CN103878034B - The renovation process of a kind of arsenic and phosphorism denitrifying catalyst with selective catalytic reduction - Google Patents
The renovation process of a kind of arsenic and phosphorism denitrifying catalyst with selective catalytic reduction Download PDFInfo
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- CN103878034B CN103878034B CN201410127771.7A CN201410127771A CN103878034B CN 103878034 B CN103878034 B CN 103878034B CN 201410127771 A CN201410127771 A CN 201410127771A CN 103878034 B CN103878034 B CN 103878034B
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Abstract
The invention discloses the renovation process of a kind of arsenic and phosphorism denitrifying catalyst with selective catalytic reduction, technical process comprises mechanical ash removing, alkaline cleaning fluid cleaning, regenerated liquid dipping and drying; Alkaline cleaning fluid is the mixed solution of strong base-weak acid salt and surfactant; Acid reclaim liquid is made up of ammonium salt, weak acid, ammonium metavanadate and ammonium molybdate.Adopt method of the present invention to after the SCR denitration regeneration of arsenic and phosphorism, substantially by arsenic and phosphorus component removing, and can have certain anti-arsenic poisoning ability, denitration rate reaches 81 ~ 88%, can keep compression strength and the tear strength of catalyst simultaneously; In addition, the regeneration technology flow process used is also comparatively simple, and treatment effeciency is high, is applicable to large-scale industrial production.
Description
Technical field
The present invention relates to SCR (SCR) field of denitration catalyst, be specifically related to the renovation process of a kind of arsenic and phosphorism denitrifying catalyst with selective catalytic reduction.
Background technology
Nitrogen oxide is one of main atmosphere pollution, and coal-fired power plant is one of primary discharge source of nitrogen oxide.Along with promulgation and the enforcement of a series of environmental protection policy of China, SCR method gas denitrifying technology is just progressively applied in coal-burning power plant of China.By the end of the year 2012, the coal steam-electric plant smoke denitration unit total capacity that put into operation, more than 2.3 hundred million kW, will account for 28% of national active service fired power generating unit capacity, will improve 10% than 2011; In 2013, the newly-increased thermoelectricity denitration installed capacity in the whole nation was 1.3 times of " 12 " the first two years total amount.SCR denitration in use activity can decline gradually, when its activity decrease extremely can not meet the requirement of " fossil-fuel power plant atmospheric pollutant emission standard ", just need to change, its replacement cycle is generally 3 years, and renewal cost accounts for 50% of SCR system total price.The SCR catalyst of inactivation is regenerated, can improve or recover its activity, reach the object of re-using.Regeneration expense only accounts for all changes 30% of catalyst costs, and saves the cost of process spent catalyst, and therefore, the regeneration of SCR catalyst has very important economic benefit and environmental benefit.
Arsenic and phosphorism are one of common causes causing catalysqt deactivation.Arsenic (As) is poisoning is that As can be oxidized to the As of gaseous state because ignition temperature is higher than 1400 DEG C
2o
3and be present in flue gas, these As
2o
3molecule enters into the micropore of catalyst, with O
2and V
2o
5reaction, forms As at catalyst surface
2o
5, cause the destruction of catalyst activity component.The poisoning main cause of phosphorus (P) is V and W that P instead of in V-OH and W-OH, generates P-OH, and it is acid not as V-OH and W-OH, can only provide more weak acidic site, cause catalyst to NH
3absorption can weaken; In addition, P also can react with the V=O active sites of catalyst surface, generates VOPO
4deng material, thus decrease the quantity of active sites.
Cause the arsenic of catalyst poisoning and the compound of phosphorus generally to present acidity, adopt Alkaline pretreatment just can reach good effect.The processing method that refer to respectively in the Chinese invention patent of publication number CN102814201A and publication number CN102026721A for arsenic poisoning and phosphorism is found in research.The former is adopt strong acid and strong base alternating action to the process of arsenic, and this sustains damage making the catalyst strength after regeneration, reduces service life; In addition, its regeneration technology more complicated, adds industrial production cost, can produce a large amount of waste liquor contamination environment simultaneously.The latter has only used highly basic when the catalyst treatment to phosphorism, supplements lack research to acidifying and active material, although the method is fine to the treatment effect of phosphorus, strength damage is also comparatively large, and is difficult to obtain higher denitration activity.
