CN108677016A - A kind of preparation method of metallurgical titanium slag and ferrotitanium vanadium alloy containing waste denitration catalyst - Google Patents
A kind of preparation method of metallurgical titanium slag and ferrotitanium vanadium alloy containing waste denitration catalyst Download PDFInfo
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- CN108677016A CN108677016A CN201810481162.XA CN201810481162A CN108677016A CN 108677016 A CN108677016 A CN 108677016A CN 201810481162 A CN201810481162 A CN 201810481162A CN 108677016 A CN108677016 A CN 108677016A
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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
- C22B7/009—General processes for recovering metals or metallic compounds 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
- C22B34/10—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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/006—Making ferrous alloys compositions used for making ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
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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 preparation method of the present invention provides a kind of metallurgical titanium slag and ferrotitanium vanadium alloy containing waste denitration catalyst.Metallurgical titanium slag provided by the invention containing waste denitration catalyst includes the component of following mass content：Waste denitration catalyst 20~52.9%, MgO 6.4~8%, Na2CO33.9~8%, CaF26.4~10% and calcium containing alloy 30~50%.Metallurgical titanium slag provided by the invention containing waste denitration catalyst can be used as alloy source to be used for smelting iron titanium vanadium alloy, wherein calcium containing alloy can restore the TiO in discarded SCR denitration as reducing agent2、V2O5Equal metal oxides so that the metallic elements mass transfer such as Ti, V enters alloying in molten steel or forms ferrotitanium vanadium alloy.The experimental results showed that when the metallurgical titanium slag provided by the invention containing waste denitration catalyst is used for smelting iron titanium vanadium alloy, for the rate of recovery of titanium up to 95%, the recovery rate of vanadium is 97%.
Description
Technical field
The present invention relates to trade waste recovery technology field, more particularly to a kind of metallurgical titanium containing waste denitration catalyst
The preparation method of slag and ferrotitanium vanadium alloy.
Background technology
The main energy sources in China are coal, and coal-burning power plant is all one of main disposal of pollutants source all the time.Although cigarette
Dirt and sulfur dioxide have been effectively controlled；NOxIt is a large amount of discharge or photochemical fog and acid rain, therefore nitrogen oxidation can be brought
Object (NOx) have become China's coal-burning power plant's pollution problem of greatest concern now.《Fossil-fuel power plant atmospheric pollutant emission standard》
Regulation in (GB13223-2011)：From 1 day January in 2014, the thermal power plant built up before on December 31st, 2003, nitrogen oxidation
The discharge capacity of object should be less than 200mg/m3, and the thermal power plant NO of key areas that on January 1st, 2004 builds up later and certainx's
Discharge capacity should be less than 100mg/m3.In addition,《Thermal power plant's nitrogen oxides technological policy for treatment》In also clearly stipulate that when emission contains
When amount cannot meet the requirement of discharged nitrous oxides, denitrating flue gas facility should be added.
In a variety of NOxIn Treatment process, selective catalytic reduction (selective catalytic reduction, SCR)
Denitration technology, because with by flue gas composition limitation is small, denitration efficiency is high and selectivity is good, device is simple, reliability is high,
The advantages that no coupling product, temperature smoke denitrating field is widely applied in the coal fired power plant in worldwide.Nowadays,
Medium temperature denitrating catalyst is mainly V2O5-WO3(MoO3)/TiO2Type vanadium Titanium series catalyst；Mainly there is cellular, flat and ripple
3 kinds of structures of formula.
The service life of denitrating catalyst is generally 3~5 years, and having many factors in the actual use process causes to urge
Agent inactivates.The yield of waste denitration catalyst is up to 25 ten thousand steres/year, and quality is up to 13.76 ten thousand tons.
The main component of waste denitration catalyst is TiO2, wherein also containing a small amount of V2O5、SiO2Deng.Denitrating catalyst
In contain plurality of heavy metal, belong to the hazardous solid waste containing all kinds of hypertoxic elements.If arbitrarily banking up, on the one hand can occupy big
The land resource of amount causes huge pollution to environment；Even meeting polluted underground water, causes damages to global biology；On the other hand
The production cost that enterprise can be improved causes the huge waste of resource.How efficiently to dispose discarded SCR denitration is our faces
The huge resource faced, environment, economic problems.
