CN103350004A - SCR denitrification catalyst regeneration method and mixture for SCR denitrification catalyst regeneration liquid - Google Patents
SCR denitrification catalyst regeneration method and mixture for SCR denitrification catalyst regeneration liquid Download PDFInfo
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- CN103350004A CN103350004A CN2013103316618A CN201310331661A CN103350004A CN 103350004 A CN103350004 A CN 103350004A CN 2013103316618 A CN2013103316618 A CN 2013103316618A CN 201310331661 A CN201310331661 A CN 201310331661A CN 103350004 A CN103350004 A CN 103350004A
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Abstract
The present invention provides a mixture for a SCR denitrification catalyst regeneration liquid, and a method for carrying out SCR denitrification catalyst regeneration by using the regeneration liquid. With the present invention, a regeneration performance of the catalyst can be effectively increased, an active substance supplement process can be eliminated, a regeneration cost is effectively reduced, and a regeneration process is simplified.
Description
Technical field
The present invention relates to the power environment protection technical field, the renovation process that is specifically related to a kind of honeycomb type SCR (SCR) denitrating catalyst reaches the mixture that is used for SCR denitrating catalyst regenerated liquid.
Background technology
The nitrogen oxide of coal fired power plant (NOx) emission control is the major tasks in energy-conserving and environment-protective field during the country " 12 ", and " fossil-fuel power plant atmospheric pollutant emission standard " of up-to-date promulgation (GB13223-2011) formulated control criterion (100mg/m the strictest in the world wide especially to the NOx concentration of emission
3).Along with the appearance of these national policies, discharging how effectively to control NOx has become one of important topic that needs to be resolved hurrily in the current power field of Environment Protection.
At present, the denitrating flue gas of coal fired power plant (DeNOx) mainly adopts SCR (SCR) technology.This technology by the SCR catalyst, is reduced into the NOx in the flue gas N of nonhazardous take ammonia as reducing agent
2And H
2O, thus reach the purpose that control NOx discharges.The SCR catalyst is the core of SCR flue gas denitrification system, and its performance directly affects denitration efficiency and denitration cost.Typical commercial SCR catalyst is with TiO
2Be carrier, V
2O
5-WO
3Or V
2O
5-MoO
3Honeycomb type catalyst for active material.This kind catalyst denitration efficiency is high, and technology maturation is reliable, is used widely.
But because this catalyst is in the working environment of high-temperature high dust for a long time, easy-sintering also forms micropore gambling plug; Alkali in the flue gas (soil) metal also very easily with the acidic site effect of catalyst surface, thereby reduce the sour figure place of catalyst surface; These all can cause the catalyst denitration activity to reduce is catalyst poisoning, and shorten service life, for example V
2O
5-WO
3/ TiO
2Usually only have 3～4 years the service life of type SCR catalyst.Because the initial investment of SCR catalyst is large, accounts for 30～50% of whole denitrating system gross investment, after catalyst poisoning, if can cause the denitration cost to increase considerably with the raw catelyst replacement; And if adopt suitable technology that catalyst is carried out active regeneration, then can effectively reduce the denitration cost; According to measuring and calculating, to typical 600 megawatt units, if adopt catalyst regeneration technical finesse poisoned catalyst, can save 100～3,000,000 RMB every year.Therefore, the SCR catalyst regeneration technology of research high efficiency, low cost seems particularly necessary and important.
Common SCR catalyst regeneration thinking is: at first purge dust on the catalyst with compressed air, then remove alkali (soil) slaine on the catalyst and recover the acid position with sulfuric acid liquid dipping, use at last active material presoma (being generally ammonium metavanadate and ammonium metatungstate) solution to soak catalyst to replenish the active material that runs off.Although above-mentioned regeneration thinking can have the denitration activity of efficient recovery poisoned catalyst, also there are the following problems: (1) sulfuric acid dipping can effectively be removed the K of catalyst surface
+And Na
+, but to alkaline-earth metal ions such as Mg
2+, Ca
2+Deng removal effect unsatisfactory; Simultaneously, acid solution can be dissolved V
2O
5And WO
3Can cause the catalyst activity material to run off, and acid strength is larger, active material runs off more seriously in the pickling rear catalyst, and this is at document (Jung Bin Lee, Seong Keun Kim, Dong Wha Kim, et al.Korean J.Chem.Eng., 270～276) and confirmation all arranged among the patent US7592283 2012,29 (2):; (2) active material presoma ammonium metatungstate price is higher, is the principal element that affects SCR Catalyst Production cost, and therefore, additional active material can significantly increase the regeneration cost of catalyst, has also increased the complexity of regeneration technology operation simultaneously.In a word, the problems referred to above cause existing SCR catalyst regeneration technology to exist regenerability to have much room for improvement, and the more high potential problems of regeneration cost are unfavorable for the through engineering approaches application.
