CN114107677A - Method for recovering vanadium and potassium from acid-making waste vanadium catalyst under assistance of microwaves - Google Patents
Method for recovering vanadium and potassium from acid-making waste vanadium catalyst under assistance of microwaves Download PDFInfo
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- CN114107677A CN114107677A CN202111467836.9A CN202111467836A CN114107677A CN 114107677 A CN114107677 A CN 114107677A CN 202111467836 A CN202111467836 A CN 202111467836A CN 114107677 A CN114107677 A CN 114107677A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 67
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000003054 catalyst Substances 0.000 title claims abstract description 60
- 239000002699 waste material Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 23
- 239000011591 potassium Substances 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 63
- 238000000120 microwave digestion Methods 0.000 claims abstract description 48
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000007787 solid Substances 0.000 claims abstract description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 6
- 238000002386 leaching Methods 0.000 claims description 31
- 238000000926 separation method Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 claims description 7
- 238000004064 recycling Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000011084 recovery Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 230000029087 digestion Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- AMAGVGJJHVRPSI-UHFFFAOYSA-N potassium vanadium Chemical compound [K].[V] AMAGVGJJHVRPSI-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 description 1
- WKXHZKXPFJNBIY-UHFFFAOYSA-N titanium tungsten vanadium Chemical compound [Ti][W][V] WKXHZKXPFJNBIY-UHFFFAOYSA-N 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical group [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 description 1
- 229940041260 vanadyl sulfate Drugs 0.000 description 1
- 229910000352 vanadyl sulfate Inorganic materials 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- 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
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering vanadium and potassium from acid-making waste vanadium catalyst by microwave assistance, which comprises the following steps: crushing the waste vanadium catalyst into particles, adding the particles and water into a microwave digestion kettle, fully stirring, screwing, adjusting microwave power, radiating and cooling to room temperature; opening the microwave digestion kettle to separate solid from liquid, washing the particles for 3 times, placing the separated particles in the microwave digestion kettle, adding water, repeating the steps, opening the microwave digestion kettle to separate solid from liquid, washing the particles for 3 times, placing the separated particles in the microwave digestion kettle, mixing the two extraction liquids, evaporating to viscous solid, and drying to obtain sylvite; adding oxalic acid solution into a microwave digestion kettle, stirring, screwing, adjusting microwave power, cooling to room temperature after radiation, opening the microwave digestion kettle to separate solid from liquid, evaporating the liquid to be viscous solid, drying and calcining to obtain vanadium pentoxide powder. The method can efficiently and quickly recover the vanadium and the potassium, realizes the recycling of resources, and is safe, environment-friendly and simple in process.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for recovering vanadium and potassium from acid-making waste vanadium catalysts by microwave assistance.
Background
The vanadium catalyst for sulfuric acid production is a multi-component catalytic system with vanadium pentoxide as an active component, potassium sulfate and sodium sulfate as cocatalysts and diatomite as a carrier. In the production process of sulfuric acid, the vanadium catalyst is easy to be blocked, collapsed and sintered by fluorine, acid mist, dust and arsenic in flue gas and reaction heat generated by reaction, so that the pore diameter of the catalyst is reduced, and meanwhile, the proportion of pentavalent vanadium is reduced due to precipitation of potassium and vanadium of the catalyst, so that the activity of the catalyst is reduced, and the production requirement cannot be met. The national waste vanadium catalyst generated by sulfuric acid production in China every year is about 1 ten thousand tons, and the vanadium catalyst is increased year by year. Because the vanadium pentoxide contained in the waste vanadium catalyst is toxic, if the vanadium pentoxide is not reasonably treated, the environment pollution is caused, the health of people is influenced, meanwhile, the waste vanadium catalyst contains a large amount of alkali metals (19-25% of potassium sulfate and 6-12% of sodium sulfate), the waste of resources is caused by random stacking, and a large amount of cultivated land is occupied.
