CN103990487A - Denitration and demercuration catalyst and preparation method thereof - Google Patents
Denitration and demercuration catalyst and preparation method thereof Download PDFInfo
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- CN103990487A CN103990487A CN201410256006.5A CN201410256006A CN103990487A CN 103990487 A CN103990487 A CN 103990487A CN 201410256006 A CN201410256006 A CN 201410256006A CN 103990487 A CN103990487 A CN 103990487A
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Abstract
The invention provides a denitration and demercuration catalyst and a preparation method thereof. The denitration and demercuration catalyst comprises the following components: 0.5wt%-10wt% of NH4X, 3wt%-7 wt% of YO3, 1 wt%-5 wt% of V2O5, 75 wt%-90 wt% of TiO2, 0.1 wt%-2 wt% of Ge(NO3)4 and 0.1wt%-1.5wt% of auxiliaries, wherein X is Cl or Br, Y is W or Mo; auxiliaries are one or more of CeO2, Nb2O5 and NiO. The denitration and demercuration catalyst disclosed by the invention can satisfy fire coal flue gas denitration and demercuration requirements of multiple industries, is long in service life, low in price and suitable for large-scale industrial production, can reduce equipment installation and operation cost, and avoids the secondary pollution of the catalyst.
Description
Technical field
The present invention relates to a kind of catalyst, relate in particular to a kind of denitration demercuration Catalysts and its preparation method, belong to Air Pollution Control field.
Background technology
Mercury is a kind of hypertoxicity, high volatile volatile and has permanent cumulative noxious material in vivo with in food chain, and the nonvalent mercury in atmosphere can be resided for a long time, thereby mercury pollution receives much concern in global pollution.China is the country of mercury use amount and discharge capacity maximum in the world, and annual mercury emissions, between 500-700 ton, accounts for 30% of global mercury emissions total amount, and wherein coal-burning power plant and Industrial Boiler account for 52% of domestic mercury emissions.The discharge standard that China has set up fire coal boiler fume mercury in " fossil-fuel power plant atmospheric pollutant emission standard " that promulgate in July, 2011 in (GB13223-2011).The existence form of Mercury In Coal Combustion Flue Gas has Elemental Mercury (Hg
0), divalence mercury (Hg
2+) and particle mercury (Hg
p) three kinds.Because the temperature in combustion furnace is high, most mercury are all broken down into Elemental Mercury and are present in flue gas with gaseous form.The divalence mercury of gaseous state is soluble in water, and is easily caught and remove by wet scrubbing system; Particle mercury is easily by removals such as electric cleaners; And Elemental Mercury volatility is high and be insoluble in water, be relatively stable form, therefore the removal of flue gas gaseous elemental mercury is that mercury in flue gas pollutes the difficult point of controlling all the time.
Most domestic coal-burning boiler has been installed electrostatic precipitator and flue gas desulfur device at present, and as installed independent denitration and demercuration control appliance additional, overall operation will produce phase mutual interference, and technical difficulty is increased considerably again, and also have economically infeasibility.Because technical development is limit, the integrated technology that removes of nitrogen oxide and element mercury also rests on laboratory stage substantially, is seldom applied in gas pollution control.
The Chinese patent application CN102366722A announcing on March 7th, 2012, denitrating catalyst of a kind of double demercuration and preparation method thereof is disclosed, it utilizes the halide of vanadium Titanium series catalyst load Fe, Cu etc. to carry out catalytic oxidation to Elemental Mercury, but under hot conditions, Fe, Cu etc. easily change its oxide into, by SO
2catalytic oxidation becomes SO
3.In running, these SO
3meeting and reducing agent NH
3reaction generates thick ammonium sulfate and stops up duct, has reduced the remove ability of catalyst to nitrogen oxide and Elemental Mercury.In the Chinese patent application CN103480371A that on January 1st, 2014 announces, a kind of denitration demercuration Catalysts and its preparation method and application are disclosed, it utilizes ruthenium component to mix and carry out denitration demercuration with Ti-base catalyst, but ruthenium used also can promote SO
2oxidation, and ruthenium is expensive, is easy to again contaminated environment, is not suitable for suitability for industrialized production.
