CN104628032B - Method for preparing high-purity ammonium metavanadate from spent catalyst - Google Patents
Method for preparing high-purity ammonium metavanadate from spent catalyst Download PDFInfo
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- CN104628032B CN104628032B CN201510004137.9A CN201510004137A CN104628032B CN 104628032 B CN104628032 B CN 104628032B CN 201510004137 A CN201510004137 A CN 201510004137A CN 104628032 B CN104628032 B CN 104628032B
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- vanadium
- molybdenum
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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
- C01G31/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for preparing high-purity ammonium metavanadate from a spent catalyst, which comprises the following steps: dephosphorization: collecting a spent catalyst leach solution in a leaching mode, filtering the leach solution, sending into an ion-exchange dephosphorization system, and carrying out phosphorus adsorption on the spent catalyst leach solution by using a resin; molybdenum-vanadium separation: sending the dephosphorized molybdenum/vanadium-containing solution into an ion-exchange system, and carrying out molybdenum adsorption by using a resin to separate the molybdenum and vanadium; and vanadium precipitation: pumping the vanadium-containing mother solution subjected to dephosphorization and separation molybdenum into a vanadium precipitation tank, and precipitating vanadium by using a weakly alkaline ammonium salt to obtain the high-purity ammonium metavanadate product. The method has the characteristics of short process, simple technique, energy saving, environmental protection, high efficiency, low cost and the like.
Description
Technical field
The present invention proposes a kind of method that dead catalyst of vanadium containing molybdenum prepares high-purity ammonium metavanadate, and it is the exchange point of molybdenum vanadium ion
Prepare high-purity ammonium metavanadate technology from a kind of separating-purifying combining with chemical precipitation method, belong to field of chemical separation and purification.
Background technology
Contain the rare metal such as molybdenum vanadium in oil refining waste catalyst, in processing disposal process due to vanadium and molybdenum property extremely
Similar, after wet-leaching molybdenum vanadium ion deep impurity-removing, carry out chemical precipitation and prepare ammonium metavanadate carrying reason secretly due to molybdenum, can only
The smart vanadium doing 98.5% prepares high-purity ammonium metavanadate it is impossible to do a precipitation, if traditional handicraft is done high-purity ammonium metavanadate and must be adopted
Use secondary recrystallization technology, with high costs.
The method of traditional Separation of vanadium and molybdenum is addition ammonium salt precipitation, vanadium shape in ph value is for the molybdate solution of 7.0-9.0
Become ammonium vanadate to be precipitated out, and molybdenum still remains in solution to reach Separation of vanadium and molybdenum.But vanadium concentration is required, and separates
Not thorough, also Separation of vanadium and molybdenum is carried out using extraction, this method 15%n263, under conditions of ph=7, o/a=1/2, Jing Guowu
Level extraction, the extraction yield of vanadium reaches 99.52%, and the extraction yield of molybdenum is 13.71% it is clear that this method is not suitable for Separation of vanadium and molybdenum.
Learn through retrieval: the patent of this respect has a cn1792819a, " separates from ammonium molybdate solution and remove the net of vanadium
Change method ".It is using large aperture chelating resin 190, d401, d411, d13, d418；Or gel chelating resin cu, wp-1,
wp-2.Vanadium in Adsorption molybdate solution, adsorption conditionses are: the ph value controlling feeding liquid is 6.5-8.5, and flow velocity is 0.2-
2 times of column volumes, control feed liquid and resin contact time to be 30-300 minute, stop inhaling when effluent vanadium content reaches and wears
Attached, with the ammonia of 4%-5% or the naoh solution drip washing of 0.1-2mol/l, using mineral acid regenerating resin.This method can have
The vanadium removing in molybdate solution of effect, but these resins also adsorb a small amount of molybdenum while adsorption of vanadium.Desorbed solution chemistry is heavy
Vanadium also cannot prepare high-purity ammonium metavanadate.
Content of the invention
It is an object of the invention to provide a kind of preparation cost low, without secondary recrystallization technology, process is simple, make full use of
In dead catalyst, utility, the dead catalyst of environmental protection prepare high-purity ammonium metavanadate method, overcome the deficiencies in the prior art.
