CN106000100A - Method for regenerating ineffective SCR catalyst under negative pressure condition - Google Patents
Method for regenerating ineffective SCR catalyst under negative pressure condition Download PDFInfo
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Abstract
The invention discloses a method for regenerating an ineffective SCR catalyst under negative pressure condition. An alkali wash solution, a pickling solution and regenerated liquid more easily reach tiny pores of the catalyst under the negative pressure, so that bound phosphorus and deposited arsenic trioxide in the pores of the catalyst are more thoroughly dissolved, sodium ions, potassium ions and the like bound on acid sites are replaced, V-OH Bronsted acid sites on the surface of the catalyst are basically recovered, the adsorption amount of NH3 of the surface of the catalyst is increased, the Bronsted acid sites and active sites are more quickly and thoroughly regenerated, and the activity of a regenerated SCR denitration catalyst is improved. Multiple catalysts ineffective due to a variety of reasons can be also subjected to comprehensive treatment in actual production, surface deposits of the catalyst can be quickly and thoroughly removed, the catalyst poisoned by acidic and alkaline substances can be quickly and thoroughly washed, the activity of the deactivated catalyst can be efficiently and rapidly restored, and further the service life of the catalyst can be prolonged.
Description
Technical field
The present invention is inefficacy SCR catalyst to be carried out regeneration method, particular by purging, negative-pressure alkali under a kind of condition of negative pressure
Wash, negative pressure pickling, negative pressure washing, the step such as negative pressure active regeneration, inactivation denitrating catalyst is carried out active regeneration.The present invention
Belong to denitrating catalyst technical field.
Background technology
Nitrogen oxides (the NO of coal-burning power plant's dischargeX) it is one of Air Pollutants.On January 1st, 2012 comes into effect
" fossil-fuel power plant atmospheric pollutant emission standard " (GB13223-2011) is to NOXDischarge has had stricter regulation: require portion
The discharge capacity of point new power plant construction nitrogen oxides is less than 100mg/m3, do not reach discharge standard regulation will be according to " charges for disposing pollutants are levied
Receive and use management rules " charge.The most effectively control NOXDischarge has become major issue in current environment protection.
Selective catalytic reduction (SCR) is the control coal-burning power plant discharged nitrous oxides most efficient method generally acknowledged at present, and is catalyzed
Agent is the core of SCR gas denitrifying technology, and its performance decides the denitration efficiency that reaction is final to a great extent.But it leads to
Often being arranged in after boiler economizer before air preheater, catalyst easily blocks, is poisoned, and has a strong impact on its life-span and economy.
SCR catalyst typically constitutes the 30%～40% of initial investment.The catalyst almost all that domestic SCR system uses is by from abroad
Import.Due to easily blocking and poisoning, catalyst in use loses activity unavoidable.If but can be to inactivation catalysis
Agent carries out detection and analyzes its main deactivation cause, and takes corresponding regeneration techniques to make catalyst activity recover and recycling, will
Save the operating cost of more than 3/4, also can reduce the decaying catalyst disposal costs as solid waste, reduce rare earth gold
Belong to the use of (vanadium, tungsten, titanium etc.), save valuable resource, it also avoid the secondary pollution to environment simultaneously.But it is the most domestic
Less for the research of renovation process after catalyst deactivation mechanisms and inactivation.Further research can accelerate drawing of advanced technology
Enter infiltration rate, break the monopolization of external denitrating catalyst technology, lay good for SCR denitration technology in the extensively application of China
Basis.Therefore, the exploitation of catalyst regeneration techniques, in China, there is huge market potential, catalyst regeneration techniques is China
An important new and developing branch in huge gas pollution control engineering.
Summary of the invention
The technical problem to be solved in the present invention is that existing SCR regenerating flue gas denitrifying catalyst technology can not be lost due to many reasons
The catalyst lived carries out quickly integrated treatment up hill and dale, as removed the deposit of surface sediment not the most thoroughly, to by basic species
Matter, acidic materials or neutral substance fouled catalyst can not regenerate the most up hill and dale, provide for this under a kind of condition of negative pressure
Inefficacy SCR catalyst is carried out regeneration method.