Summary of the invention
For the defective and the deficiency that exist in the existing SCR catalyst regeneration technology, the object of the present invention is to provide a kind of renovation process of SCR catalyst.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of renovation process of SCR denitrating catalyst is characterized in that may further comprise the steps:
(1) cleans: purge poisoning SCR catalyst with the cleaning dried compressed air, remove the dust stratification of catalyst surface; Catalyst after purging is immersed in deionized water for ultrasonic ripple preliminary treatment 10 minutes, removes the laying dust in the fine pore, then rinse well with water fog nozzle.
(2) dipping: the catalyst after step (1) processing is inserted in the regenerated liquid that is comprised of strong acid, ammonium salt, chelating agent and deionized water, flood at normal temperatures and pressures more than 2 hours;
(3) drying and roasting: the catalyst after step (2) processing is carried out drying and roasting at temperature rise rate by following temperature increasing schedule, comprise: to be less than or equal to 3 ℃/minute heating rate, be heated to 150 ℃ and maintenance from room temperature, the total duration of this part is 2 hours; Being less than or equal to 3 ℃/minute heating rate, be heated to 400 ℃ and keep from 150 ℃, the total duration of this part is 4 hours.
Further, the content of strong acid, ammonium salt and chelating agent is respectively in the described regenerated liquid: 1～2wt%, 2～5wt%, 0.5～1wt%.
Further, the strong acid in the described regenerated liquid is the concentrated sulfuric acid or red fuming nitric acid (RFNA).
Further, the ammonium salt in the described regenerated liquid is ammonium chloride.
Further, the chelating agent in the described regenerated liquid is ethylenediamine tetra-acetic acid or nitrilotriacetic acid.
A kind of mixture for SCR denitrating catalyst regenerated liquid is characterized in that: described mixture is comprised of strong acid, ammonium salt, chelating agent and deionized water.
Further, the content of strong acid, ammonium salt and chelating agent is respectively in the described mixture: 1～2wt%, 2～5wt%, 0.5～1wt%.
Technique effect of the present invention is:
The invention discloses a kind of novel regenerated liquid prescription that is used for the SCR denitrating catalyst, regenerated liquid is comprised of diluted acid, chelating agent and ammonium salt and deionized water, wherein, in order to reduce acid solution to the dissolubility of active component in the catalyst, the more traditional SCR catalyst regeneration of the acid strength liquid that the present invention selects (is generally 0.5M H
2SO
4) low; And be to improve regenerated liquid to the removal effect of alkali (soil) metal ion, select that alkali (soil) metal ion is had the chelating agent of good combination performance as one of regenerated liquid recipe ingredient; Simultaneously, can thermal decomposition and original position generation NH
3Ammonium salt introduce in the regenerated liquid prescription, can increase regeneration rear catalyst surface NH
3Adsorbance; Therefore, the regeneration effect that regenerated liquid formula Design of the present invention on the one hand can the Effective Raise catalyst can save on the other hand active material and replenish technique, effectively reduces regeneration cost, simplifies regeneration technology.
The present invention utilizes above-mentioned regenerated liquid prescription and in conjunction with suitable drying and roasting and soot blowing technique, and a kind of renovation process of new SCR catalyst is provided.
Compare with existing SCR catalyst regeneration technology, have the following advantages:
(1) by reducing acid concentration in the regenerated liquid, effectively reduces the loss of catalyst activity material in the regenerative process, reduce the necessity of replenishing active material.
(2) in regenerated liquid, add chelating agent and can improve it to the removal effect of alkali in the catalyst (soil) metal ion.
(3) add easily decomposition ammonium salt, then can improve the NH on regeneration rear catalyst surface
3Content.
In summary, the regenerability that the renovation process of SCR catalyst provided by the invention not only can the Effective Raise catalyst, and can also save active material simultaneously and replenish technique, effectively reduce regeneration cost, simplify regeneration technology.
