CN108014818A - The regeneration technology of denitrating catalyst - Google Patents

The regeneration technology of denitrating catalyst Download PDF

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Publication number
CN108014818A
CN108014818A CN201711347216.5A CN201711347216A CN108014818A CN 108014818 A CN108014818 A CN 108014818A CN 201711347216 A CN201711347216 A CN 201711347216A CN 108014818 A CN108014818 A CN 108014818A
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China
Prior art keywords
catalyst
denitrating catalyst
vanadium
tungsten
regeneration
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CN201711347216.5A
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Chinese (zh)
Inventor
张涛
何伟
陈春兴
赖晓清
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江苏龙净科杰催化剂再生有限公司
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Priority to CN201711347216.5A priority Critical patent/CN108014818A/en
Publication of CN108014818A publication Critical patent/CN108014818A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/90Regeneration or reactivation
    • B01J23/92Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/48Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/60Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids
    • B01J38/62Liquid treating or treating in liquid phase, e.g. dissolved or suspended using acids organic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00Regeneration or reactivation of catalysts, in general
    • B01J38/48Liquid treating or treating in liquid phase, e.g. dissolved or suspended
    • B01J38/68Liquid treating or treating in liquid phase, e.g. dissolved or suspended including substantial dissolution or chemical precipitation of a catalyst component in the ultimate reconstitution of the catalyst

Abstract

The invention discloses a kind of regeneration technology of denitrating catalyst, include the following steps:1)Inactivate denitrating catalyst pretreatment;2)Active material vanadium oxide and tungsten oxide are obtained into regeneration denitrating catalyst on inactivation denitrating catalyst using atomic layer deposition method;The mass percentage for regenerating vanadium oxide in denitrating catalyst is 0.1~0.5%, and the mass percentage of tungsten oxide is 0.3~1%.The regeneration technology of denitrating catalyst of the present invention, using technique for atomic layer deposition supplement activity material, active material is adsorbed inside and outside catalyst duct, and the active force between decaying catalyst is strong, and is evenly distributed in the catalyst;The amount of supplement activity material, the active material vanadium oxide and tungsten oxide controllable precise of implantation can also be regulated and controled by controlling atomic deposition number.

Description

The regeneration technology of denitrating catalyst

Technical field

The present invention relates to denitrating catalyst regeneration field, and in particular to a kind of regeneration technology of denitrating catalyst.

Background technology

As the important component of coal-burning power plant's denitrating system, denitrating catalyst expense occupies denitration total investment of engineering Nearly 40% ratio.Therefore, by taking the regeneration measure of denitrating catalyst, denitrating catalyst circulation comprehensive is improved using effect Rate, becomes the breach for reducing coal fired thermal power plant denitration operating cost.

Denitrating catalyst regeneration is the reason for inactivation by analysis of catalyst, takes corresponding process means to eliminate catalyst Inactivation factor, the inactivation denitrating catalyst activity recovery and selectivity made, is reused.Chinese patent CN201210100560.5 In catalyst the being impregnated in property replenisher cleaned, active supplement, drying will be carried out;Finally, the complete catalyst of drying is carried out Roasting, obtains regenerated denitrating catalyst.Chinese patent CN 201410165148.0 is that the catalyst after cleaning is impregnated in grass Sour vanadyl, cerous nitrate, lanthanum nitrate, copper nitrate active liquid in 25~take out after forty minutes, denitrification catalyst module is dried Dry drying.All it is that active supplement is carried out using general infusion process above, can exists in actually producing in batches and can not accurately control Active matter quality, causes that denitration efficiency is unstable, SO2Oxidation is high, high-temperature calcination improves production cost and is catalyzed in regenerative process The problem of agent damages.

The content of the invention

It is an object of the invention to provide a kind of regeneration technology of denitrating catalyst, is supplemented and lived using technique for atomic layer deposition Property material, active material adsorbed inside and outside catalyst duct, and the active force between decaying catalyst is strong, and in the catalyst It is evenly distributed;The amount of supplement activity material, the active material vanadium oxide and oxygen of implantation can also be regulated and controled by controlling atomic deposition number Change tungsten controllable precise, and inhibitory activity material sinters, and then denitration efficiency height, SO are realized in denitration reaction2Oxygenation efficiency is low, and Regenerated catalyst is without calcination processing, and whole process is to catalyst not damaged.

