CN104162456B - A kind of cleaning fluid for denitrating catalyst regeneration and cleaning method - Google Patents
A kind of cleaning fluid for denitrating catalyst regeneration and cleaning method Download PDFInfo
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- CN104162456B CN104162456B CN201410383383.5A CN201410383383A CN104162456B CN 104162456 B CN104162456 B CN 104162456B CN 201410383383 A CN201410383383 A CN 201410383383A CN 104162456 B CN104162456 B CN 104162456B
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Abstract
The invention discloses a kind of cleaning fluid for denitrating catalyst regeneration, comprise cleaning solution and cushioning liquid, cleaning solution take deionized water as solvent, add the Polyoxyethylene Ether Nonionic Surfactant of the selective heavy metal chelating agent HMCA-1 and 0.01 ~ 1% of 1 ~ 10%, cushioning liquid is hydrogen phthalate ammonium-dilution heat of sulfuric acid, hexa-sulfuric acid solution, sulfuric acid-ammonium sulfate, phosphoric acid-ammonium dibasic phosphate solution or oxalic acid-ammonium oxalate solution, the invention also discloses the method utilizing above-mentioned cleaning fluid to clean spent catalyst.The present invention adopts heavy metal chelating agent HMCA-1 to have the effect of the arsenic, mercury, calcium, beryllium, barium, magnesium, iron etc. optionally catching dead catalyst surface, simultaneous buffering solution substantially increases the quantity of the sour position of SCR catalyst Bronsted, make the ammonium metavanadate that only need add small amount in follow-up regenerated liquid, reduce costs.
Description
Technical field
The present invention relates to denitrating catalyst (SCR) technical field of regeneration, the cleaning fluid of particularly coal-burning power plant's denitrating catalyst regeneration and cleaning method.
Background technology
The exposure draft that national environmental protection portion externally discloses " waste flue gas denitration catalyst regeneration and process guide ", suggestion original text particularly points out: spent catalyst should adopt regeneration techniques to regenerate as much as possible, and the spent catalyst that cannot regenerate can carry out landfill by the requirement of " hazardous waste security landfill Environmental capacity standard " (GB-8598).Encourage high performance catalyst raw material, new catalyst, the regeneration of spent catalyst and the development and application of safe disposal technology.Under normal circumstances, a 300MW unit, complete after " 2+1 " arrange loading catalyst, annual dead catalyst is 100m3, land-fill method is adopted to cause environmental pollution, and making catalyst return to the 95-100% of original activity by the mode of regeneration, catalyst can reuse, and cost is only the 40-50% changing fresh catalyst cost.Therefore, the regeneration of exploitation denitrating catalyst both can reduce the production cost of enterprise's SCR denitration system, met again the industrial policy of country.
Cause the factor of denitrating catalyst inactivation a lot, mainly contain following three types:
(1) alkali metal in catalyst poisoning inactivation-flying dust mainly comprises these two kinds of materials of Na and K, under aqueous solution ionic condition, catalyst deep layer can be penetrated into, directly and catalyst and catalyst activity substance reaction, make catalyst acid position poisoning, to reduce it to NH
3degree of absorption and adsorption activity, then reduce the activity of catalyst.
(2) sintering deactivation-catalyst of catalyst runs for a long time and causes sintering of catalyst under excessive temperature (more than 450 DEG C) flue gas, catalytic inner duct can be caused to lose, in micropore, pore size distribution reduces, overall specific area declines, thus the area that lost part contacts with reacting gas, cause the decline of catalyst activity.
(3) the blocking inactivation-in running of catalyst, the hole plug that the ammonium salt in flue gas and flying dust granule cause and duct blocking.
At present, according to the deactivation cause of denitrating catalyst and the complexity of regeneration, summing up now main renovation process has: oxidation is made charcoal, purges, is aspirated, acid-alkali washing, solvent extraction, selection complexing water law, dipper precipitation, again shaping, acid-base function, oxidation renewal etc.Number of patent application is 201210100560.5 disclose and clean denitrating catalyst as cleaning fluid with the dilute sulfuric acid of 0.018mol/L ~ 3mol/L; Number of patent application is 201210512916.6 disclose and clean denitrating catalyst as cleaning fluid with the HF of 0.01mol/L ~ 0.02mol/L; Number of patent application is that in 201210491287.3, the dilute sulfuric acid disclosed with 1% cleans denitrating catalyst as cleaning fluid; Number of patent application is disclose in 201310331661.8 to clean denitrating catalyst as cleaning fluid with the concentrated sulfuric acid or red fuming nitric acid (RFNA).
