CN108906030A - A kind of recovery and treatment method of spent vanadium catalyst - Google Patents
A kind of recovery and treatment method of spent vanadium catalyst Download PDFInfo
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- CN108906030A CN108906030A CN201810710090.1A CN201810710090A CN108906030A CN 108906030 A CN108906030 A CN 108906030A CN 201810710090 A CN201810710090 A CN 201810710090A CN 108906030 A CN108906030 A CN 108906030A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/60—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
- B01J38/62—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids organic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/68—Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst
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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
- 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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- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of recovery and treatment methods of spent vanadium catalyst comprising following steps：Step A：Spent vanadium catalyst is washed using the solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters；Step B：The spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained；Step C：The spent vanadium catalyst of the drying is soaked in the oxalic acid solution containing mass fraction 30-80%, 30-40 DEG C of heating will be added the vanadic anhydride that mass fraction is 2-8%, heat 80-102 DEG C of the solution in above-mentioned solution, reaction 2-5 hours obtains the intermediate product containing spent vanadium catalyst；Step D：The intermediate product is roasted at 100-550 DEG C, up to the discharge of no gas, obtains the spent vanadium catalyst containing vanadic anhydride.The recovery and treatment method of spent vanadium catalyst of the present invention hinders precipitating reagent by dibasic acid esters, and the effect of the reagents such as oxalic acid does not generate polluted gas during recovery processing, do not generate waste, environmentally friendly, while to the rate of recovery of spent vanadium catalyst height, manufacturing cost is low.
Description
Technical field
The present invention relates to spent catalyst recovery technical fields, and in particular to a kind of recovery processing side of spent vanadium catalyst
Method.
Background technique
Currently, with sulfuric acid industry, petrochemical industry, the continuous development of benzene alkane industry, the consumption of spent vanadium catalyst is also therewith
Increase, spent vanadium catalyst is known noxious material.Many scholars, expert have concentrated on studies the new of spent vanadium catalyst at home and abroad
Chemical disposal process, although the process of some recycling spent vanadium catalysts is had developed, meanwhile, for the circulation for the vanadium resource that gives up
Utilize the basis for having established theory and practice.It is traditional due to containing the substances such as a large amount of sulphur, nitre, carbon, arsenic in spent vanadium catalyst
In spent vanadium catalyst recovery process method, during high-temperature roasting, make the harmful substance volatilization of sulphur, nitre, arsenic, volatilization has
Evil substance polluted the air in environment, impair the health of people.
In the technical process of the recycling of former spent vanadium catalyst, most of crushed using drying, roasting, then again
With sulfuric acid leaching V2O4Dope, V is then obtained by redox2O5Or sodium vanadate dope, metavanadic acid is synthesized using ammonium chloride
Ammonium, then vanadic anhydride is obtained after being fired, during technique roasting：When roasting, there is the volatilization of a large amount of hydrogen sulfide gas
And arsenic, ammonium volatilization and polluted air.There is a large amount of noxious material (vanadium, arsenic, thallium, chromium) powder to fly upward, damage when crushing
The body of ambient enviroment and people.Since spent vanadium catalyst failure cause is that pentavalent vanadium rush becomes tetravalence vanadium, need by Ore Leaching,
A large amount of waste water is generated after leaching synthesis, then toxic wastewater pollutes mankind water source again.It is a large amount of useless after vanadic anhydride obtains
The waste offcuts of vanadium catalyst can not be handled, and noxious material is caused to pollute environment.
In conclusion the process of the recovery processing of traditional spent vanadium catalyst, during processing, there is rows
Noxious material is placed in environment, is polluted the environment, and the technique is during the treatment, waste of resource is at high cost, it would be highly desirable to
It is further improved.
Summary of the invention
The purpose of the present invention is to provide a kind of recovery and treatment methods of spent vanadium catalyst, to solve existing useless vanadium catalysis
Agent treatment process is polluted the environment there is noxious material pollution, the defect of complex treatment process.