At present, researchers at home and abroad research many researches on recycling vanadium and potassium from waste vanadium catalysts, and certain achievements are achieved, and Chinese patent CN107416903A reports that a method for treating the waste vanadium catalysts grinds the waste vanadium catalysts, adopts a method of firstly soaking in water and then soaking in acid, adopts sulfur dioxide as a reducing agent to realize simultaneous recycling of vanadium and potassium, and needs to grind the waste catalysts into particles, soak the particles for 0.5-4 h at a certain temperature, and has long leaching time, and the problems of sulfur dioxide leakage, tail gas treatment and the like due to reduction by utilizing the sulfur dioxide.
Chinese patent CN107572586A reports that a method for recovering V2O5 from acid-making waste vanadium catalyst comprises the steps of mixing the waste vanadium catalyst with water according to a certain proportion, heating to 102-105 ℃ for dissolving for 2.5-3 h, introducing sulfur dioxide to reduce the mixture into vanadyl sulfate, stopping introducing the sulfur dioxide after vanadium pentoxide is dissolved, and preserving heat for 3-4 h. The method needs to grind the catalyst into particles of 12 mm, which causes the problems of increased catalyst treatment cost, long leaching heat preservation time, low leaching efficiency in unit time and the like.
Chinese patent CN108906030A reports that a method for recovering and treating a waste vanadium catalyst comprises the steps of soaking the waste vanadium catalyst in oxalic acid solution with the mass fraction of 30-80%, heating to 80-102 ℃, and reacting for 2-5 hours to recover vanadium from the waste vanadium catalyst, wherein the leaching time is long.
Chinese patent CN102491419A reports that a method for comprehensively recycling a waste vanadium catalyst comprises the steps of crushing the waste vanadium catalyst into particles smaller than 200 um, adding 3-40% of sulfuric acid solution and reducing agents (potassium sulfite, sulfurous acid and sulfur dioxide), and leaching for 0.5-4 h at the temperature of 30-100 ℃.
Chinese patent CN104789780A reports that a method for recovering anatase type titanium-tungsten powder from waste vanadium-tungsten-titanium catalyst adopts a microwave roasting digestion method to soak a roasting digestion sample in warm water at 80-90 ℃ for 1-3 h from the waste catalyst by using sodium carbonate and sodium chlorate as a composite digestion agent, the pH value is adjusted to 1-2 by using sulfuric acid, titanate and tungstate form solid separation, vanadium is retained in the solution, and the waste catalyst is recycled. The method has the advantages that the leaching time is long, simultaneously, sodium carbonate and sodium chlorate are used as composite digesting agents, other substances are introduced, and the cost is increased for the subsequent vanadium separation and purification.
In the traditional recovery treatment process of the waste vanadium catalyst, toxic and irritant gases exist during use or generation, and environmental pollution is easily caused. Meanwhile, the waste vanadium catalyst needs to be processed into fine particles, so that the processing cost is increased, the leaching time is longer, and the problem of low leaching efficiency in unit time is caused.
Disclosure of Invention
The invention aims to overcome the defects and provide the method for recovering the vanadium and the potassium from the acid-making waste vanadium catalyst by microwave assistance, which can efficiently and quickly recover the vanadium and the potassium from the waste vanadium catalyst, realizes resource recycling, is safe and environment-friendly, has simple process and low treatment cost and is safe and environment-friendly.
