CN113416847B - Method for recycling, reducing and harmlessly treating vanadium extraction tailings - Google Patents
Method for recycling, reducing and harmlessly treating vanadium extraction tailings Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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Abstract
The invention discloses a method for recycling, reducing and harmlessly treating vanadium extraction tailings. Through the component analysis of the vanadium extraction tailings, the vanadium extraction tailings are subjected to resource, reduction and harmless treatment by a method combining a pyrogenic process and a wet process, and the process comprises the steps of heating and dissolving, adding alkali and deaminating, filtering, preparing ammonium sulfate by sulfuric acid, sodium roasting, extracting vanadium, evaporating and concentrating, and centrifuging. The process has reasonable design, fully utilizes the properties of various chemical elements and compounds thereof under different conditions, realizes the separation and recovery of elements such as N, Na, V, Cr and the like in the vanadium extraction tailings, and has high economic benefit. The method is environment-friendly and high in resource utilization rate, can recover vanadium pentoxide and high-valence chromium, and can reasonably remove other substances such as sodium sulfate, ammonium sulfate and the like. The method has industrial application value.
Description
Technical Field
The invention relates to a method for recycling, reducing and harmlessly treating vanadium extraction tailings, belonging to the technical field of resource utilization.
Background
In the process of extracting vanadium, after vanadium pentoxide in the vanadium titano-magnetite is extracted by a sodium roasting process, high-content vanadium pentoxide still exists in tailings. The vanadium pentoxide flows out along with the process flow and finally exists in the vanadium precipitation waste liquid, and the vanadium precipitation waste liquid is evaporated and crystallized to finally form vanadium extraction tailings. Because the vanadium pentoxide content in each batch of raw ore is different, the vanadium pentoxide content in each batch of vanadium extraction tailings is different. In the process of extracting vanadium pentoxide, because the components of tailings are different from those of raw ores, certain difference exists in the extraction process and certain technical difficulty exists.
The main component of the vanadium extraction tailings is sodium sulfate crystals, and a small amount of ammonium sulfate is also contained. Also contains oxides of calcium, magnesium, aluminum, iron, silicon, vanadium, chromium, etc., and other compounds. These components are derived from raw ore.
At present, a plurality of treatment methods for some vanadium extraction tailings are adopted in China, and the methods are greatly different. However, most methods lack the overall control of the vanadium extraction tailings, and are mainly resource, reduction and harmless treatment of a plurality of steps or a plurality of metal oxides or compounds. Among them, the methods for treating and recovering vanadium pentoxide and reducing high-valence chromium are important. Most of the processes adopt a pyrogenic process to carry out sodium roasting on vanadium pentoxide to convert the vanadium pentoxide into soluble vanadate, then adopt wet acid leaching or alkali leaching to enable the vanadium to enter a liquid phase, and finally precipitate the vanadium through an extraction or precipitation method and the like.
The research results of a plurality of vanadium extraction tailings and vanadium extraction technologies are summarized in volume 36, No. 3 of 6.2015 of Steel vanadium and titanium. The method for extracting vanadium by normal-pressure acid leaching comprises the steps of destroying the crystal structure of mineral silicate minerals by using HF acid, dissolving insoluble high-valence vanadium in raw materials, oxidizing the vanadium by using an oxidant NaClO, and converting the oxidized vanadium into VOSO (volatile organic Compounds) which is more stably present in a sulfuric acid solution4The extraction of vanadium in the steel-climbing vanadium extraction tailings under normal pressure can be realized by adopting the combination of sulfuric acid, hydrofluoric acid and sodium hypochlorite. Adding fluorine-containing leaching aid CaF into normal-pressure acid leaching vanadium extraction2And (5) enhancing vanadium extraction. In addition, a method for extracting vanadium by using pressurized acid is also provided, and the fact that the mass concentration of sulfuric acid and the solid mass ratio of reaction liquid are increased to be beneficial to leaching is determined by a single-factor comparison test. And then the minerals are ground, so that the vanadium leaching rate can be obviously increased.