In addition, because different poisoned catalyst poisoning kinds and the difference of degree of intoxication, can be according to the concentration value of each composition in the concrete regenerated liquid of the detection Analysis deterrmination of catalyst poisoning kind and degree of intoxication before the regeneration.
The specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
Embodiment one
(1) domestic certain coal fired power plant has been moved more than 30000 hour poisoning SCR catalyst (V
2O
5-WO
3/ TiO
2Type, wall thickness: 0.7mm, pitch: 6.8mm), cut into the fritter of 35mm * 35mm * 90mm, use without oil drying compressed air (0.5MPa) and purge 10 minutes, to remove the dust stratification of catalyst surface; Then the catalyst after will purging is immersed in to be rinsed well with water fog nozzle after laying dust in the fine pore is removed in deionized water for ultrasonic ripple preliminary treatment 10 minutes.
(2) catalyst after step (1) processing is inserted 500ml by 1wt% sulfuric acid, in the regenerated liquid that 5wt% ammonium chloride and 0.8wt% ethylenediamine tetra-acetic acid form, flooded at normal temperatures and pressures 2 hours.
(3) catalyst after step (2) is processed carries out drying and roasting by following temperature increasing schedule: room temperature → 150 ℃/2 hours → 400 ℃/4 hours, heating rate is not more than 3 ℃/minute.Regeneration ending.
Catalyst after poisoning and the regeneration is placed respectively SCR denitration activity experimental rig, under simulated flue gas, test denitration efficiency, estimate regeneration effect.
Experiment condition is as follows: NO:350ppm, NH
3: 350ppm, O
2: 3%, SO
2: 500ppm, N
2Be balanced gas, total gas flow rate: 10000ml/min, range of reaction temperature: 280～400 ℃.Gas componant is measured by moral figure flue gas analyzer (testo350-Pro).The result shows: in 280～400 ℃ of scopes, the denitration efficiency of regenerated catalyst is higher than poisoned catalyst, and its activity can return to 89% of the front activity of poisoning.
Embodiment two
(1) domestic certain coal fired power plant has been moved more than 30000 hour poisoning SCR catalyst (V
2O
5-WO
3/ TiO
2Type, wall thickness: 0.7mm, pitch: 6.8mm), cut into the fritter of 35mm * 35mm * 90mm, use without oil drying compressed air (0.5MPa) and purge 10 minutes, to remove the dust stratification of catalyst surface; Then the catalyst after will purging is immersed in to be rinsed well with water fog nozzle after laying dust in the fine pore is removed in deionized water for ultrasonic ripple preliminary treatment 10 minutes.
(2) catalyst after step (1) processing is inserted 500ml by 2wt% sulfuric acid, in the regenerated liquid that 3wt% ammonium chloride and 0.5wt% ethylenediamine tetra-acetic acid form, flooded at normal temperatures and pressures 2 hours.
(3) catalyst after step (2) is processed carries out drying and roasting by following temperature increasing schedule: room temperature → 150 ℃/2 hours → 400 ℃/4 hours, heating rate is not more than 3 ℃/minute.Regeneration ending.
Catalyst after poisoning and the regeneration is placed respectively SCR denitration activity experimental rig, under simulated flue gas, test denitration efficiency, estimate regeneration effect.
Experiment condition is as follows: NO:350ppm, NH
3: 350ppm, O
2: 3%, SO
2: 500ppm, N
2Be balanced gas, total gas flow rate: 10000ml/min, range of reaction temperature: 280～400 ℃.Gas componant is measured by moral figure flue gas analyzer (testo350-Pro).The result shows: in 280～400 ℃ of scopes, the denitration efficiency of regenerated catalyst is higher than poisoned catalyst, and its activity can return to 93% of the front activity of poisoning.
Embodiment three
(1) domestic certain coal fired power plant has been moved more than 30000 hour poisoning SCR catalyst (V
2O
5-WO
3/ TiO
2Type, wall thickness: 0.7mm, pitch: 6.8mm), cut into the fritter of 35mm * 35mm * 90mm, use without oil drying compressed air (0.5MPa) and purge 10 minutes, to remove the dust stratification of catalyst surface; Then the catalyst after will purging is immersed in to be rinsed well with water fog nozzle after laying dust in the fine pore is removed in deionized water for ultrasonic ripple preliminary treatment 10 minutes.