To achieve the above object, the present invention provides a kind of recovery and treatment method of spent vanadium catalyst, the method includes with
Lower step：
Step A：Spent vanadium catalyst is washed using the solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters；
Step B：The spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained；
Step C：The spent vanadium catalyst of the drying is soaked in the oxalic acid solution containing mass fraction 30-80%, is added
Hot 30-40 DEG C, the vanadic anhydride that mass fraction is 2-8% will be added in above-mentioned solution, heat 80-102 DEG C of the solution, instead
It answers 2-5 hours, obtains the intermediate product containing spent vanadium catalyst；
Step D：The intermediate product is roasted at 100-550 DEG C, up to no gas is discharged, acquisition contains vanadic anhydride
Spent vanadium catalyst；
Step E：Add the white carbon black of 5%-10% to pelletize the spent vanadium catalyst containing vanadic anhydride, obtains finished product
Vanadium pentoxide catalyst.
Preferably, the general molecular formula of the spent vanadium catalyst is VC2O(R)V2O5, wherein R C2H2O4。
Preferably, in the step B, the spent vanadium catalyst needs dry 2h in 100 DEG C.
Preferably, V in the spent vanadium catalyst2O5Mass percent be 50%-100%.
Preferably, the refractive index of the finished product vanadic anhydride is 1.2-1.5.
Preferably, the dibasic acid esters resistance precipitating reagent includes the component of following mass fraction：Phosphate 84-93.8%, five oxidations
Two vanadium are 0.2-1%, polyphosphate 6-15%.
Preferably, maturing temperature is 450-550 DEG C in the step D.
Preferably, in the step A, the dibasic acid esters resistance precipitating reagent mass fraction is 0.5-1.5%, the quality of the oxalic acid
Score is 1.5-2.5%.
The recovery and treatment method of spent vanadium catalyst of the invention has the following advantages that：
The recovery and treatment method of spent vanadium catalyst of the invention, process treatment process is pollution-free, environmentally friendly, processing
It is at low cost, it is high to the processing cost of spent vanadium catalyst.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Specific embodiments of the present invention are described in more detail below.These embodiments are provided to be to be able to more thoroughly
Understand the present invention, and the scope of the present invention can be fully disclosed to those skilled in the art.
"comprising" or " comprising " as mentioned throughout the specification and claims are an open language, therefore are answered
It is construed to " including but not limited to ".Specification subsequent descriptions are to implement better embodiment of the invention, and so description is
For the purpose of the rule of specification, the range that is not intended to limit the invention.Protection scope of the present invention is when the appended power of view
Benefit requires subject to institute's defender.
Embodiment 1
The recovery and treatment method of the spent vanadium catalyst of the present embodiment comprising following steps：
Step A：Spent vanadium catalyst is washed using the protection solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters, wherein is being protected
In solution, it is 1.5% that dibasic acid esters, which hinders precipitating reagent mass fraction, and the mass fraction of oxalic acid is 2.5%.
Step B：Spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained, wherein spent vanadium catalyst needs
2h is dried in 100 DEG C.
Step C：Dry spent vanadium catalyst is soaked in the oxalic acid solution containing mass fraction 80%, heats 40 DEG C,
Will in above-mentioned solution be added mass fraction be 8% vanadic anhydride, 102 DEG C of heated solution, react 5 hours, then drain or
Drying obtains the intermediate product containing spent vanadium catalyst.In this step, convert the pentavalent vanadium that stubble in spent vanadium catalyst is stored in
Tetravalence vanadium；It, with the vanadium consumed in spent vanadium catalyst is supplemented, can be the CH of 500g/l using dope2O4V supplement.
