CN103769114A - Vanadium-modified iron-based activated carbon catalyst, preparation method and application thereof - Google Patents
Vanadium-modified iron-based activated carbon catalyst, preparation method and application thereof Download PDFInfo
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- CN103769114A CN103769114A CN201410051686.7A CN201410051686A CN103769114A CN 103769114 A CN103769114 A CN 103769114A CN 201410051686 A CN201410051686 A CN 201410051686A CN 103769114 A CN103769114 A CN 103769114A
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Abstract
The invention discloses a vanadium-modified iron-based activated carbon catalyst which comprises active components which are ferric oxide and vanadium pentoxide. Activated carbon serves as a carrier; the mass percentage of the vanadium pentoxide in the activated carbon is larger than 0 percent and smaller than or equal to 1 percent. The vanadium-modified iron-based activated carbon catalyst obtained by adding vanadium is excellent in low-temperature NH3-SCR (silicon controlled rectifier) activity and SO2 poisoning resistance; an operation temperature window is wide. Under 150 DEG C, the NOx purification efficiency of the catalyst is over 70 percent; under 175 DEG C, the NOx purification efficiency is over 80 percent; furthermore, under 200 DEG C, the catalyst is high in SO2 poisoning resistance.
Description
Technical field
The present invention relates to relate to low temperature ferrovanadium activated-carbon catalyst, the Preparation method and use that a kind of sulfur resistance is high, be specifically related to iron-based activated-carbon catalyst, preparation method and its usage that a kind of vanadium is modified.
Background technology
NO
xbe one of main pollution pollutant of atmosphere, can cause acid rain, photochemical pollution and damage the ozone layer, the mankind's production and life in serious threat.China is take fire coal as main developing country, almost 37% NO
xcome from the discharge of the stationary source such as thermal power generation, boiler combustion, thereby caused serious atmosphere pollution, therefore carry out industrial furnace NO
xemission control technique becomes the task of top priority.
With NH
3for the SCR technology of reducing agent selective catalysis reducing NOx has obtained broad research, traditional V
2o
5-WO
3/ TiO
2although catalyst has high NO at 300～400 ℃
xpurification efficiency and anti-SO
2poisoning capability, but in order to meet its active and anti-sulphur sexual demand, the SCR device in station boiler needs preheating or repacking again, and this is by increase energy consumption or cause improvement project complexity, improves operation cost.
The non-vanadium base NH of exploitation at present
3-SCR catalyst system mainly comprises the oxide-based catalyst such as Fe base, Mn base, Ce base and Fe, Cu base equimolecular sieve catalyst.There is significant low temperature active, its N although Mn is catalyst based
2selective and sulfur resistance is poor; In Fe, Ce base oxide catalyst, high temperature active is good, but sulfur poisoning easily occurs; Though Fe, Cu based molecular sieve catalyst superior performance, but still exist expensive, the shortcoming such as hydrothermal stability is poor and sulfur resistance is low.Therefore exploitation has the low temperature NH that sulfur tolerance is good
3-SCR catalyst has great importance.
Summary of the invention
For the problem of prior art, the iron-based activated-carbon catalyst that the object of the present invention is to provide a kind of vanadium to modify, described catalyst has excellent low temperature NH
3-SCR activity and sulfur tolerance.
In order to achieve the above object, the present invention has adopted following technical scheme:
The iron-based activated-carbon catalyst that vanadium is modified, by adding a small amount of vanadic anhydride, the NOx removal efficiency of catalyst is substantially uninfluenced, and low temperature sulfur resistance improves, thereby the low-temp desulfurization denitration efficiency of catalyst entirety improves.The active component of described catalyst is iron oxide and vanadic anhydride, and carrier is active carbon, and the mass percent that described vanadic anhydride accounts for carrier active carbon is greater than 0 and is less than or equal to 1%.
