CN104801182A - Regeneration method of denitration catalyst - Google Patents
Regeneration method of denitration catalyst Download PDFInfo
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- CN104801182A CN104801182A CN201510156388.9A CN201510156388A CN104801182A CN 104801182 A CN104801182 A CN 104801182A CN 201510156388 A CN201510156388 A CN 201510156388A CN 104801182 A CN104801182 A CN 104801182A
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Abstract
The invention discloses a regeneration method of a denitration catalyst. The method is characterized by comprising the following steps: (1) carrying out negative pressure dust sucking on the surface and the pore canals of a deactivated denitration catalyst at the negative pressure of 0.05-0.07 MPa, while cleaning the pore canals of the catalyst with a fur brush; (2) using a prepared cleaning solution to clean the surface and the pore canals of the catalyst with ultrasonic wave and drying the catalyst; (3) steeping the catalyst in 0.1 mole of a prepared saltpeter solution containing rare earth elements La and Ce and aluminium dihydrogen phosphate and calcining the catalyst to increase the specific surface area of the catalyst and enhance the mechanical strength of the catalyst at the same time; (4) steeping the calcined catalyst in an active-ingredients steeping solution; (5) calcining. By implementing the method, the denitration efficiency of the catalyst after deactivated catalyst generation can reach 82%-87%, and the catalyst strength can be increased by 40%; the method is easy to operate and has prominent economic and social benefits.
Description
Technical field
The present invention relates to a kind of catalyst recovery process, be specifically related to the method for a kind of Faveolate denitration catalyst activity and intensity recovery.
Background technology
The discharge of nitrogen oxide (NOx) drastically influence the health of atmospheric environment and the mankind, and selective catalytic reduction (SCR) gas denitrifying technology is one of effective ways of NO_x removal.The research regenerated after inactivation after running a period of time about denitrating catalyst in recent years becomes the focus of current SCR denitration research.A kind of SCR regenerating flue gas denitrifying catalyst method 201210100560.5P the present invention as applied for by Nanjing University of Technology adopts and is purged by catalyst to be regenerated, then catalyst is put into the cleaning of service sink cleaning fluid, dries; Again by the catalyst soakage that cleaned in active supplement solution, carry out activity supplement, dry; Finally, catalyst complete for drying is carried out roasting, cooling, finally, just can obtain the denitrating catalyst regenerated.Catalyst after regeneration, denitration efficiency reaches more than 90%.Good denitration effect is achieved by the regeneration of foregoing invention to honeycombed catalyst.
After but the denitrating catalyst industrially applied runs a period of time, there is denitration efficiency to decline and catalyst its own mechanical intensity reduces the problem of two aspects, there is not yet the pertinent literature about raising intensity while how strengthening regenerated catalyst denitration efficiency so far.
For above denitrating catalyst regeneration Problems existing, the invention provides a kind of strengthen denitrating catalyst intensity while have the method for efficient recovery catalyst activity.
Summary of the invention
In order to realize above object, the present invention regenerates the denitration honeycombed catalyst running more than 16000h, and the technical solution used in the present invention is: a kind of renovation process of denitrating catalyst, it is characterized in that being, its method comprises the following steps:
(1) hairbrush cleaning catalyst duct is used while using the negative pressure of 0.05-0.07Mpa to carry out the aspiration of negative pressure to decaying catalyst surface and duct;
(2) cleaning fluid is used to utilize ultrasonic wave to clean catalyst surface and duct;
(3) use 0.1 mole of salpeter solution containing the rare earth elements such as La, Ce and aluminium dihydrogen phosphate, impregnated catalyst, while increasing specific surface area of catalyst, within 4 hours, strengthen the mechanical strength of catalyst 550 DEG C of calcinings;
(4) use the oxalic acid solution of 2%, dissolve active ingredient maceration extract containing major catalyst effective ingredient ammonium metavanadate and co-catalyst ammonium tungstate, ammonium molybdate, niobium pentaoxide and the catalyst after reforming is flooded, effective make-up catalyst active constituent;
(5) follow procedure intensification calcining manners is calcined denitrating catalyst at maximum temperature 550 DEG C.
The renovation process of described a kind of denitrating catalyst, is characterized in that being, described catalyst is the cellular selective reduction catalyst (SCR) that coal-burning power plant's denitration uses.
The renovation process of described a kind of denitrating catalyst, is characterized in that, the negative pressure used in described step (1) is 0.05-0.07MPa, while carrying out dust suction, clears up with the hairbrush of diameter 3-5mm catalyst surface ash.