The purpose of the present invention can be achieved through the following technical solutions:
Under a kind of condition of negative pressure, inefficacy SCR catalyst is carried out regeneration method, comprises the following steps:
(1) by dry compressed air, inefficacy SCR catalyst is purged；
(2) under airtight subnormal ambient, the catalyst processed through step (1) is placed in the hydrogen-oxygen that concentration is 0.1～0.5mol/L
Change in sodium solution, carry out alkali cleaning；
(3) under airtight subnormal ambient, the catalyst processed through step (2) is placed in 10wt% sulphuric acid and 5wt% Fluohydric acid.
Mixed solution in, carry out pickling；
(4) under airtight subnormal ambient, the catalyst processed through step (3) is put in deionized water, washes, directly
Stable to deionized water intermediate ion concentration；
(5) under airtight subnormal ambient, the catalyst processed through step (4) is immersed in containing 5wt% ammonium metatungstate and 1wt%
In the active mixed solution of ammonium metavanadate, carry out active regeneration；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
In technical solution of the present invention step (1): the pressure of air is 0.6～0.8Mpa, compressed-air actuated flow is 0.6～1.0m3/ s,
Purge time is 0.5～1.0h.This step is for purging the fraction solids granule in catalyst surface and duct and dust.
In technical solution of the present invention step (2): alkali cleaning is to carry out under airtight subnormal ambient, and suction strength is 0.05～0.1Mpa,
The alkali cleaning time is 0.5～1.5h.This step for removing the acidic materials deposited in catalyst surface and duct, as phosphorus pentoxide,
Phosphate, arsenic trioxide, arsenic oxide, sulfur trioxide etc..
In technical solution of the present invention step (3): pickling is to carry out under airtight subnormal ambient, and suction strength is 0.05～0.1Mpa,
Pickling time is 0.5～1.5h.This step is the alkaline matter of deposition in removing catalyst surface and duct, such as sodium oxide, oxygen
Change potassium, calcium sulfate, calcium sulfite, calcium carbonate etc..
In technical solution of the present invention step (4): washing is to carry out under airtight subnormal ambient, and suction strength is 0.05～0.1Mpa,
Washing time is 0.5～1.0h.This step is for removing the metallic sodium ion of catalyst surface precipitation, sulfate ion, Fluohydric acid.
Radical ion etc..
In technical solution of the present invention step (5): described active regeneration is to carry out under airtight subnormal ambient, and suction strength is
0.05～0.1Mpa, the recovery time is 1～2h.This step for being re-added to the table of decaying catalyst by vanadium and tungsten active component
On face and duct.
The principle of the present invention is: the SCR denitration of inefficacy purged, negative pressure alkali cleaning, negative pressure pickling, and negative pressure is washed,
Negative pressure active regeneration, is dried；Alkali wash water, pickle, regenerated liquid under subnormal ambient more accessible in the small duct of catalyst,
Thus more up hill and dale the arsenic trioxide of the phosphorus combined in catalyst duct and deposition is dissolved out, the sodium that will combine on acid site
Ion, potassium ion etc. cement out, and make the V-OH bronsted acid position of catalyst surface substantially recover, increase catalyst surface
NH3Adsorbance so that Bronsted acidic site and avtive spot obtain regenerating the most up hill and dale, improve regeneration SCR take off
The activity of denox catalyst.The catalyst lost efficacy due to many reasons in actual production can also be carried out integrated treatment, reach the fastest
Speed removes catalyst surface deposit up hill and dale, it is also possible to carry out the catalyst after being poisoned by acid and alkali substance the most thoroughly cleaning,
Can the most promptly recover again the activity of decaying catalyst and then extend its service life.Catalyst denitration activity through regeneration
Height, decreases waste catalyst disposal costs and the secondary pollution brought to environment, it is achieved that the reusable edible of resource simultaneously,
Also save the rare earth resources of preciousness.
The invention has the beneficial effects as follows and the catalyst inactivated due to many reasons in actual production process is carried out the most comprehensive
Process, as not thorough, to the catalysis being poisoned by alkaline matter, acidic materials or neutral substance in the deposit of surface sediment is removed
Agent can not regenerate the most up hill and dale, provides the renovation process of a kind of SCR denitration that lost efficacy for this.
Accompanying drawing explanation
Fig. 1 is embodiment 1 regenerated catalyst and fresh catalyst and decaying catalyst carries out expression activitiy figure.
Fig. 2 is embodiment 2 regenerated catalyst and fresh catalyst and decaying catalyst carries out expression activitiy figure.
Fig. 3 is embodiment 3 regenerated catalyst and fresh catalyst and decaying catalyst carries out expression activitiy figure.