To achieve the above object, the technical scheme is that designing a kind of regeneration technology of denitrating catalyst, including such as Lower step:1)Inactivate denitrating catalyst pretreatment;2)Using atomic layer deposition method by active material vanadium oxide and tungsten oxide in mistake On denitrating catalyst living, regeneration denitrating catalyst is obtained;Regenerate the mass percentage of vanadium oxide in denitrating catalyst for 0.1~ 0.5%, the mass percentage of tungsten oxide is 0.3~1%.

Preferably, the regeneration technology of the denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.05~0.1% lactic acid, 0.10~0.20% oxalic acid, with 20~40HZ ultrasounds 30 ~60min, takes out after 120~150 DEG C of dry 30~90min;

2)Atomic layer deposition method is implanted into active material:By step 1)Catalyst after processing inserts the reaction of atomic layer deposition apparatus In chamber, reaction chamber is sealed;High pure nitrogen is passed through after being vacuumized in atomic layer deposition system, adjusting reaction chamber outlet valve makes chamber Interior pressure is in negative pressure, and depositing temperature is set in 300~400 DEG C;Vanadium tungsten mixing presoma, injection length are injected into reaction chamber Control in 150~300s, then pass to inert gas flushing, washing time is controlled in 30~60s;Cyclic deposition 3~5 times, obtains To regeneration denitrating catalyst.

Preferably, in the vanadium tungsten mixing presoma vanadium presoma for three isopropyl oxygen alcohol vanadium, three isopropoxy vanadium oxides, Any one in acetylacetone,2,4-pentanedione vanadium oxide.

Preferably, the presoma of tungsten is isopropanol tungsten, in ethanol tungsten, dichloro tungstocene in the vanadium tungsten mixing presoma Any one.

The advantages of the present invention are:A kind of regeneration technology of denitrating catalyst is provided, using atomic layer deposition Product technique complementary active material, active material is adsorbed inside and outside catalyst duct, and the active force between decaying catalyst is strong, And it is evenly distributed in the catalyst;The amount of supplement activity material, the active matter of implantation can also be regulated and controled by controlling atomic deposition number Matter vanadium oxide and tungsten oxide controllable precise, and inhibitory activity material sinters, so realize in denitration reaction denitration efficiency it is high, SO2Oxygenation efficiency is low, and regenerated catalyst, without calcination processing, whole process is to catalyst not damaged.

Embodiment

With reference to embodiment, the embodiment of the present invention is further described.Following embodiments are only used for more Add and clearly demonstrate technical scheme, and be not intended to limit the protection scope of the present invention and limit the scope of the invention.

In following embodiment, the content of vanadium for inactivating denitrating catalyst is 0.568%, W content 4.284%(X-ray is glimmering Light analyzer method, it is rear same), according to regenerated catalyst Active pharmaceutical, catalyst content of vanadium increase by 0.15%, W content increase by 0.3%.

Embodiment 1

The regeneration technology of denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.05% lactic acid, 0.10% oxalic acid, with 20HZ ultrasound 30min, is taken out after 120 DEG C dry 90min;

2)Atomic layer deposition method is implanted into active material:By step 1)Catalyst after processing inserts the reaction of atomic layer deposition apparatus In chamber, reaction chamber is sealed;High pure nitrogen is passed through after being vacuumized in atomic layer deposition system, adjusting reaction chamber outlet valve makes chamber Interior pressure is in negative pressure, and depositing temperature is set in 300 DEG C;Three isopropoxy vanadium oxides are injected into reaction chamber, isopropanol tungsten mixes Presoma is closed, injection length is controlled in 150s, then passes to inert gas flushing, and washing time is controlled in 60s;Cyclic deposition 5 It is secondary, obtain regeneration denitrating catalyst.

Embodiment 2

The regeneration technology of denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.1% lactic acid, 0.20% oxalic acid, with 40HZ ultrasound 60min, is taken out after 150 DEG C dry 30min;

2)Atomic layer deposition method is implanted into active material:By step 1)Catalyst after processing inserts the reaction of atomic layer deposition apparatus In chamber, reaction chamber is sealed;High pure nitrogen is passed through after being vacuumized in atomic layer deposition system, adjusting reaction chamber outlet valve makes chamber Interior pressure is in negative pressure, and depositing temperature is set in 400 DEG C;Three isopropyl oxygen alcohol vanadium, ethanol tungsten mixing forerunner are injected into reaction chamber Body, injection length are controlled in 300s, then pass to inert gas flushing, and washing time is controlled in 30s;Cyclic deposition 3 times, obtains Regenerate denitrating catalyst.