The invention discloses a method for recovering vanadium and potassium from an acid-making waste vanadium catalyst by microwave assistance, which comprises the following steps of:
(1) crushing the waste vanadium catalyst into 20-30-mesh particles, adding the particles and water into a microwave digestion kettle according to the mass ratio of 1-3: 20, and fully stirring for 5 min;
(2) screwing the microwave digestion kettle tightly, adjusting the microwave power to be 250-350W, radiating for 5-15 min, and naturally cooling to room temperature after the reaction is stopped;
(3) opening the microwave digestion kettle, carrying out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, adding water according to the mass ratio of the particles to the water of 1-3: 20, repeating the step (2), carrying out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, mixing the two extraction liquids, and marking as No. 1 leaching liquid;
(4) adding 6-9% by mass of oxalic acid solution into a microwave digestion kettle according to the mass ratio of particles to the solution of 1-3: 20, and stirring for 5 min;
(5) screwing the microwave digestion kettle, adjusting the microwave power to 250-350W, radiating for 5-15 min, naturally cooling to room temperature after the reaction is stopped, opening the microwave digestion kettle, and performing solid-liquid separation, wherein the liquid is marked as No. 2 leaching liquid;
(6) evaporating the No. 1 leaching solution at 80 ℃ to obtain viscous solid, and drying at 120 ℃ for 0.5-1h to obtain potassium salt;
(7) and (3) evaporating the No. 2 leaching solution at 80 ℃ to form viscous solid, drying at 120 ℃ for 0.5-1h, then placing in a muffle furnace, and calcining at 600 ℃ for 4-5h to obtain vanadium pentoxide powder.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can show that: the method utilizes the different solubility of pentavalent vanadium and potassium sodium in water and utilizes a microwave auxiliary method to quickly separate the potassium salt in the waste vanadium catalyst. And then oxalic acid is utilized to change the vanadium pentoxide which is difficult to dissolve in water in the waste catalyst into vanadyl oxalate which is easy to dissolve in water, and simultaneously microwave heating from inside to outside is utilized as assistance, so that the waste catalyst is uniformly heated, the heating time is greatly shortened, and the potassium vanadium can be leached by large particles or the original particle waste catalyst. Meanwhile, the microwave digestion kettle is in a high-temperature and high-pressure state, so that the leaching of vanadium and potassium in large-particle waste catalysts is more facilitated, the efficiency of recovering vanadium and potassium from the waste catalysts in unit time is obviously improved, the pretreatment process of the waste catalysts is reduced, the waste catalysts are easier to separate and purify, waste materials are changed into valuable materials, and the recycling of waste catalyst resources is realized. The waste vanadium catalyst only needs simple pretreatment, saves the pretreatment cost of the waste catalyst, and can obviously improve the recovery efficiency of vanadium and potassium in unit time.
Detailed Description
Example 1
A method for recovering vanadium and potassium from acid-making waste vanadium catalyst by microwave assistance specifically comprises the following steps:
(1) crushing the waste vanadium catalyst into particles of 20-30 meshes, adding the particles and water into a microwave digestion kettle according to the mass ratio of 1:20, and fully stirring for 5 min;
(2) screwing the microwave digestion kettle, adjusting the microwave power to 350W, radiating for 5min, and naturally cooling to room temperature after the reaction is stopped;
(3) opening the microwave digestion kettle, carrying out solid-liquid separation on the particles, washing the particles for 3 times, placing the separated particles into the microwave digestion kettle, adding water according to the mass ratio of the particles to the water of 1:20, repeating the step (2), carrying out solid-liquid separation on the particles, washing the particles for 3 times, placing the separated particles into the microwave digestion kettle, mixing the two extraction liquids, and marking as No. 1 leaching solution;
(4) adding 6% oxalic acid solution into a microwave digestion kettle according to the mass ratio of particles to the solution of 1:20, and stirring for 5 min;
(5) screwing the microwave digestion kettle, adjusting the microwave power to 250W, radiating for 15min, naturally cooling to room temperature after the reaction is stopped, opening the microwave digestion kettle to separate solid from liquid, and recording the liquid as No. 2 leaching solution:
(6) evaporating the No. 1 leaching solution at 80 ℃ to obtain viscous solid, and drying at 120 ℃ for 1h to obtain potassium salt;
(7) and (3) evaporating the No. 2 leaching solution at 80 ℃ to obtain a viscous solid, drying at 120 ℃ for 1h, then calcining in a muffle furnace at 600 ℃ for 5h to obtain vanadium pentoxide powder.