Above-mentioned patent when cleaning useless denitrating catalyst, these strong acid can and the active component V of catalyst
2o
5there is strong chemical reaction, make V
2o
5be converted into VOSO
4, thus make about 50%V
2o
5washed away, cause the catalyst activity after regeneration very low.Week, institute was known, V
2o
5with carrier TiO
2interact and the Bronsted acid position that generates is the activated centre of denitrating catalyst.Above-mentioned cleaning method can make the quantity of position, activated centre greatly reduce, thus affects the denitration activity of regenerated catalyst, and further shorten the life-span of catalyst.Even if supplement active component presoma again in follow-up: ammonium metavanadate, metatungstic acid sodium.The market price of presoma ammonium metavanadate and ammonium metatungstate is higher, is the principal element affecting SCR catalyst regeneration cost, therefore supplements the regeneration cost that active material significantly can increase catalyst, too increases the complexity of regeneration technology operation simultaneously; In addition, in the cleaning and regeneration liquid of publication, mainly for K, Na(alkali metal) and the removal of alkali metal Ca, Ba, Be, Cs, Ms, seldom there is the cleaning of the denitrating catalyst for arsenic poisoning, lead poisoning and phosphorism and mercury poisoning.
Summary of the invention
Technical problem to be solved by this invention is that the drawback existed for denitrating catalyst regeneration in background technology provides a kind of cleaning fluid for denitrating catalyst regeneration and cleaning method, significantly can increase the quantity in SCR catalyst activated centre, improve the life-span of SCR catalyst, removing blocking simultaneously arsenic, lead and mercury on a catalyst.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of cleaning fluid for denitrating catalyst regeneration, comprise for removing blocking arsenic on a catalyst, the cushioning liquid that cleaning solution that is plumbous and mercury increases with maintenance active acid bit quantity, wherein cleaning solution take deionized water as solvent, with the quality of deionized water for benchmark, add the Polyoxyethylene Ether Nonionic Surfactant of the selective heavy metal chelating agent HMCA and 0.01 ~ 1% of 1 ~ 10%, cushioning liquid is hydrogen phthalate ammonium-dilution heat of sulfuric acid, hexa-sulfuric acid solution, sulfuric acid-ammonium sulfate, phosphoric acid-ammonium dibasic phosphate solution or oxalic acid-ammonium oxalate solution.
In described hydrogen phthalate ammonium-dilution heat of sulfuric acid, hydrogen phthalate ammonium is 3:50 ~ 60 with the ratio of the amount of substance of dilute sulfuric acid, in described hexa-sulfuric acid solution, hexa is 1:260 ~ 270 with the ratio of the amount of substance of sulfuric acid, in described sulfuric acid-ammonium sulfate, sulfuric acid is 2 ~ 5:1 with the ratio of the amount of substance of ammonium sulfate, in described phosphoric acid-ammonium dibasic phosphate solution, phosphoric acid is 3 ~ 5:1 with the ratio of the amount of substance of diammonium hydrogen phosphate, and described oxalic acid-ammonium oxalate solution mesoxalic acid is 2 ~ 4:1 with the ratio of the amount of substance of ammonium oxalate.
The pH value of described cushioning liquid is 4.0 ~ 5.5.
For the method for the cleaning fluid cleaning denitrating catalyst of denitrating catalyst regeneration, step is as follows: get inactivation denitrating catalyst, with high-pressure washing 3 ~ 5 times, then uses cleaning solution and the ultrasonic immersion 0.1 ~ 6h of cushioning liquid successively.