On this basis, this patent proposes a kind of renovation process of the SCR denitration for arsenic and phosphorism newly.The method can simplification of flowsheet, and reduce production cost and reduce regenerative process to the pollution of environment, the catalyst after also can making regeneration still has higher intensity and longer service life, is therefore more conducive to large-scale industrial production.
Summary of the invention
The object of this invention is to provide the SCR denitration renovation process of a kind of new arsenic and phosphorism, succinct mode efficiently can be utilized to remove the arsenic and phosphorus component that cause catalyst poisoning, supplement impaired active component simultaneously, make catalyst recover its higher denitration activity, have certain anti-arsenic poisoning ability simultaneously.
For achieving the above object, the present invention is by the following technical solutions:
A renovation process for the SCR denitration of arsenic and phosphorism, comprises the following steps:
(1) with 2 ~ 6Mpa, flow 0.5 ~ 1.0m
3the clean dried compressed air of/s purges the SCR denitration of inactivation, and to remove the dust stratification on surface, the time is 10 ~ 20min;
(2) by blow ash process after catalyst be placed in alkaline cleaning fluid ultrasonic wave added cleaning, time 20 ~ 60min, ultrasonic power 100 ~ 500w;
(3) deionized water rinsed clean is used;
(4) by catalyst soakage in regenerated liquid, remove residual arsenic and phosphorus composition, supplement impaired active component, dip time 1 ~ 4h simultaneously;
(5) by catalyst dry 1 ~ 3h, then roasting 2 ~ 5h at 350 ~ 450 DEG C at 100 ~ 150 DEG C, the SCR denitration after regenerating namely is obtained.
Wherein, described alkaline cleaning fluid is the mixed solution of strong base-weak acid salt and surfactant, and strong base-weak acid salt is one or more of sodium carbonate, sodium acetate, sodium sulfite or sodium metasilicate, and concentration is 0.1 ~ 2mol/L; Surfactant is one or more of paregal O (AEO), micropore permeation agent JFC or alkyl phenol polyoxy ether (OP ~ (n), n=10), and content is 0.2 ~ 1wt%; Surplus is deionized water.
Wherein, described regenerated liquid consist of ammonium salt, weak acid, ammonium metavanadate and ammonium molybdate, ammonium salt is one or both of ammonium chloride or ammonium nitrate, and concentration is 0.1 ~ 2mol/L; Weak acid is one or more of oxalic acid, acetic acid or citric acid, and content is 0.1 ~ 1wt%; Ammonium metavanadate content is 0.5 ~ 4wt%; Ammonium molybdate content is 1 ~ 6wt%; Surplus is deionized water.
Further, preferred described cleaning fluid is made up of 0.8mol/L sodium carbonate, 0.3wt% paregal O.
Further, preferred described regenerated liquid is made up of 1mol/L ammonium chloride, 0.6wt% oxalic acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
Beneficial effect:
The beneficial effect of the renovation process of arsenic of the present invention and phosphorism SCR denitration is:
(1) cleaning fluid that the present invention is used presents alkalescent, while removing arsenic and phosphorus composition, can farthest keep the compression strength of catalyst, tear strength and active component; With the addition of surfactant in cleaning fluid, and adopt ultrasonic wave added cleaning, greatly improve cleaning efficiency;
(2) ammonium salt contained in regenerated liquid of the present invention and weak acid can remove residual a small amount of arsenic and phosphorus component further, reach the object purified completely; Regenerated liquid can be also catalyst make-up active component, and its denitration activity is further enhanced; Catalyst after the ammonium molybdate added can make regeneration obtains certain anti-arsenic poisoning ability.
