CN106268977A - Utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method - Google Patents
Utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method Download PDFInfo
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- CN106268977A CN106268977A CN201610647380.7A CN201610647380A CN106268977A CN 106268977 A CN106268977 A CN 106268977A CN 201610647380 A CN201610647380 A CN 201610647380A CN 106268977 A CN106268977 A CN 106268977A
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- Prior art keywords
- denitration catalyst
- waste denitration
- petroleum coke
- garbage
- coke combustion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/485—Impregnating or reimpregnating with, or deposition of metal compounds or catalytically active elements
Abstract
The invention belongs to waste material field of comprehensive utilization, be specifically related to a kind of utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method.Described method comprises the steps: the pretreatment of (1) waste denitration catalyst: first, carries out waste denitration catalyst sorting, purges, cleans, and dries after cleaning；(2) a, ammonia spirit preparation: the ammonia that mass percent is 12 17% is mixed with deionized water equal-volume, standby after stirring；B, being sieved by the garbage after petroleum coke combustion, add the ammonia spirit prepared, stirring and dissolving obtains solution；C, solution step b obtained filter, and filtrate is dipping solution；(3) regeneration: the waste denitration catalyst of drying being put in dipping solution prepared by step (2) and impregnate, piling, after drying, regeneration completes.Two kinds of garbages are re-used by the present invention, turn waste into wealth, make full use of secondary resource, carry out waste denitration catalyst regeneration.
Description
Technical field
The invention belongs to waste material field of comprehensive utilization, be specifically related to a kind of utilize the garbage after petroleum coke combustion
To waste denitration catalyst regeneration method.
Background technology
Along with the extensive consumption of resource, finding new utilizable resource is following a period of time industrial development research
Emphasis.As the petroleum coke after the oil refining of garbage, because there is high caloric value and gradually by as kiln or other
The fuel applications of firing equipment.Because petroleum coke is from the impurity in the refining process of crude oil, in crude refinement processes these
Impurity being enriched in side-product petroleum coke progressively.During after petroleum coke combustion, these impurity stay heavy oil flying dust after combustion, its
Mainly comprise that it is as shown in the table:
| Constituent content % | SiO2 | V2O5 | NiO2 | C | Al2O3 |
| Flying dust | 0.3 | 9.36 | 1.54 | 80 | 0.12 |
Be may know that by table analysis, in the flying dust after petroleum coke combustion, metallic element is mainly vanadium and a small amount of nickel, aluminum, non-
Metallic element is mainly carbon and silicon.Flying dust how is utilized to reclaim valuable element, the most not relevant research and report.
The denitrating flue gas of boiler and power plant etc. is administered, and mainly applies denitrating catalyst, the most domestic denitrating catalyst longevity
Life is substantially at 2-3, and denitrating catalyst is along with the time lengthening of process flue gas, and its denitration performance is gradually reduced, and makes the de-of flue gas
Nitre rate significantly declines, it has to be replaced, and causes and uses the environmental protection treatment cost of producer significantly to increase.How
Carry out the regeneration of catalyst and increase the service life, current patent CN201410383383.5, CN201210571417.4,
CN201410012220.6 etc. be all denitrating catalyst is carried out pretreatment after, then prepare active constituent solution and process.Arrive
So far, the method that the flying dust after the petroleum coke combustion after heavy oil refinery carries out Regeneration Treatment is not the most used.
Summary of the invention
According to above deficiency of the prior art, it is an object of the invention to provide a kind of utilize after petroleum coke combustion discarded
Two kinds of garbages, to waste denitration catalyst regeneration method, are re-used, turn waste into wealth, make full use of secondary resource and enter by thing
Row denitrating catalyst regeneration.
Of the present invention utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method, including such as
Lower step:
(1) pretreatment of waste denitration catalyst: first, waste denitration catalyst sorted, will not have breakage
Waste denitration catalyst is through hot-air blowing, then, uses cleanout fluid to be carried out, clearly the waste denitration catalyst after purging
Wash complete post-drying；
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume, after stirring by the ammonia that mass percent is 12-17%
Standby；
B, the garbage after petroleum coke combustion is sieved, after removing residue on sieve, useless after the petroleum coke combustion after sieving
Adding the ammonia spirit prepared in gurry, stirring and dissolving obtains solution；
C, being filtered by the solution that step b stirring and dissolving obtains, filtrate is dipping solution；
(3) regeneration:
Waste denitration catalyst after step (1) being dried is put in dipping solution prepared by step (2) and is impregnated, and then puts
Entering piling in spacious paulin, after drying, waste denitration catalyst has regenerated.
In step (1), described hot blast temperature is 150-200 DEG C, and purge time is 15-30min.