The method of existing discarded SCR denitration resource utilization mainly has：Sodium roasting method and concentrated base lixiviation process
Recycle TiO2；The ammonium salt precipitation method, extraction, electrolysis recycle V2O5, the heavy tungsten method recycling WO of calcium chloride3.These methods are all without an example
A large amount of strong acid and strong base has been used in other places, and economic cost is high, and environmental pollution is serious.
Invention content
The preparation of the purpose of the present invention is to provide a kind of metallurgical titanium slag and ferrotitanium vanadium alloy containing waste denitration catalyst
Method.The preparation method of metallurgical titanium slag and ferrotitanium vanadium alloy provided by the invention containing waste denitration catalyst is without strong acid and by force
Alkali can realize the resource utilization of useful metal element in waste denitration catalyst.
The present invention provides a kind of metallurgical titanium slag containing waste denitration catalyst, includes the component of following mass content：It is useless
Abandon denitrating catalyst 20~52.9%, MgO 6.4~8%, Na2CO33.9~8%, CaF26.4~10% and calcium containing alloy 30
~50%.
Preferably, the metallurgical titanium slag containing waste denitration catalyst includes waste denitration catalyst 30~45%, MgO 7
~7.5%, Na2CO35~7%, CaF27~9% and calcium containing alloy 35~45%.
Preferably, the calcium containing alloy includes containing Ca deoxidizer or Calcium treatment agent.
Preferably, the mass content of calcium is not less than 20% in the calcium containing alloy.
Preferably, the granularity of the metallurgical titanium slag containing waste denitration catalyst is 50 mesh or more.
The present invention also provides a kind of preparation methods of ferrotitanium vanadium alloy, including：Containing described in above-mentioned technical proposal is given up
Abandon denitrating catalyst metallurgical titanium slag mixed with source of iron after melting, obtain ferrotitanium vanadium alloy.
Preferably, the mass ratio of the metallurgical titanium slag and source of iron containing waste denitration catalyst is (31.06~46.59):
100。
Preferably, the temperature of the melting is 1550~1650 DEG C.
Preferably, the source of iron is molten steel.
Preferably, described mix includes：Metallurgical titanium slag containing waste denitration catalyst is added in molten steel in batches.
The present invention provides a kind of metallurgical titanium slag containing waste denitration catalyst, includes the component of following mass content：It is useless
Abandon denitrating catalyst 20~52.9%, MgO 6.4~8%, Na2CO33.9~8%, CaF26.4~10% and calcium containing alloy 30
~50%.Metallurgical titanium slag provided by the invention containing waste denitration catalyst can be used as alloy source to be closed for melting ferrotitanium vanadium
Gold, wherein calcium containing alloy can restore the TiO in discarded SCR denitration as reducing agent2、V2O5Equal metal oxides,
So that the metallic elements mass transfer such as Ti, V enters alloying in molten steel or forms ferrotitanium vanadium alloy；MgO can reduce fusing point and viscosity,
Protect furnace lining；Na2CO3It is decomposed into Na under high temperature2O reduces fusing point and viscosity；CaF2Fusing point and viscosity can be reduced；Without strong
In the case of acid and highly basic, the abundant recycling of waste denitration catalyst is realized.The experimental results showed that provided by the invention containing useless
When abandoning the metallurgical titanium slag of denitrating catalyst and being used for smelting iron titanium vanadium alloy, the rate of recovery of titanium is up to 95%, the recovery rate of vanadium
97%.
Specific implementation mode
The present invention provides a kind of metallurgical titanium slag containing waste denitration catalyst, includes the component of following mass content：It is useless
Abandon denitrating catalyst 20~52.9%, MgO 6.4~8%, Na2CO33.9~8%, CaF26.4~10% and calcium containing alloy 30
~50%.
