CN106955712B - A kind of Fe-Ce based composite catalyst and preparation method thereof suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique - Google Patents
A kind of Fe-Ce based composite catalyst and preparation method thereof suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique Download PDFInfo
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Abstract
The Fe-Ce based composite catalyst and preparation method thereof that the invention discloses a kind of suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique.The composite catalyst is with Al2O3‑TiO2For complex carrier, load active component Fe2O3‑CeO2Made of.A kind of preparation method suitable for vulcanizing the Fe-Ce based composite catalyst of hydrogen catalysis reduction and desulfurization denitrating technique is also disclosed simultaneously comprising following steps: 1) first prepares complex carrier Al2O3‑TiO2；2) composite catalyst Fe is prepared after2O3‑CeO2/Al2O3‑TiO2.Catalyst process prepared by this method is relatively easy, convenient for industrial large-scale production, and in lower 160 DEG C -240 DEG C this common Industrial Catalysis temperature sections, it is able to achieve to the preferable simultaneous removing of the two, therefore economic value with higher and promotional value.And the later period can be by further modified catalyst, the content including further increasing or reducing Ce and Fe, or the micro other components of addition, or even optimization reaction condition, realizes the conversion ratio of higher nitrogen oxides and sulfide.
Description
Technical field
The Fe-Ce based composite catalyst that the present invention relates to a kind of suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique and its
Preparation method.
Background technique
It is well known that a large amount of nitrogen oxides (NOx) and sulfide (mainly SO caused by coal-fired boiler combustion2) can lead
The aggravation of haze and photochemical fog is caused, and huge harm is caused to the health of the mankind.In addition, all kinds of discharge standards also by
Year increases.Therefore, it is necessary to in flue gas nitrogen oxides and the removing that synchronizes of sulfide so that their concentration reaches
The standard that can be discharged.
Currently, synchronized desulfuring and denitrifying method used in industry is usually based on wet process, such methods are mainly used
Solution with oxidisability is absorbing solubility SO2While insoluble NOx (mainly NO) is oxidized to it is soluble
NOx (mainly NO2) and absorbed.However, such methods, since equipment usually takes up a large area, maintenance cost is high, in addition
Absorbing liquid needs the reasons such as long-term replacement, leads to universal higher cost, thus and be not implemented large-scale and promote.And catalytic desulfurization
Denitration rule can overcome above-mentioned various drawbacks, thus just become the hot spot of current research and extension.Wherein, industrial common single
Only catalytic desulfuriation is Claus method, and used reducing agent is H2S.And individually catalytic denitration is then SCR method, used goes back
Former agent is NH3.But above-mentioned method causes catalyst and process flow used also endless since reducing agent used is different
It is exactly the same, thus it is difficult to realize the simultaneous removing of nitrogen oxides and sulfide.In addition, H2, CO, CxHy etc. also ammonia can be replaced real
Now to the removing of nitrogen oxides.But the price of this kind of gas is costly, and keeping and transport are inconvenient.In addition, this kind of urge
Catalyst needed for changing reaction is usually precious metal based catalysts, and cost is higher compared to common oxide catalyst.Above-mentioned
All kinds of technical bottlenecks also limit its further research, development and popularization to a certain extent.In fact, since Claus is anti-
Strong reductant H in answering2S can effectively be realized to SO2Removing, therefore inventors believe that, in the effect of suitable catalyst
Under, H2S is also able to achieve the removing to NO.Reaction equation is as follows:
H2S+NO→S+N2+H2O
As can be seen that it is nontoxic N that above-mentioned reaction is generated2And S, therefore there is the value further studied.In early days
There is document report with Al2O3As catalyst, it is able to achieve above-mentioned reaction.And the H invented before2Flue gas of the S as reducing agent
Catalytic desulfurization and denitrification technique shows H2S, which can be used as reducing agent, may be implemented synchronous desulphurization denitration, and H2S can pass through work
The preparation of industry enterprise sewage disposal process, can be significantly reduced the cost of flue gas desulfurization and denitrification.But since the invented technology uses
Catalyst is 4A molecular sieve, and catalytic temperature is 600 DEG C -700 DEG C, reduces the cost advantage of this new technology.Therefore, it studies
New catalyst, improving reaction efficiency, reducing reaction temperature is the task of top priority.
Currently, the research of iron (Fe) is relatively more in the research of SCR catalyst, it is not only because its cheap, list
Only denitration effect is good, and it can significantly improve the performance of other catalyst as auxiliary agent or auxiliary element, while reduce reaction
Temperature.And rare-earth element cerium (Ce) is due to its special crystal structure, so that it is with stronger oxygen storage capacity, and preferable
Redox catalysis activity.Therefore, in conjunction with factors above, present invention selection prepares compound the two of the Fe and Ce of various different ratios
The catalyst prepared is then used for H by component catalyst2The synchronized desulfuring and denitrifying of S is tested, to reach the two while remove
Purpose.