Therefore be necessary to provide a kind of denitration demercuration catalyst, it has general applicability to every profession and trade coal-fired flue-gas, can reduce installation procedure and operating cost, and the secondary pollution of avoiding catalyst to produce, realizes centralized Control.
Summary of the invention
In view of the problem that background technology exists, the object of the present invention is to provide a kind of denitration demercuration Catalysts and its preparation method, it has wider use warm area and stronger anti-SO
2the ability of oxidation, all has and removes efficiently ability nitrogen oxide and Elemental Mercury.
Another object of the present invention is to provide a kind of denitration demercuration Catalysts and its preparation method, and it is cheap, and long service life is applicable to large-scale industrial production.
In order to realize object of the present invention, aspect first, the invention provides a kind of denitration demercuration catalyst of the present invention, it comprises NH
4x, YO
3, V
2o
5, TiO
2, Ge (NO
3)
4and auxiliary agent, wherein X is Cl or Br, and Y is W or Mo, and auxiliary agent is CeO
2, Nb
2o
5or one or more in NiO.
In order to realize object of the present invention, aspect second of the present invention, the invention provides a kind of preparation method of denitration demercuration catalyst, it comprises the following steps: by a certain amount of TiO
2powder, according to TiO
2with the mass ratio of ammonium molybdate or ammonium tungstate be (9.7～24.2): 1 adds in the aqueous solution of ammonium molybdate or ammonium tungstate, after mixing at 150～200 DEG C dry 3～6h, make YO
3-TiO
2presoma; By Ge (NO
3)
4, auxiliary agent, ammonium metavanadate and YO
3-TiO
2being respectively in mass ratio of presoma (0.001～0.02): 1, (0.001～0.018): 1 and (0.013～0.078): 1 ratio takes, and add appropriate water, at 40～60 DEG C, mix, then dry 5～8h at 120～150 DEG C; Dried sample is warming up to 350～450 DEG C by the speed of 1～10 DEG C/min, roasting 4～7h, cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-YO
3-TiO
2; By a certain amount of NH
4x is dissolved in deionized water, adds in SCR denitrating catalyst, mixes and is placed at 50～100 DEG C dry 12h, is then warmed up to 200～300 DEG C and be incubated 5～10h, obtains finished catalyst.
By above technical scheme, beneficial effect of the present invention is as follows:
Catalyst of the present invention has wider active temperature windows and stronger anti-sulfur poisonous performance, and nitrogen oxide and Elemental Mercury are all had and efficiently remove ability therefore, and this catalyst can meet conglomerate coal-fired flue gas denitration demercuration; Long service life, cheap, be applicable to large-scale industrialization and produce;
Catalyst of the present invention can reduce equipment installation and operation expense, avoids the secondary pollution of catalyst.
Detailed description of the invention
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, advantage and disadvantage of the present invention will be more clear along with description.But these embodiment are only exemplary, scope of the present invention are not formed to any restriction.
The following describes according to denitration demercuration Catalysts and its preparation method of the present invention and embodiment.
First explanation denitration demercuration catalyst according to a first aspect of the invention.
Denitration demercuration catalyst according to a first aspect of the invention, comprises NH
4x, YO
3, V
2o
5, TiO
2, Ge (NO
3)
4and auxiliary agent, wherein X is Cl or Br, and Y is W or Mo, and auxiliary agent is CeO
2, Nb
2o
5or one or more in NiO.
In denitration demercuration catalyst according to a first aspect of the invention, NH
4x content is 0.5～10wt%; YO
3content is 3～7wt%; V
2o
5content is 1～5wt%; TiO
2content is 75～90wt%; Ge (NO
3)
4content is 0.1～2wt%; Auxiliary agent content is 0.1～1.5wt%.
In denitration demercuration catalyst according to a first aspect of the invention, NH
4x is preferably NH
4cl, YO
3be preferably MoO
3.
In denitration demercuration catalyst according to a first aspect of the invention, preferably,
NH
4cl content is 3.4～8wt%; MoO
3content is 4～6wt%; V
2o
5content is 2～3wt%; TiO
2content is 80～90wt%; Ge (NO
3)
4content is 0.5～1wt%; Auxiliary agent content is 0.5～1wt%.