(3) denitration activity detection is carried out to the SCR denitration after the regeneration of use this method, find that its denitration rate can reach 81 ~ 88%.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is elaborated, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Embodiment 1
(1) solution preparation
Cleaning fluid: 0.8mol/L sodium carbonate, 0.3wt% paregal O;
Regenerated liquid: 1mol/L ammonium chloride, 0.6wt% oxalic acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
(2) technological process
Institute's sample thief is the vanadium tungsten titanium system denitrating catalyst that certain power plant has run 23000 hours, and find that denitration rate is 53% after testing, deactivation cause is serious arsenic poisoning.First, 3Mpa, flow 0.5m is utilized
3the Compressed Gas of/s carries out purging 10min to the denitrification catalyst module of arsenic poisoning; Secondly, the complete catalyst of purging is inserted ultrasonic wave added cleaning 30min in cleaning fluid, utilize deionized water to carry out rinsing; Then, by the catalyst soakage 3h in regenerated liquid after process; Finally, the hot-air of 120 DEG C is utilized to carry out dry 2h to catalyst.SCR denitration regenerative process terminates.
Denitration activity test is carried out to the catalyst after regeneration, finds that its denitration rate returns to 88% by 53%.
Embodiment 2
(1) solution preparation
Cleaning fluid: 0.5mol/L sodium carbonate, 0.3wt% paregal O;
Regenerated liquid: 1mol/L ammonium chloride, 0.6wt% oxalic acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
(2) technological process
Institute's sample thief is the vanadium tungsten titanium system denitrating catalyst that certain power plant has run 23000 hours, and find that denitration rate is 53% after testing, deactivation cause is serious arsenic poisoning.First, 3Mpa, flow 0.5m is utilized
3the Compressed Gas of/s carries out purging 10min to the denitrification catalyst module of arsenic poisoning; Secondly, the complete catalyst of purging is inserted ultrasonic wave added cleaning 30min in cleaning fluid, utilize deionized water to carry out rinsing; Then, by the catalyst soakage 3h in regenerated liquid after process; Finally, the hot-air of 120 DEG C is utilized to carry out dry 2h to catalyst.SCR denitration regenerative process terminates.
Denitration activity test is carried out to the catalyst after regeneration, finds that its denitration rate returns to 82% by 53%.
Embodiment 3
(1) solution preparation
Cleaning fluid: 0.8mol/L sodium acetate, 0.3wt% micropore permeation agent JFC;
Regenerated liquid: 1mol/L ammonium chloride, 1wt% acetic acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
(2) technological process
Institute's sample thief is the vanadium tungsten titanium system denitrating catalyst that certain power plant has run 23000 hours, and find that denitration rate is 53% after testing, deactivation cause is serious arsenic poisoning.First, 3Mpa, flow 0.5m is utilized
3the Compressed Gas of/s carries out purging 10min to the denitrification catalyst module of arsenic poisoning; Secondly, the complete catalyst of purging is inserted ultrasonic wave added cleaning 30min in cleaning fluid, utilize deionized water to carry out rinsing; Then, by the catalyst soakage 3h in regenerated liquid after process; Finally, the hot-air of 120 DEG C is utilized to carry out dry 2h to catalyst.SCR denitration regenerative process terminates.
Denitration activity test is carried out to the catalyst after regeneration, finds that its denitration rate returns to 85% by 53%.
Embodiment 4
(1) solution preparation
Cleaning fluid: 1mol/L sodium sulfite, 0.3wt% paregal O;
Regenerated liquid: 0.5mol/L ammonium nitrate, 0.6wt% oxalic acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
(2) technological process
Institute's sample thief is the vanadium tungsten titanium system denitrating catalyst that certain power plant has run 23000 hours, and find that denitration rate is 53% after testing, deactivation cause is serious arsenic poisoning.First, 3Mpa, flow 0.5m is utilized
3the Compressed Gas of/s carries out purging 10min to the denitrification catalyst module of arsenic poisoning; Secondly, the complete catalyst of purging is inserted ultrasonic wave added cleaning 30min in cleaning fluid, utilize deionized water to carry out rinsing; Then, by the catalyst soakage 3h in regenerated liquid after process; Finally, the hot-air of 120 DEG C is utilized to carry out dry 2h to catalyst.SCR denitration regenerative process terminates.
