CN106622284A - Recovery and utilization technology of waste titanium-vanadium based SCR catalyst capable of being applied to reproduction - Google Patents
Recovery and utilization technology of waste titanium-vanadium based SCR catalyst capable of being applied to reproduction Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
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Abstract
The invention belongs to the technical field of catalyst recovery and regeneration, and specifically discloses a recovery and utilization technology of a waste titanium-vanadium based SCR catalyst capable of being applied to reproduction. The technology comprises the following steps: (1) carrying out a dedusting treatment; (2) carrying out a washing treatment; (3) carrying out a ball milling and filter pressing treatment; (4) carrying out acid washing; (5) carrying out judgment: judging the specific surface area, pore volume, and water retaining performance of obtained V2O5/WO3(MoO3)-TiO2-SiO2 mud, wherein qualified mud can be directly used as the raw material and can be applied to SCR catalyst production through a partial addition mode; (6) carrying out calcination and grinding: adding meta-titanic acid and tungsten salts/molybdenum salts into disqualified mud, calcining the mud at a high temperature, and grinding the mud to obtain WO3(MoO3)-TiO2-SiO2 composite oxide powder with a particle size less than 10 [mu]m. The crystal form of the composite oxide powder is anatase structure. The particle size is uniform. The specific surface area is preferably (80 to 150 m<2>/g). The recovered catalyst can be applied to SCR catalyst production. The technology has the characteristics of controllable components of product, simple operation flow, low cost, good stability, and easiness for massive industrial production.
Description
Technical field
The invention belongs to catalyst reclaiming technical field, more particularly to a kind of discarded vanadium titanium-based that can be used for reproduction
SCR catalyst recycles technique.
Background technology
Nitrogen oxides (NOx) it is one of main component of atmosphere pollution, 70% comes from China's nitrogen oxide emission
The direct burning of coal, and coal-fired station is then NOxPrimary discharge source one of.On July 29th, 2011, Chinese Ministry of Environmental Protection
It is formal to issue《Fossil-fuel power plant atmospheric pollutant emission standard》(GB13223-2011), it is current thermal power plant most stringent of in the world
NOxDischarge standard.Standard clear stipulaties key area new construction of coal-fired boiler nitrogen oxides is (with NO2Meter) emission limit be 100mg/
m3, 50% is directly reduced on the basis of original limit value, the standard is formal in 1 day January in 2012 to be implemented.2014 again
Regulation implements discharged nitrous oxides and is less than 50mg/m in East Coastal provinces and cities3Minimum discharge regulation.
Current coal-burning power plant and other coal-fired, selective catalytic reduction methods of main flow denitration technology of gas industry boiler
And two kinds of noncatalytic reduction (SNCR) (SCR).SNCR techniques are without the need for catalyst, but denitration rate is not high, generally 30%～
40%；SCR techniques need catalyst, and it has denitration rate high (maximum can be more than 90%), selective good, mature and reliable etc. excellent
Point, is widely used at present thermal power station, becomes the main flow of coal unit denitration.
Core in SCR techniques is catalyst, and its cost generally accounts for the 30%～50% of denitrification apparatus gross investment；Should
Catalyst is with TiO2For carrier, main component is V2O5-WO3(MoO3) etc. metal oxide, these compositions account for catalyst total amount
More than 90%, remaining microcomponent is added according to the concrete coal that boiler is used.Ideally, denitrating catalyst can be with one
Directly use and do not produce any change, but in actual moving process, due to sulphur ammonium deposition, catalyst pores blocking, alkali metal
With heavy metal element poisoning and the presence of the situation such as catalyst abrasion, the activity and service life of catalyst can be reduced.
For the catalyst after inactivation, ordinary priority recovers the activity of catalyst by the way of catalyst regeneration.But and
Not all catalyst can be reproduced, if its activity can not be recovered by regeneration, that can only give up dead catalyst
Abandon process.
Chinese annual dead catalyst yield is nearly 100,000 tons, if only using the general processing mode of solid waste, shown
It is not so the optimum way for processing dead catalyst；In August in 2014 5 days, the Environmental Protection Department that national environmental protection portion delivers was done
Waste flue gas denitration catalyst (vanadium titanium system) is clearly included Hazardous Wastes Management by public Room letter " ring does letter [2014] 990 ", will
It is named as " waste flue gas denitration catalyst (vanadium titanium system) that industrial smoke the selective catalytic denitrification process process is produced ".It is well known that
Vanadium, tungsten and molybdenum are all rare resources, if the metal oxides such as the titanium in SCR dead catalyst, vanadium, tungsten, molybdenum can be recycled,
The output value of more than one hundred million units can be not only produced, can also make the catalyst in whole denitrating flue gas industry realize recycling.Therefore, open
Sending out SCR catalyst reclaiming comprehensive utilization process discarded can create huge ecological and economic benefit.