Through detection: the recovery rates of potassium and vanadium in the waste catalyst are respectively 95% and 94%, and in addition, the content of vanadium pentoxide in the vanadium pentoxide powder in the product reaches 95%.
Example 2
A method for recovering vanadium and potassium from acid-making waste vanadium catalyst by microwave assistance specifically comprises the following steps:
(1) crushing the waste vanadium catalyst into 20-30-mesh particles, adding the particles and water into a microwave digestion kettle according to the mass ratio of 3:20, and fully stirring for 5 min;
(2) screwing the microwave digestion kettle, adjusting the microwave power to 250W, radiating for 15min, and naturally cooling to room temperature after the reaction is stopped;
(3) opening the microwave digestion kettle, carrying out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, adding water according to the mass ratio of the particles to the water of 3:20, repeating the step (2) to carry out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, mixing the two extraction liquids, and marking as No. 1 leaching liquid;
(4) adding an oxalic acid solution with the mass fraction of 9% into a microwave digestion kettle according to the mass ratio of particles to the solution of 3:20, and stirring for 5 min;
(5) screwing the microwave digestion kettle, adjusting the microwave power to 250W, radiating for 15min, naturally cooling to room temperature after the reaction is stopped, opening the microwave digestion kettle to separate solid from liquid, and recording the liquid as No. 2 leaching solution:
(6) evaporating the No. 1 leaching solution at 80 ℃ to obtain viscous solid, and drying at 120 ℃ for 0.5h to obtain potassium salt;
(7) and (3) evaporating the No. 2 leaching solution at 80 ℃ to form viscous solid, drying the viscous solid at 120 ℃ for 0.5h, then calcining the viscous solid in a muffle furnace at 600 ℃ for 4h to obtain vanadium pentoxide powder.
Through detection: the recovery rates of potassium and vanadium in the waste catalyst are respectively 95% and 95%, and in addition, the content of vanadium pentoxide in the vanadium pentoxide powder reaches 96%.
Example 3
A method for recovering vanadium and potassium from acid-making waste vanadium catalyst by microwave assistance specifically comprises the following steps:
(1) crushing the waste vanadium catalyst into 20-30-mesh particles, adding the particles and water into a microwave digestion kettle according to the mass ratio of 2:20, and fully stirring for 5 min;
(2) screwing the microwave digestion kettle, adjusting the microwave power to 350W, radiating for 15min, and naturally cooling to room temperature after the reaction is stopped;
(3) opening the microwave digestion kettle, carrying out solid-liquid separation on the particles, washing the particles for 3 times, placing the separated particles into the microwave digestion kettle, adding water according to the mass ratio of the particles to the water of 2:20, repeating the step (2) to carry out solid-liquid separation on the particles, washing the particles for 3 times, placing the separated particles into the microwave digestion kettle, mixing the two extraction liquids, and marking as No. 1 leaching solution;
(4) adding an oxalic acid solution with the mass fraction of 7% into a microwave digestion kettle according to the mass ratio of particles to the solution of 3:20, and stirring for 5 min;
(5) screwing the microwave digestion kettle, adjusting the microwave power to 350W, radiating for 15min, naturally cooling to room temperature after the reaction is stopped, opening the microwave digestion kettle to separate solid from liquid, and recording the liquid as No. 2 leaching solution:
(6) evaporating the No. 1 leaching solution at 80 ℃ to obtain viscous solid, and drying at 120 ℃ for 1h to obtain potassium salt;
(7) and (3) evaporating the No. 2 leaching solution at 80 ℃ to obtain a viscous solid, drying at 120 ℃ for 1h, then calcining in a muffle furnace at 600 ℃ for 5h to obtain vanadium pentoxide powder.
