CN105950873B - A method of recycling vanadium, tungsten, titanium from waste and old SCR denitration - Google Patents
A method of recycling vanadium, tungsten, titanium from waste and old SCR denitration Download PDFInfo
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- CN105950873B CN105950873B CN201610545432.XA CN201610545432A CN105950873B CN 105950873 B CN105950873 B CN 105950873B CN 201610545432 A CN201610545432 A CN 201610545432A CN 105950873 B CN105950873 B CN 105950873B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry 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
- C22B34/1218—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 dry 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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
- C22B34/225—Obtaining vanadium from spent catalysts
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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
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
- C22B34/365—Obtaining tungsten 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 present invention relates to one kind recycling vanadium from waste and old SCR denitration, tungsten, the method of titanium, vanadium is mainly realized using a step high temperature reduction lixiviation process, tungsten, the separation and recycling of titanium, i.e. by the broken rear and reducing agent of waste and old SCR catalyst, reducing leaching agent, cooling agent etc. is uniformly mixed, smelting reduction at high temperature, part volatility barium oxide is collected by vaporization at high temperature and is enriched with, vanadium after reduction, tungsten species are deposited to bottom by ferrosilicon leaching, titanium dioxide forms after melt and realizes separation of solid and liquid by toppling over, the recovery process is simple, it is easily operated, universality is strong, the separation of vanadium tungsten titanium is more apparent, energy consumption is relatively low, isolated product purity meets related sale and requires, it is nearly free from removal process " three wastes ", it is expected to recycle applied to the scale of waste and old SCR denitration.
Description
Technical field
The present invention relates to spent catalyst utilization technology fields, especially a kind of to be catalyzed from waste and old honeycomb SCR denitration
The method that vanadium, tungsten, titanium are recycled in agent.
Background technology
With the engineered completion of the extensive denitration in China, most coal-burning power plants and Industrial Stoves are all made of selectivity
Catalytic oxidation denitration technology.As the SCR denitration of the technological core component, demand is in blowout situation in recent years.SCR
The denitrating catalyst service life is generally 3-5, expires and needs replacing.According to estimates by 2018, waste and old SCR catalyst is up to tens of
Ten thousand tons, and it is annual also by sustainable growth.In August, 2014, Chinese Ministry of Environmental Protection's publication《Waste flue gas denitration catalyst hazardous waste operation permission
Demonstrate,prove guidelines for examination》Waste and old SCR denitration is clearly classified as danger wastes, to being engaged in waste flue gas denitration catalyst (vanadium titanium
System) collect, storage, transport, regeneration, using disposing movable operating unit, from technical staff, waste transport, packaging and storage,
Facility and corollary equipment, technology and technique, system and measure etc. propose related examination requirement, waste and old SCR denitration catalysis
Agent disposition also becomes unavoidable a great problem on Denitration Industry chain therewith.
Two methods of regeneration and recycling are equipped at waste and old SCR catalyst.Only fewer companies have grasped catalyst again at present
Raw technology also has correlative regeneration demonstration project, but lacks large-scale practical application.Furthermore catalyst regeneration several times after, machinery
Intensity and catalytic activity cannot meet practical denitration demand, therefore finally or be revert to the disposition of waste and old SCR catalyst
Recycling comes up.Currently, domestic waste and old SCR denitration recycling is also in the laboratory research stage, and external recovery technology is also
Inadaptable domestic waste and old denitrating catalyst is practical.With closing on for the SCR denitration stage of replacement, domestic waste and old SCR denitration is urged
The exploitation of agent recovery technology is extremely urgent, and SCR catalyst recycling research also becomes the heat of Environmental Protection in China area research
Point.In addition, for toxic element vanadium, since content is less in SCR catalyst for it, it is difficult to regular course by it from urging
It is detached in agent.
There is the relevant report that SCR catalyst recycles in patent and periodical literature at present, but there are one for the relevant technologies
A little defects, such as technology path complexity, the strong acid and strong base used in the process is more, and " three wastes " are more, and the final products of recycling are not yet
It is identical to the greatest extent, increasing SCR spent catalysts recycling demand cannot be met.Patent of invention (application number 201510535971.0)
A kind of SCR denitration processing method is disclosed, emphasis is to deviate from the vanadium in catalyst with molten iron or molten steel, i.e., will
SCR denitration processing is combined with steel-making ironmaking, and vanadium is made to be converted into calcium vanadate.But the technology path has the following disadvantages:
First, entire route is complex, to be combined with steel-making ironmaking, need a large amount of molten iron or molten steel, energy consumption higher in the process;
Second is that technology path is using restrictive.The technical finesse mode is not suitable for waste and old SCR catalyst, because waste and old SCR is urged
It can be entered in final molten iron or molten steel containing heavy metal in agent, influence the quality of final product abrasion-proof steel ball;Third, adding
Add component more, slag component differs, and the separation and recovery rate of vanadium, tungsten and titanium is not high, is not suitable for scale processing SCR denitration catalysis
Agent.Therefore, there is an urgent need for developing, a kind of route is simple, universality is strong, the technology of waste and old SCR denitration can be recycled with scale.