Embodiment 3

The regeneration technology of denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.08% lactic acid, 0.15% oxalic acid, with 28HZ ultrasound 45min, is taken out after 140 DEG C dry 60min;

2)Atomic layer deposition method is implanted into active material:By step 1)Catalyst after processing inserts the reaction of atomic layer deposition apparatus In chamber, reaction chamber is sealed;High pure nitrogen is passed through after being vacuumized in atomic layer deposition system, adjusting reaction chamber outlet valve makes chamber Interior pressure is in negative pressure, and depositing temperature is set in 350 DEG C;Acetylacetone,2,4-pentanedione vanadium oxide is injected into reaction chamber, dichloro tungstocene mixes Presoma is closed, injection length is controlled in 200s, then passes to inert gas flushing, and washing time is controlled in 45s;Cyclic deposition 4 It is secondary, obtain regeneration denitrating catalyst.

Comparative example 1

Infusion process regenerates denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.05% lactic acid, 0.10% oxalic acid, with 20HZ ultrasound 30min, is taken out after 120 DEG C dry 90min;

2)Infusion process is implanted into active material:By step 1)Catalyst after processing is impregnated in ammonium metavanadate, ammonium metatungstate aqueous solution In, after impregnating 750s, 60 DEG C of oven drying 12h are transferred to, then 6h is calcined under 300 DEG C of air atmospheres, obtain regeneration denitration catalyst Agent.

Comparative example 2

Infusion process regenerates denitrating catalyst, comprises the following specific steps that:

1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.05% lactic acid, 0.10% oxalic acid, with 20HZ ultrasound 30min, is taken out after 120 DEG C dry 90min;

2)Infusion process is implanted into active material:By step 1)Catalyst after processing is impregnated in ammonium metavanadate, ammonium metatungstate aqueous solution In, after bubbling dipping 750s, 60 DEG C of oven drying 12h are transferred to, then 6h is calcined under 300 DEG C of air atmospheres, obtain regeneration denitration Catalyst.

Regenerate the performance test of denitration denitrating catalyst

By the regeneration denitration denitrating catalyst obtained by embodiment 1~3, comparative example 1~2 according to GBT 31587-2015《Honeycomb Formula catalyst for denitrating flue gas》The denitration efficiency and Activity determination standard of middle requirement, detection denitration efficiency, activity and chemical composition contain Amount;Test condition is:NO 500ppm, NH3500ppm, O210%, SO2 1000ppm, N2For Balance Air, air speed 3500h-1, 380 DEG C of detection temperature, 20 × 20 hole of catalyst, length 500mm.Testing result is as shown in table 1.

Denitration efficiency, activity and the chemical composition content of 1 SCR denitration of table

As it can be seen from table 1 the obtained regeneration denitrating catalyst of embodiment 1~3 is substantially better than the obtained regeneration of comparative example 1~2 Denitrating catalyst, the obtained regeneration denitrating catalyst denitration efficiency of embodiment 1~3 and activity raising are more notable, and pass through inspection Chemical composition content in denitrating catalyst after survey regeneration, it is more smart that embodiment 1~3 regenerates denitrating catalyst chemical composition load capacity Really, than the SO of comparative example 1~22Oxygenation efficiency is reduced and become apparent;It can be seen that through atomic layer deposition method regeneration denitrating catalyst denitration effect Rate, activity are all significantly improved, active material vanadium tungsten load amount controllable precise.

Present invention regeneration denitrating catalyst not only increases denitration efficiency and activity, also reduces SO2Oxygenation efficiency, accurate control Active material load capacity processed, reduces production cost.Therefore, denitrating catalyst renovation process of the present invention, can effectively prolong The service life of long denitrating catalyst, ensures higher denitration effect and low SO2Oxygenation efficiency, has great economic value.