Summary of the invention
The Fe-Ce base that the purpose of the present invention is to provide a kind of suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique is compound
Catalyst and preparation method thereof.Being intended to overcome present in catalytic desulfurization and denitrification technology at this stage simultaneously to take off it
It removes and low temperature conversion rate is not high, the high temperature section technological deficiencies such as energy consumption is high.
The technical solution used in the present invention is:
A kind of Fe-Ce based composite catalyst suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique, is with Al2O3-TiO2
For complex carrier, load active component Fe2O3-CeO2Made of.
In the complex carrier, Al2O3With TiO2Molar ratio be 1:1.
Active component Fe2O3-CeO2Load capacity be 8wt%~12wt%.
The catalytic temperature of catalyst is 160 DEG C~240 DEG C.
A kind of preparation side suitable for vulcanizing the Fe-Ce based composite catalyst of hydrogen catalysis reduction and desulfurization denitrating technique
Method, comprising the following steps:
1) complex carrier Al is first prepared2O3-TiO2；
2) composite catalyst Fe is prepared after2O3-CeO2/Al2O3-TiO2。
In step 1), the Al2O3-TiO2It is to be prepared with aluminium salt and titanate esters by sol-gel method.
In step 1), the aluminium salt is aluminum nitrate；The titanate esters are butyl titanate；The aluminum nitrate and titanium
The molar ratio of sour four butyl esters is 2:1.
In step 2), the composite catalyst Fe2O3-CeO2/Al2O3-TiO2Be molysite and cerium salt mixing after, then with
Complex carrier Al2O3-TiO2It is prepared by equi-volume impregnating.
In step 2), the molysite is ferric nitrate；The cerium salt is cerous nitrate.
The active component Fe2O3With CeO2Mass ratio be (2~8): (8~2).
The beneficial effects of the present invention are:
The present invention utilizes H2S is reducing agent, by first preparing complex carrier, then prepares Fe-Ce based composite catalyst
Method realizes the simultaneous removing to nitrogen oxides and sulfide in flue gas.High installation and maintenance cost compared to wet process,
The unicity and limitation of Claus and SCR technology, and the higher catalyst cost faced are based oneself upon.
Catalyst process prepared by this method is relatively easy, convenient for industrial large-scale production, and lower 160
DEG C -240 DEG C of this common Industrial Catalysis temperature sections, are able to achieve to the preferable simultaneous removing of the two, therefore warp with higher
Ji value and promotional value.And the later period can be by further modified catalyst, including further increasing or reducing Ce's and Fe
Content, or the micro other components of addition, also replaceable component, becomes tungsten and cerium or iron and cobalt.Essentially consisting in can be after
The continuous method by this two kinds of metals of load changes ratio, finds better catalyst.Such as even optimize reaction condition, it is real
The conversion ratio of existing higher nitrogen oxides and sulfide.
Detailed description of the invention
Fig. 1 is the evaluating apparatus flow chart of catalyst of the present invention；
Fig. 2 is NO and SO of the present invention2Conversion ratio figure.
Specific embodiment
A kind of Fe-Ce based composite catalyst suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique, is with Al2O3-TiO2
For complex carrier, load active component Fe2O3-CeO2Made of.
Preferably, in the complex carrier, Al2O3With TiO2Molar ratio be 1:1.
Preferably, active component Fe2O3-CeO2Load capacity be 8wt%~12wt%；Most preferably, active component
Fe2O3-CeO2Load capacity be 10wt%.Load capacity, that is, the active component accounts for the mass fraction of catalyst gross mass.
Preferably, the catalytic temperature of catalyst is 160 DEG C~240 DEG C.
A kind of preparation side suitable for vulcanizing the Fe-Ce based composite catalyst of hydrogen catalysis reduction and desulfurization denitrating technique
Method, comprising the following steps:
1) complex carrier Al is first prepared2O3-TiO2；
2) composite catalyst Fe is prepared after2O3-CeO2/Al2O3-TiO2。
Preferably, in step 1), the Al2O3-TiO2It is to be prepared with aluminium salt and titanate esters by sol-gel method
At.
Preferably, in step 1), the aluminium salt is aluminum nitrate；The titanate esters are butyl titanate；The nitre
The molar ratio of sour aluminium and butyl titanate is 2:1；Further, the aluminum nitrate is Al (NO3)3·9H2O；The metatitanic acid
Four butyl esters are Ti (OC4H9)4。
Preferably, in step 2), the composite catalyst Fe2O3-CeO2/Al2O3-TiO2It is that molysite and cerium salt are mixed
Afterwards, then with complex carrier Al2O3-TiO2It is prepared by equi-volume impregnating.
Preferably, in step 2), the molysite is ferric nitrate；The cerium salt is cerous nitrate；Further, described
Ferric nitrate is Fe (NO3)3·9H2O；The cerous nitrate is Ce (NO3)3·6H2O。
Preferably, the active component Fe2O3With CeO2Mass ratio be (2~8): (8~2)；It is further preferred that
The active component Fe2O3With CeO2Mass ratio be 2:8,5:5 or 8:2 one of which；Most preferably, the activity
Component Fe2O3With CeO2Mass ratio be 5:5.
The contents of the present invention are described in further detail below by way of specific embodiment.