The present invention by adding vanadium to significantly improve the anti-sulphur of catalyst in catalyst, the mass percent that described vanadic anhydride accounts for active carbon is for example 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95% or 1.0%, preferably 0～0.7% and do not comprise 0, further preferably 0～0.5% and do not comprise 0, most preferably 0.5%.
Preferably, the mass percent of described iron oxide is 0～10 and do not comprise 0, for example 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, preferably 0～8% and do not comprise 0, further preferably 0～5% and do not comprise 0.
Two of object of the present invention is the preparation method of the iron-based activated-carbon catalyst that a kind of vanadium modification as above is provided, and described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after Fe source, V source and oxidation, in stirring at room temperature, then evaporate to dryness, is dried, and roasting obtains the iron-based activated-carbon catalyst that vanadium is modified.
The present invention adopts simple common dipping method to prepare the iron-based activated-carbon catalyst that vanadium is modified, first described method adopts nitric acid to carry out surface oxidation to active carbon, utilize strong oxidizer, at suitable temperature, the functional group of activated carbon surface is carried out to oxidation processes, change the surface functional group of active carbon, can make active carbon there is stronger performance, thereby improve the content of surperficial oxy radical, strengthen surperficial polarity.The active carbon that surface polarity is stronger easily adsorbs polar substances, thereby can reach the object that improves adsorptive selectivity.Then,, under oxalic acid condition, take Fe source and V source, and control mass percent that vanadic anhydride accounts for active carbon and be greater than 0 and be less than or equal to 1%, the mixture of the active carbon after Fe source, V source and oxidation is stirred to evaporate to dryness, roasting, can obtain the iron-based activated-carbon catalyst that vanadium is modified.
Preferably, described Fe source is selected from the mixture of any one or at least two kinds in ferric nitrate, ferric sulfate, ferric phosphate or iron chloride, preferably ferric nitrate.
Preferably, described vanadium source is selected from the mixture of any one or at least two kinds in ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium vanadate or sodium pyrovanadate, preferably ammonium metavanadate.
Preferably, the time of described stirring at room temperature is 0.5～10h, for example 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, 8h, 8.5h, 9h or 9.5h.
Preferably, described evaporate to dryness is realized by Rotary Evaporators, and evaporate to dryness temperature is 40～80 ℃, for example 43 ℃, 46 ℃, 49 ℃, 52 ℃, 55 ℃, 58 ℃, 61 ℃, 64 ℃, 67 ℃, 70 ℃, 73 ℃, 76 ℃ or 79 ℃.
Preferably, described dry temperature is 80～120 ℃, for example 83 ℃, 86 ℃, 89 ℃, 92 ℃, 95 ℃, 98 ℃, 101 ℃, 104 ℃, 107 ℃, 110 ℃, 113 ℃, 116 ℃ or 119 ℃, the described dry time is 10～24h, for example 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h or 23h.
Preferably, described roasting is carried out under protective atmosphere, and described protective atmosphere is the combination of any one or at least two kinds in nitrogen, helium or argon gas atmosphere.
Preferably, the temperature of described roasting is 250 ℃～700 ℃, for example 280 ℃, 310 ℃, 340 ℃, 370 ℃, 400 ℃, 430 ℃, 460 ℃, 490 ℃, 520 ℃, 550 ℃, 580 ℃, 610 ℃, 640 ℃, 670 ℃, 700 ℃, 730 ℃, 760 ℃ or 790 ℃, preferably 300 ℃～600 ℃, the time of described roasting is 1～24h, for example 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h or 22h, preferably 2～12h, further preferred 4～6h.
The preparation method of the iron-based activated-carbon catalyst that exemplary vanadium a kind of as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, the mixture of active carbon three by Fe source, V source and after being oxidized is at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 2h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Three of object of the present invention is the purposes of the iron-based activated-carbon catalyst that a kind of vanadium modification as above is provided, and described catalyst is for the SCR (NH of nitrogen oxide
3-SCR) purification process.