Beneficial effect of the present invention: (1) the present invention adopts representative nonionic surface active agent to have excellent biological degradability, is conducive to the sustainable development of environment; (2) the present invention adopts heavy metal chelating agent HMCA-1 to have the effect of the arsenic, mercury, calcium, beryllium, barium, magnesium, iron etc. optionally catching dead catalyst surface, does not have seizure effect to vanadium, tungsten and titanium; (3) the present invention can reduce regeneration cost greatly, it is the ammonium metavanadate that only need add small amount in follow-up regenerated liquid, in same kind deactivated situation, the addition of ammonium metavanadate reduces 30%, dead catalyst just can be made to reach the denitration efficiency of initial 95-105%, owing to decreasing regenerated liquid use amount, therefore shorten regeneration dip time, so to keeping the intensity of catalyst to have very large protective effect; (4) the present invention utilizes and first washes again by the operation sequence that cushioning liquid rinses, and additional Ultrasonic Cleaning, so the effect reaching good ash disposal, removing heavy metals.Cushioning liquid used is easy to obtain Bronsted acid, substantially increases the quantity of the sour position of SCR catalyst Bronsted.Bronsted acid number of acid sites can pass through temperature programmed desorption (TPD) and calculate.Utilize cleaning fluid of the present invention and cleaning method, the number of acid sites calculated by TPD can reach more than 10 times of the number of acid sites of fresh SCR catalyst, relative to spent catalyst, the catalyst acid bit quantity after cleaning can improve 15 ~ 20 times, thus reaches the object in extending catalyst life-span.
Detailed description of the invention
Embodiment 1
In cleaning device, preparation cleaning solution: be solvent with deionized water, add 0.5wt% surfactant polyoxyethylene ether and the selective heavy metal chelating agent HMCA-1 of 5wt%; Cushioning liquid is hydrogen phthalate ammonium-dilute sulfuric acid, and compound method is that the dilute sulfuric acid being 0.1mol/L 25.0mL concentration be 0.2mol/L hydrogen phthalate ammonium salt solution and 800mL concentration mixes, and being diluted with water to pH value is 4.5; Cleaning method is washed with cleaning composition according to first washing again, the operation sequence that last acidic buffer solution rinses, namely high pressure de-ionized water washes 3 times, then in the ultrasonic equipment that cleaning solution is housed, cleans 0.1h, finally in the ultrasonic equipment that acidic buffer solution is housed, cleans 6h.The heavy metal chelating agent that selective heavy metal chelating agent HMCA-1 selects Su Jing Environmental Protection Technology Co., Ltd of Suzhou City to produce.
Embodiment 2
In cleaning device, preparation cleaning solution: be solvent with deionized water, add 0.01wt% surfactant polyoxyethylene ether and the selective heavy metal chelating agent HMCA-1 of 1wt%; Cushioning liquid is oxalic acid-ammonium oxalate, and compound method is that the ammonium oxalate being 0.1mol/L 25.0mL concentration be 0.2mol/L oxalic acid solution and 17.5mL concentration mixes, and being diluted with water to pH value is 5.5; Cleaning method is washed with cleaning solution according to first washing again, the operation sequence that last acidic buffer solution rinses, namely high pressure de-ionized water washes 4 times, then in the ultrasonic equipment that cleaning solution is housed, cleans 6h, finally in the ultrasonic equipment that acidic buffer solution is housed, cleans 0.1h.The heavy metal chelating agent that selective heavy metal chelating agent HMCA-1 selects Su Jing Environmental Protection Technology Co., Ltd of Suzhou City to produce.
Embodiment 3
In cleaning device, preparation cleaning solution: be solvent with deionized water, add 1wt% surfactant polyoxyethylene ether and the selective heavy metal chelating agent HMCA-1 of 10wt%; Cushioning liquid is hexa-sulfuric acid, and compound method is: in 200mL water, dissolve hexa 40g, and adding concentration is 0.1mol/L dilute sulfuric acid 10mL, then to be diluted with water to pH value be 5; Cleaning method is washed with cleaning solution according to first washing again, the operation sequence that last acidic buffer solution rinses, namely high pressure de-ionized water washes 5 times, then in the ultrasonic equipment that cleaning solution is housed, cleans 1h, finally in the ultrasonic equipment that acidic buffer solution is housed, cleans 5h.The heavy metal chelating agent that selective heavy metal chelating agent HMCA-1 selects Su Jing Environmental Protection Technology Co., Ltd of Suzhou City to produce.
Embodiment 4
In cleaning device, preparation cleaning solution: be solvent with deionized water, add 0.05wt% surfactant polyoxyethylene ether and the selective heavy metal chelating agent HMCA-1 of 6wt%; Cushioning liquid is ammonium dihydrogen phosphate (ADP)-phosphoric acid, and compound method is: the phosphoric acid be ammonium dihydrogen phosphate and the 12.6mL concentration of 0.2mol/L 25.0mL concentration being 0.1mol/L mixes, and being diluted with water to pH value is 4.5; Cleaning method is washed with cleaning solution according to first washing again, the operation sequence that last acidic buffer solution rinses, namely high pressure de-ionized water washes 3 times, then in the ultrasonic equipment that cleaning solution is housed, cleans 2h, finally in the ultrasonic equipment that acidic buffer solution is housed, cleans 4h.The heavy metal chelating agent that selective heavy metal chelating agent HMCA-1 selects Su Jing Environmental Protection Technology Co., Ltd of Suzhou City to produce.
