CN114164348A - Method for extracting vanadium in sulfuric acid leaching solution reduced by waste vanadium-poor catalyst - Google Patents
Method for extracting vanadium in sulfuric acid leaching solution reduced by waste vanadium-poor catalyst Download PDFInfo
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- CN114164348A CN114164348A CN202111085756.7A CN202111085756A CN114164348A CN 114164348 A CN114164348 A CN 114164348A CN 202111085756 A CN202111085756 A CN 202111085756A CN 114164348 A CN114164348 A CN 114164348A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 112
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 112
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000002699 waste material Substances 0.000 title claims abstract description 60
- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- 238000002386 leaching Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 vanadyl hydroxide Chemical compound 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims abstract description 13
- 229910000352 vanadyl sulfate Inorganic materials 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 229940041260 vanadyl sulfate Drugs 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 9
- 239000012452 mother liquor Substances 0.000 claims description 8
- 235000011152 sodium sulphate Nutrition 0.000 claims description 8
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002893 slag Substances 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 description 10
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 6
- 239000003513 alkali Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical group O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000007832 Na2SO4 Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 125000005287 vanadyl group Chemical group 0.000 description 1
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
-
- 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
- C22B7/007—Wet processes by acid leaching
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for extracting vanadium from a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst, which comprises the following steps: adding a waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass fraction being more than or equal to 3% into a container, heating to 70-80 ℃, keeping the temperature, adding sodium hydroxide to adjust the pH value of the solution to 7-8, stirring and reacting for 1-2 hours, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residues into a sodium hydroxide solution with mass fraction being 8-12%, introducing air or adding hydrogen peroxide to convert vanadyl hydroxide into a colorless or light yellow sodium metavanadate solution, keeping stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, adding sodium metavanadate into the solution, filtering and washing to remove insoluble substances, concentrating, crystallizing, centrifuging and drying the filtrate to obtain a sodium metavanadate product; the method scientifically and environmentally recovers the vanadium in the waste lean vanadium catalyst, does not generate waste water and waste gas except a small amount of iron oxide slag, is environment-friendly, and is suitable for popularization.
Description
Technical Field
The invention relates to the technical field of vanadium recovery, in particular to a method for extracting vanadium in a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst.
Background
Vanadium and its compounds are important raw materials in metallurgical and chemical industries, and have wide application in industrial departments of machinery, construction, shipbuilding, automobile, national defense, electronics, and the like. However, vanadium is distributed in nature and production mining is largely recovered as a by-product in mining and processing other metal ores or from vanadium-containing waste. Vanadium recovery from spent vanadium catalysts is also an important route.
The vanadium content in the waste lean vanadium catalyst is about 2.5 percent (wt), the vanadium content in the conventional waste vanadium catalyst is about 5 percent, and compared with the conventional waste vanadium catalyst, the waste lean vanadium catalyst is low in recovery rate, higher in extraction difficulty and higher in medicament consumption, so that many enterprises do not want to recover vanadium from the waste lean vanadium catalyst as a raw material, but directly treat the waste lean vanadium catalyst as waste, and the vanadium content in the waste lean vanadium catalyst does not reach the standard and needs to be treated by professional waste treatment companies, so that the recovery benefit is not brought, and extra waste treatment cost is caused. Therefore, the development of a recovery method suitable for extracting vanadium from the waste lean vanadium catalyst realizes the purpose of recovering vanadium in the waste lean vanadium catalyst with low cost and environmental friendliness, and becomes a problem to be solved urgently in the industry.
Disclosure of Invention
The method provided by the invention aims at solving the problems that in the industry at present, because the waste lean vanadium catalyst is low in recovery rate, high in extraction difficulty and high in medicament consumption, people are very willing to recover the waste lean vanadium catalyst to extract vanadium, vanadium resources in the waste lean vanadium catalyst are wasted, and extra treatment cost is added for enterprises, and provides the method for extracting vanadium in the sulfuric acid leaching solution by reducing the waste lean vanadium catalyst.