Compared with the prior art, the present invention has following beneficial effect:
The iron-based activated-carbon catalyst that the vanadium that the present invention obtains by interpolation vanadium is modified has excellent low temperature NH
3-SCR activity and anti-SO
2poisoning performance, and operating temperature window is wide.Described catalyst is at 150 ℃ of NO that can reach more than 70%
xpurification efficiency, at 175 ℃ of NO that can reach more than 80%
xpurification efficiency, and there is comparatively excellent anti-SO at 200 ℃
2poisoning performance.
In addition, catalyst of the present invention adopts co-impregnation to prepare, simple; Active carbon is cheap, reduces the preparation cost of catalyst.
The specific embodiment
Further illustrate technical scheme of the present invention below by the specific embodiment.
Embodiment 1
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 3%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.3%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 12h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 2
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 3%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.5%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 12h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 3
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 3%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.7%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 12h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 4
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 3%, and the mass percent that described vanadic anhydride accounts for active carbon is 1.0%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 12h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 5
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 0.5%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.5%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 0.5h, at 40 ℃ through Rotary Evaporators evaporate to dryness, at 80 ℃ of dry 24h, then in tube furnace, under nitrogen atmosphere in 250 ℃ of roasting 24h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 6
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 10%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.4%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 10h, at 80 ℃ through Rotary Evaporators evaporate to dryness, at 120 ℃ of dry 10h, then in tube furnace, under nitrogen atmosphere in 700 ℃ of roasting 1h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Embodiment 7
The iron-based activated-carbon catalyst that a kind of vanadium is modified, the active component of described catalyst is iron oxide and vanadic anhydride, carrier is active carbon, and the mass percent that described iron oxide accounts for active carbon is 8%, and the mass percent that described vanadic anhydride accounts for active carbon is 0.6%.
The preparation method of the iron-based activated-carbon catalyst that vanadium as above is modified, described method is co-impregnation, comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after ferric nitrate, ammonium metavanadate and oxidation at stirring at room temperature 5h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 100 ℃ of dry 15h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 12h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
Comparative example 1
A kind of iron-based activated-carbon catalyst, the active component of described catalyst is iron oxide, carrier is active carbon.
The embodiment of the present invention 1～4 adopts simple common dipping method to prepare the iron-based activated-carbon catalyst that a series of vanadium is modified, wherein, the mass percent that described vanadic anhydride accounts for active carbon is respectively 0.3%, 0.5%, 0.7% and 1.0%, and prepare not the catalyst containing the comparative example 1 of vanadium, and investigated this catalyst series at the NOx of 100～250 ℃ of scope homeostasis removal efficiency, and 200 ℃ of this catalyst series are carried out reaching the anti-SO of 12h
2the investigation of ability, finds that a small amount of vanadium of interpolation can significantly improve the anti-sulphur of catalyst.
Get the catalyst of embodiment 1～3 and comparative example 1, catalyst volume 0.5mL, 40～60 orders, put into catalyst activity evaluating apparatus, and activity rating carries out in fixed bed reactors.Simple alternating temperature NH
3-SCR activity experiment reaction atmosphere is 500ppm NH
3, 500ppm NO, 5%O
2, N
2for Balance Air, total flow is 250mL/min, and reaction velocity is 30000h
-1.Test result is in table 1.Anti-sulphur experiment reaction atmosphere is 500ppm NH
3, 500ppm NO, 5%O
2, 100ppmSO
2, reaction temperature is 200 ℃, all the other conditions are the same.Test result is in table 2.
The NH of the catalyst of table 1 embodiment 1～3 and comparative example 1 under different temperatures
3-SCR activity
The sulfur resistance experiment of the catalyst of table 2 embodiment 1～3 and comparative example 1
As from the foregoing:
Catalyst of the present invention is at 150 ℃ of NO that can reach more than 70%
xpurification efficiency, at 175 ℃ of NO that can reach more than 80%
xpurification efficiency, and there is comparatively excellent anti-SO at 200 ℃
2poisoning performance.Wherein, vanadic anhydride accounts for the iron-based activated-carbon catalyst that vanadium that the mass percent of active carbon is 0.5% modifies and in the temperature range of 175 ℃, has more than 80% NO
xpurification efficiency, has excellent anti-SO at 200 ℃
2poisoning performance, and operating temperature window is wide.
