the 0.15-3.5 by the chemical reaction stoichiometric number doubly adds calcium oxide or calcium hydroxide, 0-110 ℃ is stirred 1-3 hour, make salt of wormwood and/or saleratus in solution partly or entirely change into potassium hydroxide, filter and obtain alkalescence containing potassium solution.
Described alkalescence is directly returned to the bone coal sulphuric leachate containing potassium solution and is used as rich potassium material except the aluminium operation; Or return to Tai-Ace S 150 arcanite operation transition as recycling containing the potassium acidity regulator.
The present invention compares and has the following advantages and effect with existing technology:
Advantage of the present invention is that the potassium that dexterously recovery obtained is partly as the recycle of rich potassium material in technical process, rationally regulates aluminium in the bone coal pickling liquor/potassium mol ratio, makes aluminium wherein and potassium with Tai-Ace S 150 arcanite (KAl (SO
4)
212H
2O) form crystallization, the Tai-Ace S 150 arcanite subsequent disposal obtained can be carried out the diversity selection, directly further purifies or dissolve to make the transition into more value product required on other market.Therefore, the present invention purifies by Tai-Ace S 150 arcanite recrystallization, or becomes solution to make the transition by the potassium aluminium sulfate dissolution of crystals, to realize the high-recovery of aluminium and potassium, reclaim the variation of product, by technique of the present invention, can obtain comprising high-purity alum, aluminium hydroxide, aluminum oxide, K
2SO
4, KHSO
4, KOH, K
2CO
3, KHCO
3Deng product, K wherein
2SO
4, KHSO
4, KOH, K
2CO
3And KHCO
3Solution can be used as rich potassium material or recycle in the recovery process of aluminium and potassium containing the potassium acidity regulator; And can not introduce the impurity harmful to the extracting vanadium from stone coal water circulation use at aluminium of the present invention and potassium recovery process process.Integral body redesign by technique of the present invention, cooperatively interacting between each step, but thereby aluminium and potassium in efficient recovery extracting vanadium by acid leaching of stone coal liquid, avoided the generation of ammonia nitrogen waste water, reduce environmental pollution, also meet the development trend of China's energy-conserving and emission-cutting technology transformation.
Embodiment
Below in conjunction with embodiment, the invention will be further described, and following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Get containing V
2O
54.86g/L, the bone coal acid dip solution 2000ml of Al 13.46g/L, K 4.31g/L, first add calcium carbonate adjust pH to 1.5, then add 60g K
2CO
3Make aluminium in solution and the potassium form crystallization with alum, filter; Crystalline mother solution adds hydrogen peroxide to make ferrous iron wherein be oxidized to ferric iron and trivalent vanadium and tetravalence vanadium to be oxidized to the pentavalent vanadium, and 85 ℃ are stirred 0.5 hour, and vanadium and iron co-precipitation in solution are separated out, and filter containing liquid after vanadium ferric oxide and precipitation; Soak the recovery vanadium containing vanadium ferric oxide alkali, after precipitation, liquid returns to bone coal acidleach operation and recycles; After the alum that crystallization obtains adds the water rising temperature for dissolving by solid-to-liquid ratio 1: 3g/ml, stir and add potassium hydroxide to adjust pH 6.5, filtration washing, obtain aluminium hydroxide and potassium sulfate solution; Aluminium hydroxide obtains alumina product in 2 hours through 950 ℃ of calcinings; The potassium sulfate solution condensing crystal obtains potassium product.
Embodiment 2
Get containing V
2O
53.61g/L, the bone coal acid dip solution 3000ml of Al 11.35g/L, K 2.48g/L, the vitriolate of tartar 75g that adds embodiment 1 to obtain, make aluminium in solution and potassium with the form crystallization of alum, filters; After crystallization, liquid adds CaCO
3Be neutralized to the filtration of pH value to 2.0, filtrate is oxidized to ferric iron and trivalent vanadium and tetravalence vanadium by ferrous iron and is oxidized to 1.2 times of pentavalent vanadium chemistry reaction stoichiometric number and adds the potassium permanganate Oxidation at room temperature 6 hours, with strong alkali resin 201 * 7 absorption of bisulfate ion type, reclaims vanadium; Handing over rear liquid to return to bone coal acidleach operation recycles; After the alum of crystallization adds the water rising temperature for dissolving by solid-to-liquid ratio 1: 5g/ml, stir and add salt of wormwood to adjust pH 7.0, filtration washing, obtain aluminium hydroxide and potassium sulfate solution; Aluminium hydroxide adds sulfuric acid dissolution and obtains the Tai-Ace S 150 product; Potassium sulfate solution changes into 1.5 times of salt of wormwood chemical reaction stoichiometric number by vitriolate of tartar and adds barium carbonate, and 80 ℃ are stirred 2 hours, filter, and the filtrate condensing crystal obtains salt of wormwood.