The invention relates to a method for extracting vanadium from a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst, which comprises the following steps: adding a waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass fraction being more than or equal to 3% into a container, heating to 70-80 ℃, keeping the temperature, adding sodium hydroxide to adjust the pH of the solution to 7-8, stirring and reacting for 1-2 hours, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residue into 8-12% sodium hydroxide solution by mass fraction, introducing air or adding hydrogen peroxide to convert vanadyl hydroxide into colorless or light yellow sodium metavanadate solution with the pH of the solution reaching 10-12, continuously stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, filtering and washing to remove insoluble substances, concentrating, crystallizing, centrifuging and drying the filtrate to obtain a sodium metavanadate product
And further, adjusting the pH value of the filtrate after filtering and removing the vanadyl hydroxide to 9.5-10.5 by using sodium hydroxide, evaporating, crystallizing, dehydrating, drying and recovering sodium sulfate, wherein trace vanadium exists in the mother liquor in the form of sodium metavanadate, when the mass fraction of vanadium in the mother liquor is accumulated to be more than 1%, the vanadium is converged into a reduction leaching solution, and a small amount of sodium sulfite is supplemented to convert the vanadium into vanadyl sulfate.
The leaching solution for reducing sulfuric acid by the waste lean vanadium catalyst is prepared by crushing the waste lean vanadium catalyst to 250-350 mu m, adding the crushed waste lean vanadium catalyst into dilute sulfuric acid with the mass fraction of 3-5%, simultaneously adding sodium bisulfite with the mass of 1-2 times of that of vanadium, stirring, dissolving and filtering to obtain the leaching solution for reducing sulfuric acid by the waste lean vanadium catalyst with the mass fraction of vanadium being more than or equal to 3%.
The process principle of the invention is as follows: firstly, the waste lean vanadium catalyst is treated by the processes of crushing, dilute sulfuric acid, sodium bisulfite leaching separation and the like to obtain a waste lean vanadium catalyst reduction sulfuric acid leaching solution containing more than 3 percent of vanadium, wherein the vanadium exists in the solution in a reduction state (mainly VOSO)4) Since vanadium in its reduced state readily forms the hydroxide VO (OH)2Precipitated and hardly dissolved in water (wherein VO (OH)2KSP of 5.9X 10-23) Thus, vanadium precipitate can be easily separated from the solution through alkali neutralization treatment, the vanadyl hydroxide obtained through separation is added with sodium hydroxide, oxygen or hydrogen peroxide is introduced to oxidize the vanadyl hydroxide into vanadic anhydride, the vanadyl pentoxide reacts with alkali to generate sodium metavanadate solution, and the sodium metavanadate solution is prepared through filtration, concentration, crystallization and centrifugation, namely the vanadium in the waste lean vanadium catalyst is easily recycled. Filtering the filtrate after vanadyl hydroxide, firstly adjusting the pH value to 10 +/-0.5 by using alkali, evaporating, crystallizing and recovering anhydrous sodium sulfate, wherein trace vanadium exists in mother liquor in the form of sodium metavanadate, adding a waste vanadium-poor catalyst to reduce sulfuric acid leaching solution when the concentration gradually accumulates to be more than 1%, and adding a small amount of sodium sulfite to convert sodium metavanadate into vanadyl sulfate. The main chemical reaction equations involved are as follows:
V2O5 + 2H2SO4 + NaHSO3 = 2VOSO4 + NaHSO4 + 2H2O;
VOSO4 + 2NaOH = VO(OH)2↓ + Na2SO4;
4VO(OH)2 + O2 = 2V2O5 + 4H2O;
V2O5 + 2NaOH = 2NaVO3 + H2O。
the method has the advantages of simple process introduction, simple operation and high vanadium recovery rate (more than 97 percent), provides a scientific, reasonable and high economic benefit extraction process for extracting vanadium from waste lean vanadium, does not generate waste water and waste gas except a small amount of iron oxide slag in the whole process, is environment-friendly, and is suitable for wide popularization and use.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The process of the present invention is further illustrated by the following specific examples, which are intended to be purely exemplary and are not intended to limit the invention in any way.