In the university of Kunming 'paper sodium extraction vanadium tailings sodium removal test research', it is mentioned that the vanadium extraction tailings are steelmaking slag (V)2O5Content of 10% -18%) through sodium salt roasting, water leaching, precipitation, alkali dissolution and ammonium salt vanadium precipitation, and finally obtaining waste residue obtained after ammonium metavanadate is pyrolyzed to obtain vanadium oxide, wherein most of soluble vanadium is extracted, the residual vanadium in the tailings exists in the form of acid-base insoluble low-valence vanadium, and the content of the vanadium is 1.5%, which is far higher than that of V in general vanadium-containing concentrate2O5Grade of (2). It is mentioned that the vanadium in the part of the vanadium extraction tailings is subjected to sodium salt roasting, and the process isThe method is a traditional vanadium extraction process, has high vanadium extraction rate, but has high energy consumption and can cause secondary environmental pollution.
Foreign research on recycling residual vanadium from vanadium extraction tailings is less, vanadium in the vanadium extraction tailings is generally recycled by carbon thermal reduction, and then vanadium is enriched into molten iron to produce vanadium-containing pig iron, and then vanadium is oxidized by an induction furnace to enter vanadium slag, so that vanadium slag with high vanadium content is obtained to recycle the vanadium.
Disclosure of Invention
The invention aims to provide a method which is reasonable in process design and can effectively realize the recycling, reduction and harmlessness of vanadium extraction tailings. The fire method-wet method combined process is adopted to efficiently recover elements such as V, Cr, Na and the like in the vanadium extraction tailings.
The invention relates to a method for recycling, reducing and harmlessly treating vanadium extraction tailings, which comprises the following specific steps:
s1, heating and dissolving: adding water into the vanadium extraction tailings, heating and stirring to dissolve soluble components in the tailings to obtain a mixture, wherein residual solids in the mixture exist in a metal oxide form;
s2: GBS reduction: adding water treatment agent GBS solution into the mixture obtained from S1, wherein the GBS solution is composed of NaOH and Na2S2O3、NaHSO3Composition of NaOH, Na2S2O3、NaHSO3The mass ratio is 5: 3: 2. adding the vanadium and the chromium which are 2-2.5 times of the sum of the mass of the vanadium and the chromium in the vanadium extraction tailings, heating, stirring and dissolving, reducing hexavalent chromium in the mixture into trivalent chromium, and reducing pentavalent vanadium into trivalent vanadium or tetravalent vanadium;
s3: adding alkali to deaminate: continuously adding 0.6-1mol/L NaOH solution into the mixture, wherein the mass ratio of the NaOH solution to the vanadium extraction tailings is 1.3-1.5:1, removing and collecting ammonium ions in the form of ammonia gas, and separating out trivalent chromium ions in the form of chromium hydroxide precipitate; preparing ammonium sulfate, dissolving the collected ammonia gas in sulfuric acid to form ammonium sulfate, and recycling the ammonium sulfate to the S6 vanadium precipitation process; filtering to separate soluble substances from insoluble substances;
s4: sodium treatment roasting: adding sodium carbonate with the mass of 1.5-2 times that of vanadium in the filter residue into the filter residue after filtration, and performing sodium salt roasting at the temperature of 580-750 ℃ for 4-6h to obtain soluble sodium vanadate, wherein the chromium hydroxide is changed into insoluble chromium sesquioxide;
s5: and (3) vanadium and chromium separation: dissolving the roasted tailings in water, and filtering and separating to obtain chromium trioxide filter residues and a mixed solution containing sodium vanadate;
s6: and (3) vanadium precipitation process: adding 1.5-2.5mol/L ammonium sulfate solution and 50-70g/L sulfuric acid into the mixed solution containing sodium vanadate, wherein the volume ratio of the ammonium sulfate solution to the mixed solution containing sodium vanadate is 0.6-0.8:1, and the volume ratio of the sulfuric acid to the solution containing sodium vanadate is 0.4-0.6:1, so that sodium vanadate is converted into ammonium polyvanadate and is separated out;
s7: pyrolysis of ammonium polyvanadate: performing solid-liquid separation, namely pyrolyzing the obtained ammonium polyvanadate filter residue for 3-5h at the temperature of 80-100 ℃ to generate a vanadium pentoxide product; evaporating and concentrating the filtrate to separate out sodium sulfate in the solution, simultaneously separating out a small part of soluble substances which are not removed in other previous steps, and then carrying out centrifugal separation on the separated soluble substances to obtain a high-purity sodium sulfate product.
