CN107175098A - One kind is used for activated carbon used for flue gas demercuration catalyst and preparation method and application - Google Patents
One kind is used for activated carbon used for flue gas demercuration catalyst and preparation method and application Download PDFInfo
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- CN107175098A CN107175098A CN201710468028.1A CN201710468028A CN107175098A CN 107175098 A CN107175098 A CN 107175098A CN 201710468028 A CN201710468028 A CN 201710468028A CN 107175098 A CN107175098 A CN 107175098A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
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- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
One kind is used for activated carbon used for flue gas demercuration catalyst, it is specifically related to a kind of to be used for activated carbon used for flue gas demercuration catalyst and preparation method and application, it is characterized in that catalyst is made up of active component and carrier, the active component is the oxide of vanadium and cerium, and each component percentage by weight composition of catalyst is respectively:Active component V2O5=1~10wt%;Active component CeO2=1~12wt%;Carrier=78~98wt%;The present invention, which has, to be prepared simply, and cost is low, the advantage of function admirable.
Description
Technical field
The invention belongs to a kind of catalyst and preparation method and application, relate in particular to a kind of for flue gas demercuration activity
Pd/carbon catalyst and preparation method and application.
Background technology
China is a rich coal, the country of oil-poor, few gas, and this energy resource structure determines coal in fossil fuel total resources
In critical role.China is the big country of an energy resource consumption again simultaneously, and coal proportion in energy resource structure is up to 75%,
Coal wherein close to annual output of coal 70% is directly used in burning.But the pollution discharged in the combustion process of a large amount of coals
It is main source that thing has turned into China's atmosphere pollution, mainly including NOx, SO2, mercury etc..Wherein, mercury and its derivative except with
The features such as hypertoxicity, persistence, easy migration and bioconcentration, can also persistently exist in air and food chain, at a distance
Migration, existence and health care belt to the mankind carry out huge threat, and therefore, a series of harm that mercury is produced can not be ignored.
Mercury is main with element mercury in coal-fired flue-gas(Hg0), oxidation state mercury(Hg2+), particle mercury(Hgp)Three kinds of forms are deposited
.HgpIt can be collected and be removed by cleaner, Hg2+It is soluble in water, wet desulphurization device can be combined and be removed,
However, due to Hg0With higher vapour pressure and water is insoluble in, utilizes existing cleaner and wet flue gas desulfurizer
It is difficult to its Direct Acquisition be removed, Hg0Almost all is with fume emission into air.Therefore, the emphasis and difficult point of flue gas demercuration
It is to Hg0Control and removing.In addition, newest promulgation《Fossil-fuel power plant atmospheric pollutant emission standard(GB 13223-
2011)》Middle clear stipulaties, from 2015, the discharge capacity of mercury and mercuric compounds must not exceed 0.03mg/ in coal-fired plant flue gas
m3.Therefore, to meet the requirements of relevant laws and regulations, developmental research high effective flue gas demercuration catalyst is particularly important.
The control technology of existing smoke mercury emission is directed to, activated carbon spraying technique is considered as that current coal-fired flue-gas takes off
One of most efficient method in mercury technology, but the absorption capture rate that non-modified activated carbon has mercury is low, adsorption capacity is low,
The problems such as consumption is big, causes its operating cost higher, therefore limits the extensive use in flue gas control field of the technology.
To make full use of the premium properties of activated carbon, therefore need to carry out Depth Study to activated carbon, find appropriate method of modifying, pass through
Appropriate modification is carried out to activated carbon, the load capacity and decentralization of active component is improved, prepared with height catalysis
The activated carbon of activity and adsorption capacity, increases its adsorption and oxidation ability, improves the removal efficiency of mercury, and then reduce using activated carbon
Cost.
The content of the invention:
Good it is an object of the invention to provide a kind of catalytic activity to solve problems of the prior art, adsorption capacity is high, mercury
Removal efficiency it is high, cost it is low be used for activated carbon used for flue gas demercuration catalyst and preparation method and application.
The catalyst of the present invention is made up of active component and carrier, and the active component is the oxide of vanadium and cerium, catalysis
The each component percentage by weight of agent is constituted:Active component V2O5=1~10wt%;Active component CeO2=1~12wt%;
Carrier=78~98wt%.
Above-mentioned carrier is activated carbon, and the oxide of above-mentioned vanadium is generated after the soluble-salt calcining of vanadium, above-mentioned cerium
Oxide be by cerium soluble-salt calcining after generate.
Above-mentioned activated carbon is wood activated charcoal, cocoanut active charcoal, coal mass active carbon, active fruit shell carbon, activated carbon
In one or two kinds of and two or more mixtures.