The preparation method of denitration demercuration catalyst according to a second aspect of the invention, it is for the preparation of the denitration demercuration catalyst described in first aspect present invention, and it comprises the following steps: by a certain amount of TiO
2powder, according to TiO
2with the mass ratio of ammonium molybdate or ammonium tungstate be (9.7～24.2): 1 adds in the aqueous solution of ammonium molybdate or ammonium tungstate, after mixing at 150～200 DEG C dry 3～6h, make YO
3-TiO
2presoma; By Ge (NO
3)
4, auxiliary agent, ammonium metavanadate and YO
3-TiO
2being respectively in mass ratio of presoma (0.001～0.02): 1, (0.001～0.018): 1 and (0.013～0.078): 1 ratio takes, and add appropriate water, at 40～60 DEG C, mix, then dry 5～8h at 120～150 DEG C; Dried sample is warming up to 350～450 DEG C by the speed of 1～10 DEG C/min, roasting 4～7h, cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-YO
3-TiO
2; By a certain amount of NH
4x is dissolved in deionized water, adds in SCR denitrating catalyst, mixes and is placed at 50～100 DEG C dry 12h, is then warmed up to 200～300 DEG C and be incubated 5～10h, obtains finished catalyst.
In the preparation method of denitration demercuration catalyst according to a second aspect of the invention, X is Cl or Br, and Y is W or Mo, and auxiliary agent is CeO
2, Nb
2o
5or one or more in NiO.
Use NH
4x is as alloy, and under high temperature, Cl or Br atom can be oxidized to Elemental Mercury the divalence mercury of solubility, thereby are absorbed by follow-up wet desulphurization device; NH
4x is to SO
2almost there is no oxidation, and easily decompose under its high temperature, can improve the NH of catalyst surface
3content.
Ge (NO in catalyst
3)
4with prevention sulfur poisoning, extending catalyst service life; The CeO adding
2, Nb
2o
5or the auxiliary agent such as NiO can expand the operative temperature window of catalyst, make it be applicable to the denitration demercuration of conglomerate coal-fired flue-gas.
Embodiment 1
By 85gTiO
2powder, 6.13g ammonium heptamolybdate ((NH
4)
6mo
7o
244H
2o, is equivalent to 5gMoO
3) and 30g water mix, at 180 DEG C, dry 4h, makes 90gMoO
3-TiO
2presoma;
By 1gGe (NO
3)
4, 0.5gCeO
2, 3.21g ammonium metavanadate (is equivalent to 2.5gV
2o
5) and 40g water and the MoO making
3-TiO
2presoma stirs at 50 DEG C, then dry 6h at 130 DEG C;
Dried sample is warming up to 400 DEG C of roasting 5h by the speed of 5 DEG C/min, and cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-MoO
3-TiO
2;
By 6gNH
4cl is dissolved in deionized water, adds in SCR denitrating catalyst, mixes and is placed on dry 12h at 80 DEG C, is then warmed up to 250 DEG C and insulation 8h, obtains afterwards finished catalyst.
Embodiment 2
By 83gTiO
2powder, 7.36g ammonium heptamolybdate (are equivalent to 6gMoO
3) and 30g water mix, at 180 DEG C, dry 4h, makes 89gMoO
3-TiO
2presoma;
By 0.5gGe (NO
3)
4, 0.5gCeO
2, 5.14g ammonium metavanadate (is equivalent to 4gV
2o
5) and 40g water and the MoO making
3-TiO
2presoma stirs at 50 DEG C, then dry 6h at 130 DEG C;
Dried sample is warming up to 400 DEG C of roasting 5h by the speed of 5 DEG C/min, and cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-MoO
3-TiO
2;
By 6gNH
4cl is dissolved in deionized water, adds in SCR denitrating catalyst, mixes and is placed on dry 12h at 80 DEG C, is then warmed up to 250 DEG C and insulation 8h, obtains afterwards finished catalyst.