Further, the main components of the vanadium extraction tailings comprise: v: 1-2.5%, Cr: 0.1-1%, O: 30-40%, S: 20-25%, Na: 20 to 25 percent.
Furthermore, the water adding amount of S1 is to add water according to 5ml/g of vanadium extraction tailings, heat the mixture to 40-50 ℃, and stir at the rotation speed of 350-400 rpm.
Further, the GBS solution S2 is heated to 40-50 ℃ and stirred to dissolve, and the stirring speed is 350-400 rpm.
The mechanism and the advantages of the invention are briefly described as follows:
by adopting the process route, the invention fully utilizes the properties of each element and compound under specific conditions and realizes the high-efficiency separation of each element. Treating elements in the vanadium extraction tailings by using a technological process combining a pyrogenic process and a wet process; the method comprises the steps of heating and adding alkali to dissolve and separate ammonia and sodium, GBS reducing chromium, sodium roasting, vanadium-chromium separation, vanadium precipitation and vanadium extraction, heating and dissolving vanadium extraction tailings, transferring soluble sodium sulfate and ammonium sulfate into a liquid phase, adding sodium hydroxide to remove ammonium sulfate, removing ammonium ions in the form of ammonia gas, dissolving in sulfuric acid to form ammonium sulfate, and introducing the ammonium sulfate into a reaction kettleAnd recycling to the process in one step. The residual sodium sulfate is evaporated, crystallized and extracted. Adding sodium carbonate into the residual solid phase tailings, and roasting at 580-750 ℃. The insoluble vanadium compound is changed into soluble vanadate, the phase structure of the vanadium slag is destroyed by an oxidation method at high temperature, vanadium is oxidized from low valence to the highest pentavalence, and simultaneously, water-soluble sodium vanadate is generated. Then adding ammonium salt and sulfuric acid to precipitate vanadium, and pyrolyzing the precipitate to obtain a final product V2O5. The reduction method for chromium is GBS reduction. The process can realize the recycling of all elements, realize harmless, reduction and recycling treatment, and does not produce secondary pollution in the process.
The chemical reaction equation generated by the invention is as follows:
(NH4)2SO4+2NaOH==Na2SO4+2NH3+2H2O
Cr3++3（OH）—==Cr3(OH)
2Cr(OH)3==Cr3O3+3H2O
2NH3+H2SO4==(NH4)2SO4
V2O3+O2==V2O5
2Na2CO3==Na2O+2CO2+0.5O2
Na2O+V2O5==2NaVO3
6NaVO3+2H2SO4+(NH4)2SO4==(NH4)2H2V6O17+3Na2SO4+H2O
(NH4)2H2V6O17==3V2O5+2NH3+2H2O
compared with the prior art, the process more comprehensively treats the vanadium extraction tailings, recovers all parts of important elements with high recovery value in the vanadium extraction tailings, is superior to singly recovering and treating one of the substances in the original process, and well realizes the recycling, reduction and harmless treatment of the vanadium extraction tailings. The process has high economic benefit and environmental protection value.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting in any way, and any modifications or alterations based on the teachings of the present invention are intended to fall within the scope of the present invention.