Step D：Intermediate product is roasted at 550 DEG C, up to no gas is discharged, useless vanadium of the acquisition containing vanadic anhydride is urged
Agent；Preferably, maturing temperature is 550 DEG C.When roasting, generation is oxalic acid nitrogen, and uncontaminated gases discharge, oxalic acid is at 159 DEG C
It rises and opens volatilization decarburization generation calcium oxalate, be warming up to 550 DEG C, generate oxalic acid nitrogen.When the nitrogen of oxalic acid is sloughed, the vanadium of spent vanadium catalyst is
It is oxidized to pentavalent vanadium (V2O5), V in spent vanadium catalyst2O5Mass percent be 50%-100%.According to the survey of QB614/88
The refractive index for the spent vanadium catalyst containing vanadic anhydride that method for testing measures is 1.2-1.5.
Step E：Add 10% white carbon black to pelletize the spent vanadium catalyst containing vanadic anhydride, obtains the oxidation of finished product five two
Vanadium catalyst.In this step, high purity vanadic anhydride can also be supplemented when granulation.
Embodiment 2
The recovery and treatment method of the spent vanadium catalyst of the present embodiment comprising following steps：
Step A：Spent vanadium catalyst is washed using the protection solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters, wherein is being protected
In solution, it is 0.5% that dibasic acid esters, which hinders precipitating reagent mass fraction, and the mass fraction of oxalic acid is 1.5%.
Step B：Spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained, wherein spent vanadium catalyst needs
2h is dried in 100 DEG C.
Step C：Dry spent vanadium catalyst is soaked in the oxalic acid solution containing mass fraction 30%, heats 30 DEG C,
Will in above-mentioned solution be added mass fraction be 2% vanadic anhydride, 80 DEG C of heated solution, react 2-5 hours, then drain or
Drying obtains the intermediate product containing spent vanadium catalyst.In this step, convert the pentavalent vanadium that stubble in spent vanadium catalyst is stored in
Tetravalence vanadium；It, with the vanadium consumed in spent vanadium catalyst is supplemented, can be the CH of 100g/l using dope2O4V supplement.
Step D：Intermediate product is roasted at 100 DEG C, up to no gas is discharged, useless vanadium of the acquisition containing vanadic anhydride is urged
Agent；Preferably, maturing temperature is 450 DEG C.When roasting, generation is oxalic acid nitrogen, and uncontaminated gases discharge, oxalic acid is at 159 DEG C
It rises and opens volatilization decarburization generation calcium oxalate, be warming up to 450 DEG C DEG C, generate oxalic acid nitrogen.When the nitrogen of oxalic acid is sloughed, the vanadium of spent vanadium catalyst
It has been oxidized to pentavalent vanadium (V2O5), V in spent vanadium catalyst2O5Mass percent be 50%.According to the test side of QB614/88
The refractive index for the spent vanadium catalyst containing vanadic anhydride that method measures is 1.2-1.5.
Step E：Add 5% white carbon black to pelletize the spent vanadium catalyst containing vanadic anhydride, obtains the oxidation of finished product five two
Vanadium catalyst.In this step, high purity vanadic anhydride can also be supplemented when granulation.
Embodiment 3
The recovery and treatment method of the spent vanadium catalyst of the present embodiment comprising following steps：
Step A：Spent vanadium catalyst is washed using the protection solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters, wherein is being protected
In solution, it is 1% that dibasic acid esters, which hinders precipitating reagent mass fraction, and the mass fraction of oxalic acid is 2%.
Step B：Spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained, wherein spent vanadium catalyst needs
2h is dried in 100 DEG C.
Step C：Dry spent vanadium catalyst is soaked in the oxalic acid solution containing mass fraction 30-80%, heating 35
DEG C, the vanadic anhydride that mass fraction is 5% will be added in above-mentioned solution, 90 DEG C of heated solution, react 3 hours, then drain
Or drying, obtain the intermediate product containing spent vanadium catalyst.In this step, the pentavalent vanadium that stubble in spent vanadium catalyst is stored in is converted
For tetravalence vanadium；It, with the vanadium consumed in spent vanadium catalyst is supplemented, can be the CH of 250g/l using dope2O4V supplement.