The renovation process of described a kind of denitrating catalyst, it is characterized in that being, cleaning fluid in described step (2) is made up of following composition: the emulsifier op-10 of the NaOH solution of 0.5 mole, the penetrating agent JFC-S of 1-2%, 0.5-1%, 0.5-1% metal-chelator HEDP, cleaning temperature about 30 DEG C, scavenging period 30 minutes, ultrasonic power are 6KW, supersonic frequency is 40HZ, and cleaning post-baking temperature is 90 DEG C.
The renovation process of described a kind of denitrating catalyst, it is characterized in that being, 0.1 molar nitric acid solution is used in described step (3), dissolve the catalyst crystalline phases reformation agent of 0.2-0.4%, 0.05-0.1%, crystalline phase stabilizing agent lanthanum nitrate and cerous nitrate, catalyst strength reinforcing agent is 2-4% solid phosphoric acid aluminum dihydrogen, floods regenerated catalyst, and dipping temperature is 30 DEG C, dip time 3 hours post-dryings, calcining, calcining heat is 550 DEG C of calcinings 4 hours.
The renovation process of described a kind of denitrating catalyst, it is characterized in that being, described step (4) uses the active ingredient maceration extract of the ammonium tungstate of the ammonium metavanadate of the oxalic acid solution of 2% dissolving containing 0.5-1%, 2-5%, the ammonium molybdate of 0.2-0.4%, the niobium pentaoxide of 0.05-0.1% to flood the catalyst after reformation, make-up catalyst active constituent.
The renovation process of described a kind of denitrating catalyst, it is characterized in that being, in described step (5), calcining heat is temperature programming calcining, calcination process is: 0-120 DEG C 20min, 120-250 DEG C 40min, 250-350 DEG C of 60min, 350-450 DEG C of 60 min, 450-550 DEG C 60min, calcines 4 hours for 550 DEG C.
Advantage of the present invention and beneficial effect as follows:
The catalyst of method of the present invention to more than 16000h running time regenerates, and regenerated catalyst denitration efficiency can reach 82-87%, and regeneration denitrating catalyst intensity can improve more than 40%, can reach 179N/CM
3, (decaying catalyst intensity 128 N/CM
3), the work period is short, and do not affect the denitrating technique flow process of enterprise, cost is low, has great economic benefit and social benefit.
This invention step (1) adopt two-section calcining mode first time calcining reforming catalyst increase the prerequisite of specific area under, adopt the calcining of secondary temperature-programmed mode that active constituent pay(useful) load can be made at catalyst surface.
(2) method cleaning fluid of the present invention adopts metal-chelator HEDP to carry out metalchelated ultrasonic cleaning of simultaneously carrying out to the element such as K, Na, Ca, Fe, As being sintered in catalytic inner, effectively can remove the impact of metallic element on catalyst poisoning inactivation.
(3) method of the present invention while the nitric acid cleaning catalyst surface of employing 0.1 mole with add high-temperature agglomerant aluminium dihydrogen phosphate, can with nitric acid generation Synergy, strengthen catalyst strength further.
(4), under the present invention adopts the prerequisite of the rare earth elements such as La, Ce first to denitrating catalyst reaming, increase specific area, catalyst is carried out to the dipping of effective active component, can effectively ensure that the active princlples such as V, W are farthest carried on catalyst surface.
(5) effectively can improve selective to NOx in flue gas of denitrating catalyst the adding of niobium pentaoxide auxiliary agent of 0.05-0.1%, improve denitration efficiency.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail
Embodiment 1
To the denitrating catalyst running 16000h, the negative pressure used in step (1) is 0.05MPa, with the hairbrush of diameter 3-5mm clears up while carrying out dust suction to catalyst surface ash.Step (2) uses cleaning fluid to clean catalyst surface and duct, cleaning fluid volume and catalyst volume are than being 7:1, cleaning fluid be configured to 0.5 moles of NaOH, 1% penetrating agent JFC-S, the emulsifier op-10 of 0.5%, metal-chelator HEDP, the ultrasonic power of 0.5% be 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, cleaning post-baking temperature is 90 DEG C.Step (3) uses the salpeter solution containing 0.1 mole of 0.2% lanthanum nitrate, 0.05% cerous nitrate, 2% aluminium dihydrogen phosphate to flood catalyst, and dipping temperature is 30 DEG C, and dip time is 3 hours, 550 DEG C of calcinings 4 hours after airing.Step (4) use the oxalic acid solution of 2% dissolve 0.5% ammonium metavanadate, 2% ammonium tungstate, the ammonium molybdate of 0.2%, the niobium pentaoxide solution of 0.05% active ingredient maceration extract to catalyst soakage, dip time 3 hours temperature 30 DEG C.Step (5) is calcined by 0-120 DEG C 20min, 120-250 DEG C 40min, 250-350 DEG C of 40min, 350-450 DEG C 60 min, 450-550 DEG C 240min program temperature above catalyst, and its denitration rate can reach 85%.
