CN109022828A - The extracting method of vanadium in spent vanadium catalyst - Google Patents
The extracting method of vanadium in spent vanadium catalyst Download PDFInfo
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- CN109022828A CN109022828A CN201810716719.3A CN201810716719A CN109022828A CN 109022828 A CN109022828 A CN 109022828A CN 201810716719 A CN201810716719 A CN 201810716719A CN 109022828 A CN109022828 A CN 109022828A
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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
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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
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Abstract
The invention discloses a kind of methods that vanadium is extracted in spent vanadium catalyst.The present invention is the following steps are included: spent vanadium catalyst is ground, water logging；Reduction obtains material liquid after reoxidizing；The material liquid pH value is adjusted to 2.0~3.0；Static Adsorption and/or Dynamic Adsorption are carried out after mixing with Dex-V anion exchange resin, obtain load vanadium resin；Gained load vanadium resin is eluted with strippant, obtains stripping liquid containing vanadium；After the pH value for adjusting gained stripping liquid containing vanadium is 8~9, ammonium chloride is added, obtains sediment, vanadic anhydride is obtained after calcining.The present invention, which saves, purifies-sinks thick vanadium-alkali soluble process, and vanadium concentration obtains the enrichment of decades of times, enormously simplifies process flow, reduces production cost, high to the adsorption rate of vanadium, resolution factor and the rate of recovery, and product purity is high, environmentally friendly.
Description
Technical field
The present invention relates to vanadium extractive technique fields, and in particular to a method of vanadium is extracted from spent vanadium catalyst.
Background technique
Vanadium is one of metal in short supply and important in the world, is widely applied in multi-field suffer from such as aviation and metallurgy.
According to statistics, current 70% or more vanadium is produced using rich ferrovanadium dregs, dead catalyst, bone coal ash as raw material；And in chemical industry
80% or more reaction needs catalyst to participate in, and vanadium containing catalysts are more important one of series catalyst, is widely used in
Sulfuric acid industry and Organic Chemicals synthesize field；But as vanadium containing catalysts use in the growth and use process of time
The influence of environmental factor, and the every annual meeting in the whole world is caused to generate a large amount of spent vanadium catalyst, such spent vanadium catalyst can not only account for
With a large amount of soil, it includes harmful components also will be distributed in air harm generated to humans and animals, and seeped with rainwater
Enter underground to poison vegetation and destroy soil texture.
Currently, common method is extracted in the recycling of vanadium chemical precipitation method, ion-exchange, solvent extraction etc..Wherein,
Chemical precipitation method is as a kind of method more early used, and device therefor is simple, technical maturity, but the tediously long complexity of technique, institute
Product purity is low, to the seriously corroded of equipment for preparation；And solvent extraction makees extractant using organic phase, there is single-stage extractions
Take effect poor, then extractant loses the problems such as big, operating condition is harsh to multitple extraction.
Therefore, it needs to research and develop a kind of environmentally friendly, simple process, the extraction that vanadium extraction is high-efficient, product purity is high
The method of vanadium.
Summary of the invention
That the technical problem to be solved in the present invention is to provide a kind of processes is simple, environmental-friendly, vanadium product purity is high from useless
The method of vanadium is extracted in vanadium catalyst, it is intended to solve current vanadium extract present in production procedure is complicated, absorption and resolution factor are low,
The technical issues of product purity is low.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
Design a kind of extracting method of vanadium in spent vanadium catalyst, comprising the following steps:
(1) spent vanadium catalyst is ground, water logging；By H2SO4It mixes, adds anhydrous according to the ratio of 2.5ml:1g with water logging slag
Na2SO3Reduction obtains material liquid after reoxidizing；
(2) the material liquid pH value is adjusted to 2.0~3.0；
(3) upper step material liquid and Dex-V anion exchange resin are mixed according to the ratio of 100~150ml:1.0g, 25~
Static Adsorption and/or Dynamic Adsorption are carried out after stirring 4~6h at 35 DEG C, obtains load vanadium resin；
(4) gained load vanadium resin in step (3) is eluted with strippant, obtains stripping liquid containing vanadium；The strippant is
The mixed liquor for the NaCl that the NaOH and mass percent concentration that mass percent concentration is 1~4% are 8%；
(5) after the pH value of gained stripping liquid containing vanadium is 8~9 in regulating step (4), ammonium chloride is added, sediment is obtained, after calcining
Obtain vanadic anhydride.
