CN110102284A - It is a kind of fail SCR catalyst regeneration and demercuration method of modifying - Google Patents
It is a kind of fail SCR catalyst regeneration and demercuration method of modifying Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/90—Regeneration or reactivation
- B01J23/92—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The present invention provides a kind of regeneration of SCR catalyst that fails and demercuration method of modifying, belong to field of denitration catalyst.This method supports Ce as modified active substance in catalyst surface by infusion process, supplements V and compensates as active material, supplements Mo or W as catalyst aid.The V active site of this method supplement inactivation, and the denitration ability added the modified collaboration demercuration ability for improving catalyst surface V active site of Ce and restore catalyst.The present invention supports Ce and V, Mo or substep by substep and supports Ce and V, W, prevent mixed regeneration liquid bring cerium vanadate sedimentation problem, optimize process flow, it is therefore prevented that catalyst activity component improves active component and support efficiency the problem of catalyst surface is reunited.It is applicable to control NO by SCR catalystxAnd the failure SCR catalyst of Hg emissions field.
Description
Technical field
The invention belongs to field of denitration catalyst, in particular to the regeneration of a kind of SCR catalyst that fails and demercuration modification side
Method.
Background technique
Coal-burning power plant is one of main anthropogenic discharge source of China's mercury contaminants.As pollutant, the discharge of mercury vapour can
The damage that can lead to nerve system of human body, respiratory system etc. seriously endangers the life and health safety of the people.2016, I
State ratifies " the Minamata pact about mercury ", and will come into effect in the year two thousand twenty.China's " thermal power plant's Air Pollutant Emission in 2011
Standard " (GB13223-2011) publication, it is required mercury as new control, specifies power plant's mercury emissions and be limited to 30 μ g/m3.With
The discharge standard of the proposition of minimum discharge concept, mercury will certainly be increasingly stringent.
Selective catalytic reduction (SCR) is most widely used in current power plant, China, the highest denitration skill of denitration efficiency
Art.Meanwhile in the technique of collaboration demercuration, SCR catalyst equally plays crucial effect.SCR catalyst can pass through by
The a large amount of difficult element mercury (Hg for adsorbing, being insoluble in water in flue gas0) it is oxidized to bivalent mercury (Hg2+), improve electric precipitation (ESP) removing
Particle mercury (the Hg adsorbed in flying dustP) and wet desulphurization (wFGD) remove the Hg that is oxidized2+Efficiency, to improve flue gas
The removal efficiency of middle mercury contaminants.The SCR catalyst often applied in industry at present is with V2O5For main active component, with WO3Or MoO3
For auxiliary agent, although such catalyst has high denitration efficiency, its oxygenation efficiency for being catalyzed mercury oxidation reaction is generally only
40%-60% (under coal-fired plant flue gas operating condition), it is difficult to meet stringent mercury emissions standard requirements.
The SCR catalyst that fails is a kind of danger wastes, is incorporated into " National Hazard waste register ".Its main active substances
V2O5Toxicity with higher.The SCR catalyst that fails is at high cost as offal treatment, difficulty is big, how to be processed into for flue gas
One emerging problem in denitration field.By clean, regenerate and etc. by dead catalyst regeneration again investment application be in solution
State an effective means of problem.Catalyst activity substance would generally be supplemented in traditional regeneration technology again, in this process
Catalyst is implemented to be modified, to improve its mercury oxidation efficiency, adapts it to the strict demand of pollutant emission standard, is a kind of
Efficiently, inexpensive method.
Studies have shown that the element modified SCR catalyst of Ce has, raising catalyst mercury oxidation is active, it is anti-to widen mercury catalysis oxidation
The effect for answering temperature window prepares regenerating and modifying catalyst as modified active substance using Ce element and is able to achieve raising catalyst mercury oxygen
Change active target.The patent of invention of publication number CN104888806A provides a kind of using Ce element as the needle of modified active component
To the regeneration method of failure SCR catalyst.The patent of invention of publication number CN104815674A provides a kind of inactivation vanadium titanium-based bee
Nest shape denitrating catalyst combined denitration demercuration modification regeneration liquid and preparation method thereof contains Ce, Cu, W, V, to cleaning in regenerated liquid
Failure SCR catalyst afterwards supplements active component.
