CN109607612A - Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method - Google Patents
Vanadium in a kind of discarded SCR denitration, tungsten, titanium resource recycling method Download PDFInfo
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- CN109607612A CN109607612A CN201811586330.8A CN201811586330A CN109607612A CN 109607612 A CN109607612 A CN 109607612A CN 201811586330 A CN201811586330 A CN 201811586330A CN 109607612 A CN109607612 A CN 109607612A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten 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
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- 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
Abstract
The method that the invention discloses a kind of to recycle vanadium, tungsten, titanium resource from discarded SCR denitration includes: pretreatment is crushed, grinds, and roasts, water logging, solid-liquor separation, ion exchange adsorption, and desorption and chemical precipitation are cleaned, drying.The present invention can extract vanadium, tungsten, the titanium in discarded SCR denitration, can both reduce the generation of danger wastes, and the secondary use of its heavy metal may be implemented.
Description
Technical field
The invention belongs to resource and environment fileds, and in particular to the separation of vanadium, tungsten, titanium in a kind of discarded SCR denitration
And the recovery method as metallurgical industry raw material.
Technical background
Waste catalyst recovery work in China's is started late, mainly with precious and rare metals recoveries such as platinum, rhenium, silver, bismuth, molybdenum, nickel, cobalts
Based on.In addition the vanadium in spent vanadium catalyst for thering are some enterprise's recycling sulfuric acid preparation industries to generate, but vanadium contains in spent vanadium catalyst
Amount 5% or more, and in useless SCR catalyst content of vanadium generally 1.5% hereinafter, and need to separate vanadium, tungsten, molybdenum, mention
Pure difficulty, technique are also immature.Major part waste catalyst is by directly as danger wastes by special waste at present
Reason company carries out landfill stabilization, the still enterprise without specially recycling useless SCR catalyst.The country to discarded SCR denitration still
Lack systematic research and corresponding organization and regulation, capital investment is also less, causes the recycling benefit of dead catalyst totality
Not high with rate, cost recovery is larger, can not form industrialization.
Summary of the invention
The present invention is directed to solve the problems, such as discarded SCR catalyst separation and recovery journey, develop that a kind of water consumption is few, helps
Agent additive amount is low, post-processing load is small, low energy consumption, is suitable for the process of scale separation and recovery.The present invention be by with
What lower step was realized:
(1) it pre-processes: purging the impurity removed in catalyst element surface and duct, pressure using compressed air high pressure nozzle
The pressure of contracting air is controlled in 2.0~5.0MPa, the flow control of single-nozzle between 0.5~1.5m3/s, gas nozzle with
The surface of catalyst keeps the distance of 0.5~1m, and gas purging direction and the angle in catalyst duct direction are less than 10 °, area
Domain moves high pressure nozzle to other regions after purging and continues to purge.Efficiency is purged to improve, multiple gases can also be sprayed
Mouth forms nozzle sets, while purging to multiple ducts.
Purging place is totally-enclosed or semi-closed structure, mating setting the aspiration of negative pressure equipment, useful vacuum degree -0.1~-
The dust collection equipment of 0.2MPa absorbs catalyst surface, in duct and the dust that is fallen off by compressed air purging, the aspiration of negative pressure are set
It is standby with compressed air purging equipment alternate run.
The metal base net for also needing to remove if it is board-like catalyst, after deashing in catalyst element could be as broken
Broken and abrasion process raw material.
(2) be crushed and grind: remove the catalyst element of dust carried out using crushing plant it is fine crushing, be broken into 15mm~
Jaw crusher, gyratory crusher, gyratory crusher, kibbler roll, hammer can be used in the block elements of 40mm, crushing plant
Crusher, impact breaker etc., it is preferential to select kibbler roll or gyratory crusher.
The powder that it is 44~74 microns for partial size that broken block elements, which use grinding machine to grind, grinding apparatus use dry type
Grinding machine, specific pattern can be used ball mill, vibromill, Raymond mill etc., preferentially select Raymond mill.
Calcination agent is added in catalyst grinding process, synchronous to crush and be uniformly mixed, calcination agent uses the hydrogen of alkali metal
One of oxide, chloride, carbonate, nitrate, sulfate, two or more mixture, calcination agent add
Dosage is the 1%~20% of SCR dead catalyst total amount, and preferably additive amount is 5%~10%.
(3) roast: the catalyst powder and calcination agent of qualified partial size enter roaster, 500~950 DEG C at a temperature of
1~5h is roasted, the specific pattern of roaster can be used rotary kiln, tunnel oven etc., preferentially select rotary kiln.
In roaster, catalyst powder with calcination agent high-temperature roasting, destroys the original of catalyst powder in an oxidizing atmosphere
Vanadium, tungsten etc. are oxidized to the oxide of high price by organized structure, and are reacted with calcination agent and generated water-soluble salt, in order to
It leaches.