Further, the Dex-V anion exchange resin is pre-processed via following methods:
It is first soaked in water, washs the resin to no brown colored foams, then impregnated 12h with 5%NaOH, be washed to efflux and be
Property, it is neutral for being impregnated 12h with 5%HCl later, be washed to efflux, is finally impregnated with the sodium chloride solution of saturation stand-by.
Preferably, in the step (1), 300~370 μm of the granularity for grinding rear spent vanadium catalyst；The water logging
The mass ratio of Shi Suoshu spent vanadium catalyst and water is 1:2~3；The H2SO4Mass fraction be 11%；The oxidant when oxidation
For sodium chlorate；
Preferably, in the step (2), the pH value control of the material liquid is 2.5.
Preferably, in the step (3), magnetic agitation 5h under the conditions of 30 DEG C of temperature is set；The stream of the Dynamic Adsorption
Speed control is 0.5~2ml/min.
Preferably, in the step (4), the strippant is the mixed liquor of 2% NaOH and 8 % NaCl.By the solution
Vapor by several times elutes the load vanadium resin, and in the lessivation, the liquid level of the strippant is kept above described
Load vanadium resin layer upper face.
Further, in actual production, in the step (4), when desorption efficiency reaches 93~94%, step is carried out
(5)；Then repeat step (4) continue to elute the load vanadium resin, will obtain described in stripping liquid containing vanadium as benefit
It is stand-by to fill strippant.
Preferably, in the step (5), the calcination temperature control is 500~600 DEG C.
Compared with prior art, the beneficial technical effect of the present invention lies in:
1. the method applied in the present invention is high to the adsorption rate of vanadium, resolution factor and the rate of recovery.
2. V of the quality better than metallurgical 99 grade standards of YB/T 5304-2011 can be made in method therefor of the present invention2O5Product.
3. the present invention extracts in the method for vanadium, eliminates and purify-sink thick vanadium-alkali soluble process, vanadium concentration obtains decades of times
Enrichment, stripping liquid can directly ammonia salt precipitation, enormously simplify process flow.
4. the present invention is added using two columns series connection adsorption and desorption agent continuous several times and the technique of segmentation desorption, not only significantly
Adsorption effect, concentration ratio and resolution factor are improved, and is convenient for precipitation operation；On the other hand it is effectively utilized the desorption of low concentration
Liquid realizes energy-saving and emission-reduction, reduces production cost.
5. production process of the present invention is simple and environmentally friendly.
Detailed description of the invention
Fig. 1 is the adsorption effect figure of different resins in embodiment 1 and comparative example 1；
Fig. 2 is embodiment 2 and the adsorption effect figure under different pH value in comparative example 2；
Fig. 3 is the adsorption effect figure in embodiment 3 and comparative example 3 under different temperatures；
Fig. 4 is the adsorption effect figure in embodiment 4 and comparative example 4 under different time；
Fig. 5 be it is different in flow rate in embodiment 6 and comparative example 6 under the adsorption effect figure.
Specific embodiment
Illustrate a specific embodiment of the invention with reference to the accompanying drawings and examples, but following embodiment is used only in detail
It describes the bright present invention in detail, does not limit the scope of the invention in any way.
Related instrument and equipment is routine instrument device unless otherwise instructed in the examples below；It is related
Reagent is commercially available conventional reagent unless otherwise instructed；Related test method is unless otherwise instructed conventional method.