Example 1
Referring to fig. 1, a method for extracting vanadium from a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst comprises the following steps: adding 1000g of waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass fraction of 3.1% into a container, heating to 70 ℃ for heat preservation, adding sodium hydroxide to adjust the pH value of the solution to 7.5, continuously stirring for reaction for 1 hour, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residue into 10% sodium hydroxide solution, adding hydrogen peroxide until the solution is light yellow and the pH value reaches 11, continuously stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, filtering and washing to remove insoluble substances (the filter residue is ferric oxide and is discarded), concentrating, crystallizing, centrifuging and drying the filtrate to obtain 74.2g of sodium metavanadate product, wherein the vanadium content in the prepared sodium metavanadate product is 41.06%, and the recovery rate of vanadium is 98.28%.
Further, filtering to remove the filtrate of the vanadyl hydroxide, adjusting the pH of the solution to 10 by using sodium hydroxide, evaporating, crystallizing, dehydrating and drying to obtain a sodium sulfate product, wherein the content of sodium sulfate is 98%. And when the mass fraction of vanadium in the mother liquor is accumulated to more than 1%, the vanadium is converged into a spent vanadium-poor catalyst reduction sulfuric acid leaching solution, and a small amount of sodium sulfite is supplemented to convert the vanadium into vanadyl sulfate.
The waste lean vanadium catalyst reduction sulfuric acid leaching solution is prepared by crushing the waste lean vanadium catalyst to 300 mu m, adding the crushed waste lean vanadium catalyst into dilute sulfuric acid with the mass fraction of 5%, simultaneously adding sodium bisulfite with the mass of 1.5 times of that of vanadium, stirring, dissolving and filtering to obtain the waste lean vanadium catalyst reduction sulfuric acid leaching solution with the mass fraction of 3.1% of vanadium.
Example 2
A method for extracting vanadium in a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst comprises the following steps: adding 1000g of waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass percentage of 3.12% into a container, heating to 75 ℃, keeping the temperature, adding sodium hydroxide to adjust the pH value of the solution to 7, continuously stirring for reaction for 1.5 hours, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residue into a sodium hydroxide solution with mass percentage of 8%, adding hydrogen peroxide until the solution is light yellow and the pH value reaches 12, continuously stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, adding insoluble substances into the solution, filtering and washing to remove insoluble substances (the filter residue is ferric oxide, discarding), concentrating, crystallizing, centrifuging and drying the filtrate to obtain 74.7g of sodium metavanadate product, wherein the vanadium content in the prepared sodium metavanadate is 41.1%, and the recovery rate of vanadium is 98.4%.
Further, the pH value of the filtrate which is filtered to remove the vanadyl hydroxide is adjusted to 9.5 by using sodium hydroxide, and sodium sulfate products are obtained by evaporation crystallization, dehydration and drying, wherein the content of the sodium sulfate is 98.3%. And when the mass fraction of vanadium in the mother liquor is accumulated to more than 1%, the vanadium is converged into a spent vanadium-poor catalyst reduction sulfuric acid leaching solution, and a small amount of sodium sulfite is supplemented to convert the vanadium into vanadyl sulfate.
The waste lean vanadium catalyst reduction sulfuric acid leaching solution is prepared by crushing the waste lean vanadium catalyst to 350 mu m, adding the crushed waste lean vanadium catalyst into dilute sulfuric acid with the mass fraction of 3%, simultaneously adding sodium bisulfite with the mass of 1 time of vanadium, stirring, dissolving and filtering to obtain the waste lean vanadium catalyst reduction sulfuric acid leaching solution with the mass fraction of 3.12% of vanadium.
Example 3
A method for extracting vanadium in a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst comprises the following steps: adding 1000g of waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass percentage of 3.09% into a container, heating to 80 ℃, preserving heat, adding sodium hydroxide to adjust the pH value of the solution to 8, continuously stirring for reacting for 2 hours, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residue into a sodium hydroxide solution with mass percentage of 12%, adding hydrogen peroxide until the solution is light yellow and the pH value reaches 10, continuously stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, adding the sodium metavanadate solution into the solution, filtering and washing to remove insoluble substances (the filter residue is ferric oxide, discarding), concentrating, crystallizing, centrifuging and drying the filtrate to obtain 74.1g of sodium metavanadate product, wherein the vanadium content in the prepared sodium metavanadate is 40.93%, and the recovery rate of vanadium is 98.15%.