Denitration activity test is carried out to the catalyst after regeneration, finds that its denitration rate returns to 82% by 53%.
Embodiment 5
(1) solution preparation
Cleaning fluid: 0.8mol/L sodium carbonate, 0.5wt%OP ~ (n), n=10;
Regenerated liquid: 0.2mol/L ammonium chloride, 0.4wt% citric acid, 2wt% ammonium metavanadate, 4wt% ammonium molybdate.
(2) technological process
Institute's sample thief is the vanadium tungsten titanium system denitrating catalyst that certain power plant has run 23000 hours, and find that denitration rate is 53% after testing, deactivation cause is serious arsenic poisoning.First, 3Mpa, flow 0.5m is utilized
3the Compressed Gas of/s carries out purging 10min to the denitrification catalyst module of arsenic poisoning; Secondly, the complete catalyst of purging is inserted ultrasonic wave added cleaning 30min in cleaning fluid, utilize deionized water to carry out rinsing; Then, by the catalyst soakage 3h in regenerated liquid after process; Finally, the hot-air of 120 DEG C is utilized to carry out dry 2h to catalyst.SCR denitration regenerative process terminates.
Denitration activity test is carried out to the catalyst after regeneration, finds that its denitration rate returns to 81% by 53%.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (3)
1. a renovation process for arsenic and phosphorism denitrifying catalyst with selective catalytic reduction, is characterized in that, comprises the following steps:
(1) with 2 ~ 6Mpa, flow 0.5 ~ 1.0m
3the clean dried compressed air of/s purges the SCR denitration of inactivation, and to remove the dust stratification on surface, the time is 10 ~ 20min;
(2) by blow ash process after catalyst be placed in alkaline cleaning fluid ultrasonic wave added cleaning, time 20 ~ 60min, ultrasonic power 100 ~ 500w;
(3) deionized water rinsed clean is used;
(4) by catalyst soakage in regenerated liquid, remove residual arsenic and phosphorus composition, supplement impaired active component, dip time 1 ~ 4h simultaneously;
(5) by catalyst dry 1 ~ 3h at 100 ~ 150 DEG C, then roasting 2 ~ 5h at 350 ~ 450 DEG C, namely the SCR denitration after regenerating is obtained, described alkaline cleaning fluid is the mixed solution of strong base-weak acid salt and surfactant, strong base-weak acid salt is one or more of sodium carbonate, sodium acetate, sodium sulfite or sodium metasilicate, and concentration is 0.1 ~ 2mol/L; Surfactant is paregal O or micropore permeation agent JFC, and content is 0.2 ~ 1wt%; Described regenerated liquid consist of ammonium salt, weak acid, ammonium metavanadate, ammonium molybdate and deionized water, ammonium salt is one or both of ammonium chloride or ammonium nitrate, and concentration is 0.1 ~ 2mol/L; Weak acid is one or more of oxalic acid, acetic acid or citric acid, and content is 0.1 ~ 1wt%; Ammonium metavanadate content is 0.5 ~ 4wt%; Ammonium molybdate content is 1 ~ 6wt%; Surplus is deionized water.
2. the renovation process according to claims 1, is characterized in that: described alkaline cleaning fluid is made up of 0.8mol/L sodium carbonate, 0.3wt% paregal O.
3. the renovation process according to claims 2, is characterized in that: in described regenerated liquid, and ammonium chloride concentration is 1mol/L, oxalic acid content is 0.6wt%, ammonium metavanadate content is 2wt%, ammonium molybdate content is 4wt%.