External relatively early attention spent catalyst recovery and utilizing.American-European-Japanese environmental law regulation dead catalyst is at will toppled over, is buried
Pay huge tax.The industry that the noble metals such as Pt, Pd, Rh are recycled from industrial waste catalyst is formed at present.Due to
Developed country's coal-burning boiler is less, therefore its SCR consumption is less, and catalyst operating condition is also superior to the country, can repeatedly regenerate, because
This annual SCR catalyst discarded on a small quantity for producing all is processed by burial.The research and application of discarded SCR catalyst recovery technology
China is concentrated mainly on, current recovery technology grows up on the basis of titanium white and metallurgical technology is absorbed.
At present SCR catalyst is reclaimed can be divided into three major types, and (1) directly addition uses technology；(2) two smelting processes, again can be by
It is divided into high-temperature melting method and alkali fusion；(3) liquid phase absorption method, can be divided into alkali solution technique and acid hydrolyzation again.To the excellent of three kinds of technique
Weaknesses analysis are as follows：
(1) raw catelyst preparation flow is just back to use after simple cleaning and crushing, first poisoning element and dust do not have
Thoroughly removed, it is impossible to which guarantee produces the performance of catalyst, particularly chemistry and mechanical life.Secondly as it compares table
Area, pore volume and water-retaining property lower limit reuse addition.Reuse amount is limited, it is impossible to realize the recovery to whole dead catalyst
Process.
(2) discarded SCR catalyst can be added in the smelting furnace of production titanium steel, is used as titanium source.But due in titanium steel
Titanium consumption is less cannot to consume discarded SCR catalysts in a large number, and the valuable element such as vanadium, molybdenum, tungsten also can be because obtaining effective profit
With and waste.And alkali fusion studies at present more, but cannot still carry out large-scale industrialized production at present.This is primarily due to
The alkali fusion reaction of SCR catalyst could occur in 800 DEG C of temperatures above, and energy consumption is higher.And have a large amount of sodium ions in alkali fusion product
Exist, it is necessary to cleaned with a large amount of water and just can guarantee that prepared titanium dioxide and meet denitration demand, 2 points of the above causes the recovery of alkali fusion
Cost is very high.
(3) alkali fusion is vanadium, tungsten, the molybdenum using high-concentration sodium hydroxide solution in 60-80 DEG C of interval makes SCR catalyst
It is changed into corresponding solubility acid sodium salt Deng valuable element oxide, and titanium dioxide keeps constant.Then by solid-liquid point
From obtaining valuable element sodium salt solution and containing the higher titanium dioxide of the magazines such as sodium.The former can obtain valuable element salt and contain by evaporation
Crude product of the amount between 30-40%, with relatively low price sales.With less than 1000 yuan/ton after the latter's drying and calcining
Price sales.Technology industrialization at present, but due to only through roughing, making, valuable element devalues and the rate of recovery is relatively low.
Acid hydrolyzation is to discard SCR catalyst using concentrated sulfuric acid dissolution, and the acidolysis reaction of discarded vanadium titanium catalyst is difficult below 300 DEG C
Carry out completely, in general the valuable element rate of recovery is very low, temperature then starts to decompose more than 300 DEG C of sulfuric acid.
Because vanadium, tungsten and molybdenum compound content are very low in discarded SCR catalyst, to extract vanadium, tungsten and molybdenum technical difficulty
All it is important bottleneck with cost recovery.Therefore, exploitation takes into account technical and economy recovery technology and could really solve to give up
Abandon SCR catalyst and reclaim problem.
The content of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of can be used for the discarded of reproduction
Vanadium titanium-based SCR catalyst recycles technique, is capable of achieving low cost, low stain, high efficiente callback using in discarded SCR catalyst
Resource metal oxide.
To achieve these goals, the technical solution used in the present invention is：
A kind of discarded SCR catalyst regeneration reclaims comprehensive utilization process, and the technique comprises the steps：
(1) dust removal process：Take discarded SCR denitration to be crushed, granularity 2-5cm is crushed to, then using whirlwind
Separator is separated dust with waste catalyst.