(2) catalyst after step (1) processing is inserted 500ml by 1wt% nitric acid, in the regenerated liquid that 4wt% ammonium chloride and 0.6wt% nitrilotriacetic acid form, flooded at normal temperatures and pressures 2 hours.
(3) catalyst after step (2) is processed carries out drying and roasting by following temperature increasing schedule: room temperature → 150 ℃/2 hours → 400 ℃/4 hours, heating rate is not more than 3 ℃/minute.Regeneration ending.
Catalyst after poisoning and the regeneration is placed respectively SCR denitration activity experimental rig, under simulated flue gas, test denitration efficiency, estimate regeneration effect.
Experiment condition is as follows: NO:350ppm, NH
3: 350ppm, O
2: 3%, SO
2: 500ppm, N
2Be balanced gas, total gas flow rate: 10000ml/min, range of reaction temperature: 280～400 ℃.Gas componant is measured by moral figure flue gas analyzer (testo350-Pro).The result shows: in 280～400 ℃ of scopes, the denitration efficiency of regenerated catalyst is higher than poisoned catalyst, and its activity can return to 85% of the front activity of poisoning.
Claims (7)
1. the renovation process of a SCR denitrating catalyst is characterized in that may further comprise the steps:
(1) cleans: purge poisoning SCR catalyst with the cleaning dried compressed air, remove the dust stratification of catalyst surface; Catalyst after purging is immersed in deionized water for ultrasonic ripple preliminary treatment 10 minutes, removes the laying dust in the fine pore, then rinse well with water fog nozzle.
(2) dipping: the catalyst after step (1) processing is inserted in the regenerated liquid that is comprised of strong acid, ammonium salt, chelating agent and deionized water, flood at normal temperatures and pressures more than 2 hours;
(3) drying and roasting: the catalyst after step (2) processing is carried out drying and roasting at temperature rise rate by following temperature increasing schedule, comprise: to be less than or equal to 3 ℃/minute heating rate, be heated to 150 ℃ and maintenance from room temperature, the total duration of this part is 2 hours; Being less than or equal to 3 ℃/minute heating rate, be heated to 400 ℃ and keep from 150 ℃, the total duration of this part is 4 hours.
2. the renovation process of SCR denitrating catalyst as claimed in claim 1, it is characterized in that: the content of strong acid, ammonium salt and chelating agent is respectively in the described regenerated liquid: 1～2wt%, 2～5wt%, 0.5～1wt%.
3. the renovation process of SCR denitrating catalyst as claimed in claim 2, it is characterized in that: the strong acid in the described regenerated liquid is the concentrated sulfuric acid or red fuming nitric acid (RFNA).
4. the renovation process of SCR denitrating catalyst as claimed in claim 3, it is characterized in that: the ammonium salt in the described regenerated liquid is ammonium chloride.
5. the renovation process of SCR denitrating catalyst as claimed in claim 4, it is characterized in that: the chelating agent in the described regenerated liquid is ethylenediamine tetra-acetic acid or nitrilotriacetic acid.
6. mixture that is used for SCR denitrating catalyst regenerated liquid, it is characterized in that: described regenerated liquid is comprised of strong acid, ammonium salt, chelating agent and deionized water.
7. the mixture for SCR denitrating catalyst regenerated liquid as claimed in claim 6, it is characterized in that: the content of strong acid, ammonium salt and chelating agent is respectively in the described regenerated liquid: 1～2wt%, 2～5wt%, 0.5～1wt%.