But pass through the study found that the ammonium metavanadate or ammonium metatungstate that use in regenerated liquid are mixed with cerous nitrate quickly to occur
Reaction generates white granular insoluble solid, precipitating is generated after standing, and regeneration liquid status is as shown in Figure 1.What is generated is precipitated as vanadium
Sour cerium, cerous tungstate precipitating, reaction principle are as follows:
Currently, being optimized without patent of invention to this phenomenon occurred during regenerating and modifying.This reaction
Dipping effect is seriously affected, and influences the uniformity of catalyst surface active substance distribution.
Summary of the invention
Precipitating occurs for the present invention now for mixed regeneration liquid present in failure vanadium titanium-based SCR catalyst regeneration modifying process
As the problem of, provide it is a kind of fail SCR catalyst regeneration and demercuration method of modifying.Compared to other regeneration or modification side
Method, this method can satisfy while realizing the regeneration of failure SCR catalyst denitration activity and the promotion of mercury catalytic oxidation performance,
And phenomena such as active component occurred because precipitating occurs for regenerated liquid is reunited is avoided, active component disperse is uniform, to mention
The high catalytic performance of catalyst.
To achieve the goals above, the present invention adopts the following technical scheme:
Simultaneously demercuration method of modifying, the failure SCR catalyst are living for a kind of regeneration of SCR catalyst that fails proposed by the present invention
Property group is divided into V2O5, auxiliary agent MoO3；It is characterized in that, simultaneously demercuration method of modifying comprises the steps of: for the regeneration
(1) SCR catalyst of failure is pre-processed with dedusting detoxification；
(2) it will sufficiently be soaked in the cerous nitrate solution that concentration is 0.08-1.00%wt by the catalyst of step (1) processing
Stain (such as 3-5h)；
(3) it will be dried at 100-120 DEG C by the catalyst of step (2) processing；
(4) 2-4h will be calcined at 450-500 DEG C by the catalyst of step (3) processing, and be cooled to room temperature；
(5) by the catalyst by step (4) processing in 0.45-0.60%wt ammonium metavanadate and 0.60-0.80%wt molybdenum
(such as 3-5h) is sufficiently impregnated in sour ammonium mixed solution；
(6) it will be dried at 100-120 DEG C by the catalyst of step (5) processing；
(7) 2-4h will be calcined at 400-450 DEG C by the catalyst of step (6) processing, and be cooled to room temperature.
The regeneration of another failure SCR catalyst proposed by the present invention and demercuration method of modifying, the failure SCR catalyst
Active component is V2O5, auxiliary agent WO3；It is characterized in that, simultaneously demercuration method of modifying comprises the steps of: for the regeneration
(1) SCR catalyst of failure is pre-processed with dedusting detoxification；
(2) it will sufficiently be soaked in the cerous nitrate solution that concentration is 0.08-1.00%wt by the catalyst of step (1) processing
Stain (such as 3-5h)；
(3) it will be dried at 100-120 DEG C by the catalyst of step (2) processing；
(4) 2-4h will be calcined at 450-500 DEG C by the catalyst of step (3) processing, and be cooled to room temperature；
(5) by the catalyst by step (4) processing in 0.45-0.60%wt ammonium metavanadate and the inclined tungsten of 2.5-4.0%wt
(such as 3-5h) is sufficiently impregnated in sour ammonium mixed solution；
(6) it will be dried at 100-120 DEG C by the catalyst of step (5) processing；
(7) 2-4h will be calcined at 400-450 DEG C by the catalyst of step (6) processing, and be cooled to room temperature.
The principle of the present invention are as follows: dust, the particulate matter on failure SCR catalyst surface are removed by purging；Pass through pickling, alkali
It washes, wash the alkalinity for removing catalyst surface, acid impurities, restore catalyst activity.Catalyst is improved to mercury oxygen by carrying Ce
The catalytic activity for changing reaction, widens catalytic temperature window.By carrying V and Mo or carrying V and W regeneration, catalyst denitration is supplemented
The active site of reaction, mercury oxidation reaction, restores the denitration activity of catalyst.The preferential principle for carrying Ce is presoma metavanadic acid
Ammonium, ammonium metatungstate is mixed with cerous nitrate to react, and forms cerium vanadate, cerous tungstate precipitating, and mixed regeneration liquid will seriously affect
The catalytic activity of regenerated catalyst, therefore be not suitable for supporting simultaneously, Ce is preferentially carried, rear bearing V and Mo or V and W are conducive to V activity
The abundant exposure in site, and then obtain higher catalytic activity.