(2) cleaning treatment：Discarded SCR catalyst after by separation utilizes the liquid phase of ultrasonic wave and Bubbling method at 30-80 DEG C
In carry out cleaning remove poisoning material (potassium (K), iron (Fe), magnesium (Mg), sodium (Na), phosphorus (P), arsenic (As), chromium (Cr), mercury (Hg)
Deng) and residual dust.
(3) ball milling, press filtration is processed：The catalyst after cleaning is milled to into less than 20 μm using ball mill, filter press is recycled
Obtain catalyst pug of the water content between 30%-40%.
(4) pickling：Using suitable inorganic acid or organic acid cleaning catalyst pug, remove residual alkalescence poisoning element and
Part barium oxide.
(5) judge：To V2O5/WO3(MoO3)-TiO2-SiO2The specific surface area of pug, pore volume and water retention property are sentenced
It is fixed.Meeting desired pug can be used as one of raw material, and by part addition manner, (adding proportion should be less than raw material gross mass
20%) SCR catalyst production is directly used in, and pug not up to standard then must be by addition metatitanic acid and tungsten salt (or molybdenum salt)
SCR catalyst production can be re-used for.
(6) calcining, crushing：(5) judge catalyst pug not up to standard, supplement addition metatitanic acid and tungsten salt (or molybdenum salt),
Through high-temperature calcination and crushing, granularity is obtained<10 μm of WO3(MoO3)-TiO2-SiO2(containing a small amount of V2O5) composite oxide powder
Body.The crystal formation of gained composite oxide powder is anatase structured, even particle size, and specific surface area is suitable, can be used for SCR and urges
Agent is produced.
The present invention efficiently separates discarded SCR catalyst and dust using cyclone separator, then by cleaning, ball milling, press filtration,
The operations such as pickling thoroughly remove poisoning element and residual dust, obtain the WO of cleaning3(MoO3)-TiO2-SiO2(containing a small amount of
V2O5) pug, directly as raw material or metatitanic acid and tungsten salt (or molybdenum salt) can be supplemented afterwards for the production of new SCR catalyst.This
The technique of invention has easy simple to operate, equipment requirement, low cost, pollutes low advantage.
Compared with prior art, can be expired completely using the SCR catalyst items physics and chemical index of this technique productions
Sufficient GB or technical protocol are required, and in normal conditions service life is more than 24000 hours.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Fig. 2 is the WO after reclaiming3-TiO2-SiO2(containing a small amount of V2O5) composite oxides XRD spectrum.
Specific embodiment
Come by the following examples to be further described the present invention (agents useful for same is pure for chemistry in embodiment), need
It should be noted that the following examples are used only as illustrating, present invention is not limited thereto.
Embodiment 1：V2O5/WO3-TiO2-SiO2It is prepared by pug.
As shown in figure 1, comprising the steps：
Step 1：Take the discarded V of 500g2O5/WO3-TiO2-SiO2Base SCR denitration coarse-cracking machine is crushed, and is crushed to
Granularity 2-5cm, is then separated dust with waste catalyst using multi-cyclone.
Step 2：Waste catalyst will be obtained after separation using cleaning 0.5h-1h in 50 DEG C of liquid phases of ultrasonic wave and Bubbling method,
And then removing poisoning material and residual dust.
Step 3：The catalyst after cleaning is milled to into less than 20 μm using ball mill, is recycled filter press to obtain water content and is existed
Catalyst pug between 30%-40%.
Step 4：Using dilution heat of sulfuric acid cleaning catalyst pug, residual alkalescence poisoning element and the oxidation of part vanadium are removed
Thing.
Step 5：Press filtration process is carried out to step 4 gained catalyst pug, and tests specific surface area, the pore volume of gained pug
With water retention property (as shown in table 1).
Table 1V2O5/WO3-TiO2-SiO2The structural property of pug
| Project | Specific surface area m2/g | Pore volume ml/g | Water-retaining property % |
| Index | 53 | 0.28 | 35 |
Embodiment 2：Desired V is met using the gained of embodiment 12O5/WO3-TiO2-SiO2Pug passes through part addition manner
(adding proportion is 15%) produces SCR catalyst.
Step 1：By the gained V of embodiment 12O5/WO3-TiO2-SiO2Pug presses 15 with new denitration titanium tungsten powder:85 mass ratio
Mixing, through mixing, pre-extruded, shaping extrusion, primary drying, redrying, calcination process processing honeycomb SCR catalysis is obtained
Agent.