Step D：Intermediate product is roasted at 300 DEG C, up to no gas is discharged, useless vanadium of the acquisition containing vanadic anhydride is urged
Agent；Preferably, maturing temperature is 500 DEG C.When roasting, generation is oxalic acid nitrogen, and uncontaminated gases discharge, oxalic acid is at 159 DEG C
It rises and opens volatilization decarburization generation calcium oxalate, be warming up to 500 DEG C, generate oxalic acid nitrogen.When the nitrogen of oxalic acid is sloughed, the vanadium of spent vanadium catalyst is
It is oxidized to pentavalent vanadium (V2O5), V in spent vanadium catalyst2O5Mass percent be 80%.According to the test method of QB614/88
The refractive index of the spent vanadium catalyst containing vanadic anhydride measured is 1.2-1.5.
Step E：Add 8% white carbon black to pelletize the spent vanadium catalyst containing vanadic anhydride, obtains the oxidation of finished product five two
Vanadium catalyst.In this step, high purity vanadic anhydride can also be supplemented when granulation.
In above-described embodiment, dibasic acid esters resistance precipitating reagent includes the component of following mass fraction：Phosphate 84-93.8%, five oxygen
Changing two vanadium is 0.2-1%, polyphosphate 6-15%.In the present invention, the preparation method of used dibasic acid esters resistance precipitating reagent in step A
For the prior art, detailed preparation method sees patent No. ZL2004100658012 patent application document.
In above-described embodiment, the general molecular formula of spent vanadium catalyst of the invention is VC2O(R)V2O5, wherein R C2H2O4。
The recovery and treatment method of spent vanadium catalyst of the invention, by dibasic acid esters hinder precipitating reagent, the effect of the reagents such as oxalic acid,
During recovery processing, polluted gas is not generated, does not generate waste, it is environmentally friendly, while spent vanadium catalyst is returned
High income, manufacturing cost are low.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (8)
1. a kind of recovery and treatment method of spent vanadium catalyst, which is characterized in that the described method comprises the following steps：
Step A：Spent vanadium catalyst is washed using the solution for hindering precipitating reagent and oxalic acid containing dibasic acid esters；
Step B：The spent vanadium catalyst is dried and is dried, dry spent vanadium catalyst is obtained；
Step C：The spent vanadium catalyst of the drying is soaked in the oxalic acid solution containing mass fraction 30-80%, 30- is heated
40 DEG C, the vanadic anhydride that mass fraction is 2-8% will be added in above-mentioned solution, heat 80-102 DEG C of the solution, react 2-5
Hour, obtain the intermediate product containing spent vanadium catalyst；
Step D：The intermediate product is roasted at 100-550 DEG C, up to no gas is discharged, acquisition is useless containing vanadic anhydride
Vanadium catalyst；
Step E：Add the white carbon black of 5%-10% to pelletize the spent vanadium catalyst containing vanadic anhydride, obtains five oxygen of finished product
Change two vanadium catalysts.
2. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
The general molecular formula of the spent vanadium catalyst is VC2O(R)V2O5, wherein R C2H2O4。
3. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
In the step B, the spent vanadium catalyst needs dry 2h in 100 DEG C.
4. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
V in the spent vanadium catalyst2O5Mass percent be 50%-100%.
5. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
The refractive index of the finished product vanadic anhydride is 1.2-1.5.
6. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
The dibasic acid esters resistance precipitating reagent includes the component of following mass fraction：Phosphate 84-93.8%, vanadic anhydride 0.2-
1%, polyphosphate 6-15%.
7. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
Maturing temperature is 450-550 DEG C in the step D.
8. the recovery and treatment method of spent vanadium catalyst according to claim 1, which is characterized in that
In the step A, the dibasic acid esters resistance precipitating reagent mass fraction is 0.5-1.5%, and the mass fraction of the oxalic acid is 1.5-
2.5%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114318015A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114318015A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
| CN114318015B (en) * | 2021-12-31 | 2023-08-15 | 马鞍山钢铁股份有限公司 | Treatment and utilization method of waste vanadium catalyst |
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| CN115155562A (en) | 2022-10-11 |
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Application publication date: 20181130 |
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