The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, some improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (4)

1. the regeneration technology of denitrating catalyst, it is characterised in that include the following steps:1)Inactivate denitrating catalyst pretreatment;2) Active material vanadium oxide and tungsten oxide are obtained into regeneration denitration catalyst on inactivation denitrating catalyst using atomic layer deposition method Agent;The mass percentage for regenerating vanadium oxide in denitrating catalyst is 0.1~0.5%, and the mass percentage of tungsten oxide is 0.3 ~1%.
2. the regeneration technology of denitrating catalyst according to claim 1, it is characterised in that comprise the following specific steps that:
1)Inactivate denitrating catalyst pretreatment:The dust on de-inactivation denitrating catalyst surface is removed by the aspiration of negative pressure device, then will Catalyst is immersed in the deionized water solution for including 0.05~0.1% lactic acid, 0.10~0.20% oxalic acid, with 20~40HZ ultrasounds 30 ~60min, takes out after 120~150 DEG C of dry 30~90min;
2)Atomic layer deposition method is implanted into active material:By step 1)Catalyst after processing inserts the reaction of atomic layer deposition apparatus In chamber, reaction chamber is sealed;High pure nitrogen is passed through after being vacuumized in atomic layer deposition system, adjusting reaction chamber outlet valve makes chamber Interior pressure is in negative pressure, and depositing temperature is set in 300~400 DEG C;Vanadium tungsten mixing presoma, injection length are injected into reaction chamber Control in 150~300s, then pass to inert gas flushing, washing time is controlled in 30~60s;Cyclic deposition 3~5 times, obtains To regeneration denitrating catalyst.
3. the regeneration technology of denitrating catalyst according to claim 2, it is characterised in that in the vanadium tungsten mixing presoma The presoma of vanadium is any one in three isopropyl oxygen alcohol vanadium, three isopropoxy vanadium oxides, acetylacetone,2,4-pentanedione vanadium oxide.
4. the regeneration technology of denitrating catalyst according to claim 3, it is characterised in that in the vanadium tungsten mixing presoma The presoma of tungsten is any one in isopropanol tungsten, ethanol tungsten, dichloro tungstocene.
CN201711347216.5A 2017-12-15 2017-12-15 The regeneration technology of denitrating catalyst CN108014818A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108893624A (en) * 2018-06-20 2018-11-27 江苏龙净科杰环保技术有限公司 The recovery system and recovery method of recovery Pd tungsten powder from useless SCR catalyst

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CN104888869A (en) * 2015-06-12 2015-09-09 河南博苑新未来环保科技有限公司 Waste flue gas denitration catalyst regeneration method and equipment
CN105749864A (en) * 2016-04-13 2016-07-13 西安近代化学研究所 Preparation method of high-specific-area magnetic adsorbent or magnetic catalyst support
CN106000409A (en) * 2016-05-19 2016-10-12 陕西师范大学 Iron-base composite oxide catalyst for producing styrene by CO2 oxidative dehydrogenation of ethylbenzene
CN106669864A (en) * 2016-12-27 2017-05-17 环境保护部华南环境科学研究所 Method for recycling and regenerating invalid denitration catalyst
CN106861683A (en) * 2015-12-10 2017-06-20 中国科学院大连化学物理研究所 A kind of Ru bases catalyst and its in CO2Application in methanation

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103949291A (en) * 2014-04-23 2014-07-30 江苏万德环保科技有限公司 Denitration catalyst regeneration solution and preparation method thereof as well as catalyst regeneration method
CN104888869A (en) * 2015-06-12 2015-09-09 河南博苑新未来环保科技有限公司 Waste flue gas denitration catalyst regeneration method and equipment
CN106861683A (en) * 2015-12-10 2017-06-20 中国科学院大连化学物理研究所 A kind of Ru bases catalyst and its in CO2Application in methanation
CN105749864A (en) * 2016-04-13 2016-07-13 西安近代化学研究所 Preparation method of high-specific-area magnetic adsorbent or magnetic catalyst support
CN106000409A (en) * 2016-05-19 2016-10-12 陕西师范大学 Iron-base composite oxide catalyst for producing styrene by CO2 oxidative dehydrogenation of ethylbenzene
CN106669864A (en) * 2016-12-27 2017-05-17 环境保护部华南环境科学研究所 Method for recycling and regenerating invalid denitration catalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108893624A (en) * 2018-06-20 2018-11-27 江苏龙净科杰环保技术有限公司 The recovery system and recovery method of recovery Pd tungsten powder from useless SCR catalyst

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