Step 2：Require to carry out performance detection to the honeycomb SCR catalyst of step 1 production according to GB/T 31587-2015
(testing result is as shown in table 2).
The honeycomb SCR catalyst service check result of table 2
Embodiment 3：WO3-TiO2-SiO2(containing a small amount of V2O5) composite oxides preparation.
Step 1：Take the discarded V of 500g2O5/WO3-TiO2-SiO2Base SCR denitration coarse-cracking machine is crushed, and is crushed to
Granularity 2-5cm, is then separated dust with discarded SCR denitration using multi-cyclone.
Step 2：Discarded SCR catalyst will be obtained after separation using cleaning 0.5h- in 50 DEG C of liquid phases of ultrasonic wave and Bubbling method
1h, and then remove poisoning material and residual dust.
Step 3：The SCR catalyst after cleaning is milled to into less than 20 μm using ball mill, recycles filter press to obtain aqueous
SCR catalyst pug of the amount between 30%-40%.
Step 4：SCR catalyst pug is cleaned using dilution heat of sulfuric acid, residual alkalescence poisoning element and part vanadium oxygen is removed
Compound.
Step 5：The pug for adding appropriate metatitanic acid and ammonium paratungstate is put in rotary kiln and is calcined.Calcining heat is
600 DEG C, programming rate is 10 DEG C/min, and calcination time is 5 hours.
Step 6：The material that calcining is obtained is put in ball mill carries out ball milling, obtains the anatase titanium dioxide that granularity is 5-10 μm
(XRD is as shown in Figure 2) WO3-TiO2-SiO2(containing a small amount of V2O5) composite oxides.
Embodiment 4：The WO that embodiment 3 is obtained3-TiO2-SiO2(containing a small amount of V2O5) composite oxides carry out honeycomb SCR
Catalyst Production and performance detection.
Step 1：By WO3-TiO2-SiO2(containing a small amount of V2O5) composite oxides through mixing, pre-extruded, shaping extrude,
Primary drying, redrying, calcination process processing obtain honeycomb SCR catalyst.
Step 2：Require to carry out performance detection to the honeycomb SCR catalyst of step 1 production according to GB/T 31587-2015
(testing result is as shown in table 1).
The honeycomb SCR catalyst service check result of table 3
Embodiment 5：MoO3-TiO2-SiO2(containing a small amount of V2O5) composite oxides preparation.
Step 1：Take the discarded V of 500g2O5/MoO3-TiO2-SiO2Base SCR denitration coarse-cracking machine is crushed, and is crushed to
Granularity 2-5cm, is then separated dust with discarded SCR denitration using multi-cyclone.
Step 2：Discarded SCR catalyst will be obtained after separation using cleaning 0.5h- in 50 DEG C of liquid phases of ultrasonic wave and Bubbling method
1h, and then remove poisoning material and residual dust.
Step 3：The SCR catalyst after cleaning is milled to into less than 20 μm using ball mill, recycles filter press to obtain aqueous
SCR catalyst pug of the amount between 30%-40%.
Step 4：SCR catalyst pug is cleaned using dilution heat of sulfuric acid, residual alkalescence poisoning element and part vanadium oxygen is removed
Compound.
Step 5：The pug for adding appropriate metatitanic acid and ammonium paramolybdate is put in rotary kiln and is calcined.Calcining heat is
600 DEG C, programming rate is 10 DEG C/min, and calcination time is 5 hours.
Step 6：The material that calcining is obtained is put in ball mill carries out ball milling, obtains the anatase titanium dioxide that granularity is 5-10 μm
(XRD is as shown in Figure 2) MoO3-TiO2-SiO2(containing a small amount of V2O5) composite oxides.
Claims (6)
1. a kind of discarded vanadium titanium-based SCR catalyst that can be used for reproduction recycles technique, it is characterised in that including following step
Suddenly：
(1) dust removal process：Taking discarded vanadium titanium-based SCR denitration carries out crushing dedusting；
(2) cleaning treatment：Waste catalyst after dedusting is carried out clearly using ultrasonic wave and Bubbling method in 30-80 DEG C of liquid phase
Wash, remove poisoning material and residual dust；
(3) ball milling, press filtration is processed：The catalyst after cleaning is milled to into less than 20 μm using ball mill, recycles filter press to obtain
Catalyst pug of the water content between 30%-40%；
(4) pickling：Using inorganic acid or organic acid cleaning catalyst pug, residual alkalescence poisoning element and the oxidation of part vanadium are removed
Thing；
(5) judge：To V2O5/WO3(MoO3)-TiO2-SiO2The specific surface area of pug, pore volume and water retention property are judged, full
The pug that foot is required can be produced by part addition manner directly as one of raw material for SCR catalyst, and mud not up to standard
Material then just must can be re-used for SCR catalyst production by addition metatitanic acid and tungsten salt；
(6) calcining, crushing：For pug not up to standard is judged, after supplementing addition metatitanic acid and tungsten salt or molybdenum salt, through high temperature
Calcining and crushing, obtain granularity<10 μm containing a small amount of V2O5Can be used for SCR catalyst production WO3(MoO3)-TiO2-
SiO2Composite oxide powder.