In step (1), described cleanout fluid be mass percent be the wang aqueous solution of 5-10%.
In step (1), described cleaning is for taking out after soaking 3-6min.
In step (1), described dries the hot-air seasoning for using 100-150 DEG C.
In step (2), the described garbage after petroleum coke combustion is the flying dust after petroleum coke combustion.
In step (2), described sieves as crossing 200-300 mesh analysis sieve.
In step a, described stirring is low rate mixing, and mixing time is 3-5min.
In step b, described residue on sieve is mainly impurity.
In step (2), described sieve after petroleum coke combustion after garbage concentration in ammonia spirit be 0.5-
0.8g/L。
In step b, described stirring, rotating speed is that 50-100 turns/min, and mixing time is 30-60min.
In step (2), the described employing middling speed quantitative filter paper that is filtered into filters.
In step (3), described dipping is 2-3 time, makes the mass content of vanadic anhydride in waste denitration catalyst
For 0.5-5%.
In step (3), described is dried as natural air drying.
Compared with prior art, the invention has the beneficial effects as follows:
(1) garbage-flying dust after the present invention utilizes petroleum coke combustion carries out waste denitration catalyst regeneration, due to oil
The vanadic anhydride in garbage-flying dust after burnt burning can reach and other materials with the ammonium salt solution of ammonia generation vanadium
The purpose of separation, the ammonium salt solution of preparation is impregnated in the waste denitration catalyst being disposed, after naturally drying, activity
Component vanadium is attached on catalyst, reaches the effect of catalysis.
(2) two kinds of trade wastes are re-used by the present invention, turn waste into wealth, make full use of secondary resource, carry out
Waste denitration catalyst regeneration.Two kinds of garbages are carried out regeneration, it is achieved waste recycling, economize on resources, improve money
The utilization ratio in source and recycle value, has development prospect widely.
Accompanying drawing explanation
Fig. 1 is that the flow process of waste denitration catalyst regeneration method is shown by the garbage after the present invention utilizes petroleum coke combustion
It is intended to.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
(1) pretreatment of waste denitration catalyst: waste denitration catalyst sorted, will not have the discarded de-of breakage
Denox catalyst is through hot-air blowing, it is desirable to hot blast temperature controls at 150 DEG C, purges 15min.By the discarded denitration catalyst after purging
Agent is carried out, to remove dust and the solid reaction material sticking to waste denitration catalyst surface.Cleanout fluid uses quality
Percentage ratio is the wang aqueous solution of 5%, takes out, by the heat of 100 DEG C after waste denitration catalyst is put in cleanout fluid immersion 3min
Wind is dried.
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 12%, low rate mixing
3min, standby.
B, the flying dust after petroleum coke combustion is sieved, it is desirable to sieved by the analysis of 200 mesh, residue on sieve is removed, sieve
Excess is mainly impurity.500g will be weighed by the flying dust of 200 mesh, be put in the beaker of 2000mL, add the ammonia prepared
Solution 1000mL, stirring and dissolving obtains solution, it is desirable to 50 turns/min of rotating speed, mixing time 30min.
The solution that c, step b stirring and dissolving obtain uses middling speed quantitative filter paper to filter, and the filtrate after filtration is leaching
Stain solution.
(3) regeneration:
Waste denitration catalyst after drying is put into and is carried out 2 dippings in dipping solution prepared by step (2) so that it is five
The mass content of V 2 O is 0.5%.Waste denitration catalyst after dipping is put into spacious paulin piling, after natural air drying,
Waste denitration catalyst has regenerated.
Embodiment 2
(1) pretreatment of waste denitration catalyst: waste denitration catalyst sorted, will not have the discarded de-of breakage
Denox catalyst is through hot-air blowing, it is desirable to hot blast temperature controls at 170 DEG C, purges 20min.By the discarded denitration catalyst after purging
Agent is carried out, to remove dust and the solid reaction material sticking to waste denitration catalyst surface.Cleanout fluid uses quality
Percentage ratio is the wang aqueous solution of 6%, takes out, by the heat of 120 DEG C after waste denitration catalyst is put in cleanout fluid immersion 4min
Wind is dried.
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 13%, low rate mixing
4min, standby.
B, the flying dust after petroleum coke combustion is sieved, it is desirable to sieved by the analysis of 300 mesh, residue on sieve is removed, sieve
Excess is mainly impurity.700g will be weighed by the flying dust of 300 mesh, be put in the beaker of 2000mL, add the ammonia prepared
Solution 1000mL, stirring and dissolving obtains solution, it is desirable to 60 turns/min of rotating speed, mixing time 40min.
The solution that c, step b stirring and dissolving obtain uses middling speed quantitative filter paper to filter, and the filtrate after filtration is leaching
Stain solution.