The preparation method of the catalyst of the present invention is as follows:
(1)Dry activated carbon is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby;
(2)Using equi-volume impregnating, by active component V2O51~10wt%;Active component CeO21~12wt%;Activated carbon
78~98wt% composition, activated carbon is immersed in the ammonium metavanadate-cerous nitrate mixed solution prepared, dry in 50~180 DEG C
Dry 5~10h, then in N2Under atmosphere, 200~500 DEG C of 4~10h of calcining, in air atmosphere finally, 180~300 DEG C of calcinings
4~10h, that is, catalyst needed for being made.
Ammonium metavanadate-cerous nitrate mixed solution as described above of preparing is by ammonium metavanadate, cerous nitrate, oxalic acid and water mixing
Dissolving.
The application of catalyst of the present invention, comprises the following steps:
Described catalyst is used for the removing of the mercury in flue gas such as coal-burning power plant, Industrial Boiler, garbage burning boiler, Industrial Stoves,
The operating temperature of the flue gas demercuration catalyst is 100~220 DEG C, and air speed is 2000h-1~51000h-1。
Compared with prior art, the present invention has the advantages that:
1)The present invention carries out impregnation process by using the mixed solution of ammonium metavanadate and cerous nitrate to activated carbon, improves activity
The internal structure of charcoal, adds the quantity of active component in activated carbon, generates more oxygen vacancy positions, makes the absorption of activated carbon
Oxidability is significantly increased, and air speed is 2000h in course of reaction-1~51000h-1, the removal efficiency of mercury is more than 90.8%, realization
The efficient removal of Mercury In Coal Combustion Flue Gas
2)The cerium modified activated-carbon catalyst preparation method of vanadium in the present invention is simple, easily prepared, raw material sources are various extensively, into
This cheap, demercuration function admirable.By activated carbon application of the vanadium after cerium modified in the removing of Mercury In Coal Combustion Flue Gas, it can greatly reduce
The usage amount of activated carbon, so as to reduce the input cost of activated carbon.
3)The application of catalyst of the present invention:By the modification to activated carbon, activated carbon is drastically increased to flue gas
The catalysis oxidation ability of middle mercury, the suction-operated for changing the conventional carbon that places one's entire reliance upon carries out the situation of demercuration, can be extensive
Removing for mercury in flue gas such as coal-burning power plant, Industrial Boiler, garbage burning boiler, Industrial Stoves.
4)The reaction temperature of the catalyst is gentle, has higher catalytic activity in 100~220 DEG C of low-temperature ranges.It is suitable
Together in low temperature demercuration, while the mercury captured will not be made to be desorbed or decompose, secondary pollution is not produced, possesses green energy conservation effect
Benefit, with wide application space and development prospect.
Brief description of the drawings:
Fig. 1 is the demercuration Activity evaluation of original activated carbon and modified activated-carbon catalyst in embodiment 1.
Fig. 2 is the demercuration Activity evaluation of original activated carbon and modified activated-carbon catalyst in embodiment 2.
Fig. 3 is the demercuration Activity evaluation of original activated carbon and modified activated-carbon catalyst in embodiment 4.
Fig. 4 is the demercuration Activity evaluation of original activated carbon and modified activated-carbon catalyst in embodiment 6.
Embodiment:
The present invention is further illustrated below by specific embodiment.
Embodiment 1:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby;
2)0.13g NH are weighed respectively4VO3, 0.26g H2C2O4·2H2O and 0.25g Ce (NO3)3·6H2O, is placed in beaker,
Add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-cerous nitrate is made
Mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 50 DEG C of dry 10h, 200 DEG C of nitrogen atmospheres are calcined 10h, finally existed
180 DEG C of air atmospheres calcine 10h, you can 1wt%V is made2O5-1wt%CeO2Modified active carbon catalyst(Abbreviation 1V-1Ce/AC).
Accurately weigh in the modified activated-carbon catalysts of 0.5g, the fixed bed reactors for being placed in 100 DEG C, total tolerance is in course of reaction
45ml/min, air speed is 2000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,American), through height
Pure nitrogen gas is carried and gone out as carrier gas, and fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, balance is used as by nitrogen
The concentration of mercury is detected using the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in gas, simulated flue gas.Experimental result
Show, in 240min, demercuration rate is maintained under more than 90.80%, same experimental conditions, the mercury of unit mass original activity charcoal
Adsorbance is 5037.24ug/g, and the mercury adsorbance of unit mass catalyst is 31627.45ug/g, is the 6.27 of original activity charcoal
Times.
Embodiment 2:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby.