(4) water logging: abrasive media surface of material after roasting occurs strong friction and impact in mechanical activation process, makes
Surface of material it is destructurized while so that a series of variations occur for material intracell, predominantly so that answering in crystal
Power increases, and lattice defect increases, and decrystallized tendency occurs；Crystal self-energy increases, and chemical activity increases, corresponding Leach reaction
Rate increase, reaction activity reduce.And then temperature and time needed for reducing water logging, while leaching rate can be improved.
Activation water logging activates the activation water seaoning combined with dump leaching method using hot-bulb grinding machine method or dry ball, preferentially
Select hot-bulb grinding machine method.Hot-bulb grinding machine method is to material grinding, mechanical activation, strong stirring after roasting and to leach the organic of process
In conjunction with can work in the case where liquid-solid ratio very little.
Water logging pressure is 0.5~1.2MPa, uses line-frequency induction to heat outside cylinder so that slurry temperature reaches 70 after roasting
~90 DEG C, wherein ratio of water to material control is in (0.4~1.6): 1, the control of activation water logging time is in 1~5h.
(5) solid-liquor separation: the slurry after activation water logging is handled by liquid-solid separation device, vanadium, tungsten and other miscellaneous
Matter is entered in liquid with ionic forms, and titanium then enters in filter residue as byproduct one；High-temperature roasting generate related vanadium, tungsten,
The salts such as silicon have biggish solubility in alkaline solution, and related metatianate, positive titanate and poly- titanate are molten in alkalinity
Solubility in liquid is minimum, when pH value is greater than 8.5, can effectively separate above-mentioned titanate from slurry, separate mode
Centrifugal separator, vacuum filter or inward flow filtration-type filter can be selected, preferentially select centrifugal separator.
Byproduct one (rich titanium filter residue) is obtained after solid-liquor separation, and vanadium, tungsten and other impurity are then worked as into filtrate
In obtain filtrate one, as liquid before the friendship of step (6) ion exchange.
(6) ion exchange: the filtrate obtained using the big channel anion exchange resin process step (5) of strong basicity, by vanadium,
Tungsten ion is adsorbed on ion exchange resin, and remaining impurity is then into after handing in liquid.The pH value control of filtrate before ion exchange
In 8.0~10.5 ranges.
Since vanadium, tungsten are all the refractory metal of transition metal element, the two outermost electron having the same, secondary outer layer
Electron number difference 1.And the two outermost electron layer is more stable, and be easy to lose the electronics of time outer shell, and form different price
The ion of state has property close each other, therefore vanadium, tungsten have similar characteristic in the solution.This process utilizes should
Feature simultaneously separates vanadium, tungsten before handing in liquid.
Process water of the filtrate after purification and impurity removal as activation water logging after exchange, which recycles, to be used.
(7) desorption and chemical precipitation: the resin after adsorption of vanadium, tungsten ion is using the mixed solution of NaOH and NaCl as solution
Imbibition is parsed, and the concentration of NaOH and NaCl control the concentration of NaOH and NaCl in solution within the scope of 0.5~2.0mol/L
Than controlling in 0.8~1.3 range.
Add calcium salt, magnesium salts or ammonium salt etc. into the stripping liquid after ion exchange resin desorption, formed corresponding tungstates,
Vanadate precipitating, by solid-liquor separation, centrifugal separator, vacuum filter or inward flow filtration-type filter is can be selected in separate mode, excellent
First select centrifugal separator.The solid obtained after solid-liquor separation is the mixture of Vanadium Concentrationin, tungsten, and as byproduct two, liquid divides admittedly
From rear while obtaining filtrate two.
Return step (4) after the purified removal of impurities of filtrate two obtained after ion exchange resin desorption and chemical precipitation and filtering
Process water as activation water logging.
It is reusable after regeneration and elution after ion exchange resin desorption.
(8) byproduct cleans: byproduct one and byproduct two are rinsed using deionized water, obtain by-product after being cleaned
Two vanadium of one titanium slag of product and byproduct, tungsten mixture.
After collecting, range activates water logging process and reuses as process water deionized water after cleaning.
(9) byproduct is dried, and the hot fume generated using calcining process dries the byproduct after cleaning as heat source
It is dry, free moisture therein is removed, to pack outward transport.The heat source of byproduct drying produces in step (3) calcining process
Raw hot fume can be auxiliary when the shortage of heat of hot fume is with free moisture in evaporating completely byproduct one and byproduct two
It helps using other heat source supplements such as electric heating, steam heating, gas furnace.