Further, the pH value of the filtrate which is filtered to remove the vanadyl hydroxide is adjusted to 10.5 by using sodium hydroxide, and sodium sulfate products are obtained by evaporation crystallization, dehydration and drying, wherein the content of the sodium sulfate is 98.1%. And when the mass fraction of vanadium in the mother liquor is accumulated to more than 1%, the vanadium is converged into a spent vanadium-poor catalyst reduction sulfuric acid leaching solution, and a small amount of sodium sulfite is supplemented to convert the vanadium into vanadyl sulfate.
The waste lean vanadium catalyst reduction sulfuric acid leaching solution is prepared by crushing the waste lean vanadium catalyst to 250 micrometers, adding the crushed waste lean vanadium catalyst into dilute sulfuric acid with the mass fraction of 4%, simultaneously adding sodium bisulfite with the mass of 2 times of vanadium, stirring for dissolving, and filtering to obtain the waste lean vanadium catalyst reduction sulfuric acid leaching solution with the mass fraction of vanadium being more than or equal to 3%.
The above-described embodiments are not intended to limit the present invention in any way, and any process scheme which is the same as or similar to the process scheme of the present invention and is carried out under the principle of the claims of the present invention is considered to fall within the protection scope of the claims of the present invention.
Claims (3)
1. A method for extracting vanadium from a sulfuric acid leaching solution reduced by a waste vanadium-poor catalyst is characterized by comprising the following steps: adding a waste vanadium-poor catalyst reduction sulfuric acid leaching solution with vanadium mass fraction being more than or equal to 3% into a container, heating to 70-80 ℃, keeping the temperature, adding sodium hydroxide to adjust the pH value of the solution to 7-8, stirring and reacting for 1-2 hours, neutralizing vanadyl sulfate in the solution to generate vanadyl hydroxide precipitate, filtering and washing, adding filter residues into a sodium hydroxide solution with mass fraction being 8-12%, introducing air or adding hydrogen peroxide to convert vanadyl hydroxide into a colorless or light yellow sodium metavanadate solution, adjusting the pH value of the solution to 10-12, continuing stirring for 30 minutes to convert vanadyl hydroxide into sodium metavanadate, introducing the sodium metavanadate solution into the solution, filtering and washing to remove insoluble substances, concentrating, crystallizing, centrifuging and drying the filtrate to obtain a sodium metavanadate product.
2. The method for extracting vanadium from sulfuric acid leaching solution reduced by waste vanadium-poor catalyst according to claim 1, characterized by comprising the following steps: the leaching solution for reducing sulfuric acid by the waste lean vanadium catalyst is prepared by crushing the waste lean vanadium catalyst to 250-350 mu m, adding the crushed waste lean vanadium catalyst into dilute sulfuric acid with the mass fraction of 3-5%, simultaneously adding sodium bisulfite with the mass of 1-2 times of that of vanadium, stirring, dissolving and filtering to obtain the leaching solution for reducing sulfuric acid by the waste lean vanadium catalyst with the mass fraction of vanadium being more than or equal to 3%.
3. The method for extracting vanadium from sulfuric acid leaching solution reduced by waste vanadium-poor catalyst according to claim 1, characterized by comprising the following steps: and (3) adjusting the pH value of the filtrate after filtering and removing the vanadyl hydroxide to 9.5-10.5 by using sodium hydroxide, evaporating, crystallizing, dehydrating, drying and recovering sodium sulfate, wherein trace vanadium exists in the mother liquor in the form of sodium metavanadate, and when the mass fraction of vanadium in the mother liquor is accumulated to be more than 1%, the vanadium is converged into a reduction leaching solution, and a small amount of sodium sulfite is supplemented to convert the vanadium into vanadyl sulfate.