Embodiment 3
By the TiO of 89g
2powder, 3.68g ammonium heptamolybdate (are equivalent to 3gMoO
3) and 30g water mix, at 180 DEG C, dry 4h, makes 92gMoO
3-TiO
2presoma;
By 0.1gGe (NO
3)
4, 0.1gCeO
2, 5.65g ammonium metavanadate (is equivalent to 4.4gV
2o
5) and 40g water and the MoO making
3-TiO
2presoma stirs at 50 DEG C, then dry 6h at 130 DEG C;
Dried sample is warming up to 400 DEG C of roasting 5h by the speed of 5 DEG C/min, and cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-MoO
3-TiO
2;
By 3.4gNH
4cl is dissolved in deionized water, adds SCR denitrating catalyst, mixes and is placed on dry 12h at 80 DEG C, is then warmed up to 250 DEG C and insulation 8h, obtains afterwards finished catalyst.
Embodiment 4
By the TiO of 75g
2powder, 7.66g ammonium tungstate ((NH
4)
10w
12o
41, be equivalent to 7gWO
3) and 30g water mix, at 200 DEG C, dry 3h, makes 82gWO
3-TiO
2presoma;
By 1.5gGe (NO
3)
4, 1.5gNiO, 6.42g ammonium metavanadate (be equivalent to 5gV
2o
5) and 40g water and the WoO making
3-TiO
2presoma stirs at 40 DEG C, then dry 5h at 150 DEG C;
Dried sample is warming up to 450 DEG C of roasting 4h by the speed of 10 DEG C/min, and cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-WO
3-TiO
2;
By 10gNH
4br is dissolved in deionized water, adds SCR denitrating catalyst, mixes and is placed on dry 12h at 100 DEG C, is then warmed up to 300 DEG C and insulation 5h, obtains afterwards finished catalyst.
Embodiment 5
By 90gTiO
2powder, 6.13g ammonium heptamolybdate (are equivalent to 5gMoO
3) and 30g water mix, at 150 DEG C, dry 6h, makes 95gMoO
3-TiO
2presoma;
By 2gGe (NO
3)
4, 1.5gNb
2o
5, 1.28g ammonium metavanadate (is equivalent to 1gV
2o
5) and 40g water and the MoO making
3-TiO
2presoma stirs at 60 DEG C, then dry 8h at 120 DEG C;
Dried sample is warming up to 350 DEG C of roasting 7h by the speed of 1 DEG C/min, and cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-MoO
3-TiO
2;
By 0.5gNH
4cl is dissolved in deionized water, adds SCR denitrating catalyst, mixes and is placed on dry 12h at 50 DEG C, is then warmed up to 200 DEG C and insulation 10h, obtains afterwards finished catalyst.
Catalyst synthetic in embodiment 1～5 is carried out respectively to activity test in fixed bed reactors, and catalyst in reactor useful load is 1ml, heavily about 1g, temperature programming instrument control reaction temperature processed.
Configuration component and the following simulated flue gas of concentration:
C
nOx=C
nH3=0.045%, C
hg=40 μ g/L, C
o2≈ 4.8%, C
h2O≈ 6.0%, C
sO2≈ 0.05%, C
cO2≈ 12%, C
hCl≈ 0.002%, N
2as Balance Air, air speed GHSV20000h
-1.This simulated flue gas does not comprise flue dust, and other components and actual flue gas composition are basically identical.
Utilize above simulated flue gas to measure Hg at 200 DEG C, 250 DEG C, 300 DEG C, 350 DEG C, 400 DEG C, 450 DEG C
0oxygenation efficiency, NO
xremoval efficiency and SO
2/ SO
3conversion ratio, after stable reaction conditions 10h, measure, the results are shown in Table 1～table 3.
Table 1 is Hg at each temperature
0conversion rate of oxidation (%)
As seen from Table 1, use the synthetic catalyst (embodiment 1～5) of the present invention, Hg in the time of 200 DEG C
0conversion rate of oxidation be more than 81%, and along with the rising of reaction temperature, its conversion ratio further improves, more than 300 DEG C time, conversion ratio is 90% left and right.
Table 2 is NO at each temperature
xremoval efficiency (%)
Table 3 is SO at each temperature
2/ SO
3conversion ratio (%)
From table 2 and table 3, flue-gas temperature, within the scope of 200～450 DEG C, adopts catalyst of the present invention (embodiment 1～5), and in coal-fired flue-gas, the removal efficiency of nitrogen oxide reaches more than 80%, SO/SO
3conversion ratio be less than 1.2%.