The features of the present invention and the utility model has the advantages that
The present invention devises step by step for the first time while realizing what failure SCR catalyst regeneration and demercuration hydrodynamics were modified
Method.The recycling of failure SCR catalyst is realized, while ensure that regenerated catalyst restores denitration activity and improves catalysis mercury
Oxidation activity.The precipitating in regenerated liquid is prevented in this method, optimizes the distribution of regenerated catalyst surface active composition.
It realizes the recycling of danger wastes and meets the demand that mercury contaminants removal efficiency improves in coal-burning power plant.This method
Complex process degree is although improved using step impregnation, but ensure that the maximum extent regenerated catalyst denitration activity and
Mercury catalytic oxidation activity.The present invention is especially suitable for need to control NO by SCR catalystxAnd the failure SCR of Hg emissions field
Catalyst.
Detailed description of the invention
Fig. 1 is existing regeneration and the modified mixed regeneration liquid of demercuration.
Fig. 2 is stepwise regeneration method regenerated liquid and modification liquid provided by the invention.
Specific embodiment
The present invention provides a kind of regeneration of SCR catalyst that fails and demercuration method of modifying.This method is existed by infusion process
Catalyst surface supports Ce as modified active substance, supplements V and compensates as active material, supplements Mo or W as catalyst aid.
The V active site of this method supplement inactivation, and add the modified collaboration demercuration ability for improving catalyst surface V active site of Ce simultaneously
Restore the denitration ability of catalyst.The present invention supports Ce and V, Mo or substep by substep and supports Ce and V, W, it is therefore prevented that mixing is again
Raw liquid bring cerium vanadate sedimentation problem, optimizes process flow, it is therefore prevented that catalyst activity component occurs in catalyst surface
The problem of reunion, improves active component and supports efficiency.
By the following examples and attached drawing the present invention is described in detail:
Embodiment one:
(1) SCR catalyst of failure is pre-processed with dedusting detoxification, specifically includes the following steps:
(1.1) failure SCR catalyst surface is purged using 0.6MPa dry compressed air.
(1.2) catalyst by step (1.1) processing is impregnated and is rinsed using the NaOH solution of 2.0%wt
0.5h, i.e. progress alkali cleaning.
(1.3) H of 5.0%wt is used the catalyst by step (1.2) processing2SO4Solution is impregnated and is rinsed
0.5h, i.e. progress pickling.
(1.4) catalyst by step (1.3) processing is impregnated and is rinsed using deionized water, until deionized water
Intermediate ion concentration is stablized.
(2) 4h will be impregnated in the cerous nitrate solution that concentration is 0.08%wt by the catalyst of step (1) processing, controlled
Dipping solid-to-liquid ratio is 87g/L.
(3) 1h will be dried at 110 DEG C by the catalyst of step (2) processing.
(4) 4h will be calcined at 500 DEG C by the catalyst of step (3) processing, and be cooled to room temperature.
(5) catalyst by step (4) processing is mixed in 0.54%wt ammonium metavanadate and 0.60%wt ammonium molybdate molten
4h is impregnated in liquid.
(6) 1h will be dried at 110 DEG C by the catalyst of step (5) processing.
(7) 3h will be calcined at 400 DEG C by the catalyst of step (6) processing, and be cooled to room temperature.
Embodiment two: other steps are as in the first embodiment, cerous nitrate solution concentration is 0.23%wt in step (2).
Embodiment three: other steps are as in the first embodiment, cerous nitrate solution concentration is 0.46%wt in step (2).
Example IV: other steps lead to embodiment one, and cerous nitrate solution concentration is 0.69%wt in step (2).
Embodiment five: other steps are as in the first embodiment, step (5) uses 0.54%wt ammonium metavanadate and the inclined tungsten of 2.5%wt
Sour ammonium mixed solution impregnates 4h.
Under the conditions of comparison example one to example four, and same regenerated liquid, it is with step (5) (6) (7) (1.4) (2) (3)
Sequentially, the sample (reference group sample) prepared.Setting reference group sample purpose is to absolutely prove to support regenerative component V and Mo
Or V and W and support the different influences to regenerating and modifying catalyst of modified component Ce sequence.Wherein step (2) nitric acid cerium concentration
For 0.08%wt person, it is denoted as reference one；Wherein step (2) nitric acid cerium concentration is 0.23%wt person, is denoted as reference two；Wherein step
(2) nitric acid cerium concentration is 0.46%wt person, is denoted as reference three；Wherein step (2) nitric acid cerium concentration is 0.69%wt person, is denoted as ginseng
Than four；Each example and reference denitration efficiency and catalysis mercury oxidation efficiency are as follows.