Embodiment 1:Dex-V resin carries out vanadium Static Adsorption
(1) spent vanadium catalyst partial size is milled to 300~370 μm, water is added in the ratio that solid-liquid mass ratio is 1:2.5,100
DEG C, water logging under the conditions of 1.5 hours etc., filter to obtain water logging filtrate and water logging filter residue, water logging filter residue washed with clear water to neutral
Water logging slag, water logging filtrate, washing lotion merge to obtain infusion, collect water logging slag respectively and infusion is spare；
(2) it is 11% that mass percent concentration, which is added, in the ratio for being 2.5ml:1g in liquid-solid ratio in the water logging slag that step obtains upwards
H2SO4, reduction acidleach is carried out under conditions of sodium sulfite is reducing agent, reduction pickle liquor and reduction acid leaching residue is obtained by filtration,
Reduction pickle liquor is merged into obtain leachate with the resulting infusion of upper step；
(3) in the leachate that step obtains upwards, oxidant sodium chlorate is added, boils to solution by blue and is changed into yellow, obtain
To material liquid: wherein content of vanadium is 5.6g/L；The pH value for adjusting material liquid is 3.0；
(4) it is first impregnated with deionized water, washing Dex-V anion exchange resin (being purchased from Zhengzhou, henan Qin Shi Science and Technology Ltd.)
To no brown and foam, filtered after then impregnating Dex-V anion exchange resin 12h with 5%NaOH solution, it is clear with deionized water
Efflux is washed till as neutrality；It is filtered after impregnating the Dex-V anion exchange resin 12h with 5%HCl solution again, uses deionized water
Cleaning to efflux is neutrality, is finally impregnated with the sodium chloride solution of saturation, obtains pretreated Dex-V anion exchange tree
Rouge.
(5) the 100ml pH material liquid for being 3.0 is mixed with the pretreated Dex-V anion exchange resin of 1.00g, often
Warm 1~14h of magnetic agitation carries out Static Adsorption.
Comparative test 1:D301, D201,717 resins carry out vanadium Static Adsorption
Unlike the first embodiment, the Dex-V anion described in D301, D201,717 resin replacement embodiments 1 is handed over respectively
Resin is changed, remaining content is all same as Example 1；The main physical and chemical performance parameter of four kinds of resins is such as in embodiment 1 and comparative example 1
Shown in table 1, embodiment 1 and the absorption result of the resin of comparative test 1 are as shown in Figure 1.
The main physical and chemical performance parameter of 1 four kinds of resins of table
。
2: Dex-V resin of embodiment carries out vanadium Static Adsorption
Difference from Example 1 is:
Spent vanadium catalyst is ground, water logging, reduction acidleach and oxidation obtain material liquid；Adjusting its pH value is 2.0,2.5,3.0；
It is first impregnated with deionized water, washing Dex-V anion exchange resin to no brown and foam, is then soaked with 5%NaOH solution
It is filtered after bubble Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux；It is impregnated again with 5%HCl solution
It is filtered after Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux, finally with the sodium chloride of saturation
Solution impregnates, and obtains pretreated Dex-V anion exchange resin, spare.
150ml material liquid is mixed with the pretreated Dex-V anion exchange resin of 1g, at normal temperature magnetic agitation 5h
It is adsorbed.
Comparative test 2:
As different from Example 2, the pH value of material liquid is 1.5,3.5,4.0,4.5, remaining content is all same as Example 2；
Embodiment 2 and the absorption result of comparative test 2 are as shown in Figure 2.
As seen from Figure 2, with the increase of pH value, Dex-V resin first rises vanadium adsorption capacity to be gradually reduced again, when
When pH value is 2.5 or so, Dex-V resin is best to vanadium adsorption effect.
Embodiment 3:Dex-V resin carries out vanadium Static Adsorption
Difference from Example 1 is:
Spent vanadium catalyst is ground, water logging, reduction acidleach and oxidation obtain material liquid liquid, and wherein the content of vanadium is 5.1g/L；It adjusts
Saving its pH value is 2.5；
It is first impregnated with deionized water, washing Dex-V anion exchange resin to no brown and foam, is then soaked with 5%NaOH solution
It is filtered after bubble Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux；It is impregnated again with 5%HCl solution
It is filtered after Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux, finally with the sodium chloride of saturation
Solution impregnates, and obtains pretreated Dex-V anion exchange resin.
Material liquid described in 150ml is mixed with the pretreated Dex-V resin of 1.0g, respectively in 30 DEG C, 35 DEG C, lower magnetic force
Stirring 5h is adsorbed.
Comparative test 3:
As different from Example 3, whipping temp is 20 DEG C, 25 DEG C, 40 DEG C, 45 DEG C, remaining content is all same as Example 3；
Embodiment 3 and the absorption result of comparative test 3 are as shown in Figure 3.