2. the discarded vanadium titanium-based SCR catalyst that can be used for reproduction according to claim 1 recycles technique, and its feature exists
In, the discarded vanadium titanium-based SCR catalyst in step (1) dust removal process be extruded type integral honeycomb catalyst, key component
For V2O5/WO3(MoO3)-TiO2-SiO2, fail because of dust blocking and/or chemical poisoning Jing after operation.
3. the discarded vanadium titanium-based SCR catalyst that can be used for reproduction according to claim 1 recycles technique, and its feature exists
In, in the step (1), granularity 2-5cm is crushed to, then dust and waste catalyst are carried out point using cyclone separator
From.
4. the discarded vanadium titanium-based SCR catalyst that can be used for reproduction according to claim 1 recycles technique, and its feature exists
In in the step (5), it is desirable to V2O5/WO3(MoO3)-TiO2-SiO2The specific surface area of pug is more than 50m2/ g, pore volume are more than
0.25ml/g, water-retaining property could meet SCR catalyst production requirement more than 30%.
5. the discarded vanadium titanium-based SCR catalyst that can be used for reproduction according to claim 1 recycles technique, and its feature exists
In in the step (5), part addition manner refers to that adding proportion should be less than the 20% of raw material gross mass.
6. the discarded vanadium titanium-based SCR catalyst that can be used for reproduction according to claim 1 recycles technique, and its feature exists
In in the step (6), between 400-500 DEG C, the metatitanic acid specific surface area of addition should be greater than 200m to calcining heat2/ g, adds
Plus tungsten salt be ammonium paratungstate or ammonium metatungstate, molybdenum salt is ammonium paramolybdate, the WO of production3(MoO3)-TiO2-SiO2Combined oxidation
Thing specific surface area is in 80-150m2It is controllable between/g.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108031466A (en) * | 2017-11-14 | 2018-05-15 | 浙江浙能催化剂技术有限公司 | Have the low SO of anti-arsenic poisoning and wide active temperature windows concurrently2Oxygenation efficiency SCR denitration and preparation method thereof |
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| CN108525709B (en) * | 2018-03-30 | 2021-05-18 | 国家电投集团远达环保催化剂有限公司 | Method for recycling waste SCR denitration catalyst and regenerated SCR denitration catalyst carrier powder |
| CN112569926A (en) * | 2019-09-30 | 2021-03-30 | 国家能源投资集团有限责任公司 | Denitration catalyst and method for preparing denitration catalyst from waste denitration catalyst |
| CN112919530A (en) * | 2019-12-06 | 2021-06-08 | 国家能源投资集团有限责任公司 | Mesoporous titanium dioxide material and preparation method thereof, catalyst and preparation method thereof, and flue gas denitration method |
| CN112919530B (en) * | 2019-12-06 | 2022-10-11 | 国家能源投资集团有限责任公司 | Mesoporous titanium dioxide material and preparation method thereof, catalyst and preparation method thereof, and flue gas denitration method |
| CN111701585A (en) * | 2020-06-12 | 2020-09-25 | 重庆大学 | Resource utilization process of waste denitration catalyst |
| CN112371109A (en) * | 2020-11-26 | 2021-02-19 | 西安建筑科技大学 | Preparation method of aged vanadium-based catalyst and rare earth regenerated denitration catalyst |
| CN114534713A (en) * | 2021-04-19 | 2022-05-27 | 中冶长天国际工程有限责任公司 | Method for preparing activated carbon by adding vanadium-containing ore |
| CN114534713B (en) * | 2021-04-19 | 2024-02-13 | 中冶长天国际工程有限责任公司 | Method for preparing activated carbon by adding vanadium-containing ore |
| CN116371469A (en) * | 2023-04-06 | 2023-07-04 | 天津中材工程研究中心有限公司 | Hollow sphere SCR catalyst and application method thereof in cement kiln |
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