It will be understood by those skilled in the art that lower without departing from the spirit and scope of the present invention and can the details of technical solution of the present invention and form be modified or be replaced, but these amendments and replacement all fall within the scope of protection of the present invention.
Claims (6)
1. a denitration demercuration catalyst, is characterized in that, comprises NH
4x, YO
3, V
2o
5, TiO
2, Ge (NO
3)
4and auxiliary agent, wherein X is Cl or Br, and Y is W or Mo, and auxiliary agent is CeO
2, Nb
2o
5or one or more in NiO.
2. denitration demercuration catalyst according to claim 1, is characterized in that,
NH
4x content is 0.5～10wt%; YO
3content is 3～7wt%; V
2o
5content is 1～5wt%; TiO
2content is 75～90wt%; Ge (NO
3)
4content is 0.1～2wt%; Auxiliary agent content is 0.1～1.5wt%.
3. denitration demercuration catalyst according to claim 1, is characterized in that,
NH
4x is preferably NH
4cl, YO
3be preferably MoO
3.
4. according to the denitration demercuration catalyst described in claim 2 or 3, it is characterized in that,
NH
4cl content is 3.4～8wt%; MoO
3content is 4～6wt%; V
2o
5content is 2～3wt%; TiO
2content is 80～90wt%; Ge (NO
3)
4content is 0.5～1wt%; Auxiliary agent content is 0.5～1wt%.
5. a preparation method for denitration demercuration catalyst, it prepares denitration demercuration catalyst according to claim 1, and it comprises the following steps:
By a certain amount of TiO
2powder, according to TiO
2with the mass ratio of ammonium molybdate or ammonium tungstate be (9.7～24.2): 1 adds in the aqueous solution of ammonium molybdate or ammonium tungstate, after mixing at 150～200 DEG C dry 3～6h, make YO
3-TiO
2presoma;
By Ge (NO
3)
4, auxiliary agent, ammonium metavanadate and YO
3-TiO
2being respectively in mass ratio of presoma (0.001～0.02): 1, (0.001～0.018): 1 and (0.013～0.078): 1 ratio takes, and add appropriate water, at 40～60 DEG C, mix, then dry 5～8h at 120～150 DEG C;
Dried sample is warming up to 350～450 DEG C by the speed of 1～10 DEG C/min, roasting 4～7h, cooling rear grinding, obtains the wide warm area SCR denitrating catalyst V of sulfur poisoning-resistant
2o
5-YO
3-TiO
2;
By a certain amount of NH
4x is dissolved in deionized water, adds in SCR denitrating catalyst, mixes and is placed at 50～100 DEG C dry 12h, is then warmed up to 200～300 DEG C and be incubated 5～10h, obtains finished catalyst.
6. a kind of preparation method according to claim 5, is characterized in that,
X is Cl or Br, and Y is W or Mo, and auxiliary agent is CeO
2, Nb
2o
5or one or more in NiO.
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| CN104841417A (en) * | 2015-04-10 | 2015-08-19 | 武汉大学 | Simultaneous denitration and demercuration catalyst and preparation method thereof |
| CN106362732A (en) * | 2016-08-30 | 2017-02-01 | 山东海润环保科技有限公司 | Denitration and demercuration catalyst |
| CN109692684A (en) * | 2019-01-28 | 2019-04-30 | 大唐南京环保科技有限责任公司 | A kind of denitration demercuration catalyst and preparation method thereof |
| CN111356525A (en) * | 2017-11-14 | 2020-06-30 | 优美科股份公司及两合公司 | SCR catalyst |
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| CN104841417A (en) * | 2015-04-10 | 2015-08-19 | 武汉大学 | Simultaneous denitration and demercuration catalyst and preparation method thereof |
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| CN109692684A (en) * | 2019-01-28 | 2019-04-30 | 大唐南京环保科技有限责任公司 | A kind of denitration demercuration catalyst and preparation method thereof |
| CN109692684B (en) * | 2019-01-28 | 2022-03-04 | 大唐南京环保科技有限责任公司 | Denitration and demercuration catalyst and preparation method thereof |
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Application publication date: 20140820 |