Fig. 4 is embodiment 4 regenerated catalyst and fresh catalyst and decaying catalyst carries out expression activitiy figure.
Fig. 5 is embodiment 5 regenerated catalyst and fresh catalyst and decaying catalyst carries out expression activitiy figure.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1: the negative-pressure operation in following steps is all carried out under conditions of suction strength is 0.05Mpa:
(1) with 0.6Mpa, flow 0.6m3/ s is dried the compressed air SCR denitration purging 0.5h to losing efficacy, catalyst
Fraction solids granule and dust in surface and duct purge；
(2) catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.2mol/L, negative pressure alkali cleaning 1h；
(3) catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., negative pressure
Pickling 1h；
(4) catalyst processed through step (3) is put in deionized water, negative pressure washing 0.5h；
(5) catalyst processed through step (4) is immersed in the activity containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate mix
Close in solution, negative pressure active regeneration 1.5h；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
Regenerated catalyst embodiment 1 obtained and fresh catalyst and decaying catalyst carry out expression activitiy test, test knot
Fruit is such as following table:
Substantially get a promotion, because at subnormal ambient from the activity after the operating procedure of embodiment 1 of decaying catalyst seen from upper table
Lower alkali wash water, pickle, deionized water and regenerated liquid, more accessible on the small duct of catalyst, will combine in catalyst duct
Phosphorus and the arsenic trioxide of deposition be dissolved out up hill and dale, the sodium ion that acid site combines, potassium ion etc. are cemented out,
Make Bronsted acid site obtain regenerating the most up hill and dale, also make catalyst add upper vanadium, tungsten activity group the most up hill and dale
Point.
Embodiment 2: the difference of embodiment 2 and embodiment 1 be negative-pressure operation be all to carry out under conditions of suction strength is 0.08Mpa
:
(1) with 0.6Mpa, flow 0.6m3/ s is dried the compressed air SCR denitration purging 0.5h to losing efficacy, catalyst
Fraction solids granule and dust in surface and duct purge；
(2) catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.2mol/L, negative pressure alkali cleaning 1h；
(3) catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., negative pressure
Pickling 1h；
(4) catalyst processed through step (3) is put in deionized water, negative pressure washing 0.5h；
(5) catalyst processed through step (4) is immersed in the activity containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate mix
Close in solution, negative pressure active regeneration 1.5h；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
The catalyst of embodiment 2 and the catalyst of embodiment 1 are carried out expression activitiy, and concrete data see table:
The activity of visible embodiment 2 is slightly above the activity of embodiment 1.
Embodiment 3: the difference of embodiment 3 and embodiment 1 be negative-pressure operation be all to carry out under conditions of suction strength is 0.1Mpa:
(1) with 0.6Mpa, flow 0.6m3/ s is dried the compressed air SCR denitration purging 0.5h to losing efficacy, catalyst
Fraction solids granule and dust in surface and duct purge；
(2) catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.1～0.5mol/L, negative-pressure alkali
Wash 1h；
(3) catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., negative pressure
Pickling 1h；
(4) catalyst processed through step (3) is put in deionized water, negative pressure washing 0.5h；
(5) catalyst processed through step (4) is immersed in the activity containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate mix
Close in solution, negative pressure active regeneration 1.5h；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
The catalyst of embodiment 3 and the catalyst of embodiment 1 are carried out expression activitiy, and concrete data see table:
The activity of visible embodiment 3 is higher than the activity of embodiment 1.
Embodiment 4: the negative-pressure operation in following steps is all carried out under conditions of suction strength is 0.05Mpa:
(1) with 0.7Mpa, flow 0.8m3/ s is dried the compressed air SCR denitration purging 0.5h to losing efficacy, catalyst
Fraction solids granule and dust in surface and duct purge；
(2) catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.2mol/L, negative pressure alkali cleaning 1h；
(3) catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., negative pressure
Pickling 1h；
(4) catalyst processed through step (3) is put in deionized water, negative pressure washing 0.5h；
(5) catalyst processed through step (4) is immersed in the activity containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate mix
Close in solution, negative pressure active regeneration 1.5h；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
The catalyst of embodiment 4 and the catalyst of embodiment 1 are carried out expression activitiy, and concrete data see table:
The activity of visible embodiment 4 is slightly above the activity of embodiment 1.