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CN115304046A (en) * | 2022-09-08 | 2022-11-08 | 四川大学 | Sodium vanadium phosphate, sodium vanadium manganese phosphate and preparation method thereof |
Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102951680A (en) * | 2011-08-25 | 2013-03-06 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of vanadyl sulfate |
CN103789550A (en) * | 2014-01-26 | 2014-05-14 | 郝喜才 | Method for recovering vanadium, potassium and silicon from waste vanadium catalyst |
CN104195342A (en) * | 2014-09-17 | 2014-12-10 | 华北电力大学 | Method for recycling vanadium pentoxide in waste SCR (Selective Catalytic Reduction) denitration catalyst |
CN104630484A (en) * | 2015-01-13 | 2015-05-20 | 漯河兴茂钛业股份有限公司 | Acid leaching extraction method for comprehensive waste denitration catalyst utilization |
CN105355955A (en) * | 2015-10-23 | 2016-02-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for high-purity vanadyl sulfate solution |
CN106495118A (en) * | 2016-11-11 | 2017-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing phosphoric acid hydrogen-oxygen vanadium |
CN106745246A (en) * | 2016-11-11 | 2017-05-31 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preparing vanadic sulfate |
CN107177737A (en) * | 2017-06-06 | 2017-09-19 | 开封大学 | Spent vanadium catalyst comprehensive reutilization method |
CN107416900A (en) * | 2017-08-31 | 2017-12-01 | 攀钢集团钒业有限公司 | A kind of method for efficiently preparing high-purity sodium metavanadate |
CN109022828A (en) * | 2018-07-03 | 2018-12-18 | 开封大学 | The extracting method of vanadium in spent vanadium catalyst |
CN110257647A (en) * | 2019-07-16 | 2019-09-20 | 昆明理工大学 | The method of vanadium is recycled from ferric vandate |
CN110273072A (en) * | 2019-07-16 | 2019-09-24 | 攀枝花学院 | The method of vanadium and iron is separated and recovered from ferric vandate |
CN110724836A (en) * | 2019-11-20 | 2020-01-24 | 河钢股份有限公司承德分公司 | Method for extracting vanadium from waste SCR denitration catalyst by taking iron salt as roasting additive |
-
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Patent Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102951680A (en) * | 2011-08-25 | 2013-03-06 | 攀钢集团钢铁钒钛股份有限公司 | Preparation method of vanadyl sulfate |
CN103789550A (en) * | 2014-01-26 | 2014-05-14 | 郝喜才 | Method for recovering vanadium, potassium and silicon from waste vanadium catalyst |
CN104195342A (en) * | 2014-09-17 | 2014-12-10 | 华北电力大学 | Method for recycling vanadium pentoxide in waste SCR (Selective Catalytic Reduction) denitration catalyst |
CN104630484A (en) * | 2015-01-13 | 2015-05-20 | 漯河兴茂钛业股份有限公司 | Acid leaching extraction method for comprehensive waste denitration catalyst utilization |
CN105355955A (en) * | 2015-10-23 | 2016-02-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method for high-purity vanadyl sulfate solution |
CN106495118A (en) * | 2016-11-11 | 2017-03-15 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing phosphoric acid hydrogen-oxygen vanadium |
CN106745246A (en) * | 2016-11-11 | 2017-05-31 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method for preparing vanadic sulfate |
CN107177737A (en) * | 2017-06-06 | 2017-09-19 | 开封大学 | Spent vanadium catalyst comprehensive reutilization method |
CN107416900A (en) * | 2017-08-31 | 2017-12-01 | 攀钢集团钒业有限公司 | A kind of method for efficiently preparing high-purity sodium metavanadate |
CN109022828A (en) * | 2018-07-03 | 2018-12-18 | 开封大学 | The extracting method of vanadium in spent vanadium catalyst |
CN110257647A (en) * | 2019-07-16 | 2019-09-20 | 昆明理工大学 | The method of vanadium is recycled from ferric vandate |
CN110273072A (en) * | 2019-07-16 | 2019-09-24 | 攀枝花学院 | The method of vanadium and iron is separated and recovered from ferric vandate |
CN110724836A (en) * | 2019-11-20 | 2020-01-24 | 河钢股份有限公司承德分公司 | Method for extracting vanadium from waste SCR denitration catalyst by taking iron salt as roasting additive |
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