The dead catalyst of the present invention prepares high-purity ammonium metavanadate method, and step is as follows:
, dephosphorization, using leach mode collect dead catalyst leachate, leachate is filtered subsequently into ion
Exchange dephosphorization system, carry out phosphorus absorption using resin, phosphorus in dead catalyst leachate is adsorbed；
, molybdenum vanadium separate, after dephosphorization vanadium solution containing molybdenum entrance ion exchange system, carry out molybdenum absorption using resin, make molybdenum
Vanadium separates；
, precipitation, vanadium settling tank will be pumped into containing vanadium mother liquid after dephosphorization, Separation of Molybdenum, carries out alkalescence ammonium salt precipitation, obtain
High-purity ammonium metavanadate product.
Described dead catalyst leachate, is to be leached and produced by containing molybdenum, vanadium dead catalyst, molten containing molybdenum, vanadium and phosphorus
Liquid.
Described using the condition that resin carries out phosphorus absorption is: the ph value of leachate is 6.5 ~ 8.5, and flow velocity is 0.2 ~ 2 times
Column volume, time of contact is 30 ~ 300 minutes, and when effluent phosphorus content reaches more than 2ppm, resin reaches saturation, stops inhaling
Attached, carry out resin parsing, resin parsing is the ammonia spirit drip washing with 4% ~ 5%, completes resin regeneration.
The condition that described ion exchange resin carries out molybdenum absorption is: the ph value of feeding liquid is 8-9, and flow velocity is 0.3-3 times
Column volume, feed liquid and resin contact time are 25-150 minute, and when effluent amount containing molybdenum is more than 0.05g/l, resin reaches full
With, stop absorption, carry out resin parsing, resin parsing is the naoh solution drip washing parsing with 1-3mol/l, completes resin regeneration,
The standby heavy molybdenum of desorbed solution.
Described adds ammonium salt precipitation containing in vanadium mother liquid, under the conditions of ph value is for 7.5-9, carries out alkalescence ammonium salt precipitation.
Described is the gel-type being capable of selective absorption phosphate anion using the resin that resin is carried out used by phosphorus absorption
Anion exchange resin；Described is being capable of selective absorption molybdenum acid ion using the resin that resin is carried out used by molybdenum absorption
Macropore-equal pass anion exchange resin.
The method of the present invention, by the dead catalyst leachate containing molybdenum vanadium, eliminates impurity with ion exchange technique deep impurity-removing
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, last only surplus pure containing vanadium mother liquid, with ammonium salt chemistry
Precipitation, filters, obtains purity more than 99.9% ammonium metavanadate.Phosphorus in this method selective absorption leachate, selective absorption is soaked
Go out the molybdenum in liquid, so that vanadium and molybdenum is efficiently separated.With existing prepare high-purity ammonium metavanadate technique compared with, used twice from
Son exchanges, and an ammonium salt precipitation prepares high-purity ammonium metavanadate, and not using secondary recrystallization technology, has that flow process is short, technique is simple
The features such as list, energy-conserving and environment-protective, efficiency high, low cost, efficiently solve the problems, such as that in ammonium metavanadate, molybdenum is carried secretly.
In the present invention, the phosphorus in the dead catalyst leachate of vanadium containing molybdenum can effectively be adsorbed by the dephosphorization resin of application, and
Resin absorption can be carried out in neutral conditions, can effectively reduce the consumption of soda acid, and molybdenum vanadium separation selectivity resin only adsorbs molybdic acid
Radical ion.
Brief description
Fig. 1 high-purity ammonium metavanadate production technological process.
Specific embodiment
It is addressed further under the technical characteristic of the present invention below by embodiment, but be not limited to embodiment, refer to the attached drawing 1.
Embodiment 1
Dead catalyst, after leaching and filtering, obtains 26m3Leachate, wherein contains phosphorus 0.67g/l, molybdenum 12.73g/l, vanadium
17.81g/l.
(1) dephosphorization
Adjusting leachate ph value is 6.5, enters ion exchange system, by ion exchange column, is handed over gel-type anion
Change resin, the phosphorus in leachate is adsorbed.Control valve, control feed flow rate is 0.2 times of column volume, after testing, feed liquid
Contact 270 minutes with resin after, effluent phosphorus content is more than 2ppm, resin absorption saturation, stops absorption immediately.
Resin carries out drip washing parsing with 4% ammonia spirit, completes to regenerate simultaneously.After ammonium phosphate solution crystallization to be concentrated, can
Standby production phosphate fertilizer.