Embodiment 2
To the denitrating catalyst running 18000h, while repeating embodiment 1, difference uses ultrasonic cleaning solution to clean catalyst surface and duct in step (2), cleaning fluid volume and catalyst volume are than being 7:1, cleaning fluid be configured to 0.5 moles of NaOH, 1% penetrating agent JFC-S, the emulsifier op-10 of 0.6%, metal-chelator HEDP, the ultrasonic power of 0.6% be 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, post-drying.Step (3) use containing 0.1 mole 0.25% lanthanum nitrate, 0.06% cerous nitrate, 2.5% aluminium dihydrogen phosphate salpeter solution catalyst is flooded, dipping temperature is 30 DEG C, and dip time is 3 hours, after drying 550 DEG C calcining 4 hours.The active ingredient maceration extract of the ammonium metavanadate of the oxalic acid solution dissolving 0.6% of step (4) use 2%, the ammonium tungstate of 4%, the ammonium molybdate of 0.25%, the niobium pentaoxide solution of 0.06% is to catalyst soakage time 3 h immersion temperature 30 DEG C, afterwards by embodiment 1 step (5) calcining, its denitration rate can reach 87%.
Embodiment 3
To the denitrating catalyst running 20000h, while repeating embodiment 2, difference uses cleaning fluid to clean catalyst surface and duct in step (2), cleaning fluid volume and catalyst volume are than being 7:1, cleaning fluid be configured to 0.5 moles of NaOH, 1.5% penetrating agent JFC-S, the emulsifier op-10 of 0.7%, metal-chelator HEDP, the ultrasonic power of 0.7% be 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, post-drying.Step (3) uses the salpeter solution containing 0.30% lanthanum nitrate, 0.08% cerous nitrate, 3% aluminium dihydrogen phosphate of 0.1 mole to flood catalyst, and dipping temperature is 30 DEG C, and dip time is 3 hours, 550 DEG C of calcinings 4 hours after drying.Step (4) uses the oxalic acid solution of 2.5% to dissolve ammonium metavanadate, the ammonium tungstate of 4.5%, the ammonium molybdate of 0.30% of 0.8%, the active ingredient maceration extract of the niobium pentaoxide solution of 0.08% was to 3 hours catalyst soakage time, dipping temperature 30 DEG C, afterwards by above embodiment 1 step (5) calcining, its denitration rate can reach 87%.
Embodiment 4
While repeating embodiment 3 to the denitrating catalyst running 22000h, difference is the negative pressure used in (1) is 0.06MPa, clears up, 30 minutes dust suction time to catalyst surface ash while carrying out dust suction with the hairbrush of diameter 3-5mm.(2) use that cleaning fluid cleans catalyst surface and duct, cleaning fluid volume and catalyst volume than is 7:1, cleaning fluid be configured to 0.5 moles of NaOH, 2% penetrating agent JFC-S, the emulsifier op-10 of 0.9%, metal-chelator HEDP, the ultrasonic power of 0.8% are 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, post-drying.(3) use the salpeter solution containing 0.35% lanthanum nitrate and 0.09% cerous nitrate, 3.5% aluminium dihydrogen phosphate of 0.1 mole to flood catalyst, dipping temperature is 30 DEG C, and dip time is after 3 hours, 550 DEG C of calcinings 4 hours after drying.(4) use 2% oxalic acid solution dissolve 0.9% ammonium metavanadate, 5% ammonium tungstate, the ammonium molybdate of 0.35%, the niobium pentaoxide solution of 0.09% active ingredient catalyst is flooded, dip time 3 h immersion temperature 30 DEG C.Afterwards by above embodiment 1 step (5) calcining, its denitration rate can reach 86%.