Based on mass content, the metallurgical titanium slag provided by the invention containing waste denitration catalyst includes waste denitration catalyst
20~52.9%, preferably 30~45%, most preferably 35~40%.In the present invention, the waste denitration catalyst at
Divide preferably as shown in table 1 (main component for measuring waste denitration catalyst through alkali soluble solution, upper ICP-IES).
The ingredient of 1 waste denitration catalyst of table
| Element species | CaO | MgO | SiO2 | Fe2O3 | Al2O3 | TiO2 | V2O5 |
| Mass fraction (wt%) | 1.0-2.5 | ＜ 0.02 | 3.0-8.0 | 0.5-2.0 | 0.5-1.5 | 70-85 | 1.5-2.5 |
In the present invention, in the waste denitration catalyst preferably further include WO3.In the present invention, when described discarded de-
Further include WO in denox catalyst3When, preferably further include W elements in the ferrotitanium vanadium alloy.In the present invention, the discarded denitration
Metal oxide in catalyst provides alloying element when for ferrotitanium vanadium alloy melting as alloy source, after carrying out reduction mass transfer
Into alloying in molten steel.
The present invention does not have special restriction to the waste denitration catalyst source, using known to those skilled in the art
Denitration process waste.In the present invention, the waste denitration catalyst is preferably being dusted processing using preceding.
The present invention operates not special restriction to the dust removal process, is by the way of blowing well known to those skilled in the art
It can.In the present invention, the dust removal process can blow away waste denitration catalyst surface dirt (main component SiO2), it avoids
SiO2The too high a large amount of consumption reducing agents of content, cinder viscosity increase, are unfavorable for restoring.
Based on mass content, the metallurgical titanium slag provided by the invention containing waste denitration catalyst includes MgO6.4~8%, excellent
It is selected as 7~7.5%.The present invention does not have the source of the MgO special restriction, using well known to those skilled in the art commercially available
Product.In the present invention, the MgO can reduce the fusing point and viscosity of melt in melting, protect furnace lining.
Based on mass content, the metallurgical titanium slag provided by the invention containing waste denitration catalyst includes Na2CO33.9~8%,
Preferably 5~7%.The present invention is to the Na2CO3Source there is no special restriction, using city well known to those skilled in the art
Sell product.In the present invention, the Na2CO3It is decomposed into Na at a high temperature of melting2O reduces the fusing point and viscosity of melt.
Based on mass content, the metallurgical titanium slag provided by the invention containing waste denitration catalyst includes CaF26.4~10%,
Preferably 7~9%.The present invention is to the CaF2Source there is no special restriction, using city well known to those skilled in the art
Sell product.In the present invention, the CaF2The fusing point and viscosity of melt can be reduced in melting.
Based on mass content, the metallurgical titanium slag provided by the invention containing waste denitration catalyst include calcium containing alloy 30~
50%, preferably 35~45%.In the present invention, the calcium containing alloy preferably includes to contain Ca deoxidizer or Calcium treatment agent, more excellent
Choosing includes one or more in Ca-Fe, Ca-Si and Si-Ca-Ba.In the present invention, the quality of calcium contains in the calcium containing alloy
Amount is preferably not less than 20%.In the present invention, the calcium containing alloy can be restored as reducing agent in discarded SCR denitration
TiO2、V2O5Equal metal oxides so that the metallic elements mass transfer such as Ti, V enters alloying in molten steel or forms the conjunction of ferrotitanium vanadium
Gold.
In the present invention, the granularity of the metallurgical titanium slag containing waste denitration catalyst is preferably 50 mesh or more, more preferably
More than 100 mesh.In the present invention, the granularity can be further ensured that each group in the metallurgical titanium slag of waste denitration catalyst
That divides is uniformly mixed, and makes it that can fully be reacted in fusion process.
The present invention restriction not special to the operation of the preparation of the metallurgical titanium slag containing waste denitration catalyst, uses
The preparation method of composition well known to those skilled in the art mixes each component.In the present invention, when each component
Granularity be 50 mesh below when, the present invention mixes after preferably respectively crushing each component.Behaviour of the present invention to the crushing
Make not special restriction, required granularity is crushed to using pulverizer well known to those skilled in the art.