(2) molybdenum vanadium separates
After dephosphorization, leachate enters molybdenum vanadium piece-rate system and carries out molybdenum absorption, adjusts leachate ph=8, by three group four arrange from
Sub- exchange column, carries out molybdenum absorption using macropore-all pass anion exchange resin.Control valve, controls feed flow rate to be 0.5 times
Column volume, after testing, after feed liquid contacts 143 minutes with resin, effluent amount containing molybdenum is more than 0.05g/l, resin absorption saturation, stands
Stop absorption, obtain pure containing vanadium mother liquid.
First use clear water washing resin, clean remaining in the vanadium solution in resin gap, then use the naoh of 1mol/l molten
Liquid drip washing parses, and completes resin regeneration, the standby heavy molybdenum of desorbed solution simultaneously.
(3) precipitation
The pure concentration of vanadium containing vanadium mother liquid is 16.64g/l, adjusts ph=7.5, adds ammonium salt precipitant by 3:1 weight ratio,
At the uniform velocity add sulfate precipitation agent in whipping process, control temperature 45 C, stirring reaction, after 1 hour, filters, immediately by plate
After frame filter pressing separates, obtain high-purity ammonium metavanadate product
This commerical test, the dead catalyst leachate ion exchange technique deep impurity-removing containing molybdenum vanadium eliminates impurity
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, obtain pure containing vanadium mother liquid, finally once with ammonium salt
Property precipitation, filter, obtain high-purity ammonium metavanadate product that purity is 99.96%.
Embodiment 2
Dead catalyst, after leaching and filtering, obtains 24.6m3Leachate, its phosphorous 1.34g/l, molybdenum 12.72g/l, vanadium
18.16g/l.
(1) dephosphorization
Adjusting leachate ph value is 7, enters ion exchange system, by ion exchange column, with being handed over gel-type anion
Change resin, the phosphorus in leachate is adsorbed.Control valve, control feed flow rate is 0.5 times of column volume, after testing, feed liquid
Contact 200 minutes with resin after, effluent phosphorus content is more than 2ppm, resin absorption saturation, stops absorption immediately.
Resin carries out drip washing parsing with 4.2% ammonia spirit, completes to regenerate simultaneously.After ammonium phosphate solution crystallization to be concentrated,
Can standby production phosphate fertilizer.
(2) molybdenum vanadium separates
After dephosphorization, leachate entrance molybdenum vanadium piece-rate system carries out molybdenum absorption, adjusts leachate ph=8.3, is arranged by three group four
Ion exchange column, macropore-all pass anion exchange resin carry out molybdenum absorption.Control valve, control feed flow rate is 1 times of cylinder
Long-pending, after testing, after feed liquid contacts 124 minutes with resin, effluent amount containing molybdenum is more than 0.05g/l, resin absorption saturation, stops immediately
Only adsorb, obtain pure containing vanadium mother liquid.
First use clear water washing resin, clean remaining in the vanadium solution in resin gap, then use the naoh of 1.3mol/l
Solution drip washing parses, and completes resin regeneration, the standby heavy molybdenum of desorbed solution simultaneously.
(3) precipitation
The pure concentration of vanadium containing vanadium mother liquid is 17.46g/l, adjusts ph=7.8, adds sulfate precipitation by 3:1 weight ratio
Agent, at the uniform velocity adds sulfate precipitation agent in whipping process, controls temperature 45 C, and stirring reaction, after 1 hour, filters immediately, leads to
After crossing filter press separation, obtain high-purity ammonium metavanadate product.
This commerical test, the dead catalyst leachate ion exchange technique deep impurity-removing containing molybdenum vanadium eliminates impurity
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, obtain pure containing vanadium mother liquid, finally once with ammonium salt
Property precipitation, filter, obtain high-purity ammonium metavanadate product that purity is 99.95%.
Embodiment 3
Dead catalyst, after leaching and filtering, obtains 21.3m3Leachate, wherein phosphorous 1.55g/l, molybdenum 18.97g/l, vanadium
23.2g/l.
(1) dephosphorization
Adjusting leachate ph value is 7.5, enters ion exchange system, by ion exchange column, with using gel-type anion
Exchanger resin, adsorbs to the phosphorus in leachate.Control valve, control feed flow rate is 1 times of column volume, after testing, feed liquid
Contact 150 minutes with resin after, effluent phosphorus content is more than 2ppm, resin absorption saturation, stops absorption immediately.
Resin carries out drip washing parsing with 4.4% ammonia spirit, completes to regenerate simultaneously.After ammonium phosphate solution crystallization to be concentrated,
Can standby production phosphate fertilizer.