Invention content
The purpose of the invention is to overcome the shortcomings of existing SCR denitration recovery technology, provide a kind of completely new
The method that vanadium, tungsten, titanium are recycled from waste and old SCR denitration, recycles vanadium, tungsten, titanium in catalyst respectively, recycles skill
Art route is simple, and universality is strong, and isolated product purity meets related request, and prospect for sales is apparent, while recycling
" three wastes " are nearly free from journey, environmental benefit is apparent.
To achieve the goals above, one kind designed by the present invention recycles vanadium, tungsten, titanium from waste and old SCR denitration
Method, include the following steps:
(1), waste and old SCR catalyst is broken into powder, the content of detection wherein vanadium, tungsten, titanium, be then added reducing agent,
Reducing leaching agent and cooling agent are simultaneously uniformly mixed;
(2), powder after mixing is added in reacting furnace and is melted, obtain clinker, stove liquid and furnace gas;
(3), furnace gas is collected by dust collecting at the top of reacting furnace, and stove liquid pours out to realize stove liquid and clinker
It is separated by solid-liquid separation, is collected after cooling of furnace slag.
Preferably, the reducing agent is that reducing metal or reproducibility are nonmetallic, and additive amount is in waste and old SCR catalyst
1-2 times of vanadium constituent content.
Preferably, the reducing metal is the mixture of iron powder or aluminium powder either the two, the non-gold of reproducibility
It is silica flour to belong to.
Preferably, the reducing leaching agent is ferrosilicon powder, and additive amount is the 1- of tungsten constituent content in waste and old SCR catalyst
2 times.
Preferably, the cooling agent is the salt that fusing point is less than 1200 DEG C, and additive amount is the 0- of waste and old SCR catalyst total amount
20%.
Preferably, the cooling agent is the mixture of calcirm-fluoride or sodium metasilicate either the two.
Preferably, the melting temperature in the step (2) is 1600-3300 DEG C, melting time 0.5-12h.
Preferably, the reacting furnace is intermediate frequency furnace or direct current electric arc furnace.The purpose of reacting furnace is carried for powder raw material melting
For hot environment, General reactions container is the refractory material that graphite crucible or other highests can bear 3300 DEG C of high temperature, and
And in order to adapt to large-scale production, reaction vessel preferably can disposably accommodate the powder raw material of 0.1-20t or so.
Further, the furnace gas includes barium oxide, in addition to barium oxide also has volatile low boilers in general furnace gas
Matter, the clinker include the vanadium metal being reduced, tungsten and reducing leaching agent, and the stove liquid includes the titanium dioxide of molten state.
Relative to existing SCR catalyst recovery technology, the present invention has the following advantages:(1) technology is novel, route is simple,
Cost is less, is only the separation for realizing vanadium, three kinds of tungsten, titanium components by a step high temperature reduction lixiviation process;(2) it is generated during
It is not related to strong acid and strong base, is nearly free from " three wastes ", the barium oxide that vaporization at high temperature goes out can be added by dust collecting
To collect and be enriched with, tungsten, titanium species can be collected by being separated by solid-liquid separation;(3) this method have universality, i.e., this method with it is waste and old
Whether vanadium tungsten component ratio is unrelated in SCR catalyst, be that honeycomb, ripple and board-like catalyst are unrelated with catalyst type, and useless
Old SCR catalyst failure cause is unrelated;(4) recycling of SCR denitration large-scale, economy effect may be implemented in the technology path
Benefit and environmental benefit are fairly obvious.
Relative to above-mentioned patent of invention (application number 201510535971.0), route of the present invention is relatively simple, only
It needs step reduction to be achieved that the separation and recycling of the key components such as vanadium, tungsten, titanium, it is valuable to reduce vanadium in removal process, tungsten etc.
The waste of component, and molten iron and molten steel need not be largely used, reduce the energy consumption in removal process.
Specific implementation mode
With reference to embodiment, the present invention is further described.