Embodiment 5
While repeating embodiment 4 to the denitrating catalyst running 24000h, difference is the negative pressure used in step (1) is 0.07MPa, clears up, 30 minutes dust suction time to catalyst surface ash while carrying out dust suction with the hairbrush of diameter 3-5mm.Step (2) uses cleaning fluid to clean catalyst surface and duct, cleaning fluid is configured to 0.5 moles of NaOH, cleaning fluid volume with catalyst volume than being 7:1, penetrating agent JFC-S, the emulsifier op-10 of 1%, metal-chelator HEDP, the ultrasonic power of 0.9% that cleaning fluid is configured to 2% are 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, post-drying.Step (3) uses the salpeter solution containing 0.4% lanthanum nitrate, 0.1% cerous nitrate, 4% aluminium dihydrogen phosphate of 0.1 mole to flood catalyst, and dipping temperature is 30 DEG C, and dip time is 3 hours, 550 DEG C of calcinings 4 hours after drying.The active ingredient of the ammonium metavanadate of the oxalic acid solution dissolving 1% of step (4) use 2%, the ammonium tungstate of 5%, the ammonium molybdate of 0.4%, the niobium pentaoxide solution of 0.1% floods catalyst, dip time 3 h immersion temperature 30 DEG C, afterwards by above embodiment 1 step (5) calcining, its denitration rate can reach 82%.
Embodiment 6
To the denitrating catalyst running 26000h, while repeating embodiment 5, difference is that step (2) uses ultrasonic cleaning solution to clean catalyst surface and duct, cleaning fluid volume and catalyst volume are than being 7:1, cleaning fluid be configured to 0.5 moles of NaOH, 2% penetrating agent JFC-S, the emulsifier op-10 of 1%, metal-chelator HEDP, the ultrasonic power of 1% be 6KW, frequency 40HZ, cleaning temperature 30 DEG C, scavenging period 30 min, post-drying.Step (3) uses the salpeter solution containing 0.4% lanthanum nitrate, 0.1% nitric acid, 4% aluminium dihydrogen phosphate of 0.1 mole to flood catalyst, and dipping temperature is 30 DEG C, and dip time is 3 hours, 550 DEG C of calcinings 4 hours after drying.Carry out active constituent dipping and embodiment 1 step (5) calcining by above embodiment 4 step (4), its denitration rate can reach 85%.
Embodiment data are as following table
Claims (7)
1. a renovation process for denitrating catalyst, is characterized in that being, its method comprises the following steps:
(1) hairbrush cleaning catalyst duct is used while using the negative pressure of 0.05-0.07Mpa to carry out the aspiration of negative pressure to denitration decaying catalyst surface and duct;
(2) cleaning fluid is used to utilize ultrasonic wave to clean catalyst surface and duct;
(3) use 0.1 mole of salpeter solution containing La, Ce rare earth element and aluminium dihydrogen phosphate, impregnated catalyst, while increasing specific surface area of catalyst, within 4 hours, strengthen the mechanical strength of catalyst 550 DEG C of calcinings;
(4) use the oxalic acid solution of 2%, dissolve active ingredient maceration extract containing major catalyst effective ingredient ammonium metavanadate and co-catalyst ammonium tungstate, ammonium molybdate, niobium pentaoxide and the catalyst after reforming is flooded, effective make-up catalyst active constituent;
(5) follow procedure intensification calcining manners is calcined denitrating catalyst at maximum temperature 550 DEG C.
2. the renovation process of a kind of denitrating catalyst according to claim 1, is characterized in that being, described catalyst is the cellular selective reduction catalyst (SCR) that coal-burning power plant's denitration uses.
3. the renovation process of a kind of denitrating catalyst according to claim 1, is characterized in that being, the negative pressure used in described step (1) is 0.05-0.07MPa, while carrying out dust suction, clears up with the hairbrush of diameter 3-5mm catalyst surface ash.
4. the renovation process of a kind of denitrating catalyst according to claim 1, it is characterized in that being, cleaning fluid in described step (2) is made up of following composition: the emulsifier op-10 of the NaOH solution of 0.5 mole, the penetrating agent JFC-S of 1-2%, 0.5-1%, 0.5-1% metal-chelator HEDP, cleaning temperature about 30 DEG C, scavenging period 30 minutes, ultrasonic power are 6KW, supersonic frequency is 40HZ, and cleaning post-baking temperature is 90 DEG C.