Embodiment 5: the negative-pressure operation in following steps is all carried out under conditions of suction strength is 0.05Mpa:
(1) with 0.8Mpa, flow 1.0m3/ s is dried the compressed air SCR denitration purging 0.5h to losing efficacy, catalyst
Fraction solids granule and dust in surface and duct purge；
(2) catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.2mol/L, negative pressure alkali cleaning 1h；
(3) catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., negative pressure
Pickling 1h；
(4) catalyst processed through step (3) is put in deionized water, negative pressure washing 0.5h；
(5) catalyst processed through step (4) is immersed in the activity containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate mix
Close in solution, negative pressure active regeneration 1.5h；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss
Calcining 3h.
The catalyst of embodiment 5 and the catalyst of embodiment 4 are carried out expression activitiy, and concrete data see table:
The activity of visible embodiment 5 is slightly above the activity of embodiment 4.
Claims (6)
1. under a condition of negative pressure, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: comprise the following steps:
(1) by dry compressed air, inefficacy SCR catalyst is purged；
(2) under airtight subnormal ambient, the catalyst processed through step (1) is placed in the sodium hydroxide solution that concentration is 0.1 ~ 0.5mol/L, carries out alkali cleaning；
(3) under airtight subnormal ambient, the catalyst processed through step (2) is placed in the mixed solution of 10wt% sulphuric acid and 5wt% Fluohydric acid., carries out pickling；
(4) under airtight subnormal ambient, the catalyst processed through step (3) is put in deionized water, washes, until deionized water intermediate ion concentration is stable；
(5) under airtight subnormal ambient, the catalyst processed through step (4) is immersed in the active mixed solution containing 5wt% ammonium metatungstate and 1wt% ammonium metavanadate, carries out active regeneration；
(6) catalyst processed through step (5) is put in the KSL box high temperature sintering furnace of series, under 300 DEG C of temperature conditionss, calcine 3h.
Under condition of negative pressure the most according to claim 1, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: in step (1), compressed-air actuated pressure is 0.6 ~ 0.8Mpa, and compressed-air actuated flow is 0.6 ~ 1.0m3/ s, purge time is 0.5 ~ 1.0h.
Under condition of negative pressure the most according to claim 1, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: in described step (2), its suction strength is 0.05 ~ 0.1Mpa, and the alkali cleaning time is 0.5 ~ 1.5h.
Under condition of negative pressure the most according to claim 1, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: in described step (3), its suction strength is 0.05 ~ 0.1Mpa, and pickling time is 0.5 ~ 1.5h.
Under condition of negative pressure the most according to claim 1, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: in described step (4), its suction strength is 0.05 ~ 0.1Mpa, and washing time is 0.5 ~ 1.0h.
Under condition of negative pressure the most according to claim 1, inefficacy SCR catalyst is carried out regeneration method, it is characterised in that: in described step (5), its suction strength is 0.05 ~ 0.1Mpa, and the recovery time is 1 ~ 2h.
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Cited By (5)
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| CN106480320A (en) * | 2016-11-23 | 2017-03-08 | 河钢股份有限公司承德分公司 | A kind of method for reclaiming valuable metal from discarded SCR denitration |
| CN106799265A (en) * | 2017-02-20 | 2017-06-06 | 武汉大学 | A kind of method that positive/negative-pressure alternately changes regeneration of deactivated SCR catalyst |
| CN106861772A (en) * | 2017-02-13 | 2017-06-20 | 武汉大学 | A kind of negative pressure combination ultrasonic wave carries out regeneration method to inactivation SCR 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 |
| CN113477083A (en) * | 2021-07-05 | 2021-10-08 | 国家电投集团远达环保催化剂有限公司 | Regeneration method of inactivated denitration dedusting ceramic tube |
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| CN106480320A (en) * | 2016-11-23 | 2017-03-08 | 河钢股份有限公司承德分公司 | A kind of method for reclaiming valuable metal from discarded SCR denitration |
| CN106861772A (en) * | 2017-02-13 | 2017-06-20 | 武汉大学 | A kind of negative pressure combination ultrasonic wave carries out regeneration method to inactivation SCR denitration catalyst |
| CN106799265A (en) * | 2017-02-20 | 2017-06-06 | 武汉大学 | A kind of method that positive/negative-pressure alternately changes regeneration of deactivated SCR 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 |
| CN113477083A (en) * | 2021-07-05 | 2021-10-08 | 国家电投集团远达环保催化剂有限公司 | Regeneration method of inactivated denitration dedusting ceramic tube |
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