Embodiment 5
In cleaning device, preparation cleaning solution: be solvent with deionized water, add 0.5wt% surfactant polyoxyethylene ether and the selective heavy metal chelating agent HMCA-1 of 5wt%; Cushioning liquid is sulfuric acid-ammonium sulfate, and compound method is that the dilute sulfuric acid being 0.15mol/L 25.0mL concentration be 0.2mol/L this dioctyl phthalate of neighbour hydrogen ammonium salt solution and 30.0mL concentration mixes, and being diluted with water to pH value is 4.0; Cleaning method is washed with cleaning solution according to first washing again, the operation sequence that last acidic buffer solution rinses, namely high pressure de-ionized water washes 5 times, then in the ultrasonic equipment that cleaning solution is housed, cleans 0.5h, finally in the ultrasonic equipment that acidic buffer solution is housed, cleans 1h.The heavy metal chelating agent that selective heavy metal chelating agent HMCA-1 selects Su Jing Environmental Protection Technology Co., Ltd of Suzhou City to produce.
Embodiment 6
The cushioning liquid of the present embodiment is hydrogen phthalate ammonium-dilution heat of sulfuric acid, and pH value is 4.5, and wherein hydrogen phthalate ammonium is 3:50 with the ratio of the amount of substance of dilute sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 1.
Embodiment 7
The cushioning liquid of the present embodiment is hydrogen phthalate ammonium-dilution heat of sulfuric acid, and pH value is 5.5, and wherein hydrogen phthalate ammonium is 3:60 with the ratio of the amount of substance of dilute sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 1.
Embodiment 8
The cushioning liquid of the present embodiment is hydrogen phthalate ammonium-dilution heat of sulfuric acid, and pH value is 5, and wherein hydrogen phthalate ammonium is 3:55 with the ratio of the amount of substance of dilute sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 1.
Embodiment 9
The cushioning liquid of the present embodiment is oxalic acid-ammonium oxalate solution, and pH value is 4.5, and its mesoxalic acid is 2:1 with the ratio of the amount of substance of ammonium oxalate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 2.
Embodiment 10
The cushioning liquid of the present embodiment is oxalic acid-ammonium oxalate solution, and pH value is 5.5, and its mesoxalic acid is 4:1 with the ratio of the amount of substance of ammonium oxalate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 2.
Embodiment 11
The cushioning liquid of the present embodiment is oxalic acid-ammonium oxalate solution, and pH value is 5, and its mesoxalic acid is 3:1 with the ratio of the amount of substance of ammonium oxalate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 2.
Embodiment 12
The cushioning liquid of the present embodiment is hexa-sulfuric acid solution, and pH value is 4.5, and wherein hexa is 1:260 with the ratio of the amount of substance of sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 3.
Embodiment 13
The cushioning liquid of the present embodiment is hexa-sulfuric acid solution, and pH value is 5.5, and wherein hexa is 1:270 with the ratio of the amount of substance of sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 3.
Embodiment 14
The cushioning liquid of the present embodiment is hexa-sulfuric acid solution, and pH value is 5, and wherein hexa is 1:265 with the ratio of the amount of substance of sulfuric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 3.
Embodiment 15
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 4.5, and wherein ammonium dihydrogen phosphate (ADP) is 1:3 with the ratio of the amount of substance of phosphoric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 4.
Embodiment 16
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 5.5, and wherein ammonium dihydrogen phosphate (ADP) is 1:5 with the ratio of the amount of substance of phosphoric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 4.
Embodiment 17
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 5, and wherein ammonium dihydrogen phosphate (ADP) is 1:4 with the ratio of the amount of substance of phosphoric acid, and the cleaning solution of the present embodiment and cleaning method are with embodiment 4.
Embodiment 18
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 4, and wherein sulfuric acid is 2:1 with the ratio of the amount of substance of ammonium sulfate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 5.
Embodiment 19
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 5.5, and wherein sulfuric acid is 5:1 with the ratio of the amount of substance of ammonium sulfate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 5.