5. the renovation process of a kind of denitrating catalyst according to claim 1, it is characterized in that being, 0.1 molar nitric acid solution is used in described step (3), dissolve the catalyst crystalline phases shaping agent of 0.2-0.4%, 0.05-0.1%, crystalline phase stabilizing agent lanthanum nitrate and cerous nitrate, catalyst strength reinforcing agent is 2-4% solid phosphoric acid aluminum dihydrogen, floods regenerated catalyst, and dipping temperature is 30 DEG C, dip time 3 hours, 550 DEG C of calcinings 4 hours after drying.
6. the renovation process of a kind of denitrating catalyst according to claim 1, it is characterized in that being, described step (4) uses the active ingredient maceration extract of the ammonium tungstate of the ammonium metavanadate of the oxalic acid solution of 2% dissolving containing 0.5-1%, 2-5%, the ammonium molybdate of 0.2-0.4%, the niobium pentaoxide of 0.05-0.1% to flood the catalyst after shaping, make-up catalyst active constituent.
7. the renovation process of a kind of denitrating catalyst according to claim 1, it is characterized in that being, in described step (5), calcining heat is temperature programming calcining, calcination process is: 0-120 DEG C of 20min, 120-250 DEG C of 40min, 250-350 DEG C of 60min, 350-450 DEG C 60 min, 450-550 DEG C of 60min, calcines 4 hours for 550 DEG C.
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Cited By (9)
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| CN105289758A (en) * | 2015-10-20 | 2016-02-03 | 清华大学 | Efficient chelating regeneration method for calcium-poisoned denitration catalyst |
| CN105435634A (en) * | 2015-12-14 | 2016-03-30 | 江苏肯创催化剂再生技术有限公司 | Regeneration method for As-poisoned SCR denitration catalyst |
| CN106040317A (en) * | 2016-06-01 | 2016-10-26 | 龙岩紫荆创新研究院 | Method for structure reinforcement and activity recovery of inactivated denitration catalyst and regenerated catalyst |
| CN110102284A (en) * | 2019-05-28 | 2019-08-09 | 清华大学 | It is a kind of fail SCR catalyst regeneration and demercuration method of modifying |
| CN111530508A (en) * | 2020-06-18 | 2020-08-14 | 江苏龙净科杰环保技术有限公司 | Method for regenerating deactivated denitration catalyst containing organic matters |
| CN111715217A (en) * | 2020-07-27 | 2020-09-29 | 江苏龙净科杰环保技术有限公司 | Method for regenerating 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 |
| CN113019471A (en) * | 2021-02-07 | 2021-06-25 | 铜仁市诚一环保科技有限公司 | Cleaning method and equipment for denitration catalyst |
| CN113289609A (en) * | 2021-06-09 | 2021-08-24 | 大唐环境产业集团股份有限公司 | High-wear-resistance wide-temperature denitration catalyst and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105289758A (en) * | 2015-10-20 | 2016-02-03 | 清华大学 | Efficient chelating regeneration method for calcium-poisoned denitration catalyst |
| CN105435634A (en) * | 2015-12-14 | 2016-03-30 | 江苏肯创催化剂再生技术有限公司 | Regeneration method for As-poisoned SCR denitration catalyst |
| CN106040317A (en) * | 2016-06-01 | 2016-10-26 | 龙岩紫荆创新研究院 | Method for structure reinforcement and activity recovery of inactivated denitration catalyst and regenerated catalyst |
| CN106040317B (en) * | 2016-06-01 | 2018-10-02 | 龙岩学院 | Inactivate the method and regenerated catalyst of the enhancing of denitrating catalyst structure and activation recovering |
| CN110102284A (en) * | 2019-05-28 | 2019-08-09 | 清华大学 | It is a kind of fail SCR catalyst regeneration and demercuration method of modifying |
| CN111530508A (en) * | 2020-06-18 | 2020-08-14 | 江苏龙净科杰环保技术有限公司 | Method for regenerating deactivated denitration catalyst containing organic matters |
| CN111715217A (en) * | 2020-07-27 | 2020-09-29 | 江苏龙净科杰环保技术有限公司 | Method for regenerating 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 |
| CN113019471A (en) * | 2021-02-07 | 2021-06-25 | 铜仁市诚一环保科技有限公司 | Cleaning method and equipment for denitration catalyst |
| CN113019471B (en) * | 2021-02-07 | 2023-05-23 | 铜仁市诚一环保科技有限公司 | Method and equipment for cleaning denitration catalyst |
| CN113289609A (en) * | 2021-06-09 | 2021-08-24 | 大唐环境产业集团股份有限公司 | High-wear-resistance wide-temperature denitration catalyst and preparation method and application thereof |
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