Embodiment 1:
A kind of method recycling vanadium, tungsten, titanium from waste and old SCR denitration provided by the invention, includes the following steps:
(1), waste and old SCR catalyst is broken into powder, utilizes x-ray fluorescence analyzer detection wherein vanadic anhydride, three oxygen
Change the content of tungsten, titanium dioxide, content is followed successively by 1.0%, 3.5%, 87.0% in the present embodiment;
(2) according to above components content, aluminium powder, ferrosilicon powder and calcirm-fluoride, and its quality are added into catalyst fines
Percentage is respectively 1.2%, 5%, 10%, then stirs 30min, it is made to be uniformly mixed;
(3), above-mentioned uniformly mixed raw material 0.5t is disposably put into reacting furnace, startup power supply, cooling device and
Dust collecting starts melting, the melting 1h under 1800 DEG C of melting temperature;
(4), in fusion process, the dust collecting in the reacted furnace roof portion of furnace gas is collected, and stove is formed in reacting furnace
The solid-liquid state of liquid and clinker;
(5) upper layer stove liquid is poured out into collection, is collected after lower layer's cooling of furnace slag;
(6), above-mentioned furnace gas, clinker and stove liquid are analyzed, wherein stove liquid main component is titanium dioxide, and content is big
In 90%, tungstic acid is less than 0.2%, and vanadium component is not detected;Clinker is mainly ferrotungsten component, and wherein tungstic acid content is big
In 22%, vanadium component is not detected, furnace gas includes the vanadium component that content is more than 5%.
Embodiment 2
A kind of method recycling vanadium, tungsten, titanium from waste and old SCR denitration provided by the invention, includes the following steps:
(1), waste and old SCR catalyst is crushed powder, utilizes x-ray fluorescence analyzer detection wherein vanadic anhydride, three oxidations
The content of tungsten, titanium dioxide, content is followed successively by 1.0%, 3.5%, 87.0% in the present embodiment;
(2) according to above components content, iron powder, ferrosilicon powder and sodium metasilicate, and quality hundred are added into catalyst fines
Divide than being respectively 2%, 7%, 20%, then stirs 30min, it is made to be uniformly mixed;
(3), above-mentioned uniformly mixed raw material 0.5t is disposably put into reacting furnace, startup power supply, cooling device and
Dust collecting starts melting, the melting 3h under 2200 DEG C of melting temperature;
(4), in fusion process, the dust collecting in the reacted furnace roof portion of furnace gas is collected, and stove is formed in reacting furnace
The solid-liquid state of liquid and clinker;
(5), upper layer stove liquid is poured out into collection, is collected after lower layer's cooling of furnace slag;
(6), above-mentioned furnace gas, clinker and stove liquid are analyzed, wherein stove liquid main component is titanium dioxide, content
84%, tungstic acid is less than 1%, and vanadium component is not detected;Clinker is mainly ferrotungsten component, and wherein tungstic acid content is more than
15%, it is not apparent from and detects vanadium component, furnace gas includes the vanadium component that content is more than 3%.
Embodiment 3
A kind of method recycling vanadium, tungsten, titanium from waste and old SCR denitration provided by the invention, includes the following steps:
(1), waste and old SCR catalyst is crushed powder, utilizes x-ray fluorescence analyzer detection wherein vanadic anhydride, three oxidations
The content of tungsten, titanium dioxide, content is followed successively by 1.0%, 3.5%, 87.0% in the present embodiment;
(2) according to above components content, silica flour, ferrosilicon powder and calcirm-fluoride, and quality hundred are added into catalyst fines
Divide than being respectively 2%, 7%, 15%, then stirs 30min, it is made to be uniformly mixed;
(3), above-mentioned uniformly mixed raw material 0.5t is disposably put into reacting furnace, startup power supply, cooling device and
Dust collecting starts melting, the melting 1h under 2800 DEG C of melting temperature;
(4), in fusion process, the dust collecting in the reacted furnace roof portion of furnace gas is collected, and stove is formed in reacting furnace
The solid-liquid state of liquid and clinker;
(5) upper layer stove liquid is poured out into collection, is collected after lower layer's cooling of furnace slag;
(6), above-mentioned furnace gas, clinker and stove liquid are analyzed, wherein stove liquid main component is titanium dioxide, content
87%, tungstic acid is less than 0.7%, and vanadium component is not detected;Clinker is mainly ferrotungsten component, and wherein tungstic acid content is more than
20%, it is not apparent from and detects vanadium component;Furnace gas includes the vanadium component that content is more than 3.5%.
Reacting furnace in embodiment 1-3 can be intermediate frequency furnace, can also be direct current electric arc furnace, it might even be possible to be other energy
The reacting furnace of 3300 DEG C of high temperature is enough born, and in order to adapt to large-scale production, reacting furnace preferably can be accommodated disposably
The powder raw material of 0.1-20t or so.