2)0.13g NH are weighed respectively4VO3, 0.26g H2C2O4·2H2O and 3.03g Ce (NO3)3·6H2O, is placed in beaker
In, add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-nitre is made
Sour cerium mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 80 DEG C of dry 9h, 300 DEG C of nitrogen atmospheres calcine 8h, finally 200
DEG C air atmosphere calcining 8h, you can 1wt%V is made2O5-12wt%CeO2Modified active carbon catalyst(Abbreviation 1V-12Ce/AC).It is accurate
Really weigh in the modified activated-carbon catalysts of 0.2g, the fixed bed reactors for being placed in 120 DEG C, total tolerance is in course of reaction
460ml/min, air speed is 51000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,American), warp
High pure nitrogen is carried and gone out as carrier gas, and fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, balance is used as by nitrogen
The concentration of mercury is detected using the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in gas, simulated flue gas.Experimental result
Show, in 240min, demercuration rate is maintained under more than 96.93%, same experimental conditions, the mercury of unit mass original activity charcoal
Adsorbance is 4843.41 ug/g, and the mercury adsorbance of unit mass catalyst is 36698.16ug/g, is original activity charcoal
7.58 again.
Embodiment 3:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby.
2)0.78g NH are weighed respectively4VO3, 1.56g H2C2O4·2H2O and 1.52g Ce (NO3)3·6H2O, is placed in beaker
In, add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-nitre is made
Sour cerium mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 100 DEG C of dry 8h, 350 DEG C of nitrogen atmospheres are calcined 7h, finally existed
240 DEG C of air atmospheres calcine 7h, you can 6wt%V is made2O5-6wt%CeO2Modified active carbon catalyst(Abbreviation 6V-6Ce/AC).
Accurately weigh in the modified activated-carbon catalysts of 0.2g, the fixed bed reactors for being placed in 140 DEG C, total tolerance is in course of reaction
272ml/min, air speed is 30000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,American), warp
High pure nitrogen is carried and gone out as carrier gas, and fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, balance is used as by nitrogen
The concentration of mercury is detected using the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in gas, simulated flue gas.Experimental result
Show, in 240min, demercuration rate is maintained under more than 92.61%, same experimental conditions, the mercury of unit mass original activity charcoal
Adsorbance is 5237.42ug/g, and the mercury adsorbance of unit mass catalyst is 37625.17ug/g, is the 7.18 of original activity charcoal
Times.
Embodiment 4:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby.
2)0.26g NH are weighed respectively4VO3, 0.52g H2C2O4·2H2O and 2g Ce (NO3)3·6H2O, is placed in beaker,
Add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-cerous nitrate is made
Mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 140 DEG C of dry 7h, 400 DEG C of nitrogen atmospheres are calcined 6h, finally existed
260 DEG C of air atmospheres calcine 6h, you can 2wt%V is made2O5-8wt%CeO2Modified active carbon catalyst(Abbreviation 1V-8Ce/AC).
Accurately weigh in the modified activated-carbon catalysts of 0.2g, the fixed bed reactors for being placed in 160 DEG C, total tolerance is in course of reaction
460ml/min, air speed is 51000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,American), warp
High pure nitrogen is carried and gone out as carrier gas, and fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, balance is used as by nitrogen
The concentration of mercury is detected using the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in gas, simulated flue gas.Experimental result
Show, in 240min, demercuration rate is maintained under more than 99.25%, same experimental conditions, the mercury of unit mass original activity charcoal
Adsorbance is 4843.41 ug/g, and the mercury adsorbance of unit mass catalyst is 38372.58ug/g, is original activity charcoal
7.92 again.
Embodiment 5:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby.
2)1.3g NH are weighed respectively4VO3, 2.6g H2C2O4·2H2O and 0.25g Ce (NO3)3·6H2O, is placed in beaker
In, add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-nitre is made
Sour cerium mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 160 DEG C of dry 6h, 450 DEG C of nitrogen atmospheres are calcined 5h, finally existed
280 DEG C of air atmospheres calcine 5h, you can 10wt%V is made2O5-1wt%CeO2Modified active carbon catalyst(Abbreviation 10V-1Ce/
AC).Accurately weigh in the modified activated-carbon catalysts of 0.2g, the fixed bed reactors for being placed in 200 DEG C, total gas in course of reaction
Measure as 460ml/min, air speed is 51000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,
American), carry and go out as carrier gas through high pure nitrogen, fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, by
Nitrogen is as Balance Air, and the concentration of mercury uses the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in simulated flue gas
Detection.Test result indicates that, in 240min, demercuration rate is maintained under more than 94.87%, same experimental conditions, and unit mass is former
The mercury adsorbance of beginning activated carbon is 4843.41 ug/g, and the mercury adsorbance of unit mass catalyst is 30275.83ug/g, is former
6.25 times of beginning activated carbon.