Applicant's statement, the present invention illustrates detailed composition of the present invention and method by above-described embodiment, but the present invention is not limited to above-mentioned detailed composition and method, does not mean that the present invention must rely on above-mentioned detailed composition and method could be implemented.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the each raw material of product of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. the iron-based activated-carbon catalyst that vanadium is modified, is characterized in that, the active component of described catalyst is iron oxide and vanadic anhydride, and carrier is active carbon, and the mass percent that described vanadic anhydride accounts for active carbon is greater than 0 and be less than or equal to 1%.
2. catalyst as claimed in claim 1, is characterized in that, the mass percent example that described vanadic anhydride accounts for active carbon is 0～0.7% and do not comprise 0, preferably 0～0.5% and do not comprise 0, further preferably 0.5%;
Preferably, the mass percent that described iron oxide accounts for active carbon is 0～10% and do not comprise 0, preferably 0～8% and do not comprise 0, further preferably 0～5% and do not comprise 0.
3. a preparation method for the iron-based activated-carbon catalyst that vanadium as claimed in claim 1 or 2 is modified, is characterized in that, described method comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, by the mixture of the active carbon three after Fe source, V source and oxidation, in stirring at room temperature, then evaporate to dryness, is dried, and roasting obtains the iron-based activated-carbon catalyst that vanadium is modified.
4. method as claimed in claim 3, is characterized in that, described Fe source is selected from the mixture of any one or at least two kinds in ferric nitrate, ferric sulfate, ferric phosphate or iron chloride, preferably ferric nitrate;
Preferably, described vanadium source is selected from the mixture of any one or at least two kinds in ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium vanadate or sodium pyrovanadate, preferably ammonium metavanadate.
5. the method as described in claim 3 or 4, is characterized in that, the time of described stirring at room temperature is 0.5h～10h.
6. the method as described in one of claim 3-5, is characterized in that, described evaporate to dryness is realized by Rotary Evaporators, and evaporate to dryness temperature is 40 ℃～80 ℃.
7. the method as described in one of claim 3-6, is characterized in that, described dry temperature is 80 ℃～120 ℃, and the described dry time is 10h～24h.
8. the method as described in one of claim 3-7, is characterized in that, described roasting is carried out under protective atmosphere, and described protective atmosphere is the combination of any one or at least two kinds in nitrogen, helium or argon gas atmosphere;
Preferably, the temperature of described roasting is 250 ℃～700 ℃, and preferably 300 ℃～600 ℃, the time of described roasting is 1～24h, preferably 2～12h, further preferred 4～6h.
9. the method as described in one of claim 3-8, is characterized in that, described method comprises the steps:
(1) adopt nitric acid to carry out surface oxidation to active carbon;
(2) under oxalic acid existence condition, the mixture of active carbon three by Fe source, V source and after being oxidized is at stirring at room temperature 2h, at 60 ℃ through Rotary Evaporators evaporate to dryness, at 110 ℃ of dry 12h, then in tube furnace, under nitrogen atmosphere in 500 ℃ of roasting 5h, obtain the iron-based activated-carbon catalyst that vanadium is modified.
10. a purposes for the iron-based activated-carbon catalyst that vanadium as claimed in claim 1 or 2 is modified, is characterized in that, described catalyst is for the SCR purification process of nitrogen oxide.
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| CN114345317A (en) * | 2020-10-13 | 2022-04-15 | 中石化南京化工研究院有限公司 | V/Fe bimetallic desulfurization and denitrification catalyst and preparation method and application thereof |
| CN113522299A (en) * | 2021-05-25 | 2021-10-22 | 宁夏亘峰嘉能能源科技股份有限公司 | Desulfurization, denitrification and mercury removal catalyst and preparation method thereof |
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Application publication date: 20140507 |