(3) regeneration:
Waste denitration catalyst after drying is put into and is carried out 3 dippings in dipping solution prepared by step (2) so that it is five
The mass content of V 2 O is 1.0%.Waste denitration catalyst after dipping is put into spacious paulin piling, after natural air drying,
Waste denitration catalyst has regenerated.
Embodiment 3
(1) pretreatment of waste denitration catalyst: waste denitration catalyst sorted, will not have the discarded de-of breakage
Denox catalyst is through hot-air blowing, it is desirable to hot blast temperature controls at 170 DEG C, purges 25min.By the discarded denitration catalyst after purging
Agent is carried out, to remove dust and the solid reaction material sticking to waste denitration catalyst surface.Cleanout fluid uses quality
Percentage ratio is the wang aqueous solution of 7%, takes out, by the heat of 120 DEG C after waste denitration catalyst is put in cleanout fluid immersion 5min
Wind is dried.
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 14%, low rate mixing
5min, standby.
B, the flying dust after petroleum coke combustion is sieved, it is desirable to sieved by the analysis of 250 mesh, residue on sieve is removed, sieve
Excess is mainly impurity.800g will be weighed by the flying dust of 250 mesh, be put in the beaker of 2000mL, add the ammonia prepared
Solution 1000mL, stirring and dissolving obtains solution, it is desirable to 70 turns/min of rotating speed, mixing time 50min.
The solution that c, step b stirring and dissolving obtain uses middling speed quantitative filter paper to filter, and the filtrate after filtration is leaching
Stain solution.
(3) regeneration:
Waste denitration catalyst after drying is put into and is carried out 3 dippings in dipping solution prepared by step (2) so that it is five
The mass content of V 2 O is 3.0%.Waste denitration catalyst after dipping is put into spacious paulin piling, after natural air drying,
Waste denitration catalyst has regenerated.
Embodiment 4
(1) pretreatment of waste denitration catalyst: waste denitration catalyst sorted, will not have the discarded de-of breakage
Denox catalyst is through hot-air blowing, it is desirable to hot blast temperature controls at 180 DEG C, purges 30min.By the discarded denitration catalyst after purging
Agent is carried out, to remove dust and the solid reaction material sticking to waste denitration catalyst surface.Cleanout fluid uses quality
Percentage ratio is the wang aqueous solution of 9%, takes out, by the heat of 140 DEG C after waste denitration catalyst is put in cleanout fluid immersion 56min
Wind is dried.
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 16%, low rate mixing
3min, standby.
B, the flying dust after petroleum coke combustion is sieved, it is desirable to sieved by the analysis of 200 mesh, residue on sieve is removed, sieve
Excess is mainly impurity.700g will be weighed by the flying dust of 200 mesh, be put in the beaker of 2000mL, add the ammonia prepared
Solution 1000mL, stirring and dissolving obtains solution, it is desirable to 90 turns/min of rotating speed, mixing time 60min.
The solution that c, step b stirring and dissolving obtain uses middling speed quantitative filter paper to filter, and the filtrate after filtration is leaching
Stain solution.
(3) regeneration:
Waste denitration catalyst after drying is put into and is carried out 3 dippings in dipping solution prepared by step (2) so that it is five
The mass content of V 2 O is 3%.Waste denitration catalyst after dipping is put into spacious paulin piling, after natural air drying, useless
Abandon denitrating catalyst to have regenerated.
Embodiment 5
(1) pretreatment of waste denitration catalyst: waste denitration catalyst sorted, will not have the discarded de-of breakage
Denox catalyst is through hot-air blowing, it is desirable to hot blast temperature controls at 200 DEG C, purges 30min.By the discarded denitration catalyst after purging
Agent is carried out, to remove dust and the solid reaction material sticking to waste denitration catalyst surface.Cleanout fluid uses quality
Percentage ratio is the wang aqueous solution of 10%, takes out, by the heat of 150 DEG C after waste denitration catalyst is put in cleanout fluid immersion 6min
Wind is dried.
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 17%, low rate mixing
5min, standby.
B, the flying dust after petroleum coke combustion is sieved, it is desirable to sieved by the analysis of 300 mesh, residue on sieve is removed, sieve
Excess is mainly impurity.500g will be weighed by the flying dust of 300 mesh, be put in the beaker of 2000mL, add the ammonia prepared
Solution 1000mL, stirring and dissolving obtains solution, it is desirable to 100 turns/min of rotating speed, mixing time 60min.
The solution that c, step b stirring and dissolving obtain uses middling speed quantitative filter paper to filter, and the filtrate after filtration is leaching
Stain solution.