Through detection: the recovery rates of potassium and vanadium in the waste catalyst are 97% and 96.8%, respectively, and in addition, the content of vanadium pentoxide in the vanadium pentoxide powder reaches 96%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (3)
1. A method for recovering vanadium and potassium from acid-making waste vanadium catalyst by microwave assistance comprises the following steps:
(1) crushing the waste vanadium catalyst into 20-30-mesh particles, adding the particles and water into a microwave digestion kettle according to the mass ratio of 1-3: 20, and fully stirring for 5 min;
(2) screwing the microwave digestion kettle tightly, adjusting the microwave power to be 250-350W, radiating for 5-15 min, and naturally cooling to room temperature after the reaction is stopped;
(3) opening the microwave digestion kettle, carrying out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, adding water according to the mass ratio of the particles to the water of 1-3: 20, repeating the step (2), carrying out solid-liquid separation on the particles, washing the particles for 3 times by using water, placing the separated particles into the microwave digestion kettle, mixing the two extraction liquids, and marking as No. 1 leaching liquid;
(4) adding 6-9% by mass of oxalic acid solution into a microwave digestion kettle according to the mass ratio of particles to the solution of 1-3: 20, and stirring for 5 min;
(5) screwing the microwave digestion kettle, adjusting the microwave power to 250-350W, radiating for 5-15 min, naturally cooling to room temperature after the reaction is stopped, opening the microwave digestion kettle, and performing solid-liquid separation, wherein the liquid is marked as No. 2 leaching liquid;
(6) evaporating the No. 1 leaching solution to be viscous solid, and drying to obtain potassium salt;
(7) and evaporating the No. 2 leaching solution to be viscous solid, drying and calcining to obtain vanadium pentoxide powder.
2. The microwave-assisted method for recovering vanadium and potassium from acid-making waste vanadium catalyst as claimed in claim 1, wherein: and (3) evaporating the No. 1 leaching solution in the step (6) at 80 ℃ to obtain a viscous solid, and drying at 120 ℃ for 0.5-1h to obtain the potassium salt.
3. The microwave-assisted method for recovering vanadium and potassium from acid-making waste vanadium catalyst as claimed in claim 1, wherein: and (3) evaporating the No. 2 leaching solution in the step (7) at 80 ℃ to form viscous solid, drying the viscous solid at 120 ℃ for 0.5 to 1 hour, then placing the viscous solid in a muffle furnace, and calcining the viscous solid at 600 ℃ for 4 to 5 hours to obtain vanadium pentoxide powder.
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| EP2412675A1 (en) * | 2010-07-26 | 2012-02-01 | Greenshores Patent BV | Process for isolating vanadium |
| CN103789550A (en) * | 2014-01-26 | 2014-05-14 | 郝喜才 | Method for recovering vanadium, potassium and silicon from waste vanadium catalyst |
| CN107416903A (en) * | 2017-04-21 | 2017-12-01 | 广东工业大学 | A kind of method for handling spent vanadium catalyst |
| CN108160109A (en) * | 2017-11-17 | 2018-06-15 | 昆明理工大学 | A kind of microwave-assisted regeneration FCC dead catalyst methods |
| CN111455186A (en) * | 2020-06-08 | 2020-07-28 | 江苏美东环境科技有限公司 | Method for preparing vanadium pentoxide by treating vanadium-containing waste sulfuric acid catalyst through two-step method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2412675A1 (en) * | 2010-07-26 | 2012-02-01 | Greenshores Patent BV | Process for isolating vanadium |
| CN103789550A (en) * | 2014-01-26 | 2014-05-14 | 郝喜才 | Method for recovering vanadium, potassium and silicon from waste vanadium catalyst |
| CN107416903A (en) * | 2017-04-21 | 2017-12-01 | 广东工业大学 | A kind of method for handling spent vanadium catalyst |
| CN108160109A (en) * | 2017-11-17 | 2018-06-15 | 昆明理工大学 | A kind of microwave-assisted regeneration FCC dead catalyst methods |
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