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| CN104128212A (en) * | 2014-08-01 | 2014-11-05 | 焦占付 | SCR (selective catalytic reduction) denitration catalyst deactivation repair agent and inactivation regeneration process |
| CN104162456B (en) * | 2014-08-05 | 2016-03-16 | 洛阳昊海工贸有限公司 | A kind of cleaning fluid for denitrating catalyst regeneration and cleaning method |
| CN105396626B (en) * | 2014-09-10 | 2018-06-29 | 大唐国际化工技术研究院有限公司 | A kind of regeneration method of SCR denitration regenerated liquid and SCR denitration |
| CN104548935B (en) * | 2014-12-30 | 2017-02-22 | 中国华电科工集团有限公司 | Regeneration method of SCR (selective catalytic reduction) catalyst |
| CN104624050A (en) * | 2015-01-22 | 2015-05-20 | 李灏呈 | Method for recycling wasted SCR denitrification catalyst |
| CN104826669B (en) * | 2015-04-26 | 2017-05-17 | 重庆大学 | Alkali washing liquid for regenerating SCR denitration catalysts and application thereof |
| CN104857998B (en) * | 2015-06-02 | 2017-03-22 | 清华大学 | Efficient regenerating method for As-poisoned denitration catalyst |
| CN105148940A (en) * | 2015-08-20 | 2015-12-16 | 天河（保定）环境工程有限公司 | Regeneration impregnation liquid and regeneration technology for vanadium-titanium corrugated plate type denitrification catalyst |
| CN106607106A (en) * | 2015-10-26 | 2017-05-03 | 浙江浙能技术研究院有限公司 | Activity regenerating and performance optimizing method of SCR catalyst for sulfur, arsenic and phosphorus poisoning |
| CN105618162B (en) * | 2016-01-04 | 2018-11-06 | 大唐国际化工技术研究院有限公司 | A kind of recycling method of discarded vanadium tungsten titanium-based denitrating catalyst |
| CN105728064A (en) * | 2016-03-04 | 2016-07-06 | 北京科林佰德化工科技有限公司 | Method for cleaning and regenerating SCR denitration catalyst for potassium and sodium poisoning deactivation |
| CN106378208A (en) * | 2016-08-19 | 2017-02-08 | 安徽元琛环保科技股份有限公司 | A regenerating method for a power plant flue gas denitration catalyst |
| CN107442135B (en) * | 2017-08-25 | 2020-04-21 | 华北电力大学 | Regeneration method of arsenic poisoning SCR denitration catalyst |
| CN108671931A (en) * | 2018-04-23 | 2018-10-19 | 清华大学 | A kind of method of modifying of the denitrating catalyst with anti-toxicity energy |
| CN111036310A (en) * | 2019-12-25 | 2020-04-21 | 中节能万润股份有限公司 | Regenerated monolithic molecular sieve-based denitration catalyst, and regeneration method and application thereof |
| CN114558625A (en) * | 2022-03-14 | 2022-05-31 | 龙净科杰环保技术（上海）有限公司 | SCR denitration catalyst regeneration process in steel industry |
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| US6395665B2 (en) * | 1998-07-24 | 2002-05-28 | Mitsubishi Heavy Industries, Ltd. | Methods for the regeneration of a denitration catalyst |
| CN102059156B (en) * | 2010-12-21 | 2013-01-23 | 重庆远达催化剂制造有限公司 | Denitration catalyst regenerating solution and regenerating method thereof |
| CN103143401A (en) * | 2011-12-07 | 2013-06-12 | 徐树元 | Flue gas denitrification catalyst on-line regeneration activator liquid and preparation method thereof |
| CN102814201A (en) * | 2012-07-18 | 2012-12-12 | 西安交通大学 | Cleaning and regeneration method for SCR denitration catalyst poisoned by arsenic component in flue |
| CN102974404A (en) * | 2012-11-22 | 2013-03-20 | 中节能六合天融环保科技有限公司 | Denitrification catalyst regeneration method |
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Effective date of registration: 20160511 Address after: 101111, room 2, No. 064, government road, Tongzhou District light industrial park, Zhongguancun science and Technology Park, Tongzhou, Beijing Patentee after: Beijing macro environmental protection technology Co., Ltd. Address before: 100095, 408 hot springs town, Beijing, Haidian District Patentee before: Li Haocheng |
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