Example 1:
the main materials in the vanadium extraction tailings comprise the following components: the vanadium extraction tailings comprise the following main components in percentage by mass, 1.34% of V, 0.19% of Cr, 34.87% of O, 20.35% of S and 22.82% of Nas. Weighing 100g of vanadium extraction tailings, and grinding the vanadium extraction tailings into powder with the size of 200-400 meshes. The powder was dissolved in 500ml of water, heated to 40 ℃ and stirred for 1h at 350rpm to dissolve all the solubles. Adding 3.8g GBS solution into the mixture, stirring at 45 deg.C and 400rpm for 1h, adding 1mol/L NaOH solution 150ml into the stirred solution, filtering to obtain 4.9296g filter residue, adding Na into the filter residue2CO32.0g, uniformly mixed and then put into a muffle furnace to be roasted for 4 hours at 750 ℃. And dissolving the roasted tailings, and filtering and separating to obtain 2.3321g of chromic oxide-containing slag. And adding 400ml of 1.5mol/L ammonium sulfate solution and 200ml of 50g/L sulfuric acid into the mixed solution, filtering to obtain ammonium polyvanadate, and pyrolyzing the ammonium polyvanadate for 3 hours to obtain vanadium pentoxide.
Example 2:
the main materials in the vanadium extraction tailings comprise the following components: the vanadium extraction tailings comprise the following main components in percentage by mass, 1.96% of V, 0.67% of Cr, 35.73% of O, 22.61% of S and 24.62% of Na24.62%. Weighing 100g of vanadium extraction tailings, and grinding the vanadium extraction tailings into powder with the size of 200-400 meshes. The powder was dissolved in 500ml of water, heated to 45 ℃ and stirred for 1.5h at 400rpm to dissolve all the solubles. To the mixture was added 5.2g of GBS solution, and the mixture was stirred at 50 ℃ for 2 hours at 350rpm, and 140ml of 0.8mol/L NaOH solution was added to the stirred solution, which was then filtered,5.2614g of filter residue is obtained, and Na is added into the filter residue2CO33.4g, uniformly mixing, putting into a muffle furnace, and roasting at 750 ℃ for 5 hours. And dissolving the roasted tailings, and filtering and separating to obtain 2.3321g of chromic oxide-containing slag. And adding 350ml of 2mol/L ammonium sulfate solution and 250ml of 70g/L sulfuric acid into the mixed solution, filtering to obtain ammonium polyvanadate, and pyrolyzing the ammonium polyvanadate for 4 hours to obtain vanadium pentoxide.
Example 3:
the main materials in the vanadium extraction tailings comprise the following components: the vanadium extraction tailings comprise the following main components in percentage by mass, 1.67% of V, 0.48% of Cr, 35.24% of O, 19.63% of S and 23.71% of Na23. Weighing 100g of vanadium extraction tailings, and grinding the vanadium extraction tailings into powder with the size of 200-400 meshes. The powder was dissolved in 500ml of water, heated to 40 ℃ and stirred for 1h at 350rpm to dissolve all the solubles. The insoluble matter was separated from the soluble matter by centrifugation, and the insoluble matter was dried to obtain 28.5016 g. Adding 4.8g GBS solution, stirring at 45 deg.C and 400rpm for 1h, adding 0.6mol/L NaOH solution 130ml into the stirred solution, filtering to obtain 4.7296g residue, adding Na into the residue2CO33.3g, uniformly mixing, putting into a muffle furnace, and roasting at 750 ℃ for 6 hours. And dissolving the roasted tailings, and filtering and separating to obtain 2.3321g of chromic oxide-containing slag. And adding 200ml of 1.5mol/L ammonium sulfate solution and 100ml of 50g/L sulfuric acid into the mixed solution, filtering to obtain ammonium polyvanadate, and pyrolyzing the ammonium polyvanadate for 5 hours to obtain vanadium pentoxide.