Embodiment 3
Get containing V
2O
55.73g/L, the bone coal acid dip solution 1000ml of Al 9.13g/L, K 6.52g/L, first add calcium carbonate adjust pH to 1.6, then the salt of wormwood 15g that adds embodiment 2 to obtain, make aluminium in solution and potassium with the form crystallization of alum, filter; Crystalline mother solution first adds iron powder makes the ferric iron in solution be oxidized to ferrous iron, then reclaims vanadium with the P204 extraction; Raffinate returns to bone coal acidleach operation and recycles; After the alum of crystallization adds the water rising temperature for dissolving by solid-to-liquid ratio 1: 4g/ml, stir the salt of wormwood that adds embodiment 2 to obtain and adjust pH 72, filtration washing, obtain aluminium hydroxide and potassium sulfate solution; Aluminium hydroxide adds hydrochloric acid and dissolves to obtain the aluminum chloride product; Potassium sulfate solution changes into 2 times of salt of wormwood chemical reaction stoichiometric number by vitriolate of tartar and adds calcium carbonate, and 60 ℃ are stirred 3 hours transition, filtration washing; After transition, liquid adds 95 ℃, lime to stir 2 hours by 2 times of salt of wormwood causticization chemical reaction stoichiometric number again, filters to obtain potassium hydroxide solution.
Claims (6)
1. an extracting vanadium from stone coal aluminium, potassium comprehensive recovering process comprise the following steps: in the bone coal sulphuric leachate, add rich potassium material except aluminium, make aluminium in solution and potassium with Tai-Ace S 150 arcanite KAl (SO
4)
212H
2The form of O crystal is separated out, after crystallization in liquid the concentration of K maintain 0.1-15g/L; The Tai-Ace S 150 arcanite of gained reclaims respectively aluminium and potassium after transition, and wherein Separation and Recovery obtains containing potassium solution, as rich potassium material, return except the aluminium operation or join in Tai-Ace S 150 arcanite transformation process recycles; Except liquid after aluminium adopts solvent extration or ion exchange method or vanadium iron coprecipitation method Separation and Recovery vanadium wherein, after vanadium extraction, liquid returns to bone coal acidleach operation and recycles;
Described rich potassium material is K
2SO
4, KHSO
4, KOH, K
2CO
3, KHCO
3In one or more;
It is that Tai-Ace S 150 arcanite crystallisate is added to the water rising temperature for dissolving that described Tai-Ace S 150 arcanite makes the transition, add containing the potassium acidity regulator, regulate pH value to 4.0~8.0, the aluminium in solution is separated out with aluminum hydroxide precipitation, filter to obtain aluminum hydroxide filter cake, and vitriolate of tartar and/or potassium hydrogen sulfate solution;
Described vitriolate of tartar and/or potassium hydrogen sulfate solution directly return to the bone coal sulphuric leachate and are used as rich potassium material except the aluminium operation; Or directly condensing crystal obtains vitriolate of tartar and/or sal enixum; Or add calcium carbonate or barium carbonate transition, filter to obtain gypsum or barium sulfate, and salt of wormwood and/or potassium bicarbonate solution.
2. method according to claim 1, is characterized in that, the described water rising temperature for dissolving that adds refers to first and add water by solid-to-liquid ratio 1:1~10g/ml, and 25~125 ℃ of stirrings make Tai-Ace S 150 arcanite dissolution of crystals.
3. method according to claim 1 and 2, is characterized in that, described is KOH, K containing the potassium acidity regulator
2CO
3, KHCO
3In one or more.
4. method according to claim 1 and 2, described aluminium hydroxide, through calcining to obtain aluminum oxide; Or add sulfuric acid or dissolving with hydrochloric acid obtains Tai-Ace S 150 or aluminum chloride.
5. method according to claim 4, is characterized in that, described calcining refers to that aluminium hydroxide obtains alumina product in 1-5 hour through 800-1250 ℃ of calcining.
6. method according to claim 1, it is characterized in that, described vitriolate of tartar and/or potassium hydrogen sulfate solution add calcium carbonate or barium carbonate refer to transition form the chemical reaction stoichiometric number by calcium sulfate or barium sulfate 0.5-5 doubly, add calcium carbonate or barium carbonate, 0-100 ℃ is stirred 0.5-5 hour, make vitriolate of tartar or sal enixum in solution change into salt of wormwood or saleratus, filter to obtain calcium sulfate or barium sulfate solid, and salt of wormwood and/or potassium bicarbonate solution.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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EP3214190A1 (en) * | 2016-03-01 | 2017-09-06 | SMS Siemag Process Technologies GmbH | Process for the separation of vanadium |
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CN112125325A (en) * | 2020-09-29 | 2020-12-25 | 福州大学 | Process for producing alumina by aluminosilicate mineral acid method |
CN114797768B (en) * | 2022-03-22 | 2023-08-11 | 中南大学 | Magnesium phosphate double salt-activated carbon composite material, preparation method thereof and application thereof as potassium ion adsorption material |
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CN101898791B (en) * | 2010-06-25 | 2012-10-03 | 四川龙蟒钛业股份有限公司 | Method for preparing rutile titanium dioxide from new process titanium slag |
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Publication number | Priority date | Publication date | Assignee | Title |
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EP3214190A1 (en) * | 2016-03-01 | 2017-09-06 | SMS Siemag Process Technologies GmbH | Process for the separation of vanadium |
WO2017148922A1 (en) * | 2016-03-01 | 2017-09-08 | Sms Group Process Technologies Gmbh | Process for the separation of vanadium |
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