(2) molybdenum vanadium separates
After dephosphorization, leachate entrance molybdenum vanadium piece-rate system carries out molybdenum absorption, adjusts leachate ph=8.5, is arranged by three group four
Ion exchange column, carries out molybdenum absorption using macropore-all pass anion exchange resin.Control valve, controls feed flow rate to be 1.8
Times column volume, after testing, after feed liquid contacts 95 minutes with resin, effluent amount containing molybdenum is more than 0.05g/l, resin absorption saturation,
Stop absorption immediately, obtain pure containing vanadium mother liquid.
First use clear water washing resin, clean remaining in the vanadium solution in resin gap, then use the naoh of 1.8mol/l
Solution drip washing parses, and completes resin regeneration, the standby heavy molybdenum of desorbed solution simultaneously.
(3) precipitation
The pure concentration of vanadium containing vanadium mother liquid is 21.31g/l, adjusts ph=8.2, adds sulfate precipitation by 3:1 weight ratio
Agent, at the uniform velocity adds sulfate precipitation agent in whipping process, controls temperature 45 C, and stirring reaction, after 1 hour, filters immediately, leads to
After crossing filter press separation, obtain high-purity ammonium metavanadate product.
This commerical test, the dead catalyst leachate ion exchange technique deep impurity-removing containing molybdenum vanadium eliminates impurity
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, obtain pure containing vanadium mother liquid, finally once with ammonium salt
Property precipitation, filter, obtain high-purity ammonium metavanadate product that purity is 99.97%.
Embodiment 4
Dead catalyst, after leaching and filtering, obtains 22.4m3Leachate, wherein phosphorous 1.85g/l, molybdenum 12.78g/l, vanadium
17.87g/l .
(1) dephosphorization
Adjusting leachate ph value is 8, enters ion exchange system, by ion exchange column, with being handed over gel-type anion
Change resin, the phosphorus in leachate is adsorbed.Control valve, control feed flow rate is 1.5 times of column volumes, after testing, feed liquid
Contact 102 minutes with resin after, effluent phosphorus content is more than 2ppm, resin absorption saturation, stops absorption immediately.
Resin carries out drip washing parsing with 4.7% ammonia spirit, completes to regenerate simultaneously.After ammonium phosphate solution crystallization to be concentrated,
Can standby production phosphate fertilizer.
(2) molybdenum vanadium separates
After dephosphorization, leachate entrance molybdenum vanadium piece-rate system carries out molybdenum absorption, adjusts leachate ph=8.7, is arranged by three group four
Ion exchange column, carries out molybdenum absorption using macropore-all pass anion exchange resin.Control valve, controls feed flow rate to be 2.4
Times column volume, after testing, after feed liquid contacts 72 minutes with resin, effluent amount containing molybdenum is more than 0.05g/l, resin absorption saturation,
Stop absorption immediately, obtain pure containing vanadium mother liquid.
First use clear water washing resin, clean remaining in the vanadium solution in resin gap, then use the naoh of 2.5mol/l
Solution drip washing parses, and completes resin regeneration, the standby heavy molybdenum of desorbed solution simultaneously.
(3) precipitation
The pure concentration of vanadium containing vanadium mother liquid is 16.69g/l, adjusts ph=8.6, adds sulfate precipitation by 3:1 weight ratio
Agent, at the uniform velocity adds sulfate precipitation agent in whipping process, controls temperature 45 C, and stirring reaction, after 1 hour, filters immediately, leads to
After crossing filter press separation, obtain high-purity ammonium metavanadate product.
This commerical test, the dead catalyst leachate ion exchange technique deep impurity-removing containing molybdenum vanadium eliminates impurity
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, obtain pure containing vanadium mother liquid, finally once with ammonium salt
Property precipitation, filter, obtain high-purity ammonium metavanadate product that purity is 99.96%.
Embodiment 5
Dead catalyst, after leaching and filtering, obtains 18.9m3Leachate, wherein phosphorous 2.06g/l, molybdenum 18.2g/l, vanadium
22.36g/l.
(1) dephosphorization
Adjusting leachate ph value is 8.5, enters ion exchange system, by ion exchange column, with using gel-type anion
Exchanger resin, adsorbs to the phosphorus in leachate.Control valve, control feed flow rate is 2 times of column volumes, after testing, feed liquid
Contact 56 minutes with resin after, effluent phosphorus content is more than 2ppm, resin absorption saturation, stops absorption immediately.