Claims (7)
1. A method for recycling, reducing and harmlessly treating vanadium extraction tailings is characterized by comprising the following steps:
s1, heating and dissolving: adding water into the vanadium extraction tailings, heating and stirring to dissolve soluble components in the tailings to obtain a mixture, wherein residual solids in the mixture exist in a metal oxide form;
s2: GBS reduction: adding a water treatment agent GBS solution into the mixture obtained in the step S1, heating, stirring and dissolving, reducing hexavalent chromium in the mixture into trivalent chromium, and reducing pentavalent vanadium into trivalent vanadium or tetravalent vanadium; the GBS solution is composed of NaOH and Na2S2O3、NaHSO3Composition of NaOH, Na2S2O3、NaHSO3The mass ratio is 5: 3: 2; the adding mass of the GBS solution is 2-2.5 times of the sum of the mass of vanadium and chromium in the vanadium extraction tailings;
s3: adding alkali to deaminate: continuously adding 0.6-1mol/L NaOH solution into the mixture, removing and collecting ammonium ions in the form of ammonia gas, and separating out trivalent chromium ions in the form of chromium hydroxide precipitate; dissolving the collected ammonia gas in sulfuric acid to form ammonium sulfate, and recycling the ammonium sulfate to S6 vanadium precipitation process;
s4: sodium treatment roasting: filtering, adding sodium carbonate into the filtered filter residue, and performing sodium treatment roasting at 580-750 ℃ to obtain soluble sodium vanadate, wherein the chromium hydroxide is changed into insoluble chromium sesquioxide;
s5: and (3) vanadium and chromium separation: dissolving the roasted tailings in water, and filtering and separating to obtain chromic oxide filter residues and a mixed solution containing sodium vanadate;
s6: and (3) vanadium precipitation process: adding 1.5-2.5mol/L ammonium sulfate solution and 50-70g/L sulfuric acid into the mixed solution containing sodium vanadate to convert the sodium vanadate into ammonium polyvanadate and separate out;
s7: pyrolysis of ammonium polyvanadate: and (3) performing solid-liquid separation, evaporating and concentrating the filtrate, performing centrifugal separation to obtain a high-purity sodium sulfate product, and pyrolyzing the obtained ammonium polyvanadate filter residue for 3-5h at the temperature of 80-100 ℃ to generate a vanadium pentoxide product.
2. The method for recycling, reducing and harmlessly treating the vanadium extraction tailings according to claim 1, wherein the vanadium extraction tailings mainly comprise the following components: v: 1-2.5%, Cr: 0.1-1%, O: 30-40%, S: 20-25%, Na: 20 to 25 percent.
3. The method for resource, reduction and innocent treatment of the vanadium extraction tailings as claimed in claim 1, wherein the water addition amount of S1 is that water is added according to 5ml/g of the vanadium extraction tailings, the mixture is heated to 40-50 ℃, and the stirring speed is 350-400 rpm.
4. The method for recycling, reducing and harmlessly treating the vanadium extraction tailings as claimed in claim 1, wherein the GBS solution of S2 is heated to 40-50 ℃ and stirred to dissolve, and the stirring speed is 350-400 rpm.
5. The method for resource, reduction and harmless treatment of the vanadium extraction tailings according to claim 1, wherein the addition amount of the NaOH solution in S3 is 1.3-1.5:1 of the mass ratio of the NaOH solution to the vanadium extraction tailings.
6. The method for recycling, reducing and harmlessly treating the vanadium extraction tailings according to claim 1, wherein the addition amount of S4 sodium carbonate is 1.5-2 times of the mass of the added vanadium filter residue, and the roasting time is 4-6 h.
7. The method for recycling, reducing and harmlessly treating the vanadium extraction tailings according to claim 1, wherein the volume ratio of the mixed solution of the ammonium sulfate solution and the sodium vanadate in S6 is 0.6-0.8:1, and the volume ratio of the mixed solution of the sulfuric acid and the sodium vanadate is 0.4-0.6: 1.
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| CN111087019A (en) * | 2018-10-23 | 2020-05-01 | 宜宾学院 | Method for extracting vanadium and chromium from vanadium slag vanadium extraction wastewater |
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| CN103276205B (en) * | 2013-05-29 | 2014-12-10 | 东北大学 | Method for separating and extracting vanadium and chromium from vanadium chromium leaching liquor |
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