Compared with prior art, the present invention beneficial effect is:
1. it is preferential to select hot-bulb grinding machine method using activation water logging process, water is significantly reduced compared with traditional water logging technique
Liquid-solid ratio needed for soaking process, reduces the water consume of water logging technique；Simultaneously shorten water logging technique needed for dip time and
Dipping temperature needed for reducing is a kind of energy saving, water-saving technique.
2. substantially reducing process flow using ion-exchange process while the compound of isolated vanadium, tungsten.
3. the heat source secondary use that the high-temperature flue gas that roaster generates is dried as byproduct, reduces the energy of whole flow process
Consumption.
4. byproduct flushing water, filtrate etc. is after processing or simple process without recycling, only a small amount of waste water of outlet,
Reduce the water consume of whole flow process.
Detailed description of the invention
Fig. 1 be vanadium in a kind of SCR denitration, tungsten, titanium resource recycling flow chart
Specific embodiment
Embodiment 1:
Take the SCR catalyst that 500g is discarded, by removing, it is broken after, it is 60 that 20gNaOH and 10gNa2CO3, which is added, and grinds
The powder of micron is sent into roaster, in 700 DEG C of roasting temperature 2h.Hot-bulb grinding machine is poured into after solid after roasting is cooled,
200mL water is added, controlled at 70 DEG C, pressure 1MPa, running water soaks time control in 2h.It is (unactivated during alkali leaching
The leaching rate of vanadium is 83.4%, and the leaching rate of tungsten is 79.3%, and up to 98.1%, the leaching rate of tungsten reaches the leaching rate of vanadium after activation
96.7%, and the time for reaching leaching equalization point can shorten 30min or so.) mixture is subjected to solid-liquor separation, obtain byproduct
One solid-state richness titanium filter residue and the filtrate containing vanadium, tungsten and other impurity.Using ion exchange resin adsorption of vanadium tungsten ion, then exist
Vanadium tungsten is parsed in the mixed solution of NaOH and NaCl, wherein the concentration of NaOH is 0.8mol/L, and the concentration of NaCl is 0.8mol/
Then L will add enough calcium chloride in stripping liquid, form corresponding tungstates, vanadate precipitating, by solid-liquor separation, obtain
To the calcium salt of vanadium tungsten, i.e. byproduct two.Two byproducts are respectively washed drying.Ti-rich compounds 428g (its obtained in it
In contain TiO2 96.4%, WO3 0.36%, V2O5 0.28%, SiO2 1.54%, CaO 0.57%, Al2O3 0.06%,
MgO 0.42%, other are 0.42%).Obtain vanadium tungsten compound 68.2g (wherein containing calcium vanadate 3.47%, artificial schellite 83.26%,
Moisture content 10.1%, it is other 3.17%).
Embodiment 2:
Take the SCR catalyst that 500g is discarded, by removing, it is broken after, it is 60 that 20gNaOH and 10gNa2CO3, which is added, and grinds
The powder of micron is sent into roaster, in 800 DEG C of roasting temperature 2h.Hot-bulb grinding machine is poured into after solid after roasting is cooled,
400mL water is added, controlled at 70 DEG C, pressure 1MPa, running water soaks time control in 2.5h.Mixture progress liquid is divided admittedly
From obtaining one solid-state richness titanium filter residue of byproduct and the filtrate containing vanadium, tungsten and other impurity.Using ion exchange resin adsorption of vanadium
Then tungsten ion parses vanadium tungsten in the mixed solution of NaOH and NaCl, wherein the concentration of NaOH is 0.8mol/L, NaCl's
Concentration is 0.8mol/L, then enough calcium chloride will be added in stripping liquid, forms corresponding tungstates, vanadate precipitating, warp
Solid-liquor separation is crossed, the calcium salt of vanadium tungsten, i.e. byproduct two are obtained.Two byproducts are respectively washed drying.Obtain Ti-rich compounds
432g (wherein contains TiO2 95.7%, WO3 0.41%, V2O5 0.34%, SiO2 1.63%, CaO 0.49%, Al2O3
0.08%, MgO 0.37%, other are 0.98%).Vanadium tungsten compound 65.9g is obtained (wherein containing calcium vanadate 3.43%, artificial schellite
83.98%, moisture content 10.3%, it is other 2.29%).