Resin carries out drip washing parsing with 5% ammonia spirit, completes to regenerate simultaneously.After ammonium phosphate solution crystallization to be concentrated, can
Standby production phosphate fertilizer.
(2) molybdenum vanadium separates
After dephosphorization, leachate enters molybdenum vanadium piece-rate system and carries out molybdenum absorption, adjusts leachate ph=9, by three group four arrange from
Sub- exchange column, carries out molybdenum absorption using macropore-all pass anion exchange resin.Control valve, control feed flow rate is 3 times of posts
Volume, after testing, after feed liquid contacts 38 minutes with resin, effluent amount containing molybdenum be more than 0.05g/l, resin absorption saturation, immediately
Stop absorption, obtain pure containing vanadium mother liquid.
First use clear water washing resin, clean remaining in the vanadium solution in resin gap, then use the naoh of 3mol/l molten
Liquid drip washing parses, and completes resin regeneration, the standby heavy molybdenum of desorbed solution simultaneously.
(3) precipitation
The pure concentration of vanadium containing vanadium mother liquid is 21.49g/l, adjusts ph=9, adds sulfate precipitation agent by 3:1 weight ratio,
At the uniform velocity add sulfate precipitation agent in whipping process, control temperature 45 C, stirring reaction, after 1 hour, filters, immediately by plate
After frame filter pressing separates, obtain high-purity ammonium metavanadate product.
This commerical test, the dead catalyst leachate ion exchange technique deep impurity-removing containing molybdenum vanadium eliminates impurity
Phosphorus, then makes molybdenum vanadium metal ion isolation with ion exchange technique again, obtain pure containing vanadium mother liquid, finally once with ammonium salt
Property precipitation, filter, obtain high-purity ammonium metavanadate product that purity is 99.98%.
Claims (2)
1. a kind of dead catalyst prepare high-purity ammonium metavanadate method it is characterised in that: processing step is as follows:
, dephosphorization, using leach mode collect dead catalyst leachate, leachate is filtered subsequently into ion exchange
Dephosphorization system, carries out phosphorus absorption using resin；
, molybdenum vanadium separate, after dephosphorization vanadium solution containing molybdenum entrance ion exchange system, carry out molybdenum absorption using resin, so that molybdenum vanadium is divided
From；
, precipitation, vanadium settling tank will be pumped into containing vanadium mother liquid after dephosphorization, Separation of Molybdenum, carries out alkalescence ammonium salt precipitation, obtain high-purity partially
Ammonium vanadate product；
Described using the condition that resin carries out phosphorus absorption is: the ph value of leachate is 6.5 ~ 8.5, and flow velocity is 0.2 ~ 2 times of cylinder
Long-pending, time of contact is 30 ~ 300 minutes, and when effluent phosphorus content reaches more than 2ppm, resin reaches saturation, stops absorption, enters
Row resin parses.
2. dead catalyst according to claim 1 prepare high-purity ammonium metavanadate method it is characterised in that: described resin solution
Analysis is the ammonia spirit drip washing with 4% ~ 5%, completes resin regeneration.
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| CN107500353A (en) * | 2017-09-19 | 2017-12-22 | 芜湖人本合金有限责任公司 | High-purity sodium metavanadate and preparation method thereof |
| CN108754185B (en) * | 2018-05-25 | 2021-02-02 | 中国科学院过程工程研究所 | Method for purifying silicon, phosphorus and arsenic in vanadium-containing solution |
| CN115198118A (en) * | 2022-06-29 | 2022-10-18 | 安庆市月铜钼业有限公司 | Process for producing sodium molybdate by using vanadium-molybdenum-containing calcine |
| CN116445717B (en) * | 2023-03-17 | 2023-10-20 | 浙江大学 | Resource utilization method of plate-type waste flue gas denitration catalyst |
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| CN1083802C (en) * | 1998-12-05 | 2002-05-01 | 中南工业大学 | Elimination of molybdenum from tungstate soltuion |
| CN1319863C (en) * | 2004-09-24 | 2007-06-06 | 刘亚光 | Method of producing ranadium pentoxide using vanadium containing waste catalyst |
| CN100482814C (en) * | 2005-09-30 | 2009-04-29 | 沈阳华瑞钒业有限公司 | Extraction of vanadium and molybdenum compound from refused materials containing vanadium and molybdenum etc. multiple elements |
| CN101343093B (en) * | 2008-09-03 | 2011-07-13 | 南京大学 | Method for deeply purifying minim phosphor in water with composite resin |
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