Table 1
Denitration efficiency detection method are as follows: if catalyst sample is cut into 2.9cm × 16.5cm dry plate, be put into fixed bed simulation
Denitration efficiency detection is carried out in reactor, simulates gas with N2For carrier gas, wherein NO:400mg/m3、SO2: 1000mg/m3、O2:
3%, H2O:10.0%, n (NH3)/n (NO)=1, N2For balanced gas, 370 DEG C of reaction temperature.
Using NO in the infrared flue gas analyzer NGA2000 type flue gas analyzer detection gas of German RosemountxContent.
The above result shows that Ce, which is supported, has covering to catalyst surface V active site, the increase of Ce loading is for catalysis
The denitration activity of agent has negative effect.By comparison example and reference as a result, the technological process of production that the present invention designs can be most
Limits ground exposed surface V active site, and then good SCR catalyst regeneration denitration efficiency is provided.
Table 2
| Catalyst sample title | Mercury oxidation rate detected value |
| Fail SCR catalyst | 51.0% |
| Example one | 78.4% |
| Example two | 54.7% |
| Example three | 58.9% |
| Example four | 27.3% |
Reaction condition are as follows: flue gas flow: 2L/min, N2Carrier gas.Smoke components: 800ppm SO2, 300ppm NO, 5%O2,
12%CO2, 10ppm HCl, Hg concentration: 30 μ g/m3.Reaction temperature is 350 DEG C.Reaction velocity is 20000h-1。
Detection method are as follows: the mono- optical path pool measurement of Lumex.
Measurement result shows that Ce modified catalyst can significantly improve the mercury oxidation reaction after failing SCR catalyst regeneration and urge
Change activity, for the performance for distinguishing different loading catalyst, using significantly larger than coal-burning power plant's SCR catalyst application air speed
Reaction condition still realizes higher mercury catalysis oxidation rate.Meanwhile comparison example and reference catalyst, the work that the present invention designs
Skill process also has positive effect for the mercury oxidation catalytic performance of raising regenerating and modifying catalyst.
Fig. 2 illustrates the regenerated liquid and modification liquid that the present invention uses, and will not sink under conditions of distributed regeneration is modified
It forms sediment.
The above case study on implementation is merely illustrative of the technical solution of the present invention, rather than its limitations；Although referring to aforementioned implementation
Invention is explained in detail for example, those skilled in the art should understand that: it still can be to aforementioned each reality
Technical solution documented by example is applied to modify or equivalent replacement of some of the technical features；And these modification or
Person's replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. simultaneously demercuration method of modifying, the failure SCR catalyst activity group are divided into V for a kind of regeneration for the SCR catalyst that fails2O5, help
Agent is MoO3；It is characterized in that, simultaneously demercuration method of modifying comprises the steps of: for the regeneration
(1) SCR catalyst of failure is pre-processed with dedusting detoxification；
(2) it will be sufficiently impregnated in the cerous nitrate solution that concentration is 0.08-1.00%wt by the catalyst of step (1) processing；
(3) it will be dried at 100-120 DEG C by the catalyst of step (2) processing；
(4) 2-4h will be calcined at 450-500 DEG C by the catalyst of step (3) processing, and be cooled to room temperature；
(5) by the catalyst by step (4) processing in 0.45-0.60%wt ammonium metavanadate and 0.60-0.80%wt ammonium molybdate
It is sufficiently impregnated in mixed solution；
(6) it will be dried at 100-120 DEG C by the catalyst of step (5) processing；
(7) 2-4h will be calcined at 400-450 DEG C by the catalyst of step (6) processing, and be cooled to room temperature.
2. regeneration according to claim 1 and demercuration method of modifying, which is characterized in that obtained by step (7) processing
V loading 0.8-1.2%, Mo loading 1.3-1.8%, the Ce loading 0.1-0.5% of SCR catalyst.