Embodiment 3:
Take the SCR catalyst that 500g is discarded, by removing, it is broken after, it is 60 that 20gNaOH and 10gNa2CO3, which is added, and grinds
The powder of micron is sent into roaster, in 800 DEG C of roasting temperature 2h.Hot-bulb grinding machine is poured into after solid after roasting is cooled,
300mL water is added, controlled at 70 DEG C, pressure 1.2MPa, running water soaks time control in 1h.Mixture progress liquid is divided admittedly
From obtaining one solid-state richness titanium filter residue of byproduct and the filtrate containing vanadium, tungsten and other impurity.Using ion exchange resin adsorption of vanadium
Then tungsten ion parses vanadium tungsten in the mixed solution of NaOH and NaCl, wherein the concentration of NaOH is 0.8mol/L, NaCl's
Concentration is 0.8mol/L, then enough calcium chloride will be added in stripping liquid, forms corresponding tungstates, vanadate precipitating, warp
Solid-liquor separation is crossed, the calcium salt of vanadium tungsten, i.e. byproduct two are obtained.Two byproducts are respectively washed drying.Obtain Ti-rich compounds
425g (wherein contains TiO2 96.3%, WO3 0.49%, V2O5 0.37%, SiO2 1.57%, CaO 0.54%, Al2O3
0.09%, MgO 0.34%, other are 0.3%).Vanadium tungsten compound 66.2g is obtained (wherein containing calcium vanadate 3.52%, artificial schellite
83.77%, moisture content 10.2%, it is other 2.51%).
Claims (4)
1. a kind of method that vanadium, tungsten, titanium resource recycle in discarded SCR denitration, which comprises the following steps:
(1) it pre-processes: the impurity in catalyst module surface and duct is removed using compressed air；
(2) it is crushed and grinds: the waste catalyst for being 44~74 microns at partial size by catalyst preparation by broken and grinding apparatus
Agent powder, while the calcination agent of suitable dosage is added, it is sufficiently mixed with catalyst powder；
(3) roast: the catalyst powder and calcination agent of qualified partial size enter roaster, in 500~950 DEG C of roasting temperature
1~5h；
(4) water logging: the roasting material after roasting enters wet type mechanical activation device, while carrying out water logging, and temperature is controlled 70~90
DEG C, pressure control is in 0.5~1.2MPa, and wherein ratio of water to material control is in (0.4~1.6): 1.Activate the control of water logging time 1~
5h；
(5) solid-liquor separation: activation water logging after slurry handled by liquid-solid separation device, vanadium, tungsten and other impurity with
Ionic forms enter in liquid, and titanium then enters in filter residue as byproduct one；
(6) ion exchange: the filtrate obtained using the big channel anion exchange resin process step (5) of strong basicity is inhaled vanadium, tungsten
It is attached on ion exchange resin；
(7) desorption and chemical precipitation: wherein the concentration of NaOH and NaCl controls within the scope of 0.5~2.0mol/L in stripping liquid,
In solution then enough precipitating reagents will be added than control in 0.8~1.3 range in the concentration of NaOH and NaCl in stripping liquid,
Obtain the byproduct two of Vanadium Concentrationin, tungsten compound；
(8) byproduct cleans: byproduct one and byproduct two after water logging after slurry solid-liquor separation are rinsed using deionized water,
Two vanadium of one titanium slag of byproduct and byproduct, tungsten mixture are obtained after being cleaned；
(9) byproduct is dried, and the hot fume generated using calcining process dries the byproduct after cleaning as heat source,
Remove free moisture therein.
2. the method that vanadium, tungsten, titanium resource recycle in discarded SCR denitration according to claim 4, feature exist
In: the calcination agent added in step (2) is using in the hydroxide of alkali metal, chloride, carbonate, nitrate, sulfate
A kind of, two or more mixture, the additive amount of calcination agent are the 1%~20% of SCR dead catalyst total amount.
3. the method that vanadium, tungsten, titanium resource recycle in discarded SCR denitration according to claim 1, feature exist
In: the pH value of filtrate controls in 8.0~10.5 ranges before step (6) ion exchange.
4. the method that vanadium, tungsten, titanium resource recycle in discarded SCR denitration according to claim 1, feature exist
In: the precipitating reagent added in stripping liquid in step (7) is calcium salt, magnesium salts or ammonium salt.
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| CN110643808A (en) * | 2019-11-07 | 2020-01-03 | 赣州有色冶金研究所 | Method for extracting tungsten from low-grade wolframite |
| CN111020193A (en) * | 2019-11-06 | 2020-04-17 | 北京华电光大环境股份有限公司 | Method for recovering vanadium, tungsten and titanium elements from waste SCR denitration catalyst |
| CN112028122A (en) * | 2020-09-07 | 2020-12-04 | 江西善纳新材料科技有限公司 | Microwave solid phase preparation method of nano calcium tungstate |
| CN112342392A (en) * | 2020-10-27 | 2021-02-09 | 江西理工大学 | Method for respectively recovering titanium, tungsten and vanadium from waste denitration catalyst |
| CN112960697A (en) * | 2021-02-23 | 2021-06-15 | 北京华电光大环境股份有限公司 | Efficient waste SCR denitration catalyst recovery method |
| CN114086001A (en) * | 2022-01-18 | 2022-02-25 | 国能龙源环保有限公司 | Method for simultaneously recovering vanadium and tungsten from reconstructed titanium dioxide of waste SCR denitration catalyst |
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