As seen from Figure 3, as the temperature rises, the adsorption rate of V (V) is increased to 99.2% from 86.1%, and temperature is 30 DEG C of left sides
When right, the exchange adsorption of vanadium basically reaches dynamic equilibrium in resin and solution.
Embodiment 4:Dex-V resin carries out vanadium Static Adsorption
Difference from Example 1 is:
Spent vanadium catalyst is ground, water logging, reduction acidleach and oxidation obtain material liquid；Adjusting its pH value is 2.5；
It is first impregnated with deionized water, washing Dex-V anion exchange resin to no brown and foam, is then soaked with 5%NaOH solution
It is filtered after bubble Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux；It is impregnated again with 5%HCl solution
It is filtered after Dex-V anion exchange resin 12h, it is neutral for being cleaned with deionized water to efflux, finally with the sodium chloride of saturation
Solution impregnates, and obtains pretreated Dex-V anion exchange resin.
Material liquid described in 150ml is mixed with the pretreated Dex-V anion exchange resin of 1.0g, at 30 DEG C respectively
Magnetic agitation 4,5,6h are adsorbed.
Comparative test 4:
As different from Example 4, mixing time 0.5,1,2,3h, remaining content are all same as Example 4；Embodiment 4 with
The absorption result of comparative test 4 is as shown in Figure 4.
As seen from Figure 4, with the increase in reaction time, Dex-V resin gradually rises the Static Adsorption rate of vanadium.But
Preceding half an hour, resin is very fast to the adsorption rate of vanadium, adsorption rate is more than 50%；Time continues growing, and adsorption rate amplification becomes smaller；
When reacting 5h, the exchange adsorption of vanadium basically reaches dynamic equilibrium in resin and solution.
Embodiment 5:Dex-V resin carries out vanadium Static Adsorption
Strippant: 1%NaOH+8% NaCl, 2%NaOH+8% NaCl, 3%NaOH+8% NaCl, 4%NaOH+8% NaCl is used respectively
Embodiment 4(adsorption time is eluted for gained load vanadium resin in 5h), obtains stripping liquid containing vanadium.
Comparative test 5:
As different from Example 5, strippant 2%, 4%, 6%, 8%NaCl, 1%, 2%, 3%, 4%NaOH, remaining content all with reality
It is identical to apply example 5；
The results are shown in Table 2 for the vanadium desorption efficiency of embodiment 5 and comparative test 5:
The vanadium desorption efficiency of the different composition strippants of table 2
。
Embodiment 6:Dex-V resin carries out vanadium Dynamic Adsorption
Difference from Example 1 is:
Dex-V wet resin is taken to be fitted into self-control glass column (10mm × 500mm), the material liquid that by pH value be 2.5, temperature is 30 DEG C
Respectively with 0.5,1, the flow velocity of 1.5ml/min flow countercurrently through glass column, investigate flow velocity to the shadow of Dex-V resin Dynamic Adsorption vanadium
It rings.
Comparative test 6:
As different from Example 6, flow velocity 2,2.5,3ml/min, remaining content are all same as Example 6；Embodiment 6 with it is right
Absorption result than test 6 is as shown in Figure 5.
As seen from Figure 5, resin is gradually reduced the adsorption rate of vanadium with the increasing of flow velocity.When flow velocity is bigger
When, the time that material liquid contacts in ion exchange column with resin is short, and vanadium complex anion is caused to exchange with chloride ion in resin
Possibility decline；And flow velocity is too small, although adsorption rate can improve, will increase the time that resin reaches adsorption saturation, prolongs instead
The long entire ion exchange period.
In actual production, column effect can be improved using the concatenated adsorption operations mode of two columns: is equivalent to raising exchange column
Column diameter ratio, can significantly improve resin utilization rate and carry vanadium amount, and then improve vanadium concentration ratio, accelerate subsequent precipitation speed.
Actual production the result shows that: compared with single-column mode, adsorption time can save 30% or more, vanadium enrichment multiple can be improved 20% with
On, while ammonium salt consumption is reduced when precipitation, continuous production is good, production cost decline.
Embodiment 7: elution parses vanadium by several times
Be 5h to embodiment 4(adsorption time with strippant 2%NaOH+8% NaCl) in gained load vanadium resin continuous several times into
Row elution, obtains stripping liquid containing vanadium, wherein the quality of strippant used is 4 times for loading vanadium resin, the liquid level of strippant is always
In resin layer top, measured desorption efficiency is 99.5%.