The present invention also provides a kind of preparation methods of ferrotitanium vanadium alloy, including：Containing described in above-mentioned technical proposal is given up
Abandon denitrating catalyst metallurgical titanium slag mixed with source of iron after melting, obtain ferrotitanium vanadium alloy.
In the present invention, the mass ratio of the metallurgical titanium slag and source of iron containing waste denitration catalyst be preferably (31.06~
46.59):100, more preferably (35~40):100.In the present invention, the ratio can ensure the matter of titanium in ferrotitanium vanadium alloy
It is 3% or more to measure content.
In the present invention, the temperature of the melting is preferably 1550~1650 DEG C, more preferably 1580~1620 DEG C, optimal
It is selected as 1600 DEG C.The present invention does not have the time of the melting special restriction, is adjusted according to the amount of material.
In the present invention, the source of iron is preferably molten steel；The temperature of the molten steel is preferably 1550~1650 DEG C, more preferably
It is 1580~1620 DEG C, most preferably 1600 DEG C.In the present invention, when the source of iron is molten steel, the present invention is to the molten steel
Ingredient there is no special restriction, using molten steel well known to those skilled in the art.In the present invention, the mixing is preferred
Including：Metallurgical titanium slag containing waste denitration catalyst is added in molten steel in batches.In the present invention, described to be in batches added
Mode can reduce TiO in slag2Content avoids TiO in slag2Slag melting point and viscosity are higher caused by content height, are unfavorable for also
It is former.
In the present invention, the metallurgical titanium slag containing waste denitration catalyst is preferably added in molten steel in three times.In this hair
In bright, the time interval between every batch of is preferably 8~12min, more preferably 10min.In the present invention, the time interval
It can ensure the abundant reduction of metal oxide.
Present invention preferably employs iron sheets to wrap up the metallurgical titanium slag containing waste denitration catalyst, is then bundled in iron staff
Upper insertion iron liquid.In the present invention, the quality of the iron sheet is negligible.
The preparation method of metallurgical titanium slag and ferrotitanium vanadium alloy provided by the invention containing waste denitration catalyst recycles
The plurality of heavy metal contained in discarded SCR denitration and all kinds of hypertoxic elements (vanadium) etc., avoid such hazardous solid
Waste, which is arbitrarily banked up, occupies a large amount of land resource, while avoiding pollution on the environment, especially to the dirt of underground water
Dye；The metal of the high added values such as vanadium in catalyst and titanium is carried out resource utilization utilization by the present invention；Avoid the huge of resource
Waste；Additional economic interests are brought to enterprise；TiO is recycled compared to sodium roasting method, concentrated base lixiviation process2, extraction, ammonium salt are heavy
Shallow lake method, electrolysis recycling vanadium and its oxide；The methods of heavy tungsten method recycling tungsten of calcium chloride, the invention avoids a large amount of strong acid and strong bases
Use, it is more friendly to environment；Method provided by the invention can operate under neutral atmosphere, need not blow protection gas,
Production cost is relatively low.
In order to further illustrate the present invention, with reference to embodiment to the smelting provided by the invention containing waste denitration catalyst
The preparation method of golden titanium slag and ferrotitanium vanadium alloy is described in detail, but they cannot be interpreted as to the scope of the present invention
Restriction.
Embodiment 1
Metallurgical titanium slag composition：Waste denitration catalyst 50%, MgO 6.4%, Na2CO3(provide Na2O) 3.9%, CaF2
6.4%, calcium containing alloy 33.3%.
The preparation method of metallurgical titanium slag is：
Waste denitration catalyst surface dirt is blown away with Wind Volume hair-dryer；
Discarded SCR denitration and calcium containing alloy are broken into the powder of 50 mesh or more respectively；
Each component is mixed into 1h in high speed mixer, obtains metallurgical titanium slag.
The preparation method of ferrotitanium vanadium alloy is：
The ratio that metallurgical titanium slag 42g is prepared according to every 100g molten steel is wrapped up the metallurgical titanium slag of mixing point for 3 batches with sheet iron
Tightly in case feeding intake；
When mild steel is heated to 1600 DEG C, the metallurgical titanium slag that iron sheet wraps up is bundled on thin iron staff point 3 batches of insertion molten steel
In；It is 10 minutes that every batch of metallurgy titanium slag, which is inserted into time interval,；
It waits for that the metallurgical titanium slag of third batch is added to smelt after ten minutes to finish, molten steel is poured out is to get the mass fraction to titanium
8.21% ferrotitanium vanadium alloy.