(3) regeneration:
Waste denitration catalyst after drying is put into and is carried out 3 dippings in dipping solution prepared by step (2) so that it is five
The mass content of V 2 O is 5%.Waste denitration catalyst after dipping is put into spacious paulin piling, after natural air drying, useless
Abandon denitrating catalyst to have regenerated.
Claims (10)
1. one kind utilizes the garbage after petroleum coke combustion to waste denitration catalyst regeneration method, it is characterised in that: include
Following steps:
(1) pretreatment of waste denitration catalyst: first, waste denitration catalyst sorted, will not have the discarded of breakage
Denitrating catalyst is through hot-air blowing, then, uses cleanout fluid to be carried out the waste denitration catalyst after purging, has cleaned
Finish post-drying；
(2) waste denitration catalyst dipping solution is prepared with the garbage after petroleum coke combustion:
A, ammonia spirit are prepared: mixed with deionized water equal-volume by the ammonia that mass percent is 12-17%, stir standby
With；
B, the garbage after petroleum coke combustion is sieved, after removing residue on sieve, the garbage after petroleum coke combustion after sieving
The ammonia spirit that middle addition prepares, stirring and dissolving obtains solution；
C, being filtered by the solution that step b stirring and dissolving obtains, filtrate is dipping solution；
(3) regeneration:
Waste denitration catalyst after step (1) being dried is put in dipping solution prepared by step (2) and is impregnated, and is then placed in opening
Piling in paulin, after drying, waste denitration catalyst has regenerated.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (1), described hot blast temperature is 150-200 DEG C, purge time is 15-30min.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (1), described cleanout fluid be mass percent be the wang aqueous solution of 5-10%.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (1), described cleaning is for taking out after soaking 3-6min.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (1), described dries the hot-air seasoning for using 100-150 DEG C.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (2), the described garbage after petroleum coke combustion is the flying dust after petroleum coke combustion.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (2), described sieves as crossing 200-300 mesh analysis sieve.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (2), described sieve after petroleum coke combustion after garbage concentration in ammonia spirit be
0.5-0.8g/L。
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (2), the described employing middling speed quantitative filter paper that is filtered into filters.
The most according to claim 1 utilize the garbage after petroleum coke combustion to waste denitration catalyst regeneration method,
It is characterized in that: in step (3), described dipping is 2-3 time, make the quality of the vanadic anhydride in waste denitration catalyst contain
Amount is 0.5-5%.
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Citations (7)
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|---|---|---|---|---|
| US4539186A (en) * | 1984-03-15 | 1985-09-03 | Intevep, S.A. | Method for leaching and recovering vanadium from vanadium bearing by-product materials |
| EP0499351A1 (en) * | 1991-02-15 | 1992-08-19 | Mitsubishi Jukogyo Kabushiki Kaisha | Method for treating a solution used for the regeneration of a denitration catalyst |
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| CN104475174A (en) * | 2014-11-25 | 2015-04-01 | 安徽迪诺环保新材料科技有限公司 | Regenerating method of invalid SCR denitration catalyst |
| CN104907106A (en) * | 2015-05-11 | 2015-09-16 | 华电高科环保技术有限公司 | Waste SCR flue gas denitration catalyst regeneration and recovery integration processing method |
| CN105080622A (en) * | 2015-09-14 | 2015-11-25 | 中建中环工程有限公司 | Regeneration method for inactivated selective catalytic reduction (SCR) denitration catalyst |
| CN105170198A (en) * | 2015-09-21 | 2015-12-23 | 武汉钢铁(集团)公司 | Industrialized regeneration method of SCR plate-type denitration catalyst |
-
2016
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| US4539186A (en) * | 1984-03-15 | 1985-09-03 | Intevep, S.A. | Method for leaching and recovering vanadium from vanadium bearing by-product materials |
| EP0499351A1 (en) * | 1991-02-15 | 1992-08-19 | Mitsubishi Jukogyo Kabushiki Kaisha | Method for treating a solution used for the regeneration of a denitration catalyst |
| CN104190477A (en) * | 2014-09-09 | 2014-12-10 | 华电高科（高碑店）环保技术有限公司 | Method for regenerating titanium-based vanadium-series SCR (Selective Catalytic Reduction) denitration catalyst |
| CN104475174A (en) * | 2014-11-25 | 2015-04-01 | 安徽迪诺环保新材料科技有限公司 | Regenerating method of invalid SCR denitration catalyst |
| CN104907106A (en) * | 2015-05-11 | 2015-09-16 | 华电高科环保技术有限公司 | Waste SCR flue gas denitration catalyst regeneration and recovery integration processing method |
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| CN105170198A (en) * | 2015-09-21 | 2015-12-23 | 武汉钢铁(集团)公司 | Industrialized regeneration method of SCR plate-type denitration catalyst |
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