Embodiment 8: segmentation parses vanadium
When desorption efficiency is 99.5% in embodiment 7, ammonium chloride is added to carry out precipitation processing gained stripping liquid containing vanadium, then with solution
The stripping liquid containing vanadium that vapor continues to obtain load vanadium resin elution low concentration desorbs the supplement solution of load vanadium resin as next time
Vapor, the method can make full use of the stripping liquid of low concentration in actual production, realize energy-saving and emission-reduction, and concentration ratio can be at double
It improves, is conducive to precipitation operation.
Embodiment 9: V is produced2O5Product
The pH value for adjusting 7 gained stripping liquid of embodiment is 8, and ammonium chloride is added, obtains ammonium metavanadate precipitate, ammonium metavanadate is calcined
Rufous vanadic anhydride product is obtained, the results are shown in Table 3 to vanadic anhydride analysis:
3 vanadic anhydride test products value of table and YB/T 5304-2011 Comparison of standards table
。
As seen from the above table, test products quality reaches 99 grades of V of YB/T 5304-2011 metallurgy2O5Standard.
The present invention is described in detail above in conjunction with drawings and examples, still, those of skill in the art
Member is it is understood that without departing from the purpose of the present invention, can also carry out each design parameter in above-described embodiment
Change, forms multiple specific embodiments, is common variation range of the invention, is no longer described in detail one by one herein.
Claims (10)
1. the extracting method of vanadium in a kind of spent vanadium catalyst, comprising the following steps:
(1) spent vanadium catalyst is ground, water logging；By H2SO4It is mixed with water logging slag according to the ratio of 2.5ml:1g, adds anhydrous Na2SO3
Reduction obtains material liquid after reoxidizing；
(2) the material liquid pH value is adjusted to 2.0~3.0；
(3) upper step material liquid and Dex-V anion exchange resin are mixed according to the ratio of 100~150ml:1.0g, 25~
Static Adsorption and/or Dynamic Adsorption are carried out after stirring 4~6h at 35 DEG C, obtains load vanadium resin；
(4) gained load vanadium resin in step (3) is eluted with strippant, obtains stripping liquid containing vanadium；The strippant is
The mixed liquor for the NaCl that the NaOH and mass percent concentration that mass percent concentration is 1~4% are 8%；
(5) after the pH value of gained stripping liquid containing vanadium is 8~9 in regulating step (4), ammonium chloride is added, sediment is obtained, after calcining
Obtain vanadic anhydride.
2. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that the Dex-V anion
Exchanger resin is pre-processed via following methods:
It is first soaked in water, washs the resin to no brown colored foams, then impregnated 12h with 5%NaOH, be washed to efflux and be
Property, it is neutral for being impregnated 12h with 5%HCl later, be washed to efflux, is finally impregnated with the sodium chloride solution of saturation stand-by.
3. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (1),
The granularity control for grinding rear spent vanadium catalyst is 300~370 μm；The quality of the spent vanadium catalyst and water when the water logging
Than for 1:2~3；The H2SO4Mass fraction be 11%；Oxidant is sodium chlorate when the oxidation.
4. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (2),
The pH value control of the material liquid is 2.5.
5. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (3),
Set magnetic agitation 5h under the conditions of 30 DEG C of temperature.
6. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (3),
The flow control of the Dynamic Adsorption is 0.5~2ml/min.
7. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (4),
The strippant is the mixed liquor of 2% NaOH and 8 % NaCl.
8. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (4),
The strippant by several times elutes the load vanadium resin, in the lessivation, the liquid level of the strippant is kept
Higher than the load vanadium resin layer upper face.
9. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in actual production, in institute
It states in step (4), when desorption efficiency reaches 93~94%, carries out step (5)；Then step (4) are repeated to continue to the load vanadium
Resin is eluted, will obtain described in stripping liquid containing vanadium as supplement strippant it is stand-by.
10. the extracting method of vanadium in spent vanadium catalyst according to claim 1, which is characterized in that in the step (5)
In, the calcination temperature control is 500~600 DEG C.
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