Embodiment 20
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 5.5, and wherein sulfuric acid is 3:1 with the ratio of the amount of substance of ammonium sulfate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 5.
Embodiment 21
The cushioning liquid of the present embodiment is ammonium dihydrogen phosphate (ADP)-phosphoric acid solution, and pH value is 5, and wherein sulfuric acid is 3:1 with the ratio of the amount of substance of ammonium sulfate, and the cleaning solution of the present embodiment and cleaning method are with embodiment 5.
To embodiment 1 ~ 21 clean after catalyst characterize and active testing result as shown in table 1.
Catalyst characterization after table 1 cleans and active testing result
In upper table, the quantity of Bronsted acid represents with the multiple of spent catalyst.
As shown in Table 1, through the catalyst of cleaning fluid process of the present invention, denitration efficiency is enhanced about more than once, and reaches 98%, and specific area reaches 66m
2/ g, after cleaning, the quantity of catalyst B ronsted acid improves 20 times relative to spent catalyst, obtains more satisfactory catalyst regeneration effect.
Claims (4)
1. the cleaning fluid for denitrating catalyst regeneration, it is characterized in that: comprise for removing blocking arsenic on a catalyst, the cushioning liquid that cleaning solution that is plumbous and mercury increases with maintenance active acid bit quantity, wherein cleaning solution take deionized water as solvent, with the quality of deionized water for benchmark, add the Polyoxyethylene Ether Nonionic Surfactant of the selective heavy metal chelating agent HMCA-1 and 0.01 ~ 1% of 1 ~ 10%, cushioning liquid is hydrogen phthalate ammonium-dilution heat of sulfuric acid, hexa-sulfuric acid solution, sulfuric acid-ammonium sulfate, phosphoric acid-ammonium dibasic phosphate solution or oxalic acid-ammonium oxalate solution.
2. the cleaning fluid for denitrating catalyst regeneration according to claim 1, it is characterized in that: in described hydrogen phthalate ammonium-dilution heat of sulfuric acid, hydrogen phthalate ammonium is 3:50 ~ 60 with the ratio of the amount of substance of dilute sulfuric acid, in described hexa-sulfuric acid solution, hexa is 1:260 ~ 270 with the ratio of the amount of substance of sulfuric acid, in described sulfuric acid-ammonium sulfate, sulfuric acid is 2 ~ 5:1 with the ratio of the amount of substance of ammonium sulfate, in described phosphoric acid-ammonium dibasic phosphate solution, phosphoric acid is 3 ~ 5:1 with the ratio of the amount of substance of diammonium hydrogen phosphate, described oxalic acid-ammonium oxalate solution mesoxalic acid is 2 ~ 4:1 with the ratio of the amount of substance of ammonium oxalate.
3. the cleaning fluid for denitrating catalyst regeneration according to claim 1, is characterized in that: the pH value of described cushioning liquid is 4.0 ~ 5.5.
4. the method for the cleaning fluid cleaning denitrating catalyst for denitrating catalyst regeneration according to claim 1 and 2, it is characterized in that step is as follows: get inactivation denitrating catalyst, by high pressure de-ionized water rinse 3 ~ 5 times, then use cleaning solution and the ultrasonic immersion 0.1 ~ 6h of cushioning liquid successively.
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| CN105251543B (en) * | 2015-10-20 | 2018-08-28 | 清华大学 | A kind of hydrogen reducing regeneration method of the out of stock catalyst of arsenic poisoning |
| CN107126977B (en) * | 2016-02-29 | 2020-04-17 | 神华集团有限责任公司 | Cleaning agent composition and method for regenerating deactivated denitration catalyst |
| CN107260666A (en) * | 2017-07-04 | 2017-10-20 | 江西傲新生物科技有限公司 | A kind of long-acting cefquinome sulfate injection and preparation method thereof |
| CN110721754B (en) * | 2019-11-15 | 2023-07-25 | 清大国华环境集团股份有限公司 | Regeneration and recovery method of waste SCR denitration catalyst |
| CN113926465A (en) * | 2020-06-29 | 2022-01-14 | 攀枝花学院 | Desulfurization and denitrification catalyst, preparation method and regeneration method thereof |
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| KR101083308B1 (en) * | 2009-09-10 | 2011-11-15 | 한국전력공사 | REGENERATION METHOD AND APPARATUS OF DE-NOx SPENT CATALYST BY CONTROLLING THE pH OF ACID SOLUTION |
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