From embodiment 1-3 it is found that being only point for realizing vanadium, three kinds of tungsten, titanium components by a step high temperature reduction lixiviation process
From route is simple, easy to operate, the recycling of SCR denitration large-scale may be implemented, economic benefit and environmental benefit are very
Obviously, and the vanadium as toxic element largely reacted furnace roof portion dust collecting collect, make it easier to from catalysis
It is separated in agent, and is conducive to the post-processing of vanadium component.
The above described is only a preferred embodiment of the present invention, be not the limitation for making other forms to invention, it is any
Those skilled in the art are changed or are modified as the equivalent of equivalent variations possibly also with the technology contents of the disclosure above
Embodiment.But it is every without departing from technical solution of the present invention content, above example is made according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (5)
1. a kind of method recycling vanadium, tungsten, titanium from waste and old SCR denitration, it is characterised in that include the following steps:
(1), waste and old SCR catalyst is broken into powder, then reducing agent, reduction is added in the content of detection wherein vanadium, tungsten, titanium
Leaching agent and cooling agent are simultaneously uniformly mixed;
(2), powder after mixing is added in reacting furnace and is melted, obtain clinker, stove liquid and furnace gas, wherein melting temperature
Degree is 1600-3300 DEG C, melting time 0.5-12h;
(3), furnace gas is collected by the dust collecting at the top of reacting furnace, and stove liquid is poured out to realize the solid-liquid of stove liquid and clinker
Separation is collected after cooling of furnace slag, and the furnace gas includes barium oxide, the clinker include the vanadium metal being reduced, tungsten with
And reducing leaching agent, the stove liquid include the titanium dioxide of molten state,
Wherein, the reducing agent is that reducing metal or reproducibility are nonmetallic, the reducing metal be iron powder or aluminium powder or
Person is the mixture of the two, and the nonmetallic reproducibility is silica flour;The reducing leaching agent is ferrosilicon powder;The cooling agent is fluorine
Change the mixture of calcium or sodium metasilicate either the two.
2. the method according to claim 1 for recycling vanadium, tungsten, titanium from waste and old SCR denitration, it is characterised in that:
The additive amount of the reducing agent is 1-2 times of vanadium constituent content in waste and old SCR catalyst.
3. the method according to claim 1 for recycling vanadium, tungsten, titanium from waste and old SCR denitration, it is characterised in that:
The additive amount of the reducing leaching agent is 1-2 times of tungsten constituent content in waste and old SCR catalyst.
4. the method according to claim 1 for recycling vanadium, tungsten, titanium from waste and old SCR denitration, it is characterised in that:
The additive amount of the cooling agent is the 0-20% of waste and old SCR catalyst total amount.
5. the method according to claim 1 for recycling vanadium, tungsten, titanium from waste and old SCR denitration, it is characterised in that:
The reacting furnace is intermediate frequency furnace or direct current electric arc furnace.
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CN106350679B (en) * | 2016-09-23 | 2018-09-21 | 攀枝花学院 | A method of recycling valuable metal titanium vanadium tungsten from useless SCR denitration |
CN106337133B (en) * | 2016-09-30 | 2018-06-29 | 攀枝花学院 | The recovery method of titanium vanadium tungsten in a kind of useless SCR denitration |
CN106480318A (en) * | 2016-10-21 | 2017-03-08 | 北京矿冶研究总院 | Method for recovering nickel and vanadium from waste FCC catalyst by reduction smelting |
CN106319230B (en) * | 2016-11-08 | 2018-06-22 | 南通市多乾新材料科技有限公司 | A kind of Dry recovery is given up the method for Titanium vanadium tungsten in SCR catalyst |
CN106512716A (en) * | 2016-11-15 | 2017-03-22 | 东莞市联洲知识产权运营管理有限公司 | Low-temperature flue gas SCR denitration and tungsten, vanadium and titanium comprehensive recovery method |
CN106521165B (en) * | 2016-11-25 | 2018-08-31 | 东莞市联洲知识产权运营管理有限公司 | A method of extraction discards valuable metal in SCR catalyst and prepares alloy |
CN106756050B (en) * | 2016-12-26 | 2018-07-27 | 北京国电龙源环保工程有限公司 | The method that conbustion synthesis recycles waste denitration catalyst |
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DE2908570C2 (en) * | 1979-03-05 | 1982-12-16 | Fa. Hermann C. Starck Berlin, 1000 Berlin | Process for the recovery of valuable metals from catalysts |
CN1024469C (en) * | 1991-07-12 | 1994-05-11 | 齐鲁石油化工公司研究院 | Method of nickel retrieved from waste catalyst by pyrogenic process |
CN1257295C (en) * | 2004-11-15 | 2006-05-24 | 四川川投峨眉铁合金(集团)有限责任公司 | Production process for dry method extraction of nickel |
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