The recovery rate of titanium is about 95%, and the recovery rate of vanadium is 97%.
Embodiment 2
Metallurgical titanium slag composition：Waste denitration catalyst 20%, MgO 6.4%, Na2CO3(provide Na2O) 3.9%, CaF2
6.4%, calcium containing alloy 62.9%.
The preparation method of metallurgical titanium slag is：
Waste denitration catalyst surface dirt is blown away with Wind Volume hair-dryer；
Discarded SCR denitration and calcium containing alloy are broken into the powder of 50 mesh or more respectively；
Each component is mixed into 2h in high speed mixer, obtains metallurgical titanium slag.
The preparation method of ferrotitanium vanadium alloy is：
The metallurgical titanium slag of mixing is divided 3 batches by the ratio that metallurgical titanium slag 46.59g is prepared according to every 100g molten steel with sheet iron
Package is tight in case feeding intake；
When molten steel is heated to 1600 DEG C, the metallurgical titanium slag that iron sheet wraps up is bundled on thin iron staff in point 3 batches of insertion molten steel；
It is 10 minutes that every batch of metallurgy titanium slag, which is inserted into time interval,；
It waits for that the metallurgical titanium slag of third batch is added to smelt after ten minutes to finish, molten steel is poured out is to get the mass fraction to titanium
4.02% ferrotitanium vanadium alloy.
The recovery rate of titanium is about 95%, and the recovery rate of vanadium is 97%.
As can be seen from the above embodiments, metallurgical titanium slag and ferrotitanium vanadium provided by the invention containing waste denitration catalyst close
The preparation method of gold can realize the resource utilization of useful metal element in waste denitration catalyst without strong acid and highly basic.
The above is only a preferred embodiment of the present invention, it is not intended to limit the present invention in any form.It should
It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of metallurgical titanium slag containing waste denitration catalyst, includes the component of following mass content：Waste denitration catalyst 20
~52.9%, MgO 6.4~8%, Na2CO33.9~8%, CaF26.4~10% and calcium containing alloy 30~50%.
2. the metallurgical titanium slag according to claim 1 containing waste denitration catalyst, which is characterized in that urged including discarded denitration
Agent 30~45%, MgO 7~7.5%, Na2CO35~7%, CaF27~9% and calcium containing alloy 35~45%.
3. the metallurgical titanium slag according to claim 1 or 2 containing waste denitration catalyst, which is characterized in that the calcic closes
Gold includes containing Ca deoxidizer or Calcium treatment agent.
4. the metallurgical titanium slag according to claim 3 containing waste denitration catalyst, which is characterized in that in the calcium containing alloy
The mass content of calcium is not less than 20%.
5. the metallurgical titanium slag according to claim 1 containing waste denitration catalyst, which is characterized in that described containing discarded denitration
The granularity of the metallurgical titanium slag of catalyst is 50 mesh or more.
6. a kind of preparation method of ferrotitanium vanadium alloy, including：It will be urged containing discarded denitration described in Claims 1 to 5 any one
Melting after the metallurgical titanium slag of agent is mixed with source of iron, obtains ferrotitanium vanadium alloy.
7. preparation method according to claim 6, which is characterized in that the metallurgical titanium slag containing waste denitration catalyst with
The mass ratio of source of iron is (31.06~46.59):100.
8. the preparation method described according to claim 6 or 7, which is characterized in that the temperature of the melting is 1550~1650 DEG C.
9. preparation method according to claim 6, which is characterized in that the source of iron is molten steel.
10. preparation method according to claim 9, which is characterized in that the mixing includes：Waste denitration catalyst will be contained
Metallurgical titanium slag be added in molten steel in batches.
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2018
- 2018-05-18 CN CN201810481162.XA patent/CN108677016B/en not_active Expired - Fee Related
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