3. simultaneously demercuration method of modifying, the failure SCR catalyst activity group are divided into V for a kind of regeneration for the SCR catalyst that fails2O5, help
Agent is WO3；It is characterized in that, simultaneously demercuration method of modifying comprises the steps of: for the regeneration
(1) SCR catalyst of failure is pre-processed with dedusting detoxification；
(2) it will be sufficiently impregnated in the cerous nitrate solution that concentration is 0.08-1.00%wt by the catalyst of step (1) processing；
(3) it will be dried at 100-120 DEG C by the catalyst of step (2) processing；
(4) 2-4h will be calcined at 450-500 DEG C by the catalyst of step (3) processing, and be cooled to room temperature；
(5) by the catalyst by step (4) processing in 0.45-0.60%wt ammonium metavanadate and 2.5-4.0%wt ammonium metatungstate
It is sufficiently impregnated in mixed solution；
(6) it will be dried at 100-120 DEG C by the catalyst of step (5) processing；
(7) 2-4h will be calcined at 400-450 DEG C by the catalyst of step (6) processing, and be cooled to room temperature.
4. regeneration according to claim 3 and demercuration method of modifying, which is characterized in that obtained by step (7) processing
V loading 0.8-1.2%, W loading 5.0-8.0%, the Ce loading 0.1-0.5% of SCR catalyst.
5. regeneration according to claim 1 or 3 and demercuration method of modifying, which is characterized in that step (1) includes following step
It is rapid:
(1.1) failure SCR catalyst surface is purged using 0.5-1.0MPa compressed air using dry compressed air；
(1.2) catalyst by step (1.1) processing is impregnated and is rinsed using the NaOH solution of 1.2-4.0%wt
0.5-1.0h；
(1.3) H of 3.0-9.8%wt is used the catalyst by step (1.2) processing2SO4Solution is impregnated and is rinsed
0.5-1.0h；
(1.4) to by step (1.3) processing catalyst impregnated and rinsed using deionized water, until in deionized water from
Sub- concentration is stablized.
6. regeneration according to claim 1 or 3 and demercuration method of modifying, which is characterized in that in step (2), dip time
For 3-5h.
7. regeneration according to claim 1 or 3 and demercuration method of modifying, which is characterized in that in step (5), dip time
For 3-5h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112642495A (en) * | 2020-11-18 | 2021-04-13 | 苏州西热节能环保技术有限公司 | Realize low SO2Catalyst regeneration and modification method for conversion rate and high zero-valent mercury oxidation performance |
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| KR20120028049A (en) * | 2010-09-14 | 2012-03-22 | 한국전력공사 | A catalyst for selective catalytic reduction of nitrogen oxides and method for regeneration thereof |
| CN104707482A (en) * | 2015-03-19 | 2015-06-17 | 南京宇行环保科技有限公司 | Regeneration method of deactivated catalyst |
| CN104801182A (en) * | 2015-04-03 | 2015-07-29 | 青海省化工设计研究院有限公司 | Regeneration method of denitration catalyst |
| WO2016187674A1 (en) * | 2015-05-27 | 2016-12-01 | Newsouth Innovations Pty Limited | Method for assisting thermally-induced changes |
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- 2019-05-28 CN CN201910449389.0A patent/CN110102284A/en active Pending
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| KR20120028049A (en) * | 2010-09-14 | 2012-03-22 | 한국전력공사 | A catalyst for selective catalytic reduction of nitrogen oxides and method for regeneration thereof |
| CN104707482A (en) * | 2015-03-19 | 2015-06-17 | 南京宇行环保科技有限公司 | Regeneration method of deactivated catalyst |
| CN104801182A (en) * | 2015-04-03 | 2015-07-29 | 青海省化工设计研究院有限公司 | Regeneration method of denitration catalyst |
| WO2016187674A1 (en) * | 2015-05-27 | 2016-12-01 | Newsouth Innovations Pty Limited | Method for assisting thermally-induced changes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112642495A (en) * | 2020-11-18 | 2021-04-13 | 苏州西热节能环保技术有限公司 | Realize low SO2Catalyst regeneration and modification method for conversion rate and high zero-valent mercury oxidation performance |
| CN112642495B (en) * | 2020-11-18 | 2024-01-19 | 苏州西热节能环保技术有限公司 | Realize low SO 2 Catalyst regeneration and modification method with conversion rate and high zero-valent mercury oxidation performance |
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Application publication date: 20190809 |