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| CN103599816A (en) * | 2013-11-18 | 2014-02-26 | 涿州西热环保催化剂有限公司 | Cleaning agent and cleaning method for off-line cleaning calcium-poisoned SCR (Selective Catalytic Reduction) denitration catalyst |
| CN103949290A (en) * | 2014-05-08 | 2014-07-30 | 北京中南亚太环境科技发展有限公司 | Method for recycling denitration catalyst |
| CN104226380A (en) * | 2014-09-24 | 2014-12-24 | 清华大学 | Method for regenerating flue gas denitration catalyst with high phosphorus and high alkali metal content |
| CN104815675A (en) * | 2015-04-09 | 2015-08-05 | 北京大学包头创新研究院 | Selective catalytic reduction denitration catalyst and regeneration method and application thereof |
| CN104923318A (en) * | 2015-06-09 | 2015-09-23 | 浙江大学 | Method for regenerating inactivated SCR denitration catalyst |
| CN105396626A (en) * | 2014-09-10 | 2016-03-16 | 大唐国际化工技术研究院有限公司 | Regeneration liquid of SCR denitration catalyst and regeneration method of SCR denitration catalyst |
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| CN105944770A (en) * | 2016-04-26 | 2016-09-21 | 华北电力大学（保定） | Organic acid regeneration method of alkali inactivated SCR denitration catalyst |
| CN106179526A (en) * | 2016-07-07 | 2016-12-07 | 无锡市华东电力设备有限公司 | A kind of renovation process of honeycomb type SCR denitrating catalyst |
| CN106179528A (en) * | 2016-06-30 | 2016-12-07 | 大唐南京环保科技有限责任公司 | A kind of renovation process of alkali metal poisoning denitrating catalyst |
| CN106475156A (en) * | 2016-08-30 | 2017-03-08 | 苏州华乐大气污染控制科技发展有限公司 | The recovery and treatment method of waste flue gas denitration catalyst and the preparation method of catalyst |
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| CN108355722A (en) * | 2018-04-10 | 2018-08-03 | 中国华能集团清洁能源技术研究院有限公司 | Liquid living, which is mended, using regeneration carries out vanadium titanium system SCR denitration regeneration method |
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| CN111715210A (en) * | 2020-07-09 | 2020-09-29 | 江苏龙净科杰环保技术有限公司 | Regeneration method of cement kiln thallium poisoning SCR denitration catalyst |
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| CN103599816B (en) * | 2013-11-18 | 2015-12-30 | 涿州西热环保催化剂有限公司 | A kind of cleaning agent of off-line cleaning calcium intoxication SCR denitration and cleaning method |
| CN103599816A (en) * | 2013-11-18 | 2014-02-26 | 涿州西热环保催化剂有限公司 | Cleaning agent and cleaning method for off-line cleaning calcium-poisoned SCR (Selective Catalytic Reduction) denitration catalyst |
| CN103949290A (en) * | 2014-05-08 | 2014-07-30 | 北京中南亚太环境科技发展有限公司 | Method for recycling denitration catalyst |
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| CN104815675A (en) * | 2015-04-09 | 2015-08-05 | 北京大学包头创新研究院 | Selective catalytic reduction denitration catalyst and regeneration method and application thereof |
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| CN105665037A (en) * | 2016-02-23 | 2016-06-15 | 洛阳万山高新技术应用工程有限公司 | Regenerative activation treatment method for inactivated SCR denitrated catalyst |
| CN105944770A (en) * | 2016-04-26 | 2016-09-21 | 华北电力大学（保定） | Organic acid regeneration method of alkali inactivated SCR denitration catalyst |
| CN106179528A (en) * | 2016-06-30 | 2016-12-07 | 大唐南京环保科技有限责任公司 | A kind of renovation process of alkali metal poisoning denitrating catalyst |
| CN106179526A (en) * | 2016-07-07 | 2016-12-07 | 无锡市华东电力设备有限公司 | A kind of renovation process of honeycomb type SCR denitrating catalyst |
| CN106475156A (en) * | 2016-08-30 | 2017-03-08 | 苏州华乐大气污染控制科技发展有限公司 | The recovery and treatment method of waste flue gas denitration catalyst and the preparation method of catalyst |
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| CN108355722B (en) * | 2018-04-10 | 2023-04-25 | 中国华能集团清洁能源技术研究院有限公司 | Method for regenerating vanadium-titanium SCR denitration catalyst by using regeneration and rejuvenation liquid |
| CN110354914A (en) * | 2019-08-09 | 2019-10-22 | 华北电力大学 | A kind of inactivation SCR denitration catalyst reuse method |
| CN111715210A (en) * | 2020-07-09 | 2020-09-29 | 江苏龙净科杰环保技术有限公司 | Regeneration method of cement kiln thallium poisoning SCR denitration catalyst |
| CN114870907A (en) * | 2022-06-13 | 2022-08-09 | 苏州西热节能环保技术有限公司 | Regeneration method of alkali/alkaline earth metal poisoned denitration catalyst |
| CN114870907B (en) * | 2022-06-13 | 2023-10-20 | 苏州西热节能环保技术有限公司 | Regeneration method of denitration catalyst for alkali/alkaline earth metal poisoning |
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