Embodiment 6:
1)Dry wood activated charcoal is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby.
2)1.3g NH are weighed respectively4VO3, 2.6g H2C2O4·2H2O and 3.03g Ce (NO3)3·6H2O, is placed in beaker
In, add 15mlH2O, heats and is stirred with magnetic stirring apparatus, is in navy blue to solution, ammonium metavanadate-nitre is made
Sour cerium mixed solution.
3)Weigh step 1)In granular activated carbon 10g, be added to step 2)Ammonium metavanadate-cerous nitrate mixed solution
In, using incipient impregnation.By the solid matter of gained, in 180 DEG C of dry 5h, 500 DEG C of nitrogen atmospheres are calcined 4h, finally existed
300 DEG C of air atmospheres calcine 4h, you can 10wt%V is made2O5-12wt%CeO2Modified active carbon catalyst(Abbreviation 10V-12Ce/
AC).Accurately weigh in the modified activated-carbon catalysts of 0.2g, the fixed bed reactors for being placed in 220 DEG C, total gas in course of reaction
Measure as 460ml/min, air speed is 51000h-1, mercury osmos tube of the mercury vapour in U-tube(VICI Metronics,
American), carry and go out as carrier gas through high pure nitrogen, fixed bed reactors import mercury concentration is 300ug/m3,O2=5%, by
Nitrogen is as Balance Air, and the concentration of mercury uses the online mercury vapourmeters of RA-915M (Lumex Co, Ltd, Russia) in simulated flue gas
Detection.Test result indicates that, in 240min, demercuration rate is maintained under more than 93.54%, same experimental conditions, and unit mass is former
The mercury adsorbance of beginning activated carbon is 4843.41 ug/g, and the mercury adsorbance of unit mass catalyst is 37214.45ug/g, is former
7.68 times of beginning activated carbon.
Claims (6)
1. one kind is used for activated carbon used for flue gas demercuration catalyst, it is characterised in that catalyst is made up of active component and carrier, described
Active component is the oxide of vanadium and cerium, and each component percentage by weight composition of catalyst is respectively:Active component V2O5=1~
10wt%;Active component CeO2=1~12wt%;Carrier=78~98wt%.
2. it is as claimed in claim 1 a kind of for activated carbon used for flue gas demercuration catalyst, it is characterised in that described carrier is work
Property charcoal.
3. as claimed in claim 2 a kind of be used for activated carbon used for flue gas demercuration catalyst, it is characterised in that described activated carbon is
One or two kinds of in wood activated charcoal, cocoanut active charcoal, coal mass active carbon, active fruit shell carbon, activated carbon and two kinds
Mixture above.
4. a kind of preparation method for activated carbon used for flue gas demercuration catalyst as described in claim any one of 1-3, its feature
It is to comprise the following steps:
(1)Dry activated carbon is crushed, sieved, the granular activated carbon for filtering out particle diameter in 30~60 mesh is standby;
(2)Using equi-volume impregnating, by active component V2O51~10wt%;Active component CeO21~12wt%;Activated carbon
78~98wt% composition, activated carbon is immersed in the ammonium metavanadate-cerous nitrate mixed solution prepared, dry in 50~180 DEG C
Dry 5~10h, then in N2Under atmosphere, 200~500 DEG C of 4~10h of calcining, in air atmosphere finally, 180~300 DEG C of calcinings
4~10h, that is, catalyst needed for being made.
5. a kind of preparation method for activated carbon used for flue gas demercuration catalyst as claimed in claim 4, it is characterised in that prepare
Ammonium metavanadate-cerous nitrate mixed solution is by ammonium metavanadate, cerous nitrate, oxalic acid and water mixed dissolution.
6. a kind of application for activated carbon used for flue gas demercuration catalyst as described in claim any one of 1-3, it is characterised in that
Comprise the following steps:
Described catalyst is used for the removing of the mercury in flue gas such as coal-burning power plant, Industrial Boiler, garbage burning boiler, Industrial Stoves,
The operating temperature of the flue gas demercuration catalyst is 100~220 DEG C, and air speed is 2000h-1~51000h-1。
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CN110013828A (en) * | 2019-03-19 | 2019-07-16 | 杭州电子科技大学 | A kind of preparation method of the new modified absorbent charcoal material for flue gas demercuration |
CN110013828B (en) * | 2019-03-19 | 2021-09-21 | 杭州电子科技大学 | Preparation method of modified activated carbon material for flue gas demercuration |
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Application publication date: 20170919 |