Embodiment:
A- complex carrier AT (Al2O3-TiO2) preparation method:
(1) in the beaker of 250ml, 2.4molC is sequentially added2H5OH、0.9molCH3COOH and 1.8mol deionization
Water, then by its uniform stirring 1min until being mixed thoroughly, to prepare mixed solvent.
(2) Al (NO of 0.2mol is weighed3)3·9H2O is then poured into the in the mixed solvent of above-mentioned preparation, stirring, directly
To whole dissolutions.
(3) by the Ti (OC of 0.1mol4H9)4It is slowly added dropwise and above-mentioned has dissolved Al (NO3)3·9H2The mixed solution of O
In.It is stirred after adding, is stood, until forming single uniform mixed solution.
(4) above-mentioned solution is put into magnetic stirring apparatus and carries out heating stirring, until solution is completely solidified into white size
Until shape object.
(5) the white gum object of generation is aged 12h, is subsequently placed into 110 DEG C of baking oven and is dried, it is white until being formed
Coloured particles object.
(6) white particulate material after above-mentioned drying is put into crucible, then calcines 4h in 550 DEG C of Muffle furnace.
(7) calcined product is sieved, takes the particle of 20-40 mesh size, in case further use.
Preparation method (the active component CeO of b- composite catalyst CeFe-AT2And Fe2O3Total load amount be 10%):
(1) it is uniformly layered on culture dish by the finished product carrier AT4.5g for weighing above-mentioned preparation.
(2) several (Fe (NO of predecessor are weighed3)3·9H2O and Ce (NO3)3·6H2O, needed for the catalyst of different ratio
Quality is different, and specific value see the table below), it pours into the beaker of 10ml, the deionized water that 5ml is then added is dissolved.
(3) above-mentioned precursor solution is uniformly added drop-wise on carrier AT dropwise, guarantee carrier is in completely wet
State.
(4) above-mentioned particulate matter is put into 110 DEG C of baking oven and is dried, until quality is no longer changed.
(5) solid after drying is put into crucible, then calcines 4h in 550 DEG C of Muffle furnace.
(6) calcined solid is sieved again, takes the particle of 20-40 mesh size, as the Fe-Ce base catalysis of finished product
Agent.
The evaluating apparatus and method of c- catalyst performance:
Attached drawing 1 is the evaluating apparatus flow chart of catalyst of the present invention.In Fig. 1,1.Ar steel cylinder；2.H2S steel cylinder；3.SO2Steel
Bottle；4.NO steel cylinder；5.O2Steel cylinder；6. flow regulator；7. gas bottle；8. electric heater；9. thermoregulator；10. quartzy glass
Glass reaction tube；11. thermocouple；12. sulphur powder absorption bottle；13. lye absorption bottle；14. gas buffer bottle；15. flue gas analysis
Instrument.
Due to H2S and SO2The molar ratio of reaction is 2:1, and H2The molar ratio of S and NO reaction is 1:1, therefore, H2S、SO2With
The molar ratio of NO three's reaction is 3:1:1.In the present invention, controlling its concentration is respectively 1500ppm, 500ppm and 500ppm.
And in order to reach the concentration, the numerical value in Flow Measurement Display Meter need to be adjusted.Specific method is incited somebody to action in the case where not heating
Empty glass tube is connected on heater, is then turned on carrier and three kinds of reaction gas, with flue gas analyzer measure its concentration (its according to
According to for low temperature, in the case where no catalyst, three hardly happens reaction), then stream is adjusted by adjusting Flow Measurement Display Meter
Amount makes its registration stablize the concentration or so in needs.In practice, by adjusting, the H finally obtained2S、SO2With the practical stream of NO
Amount is respectively 15.3ml/min, 5.0ml/min, 2.76ml/min.
After having adjusted registration, catalyst can be evaluated.The quartz glass reaction Guan Gu of catalyst will be housed first
It is scheduled on electric heater.And the catalyst in glass tube need to be fixed in glass tube with silica wool, the used in amounts of silica wool will fit
In, dosage will lead to greatly very much air-flow and be difficult to pass through, and dosage is too small, will lead to filler and is dispelled by air-flow.And glass tube needs closely
Fixation, cause safety accident with anti-gas-leak.
After completing the above item, Flow Measurement Display Meter and Ar carrier gas are opened, the pointer of pressure gauge is made to reach 0.1Mpa, it is therefore an objective to
Flushing pipeline, required time are about 30min.Thermoregulator is opened simultaneously, setting reaction required temperature is (due to the lag of temperature control
Property, the temperature being normally set up will be lower than reaction required temperature, and required temperature is lower, and the temperature difference of the two is bigger), when temperature liter
When to required reaction temperature, then set temperature is transferred to the reaction temperature.Reacting gas steel cylinder is opened simultaneously, makes its pressure gauge
Pointer reach 0.2Mpa.
Then, flue gas analyzer is opened, and connects air inlet pipe and escape pipe, after its test program is stablized, by air inlet pipe
One connection of the escape pipe of one and reaction system, to measure the concentration of gas.It should be noted that since the reaction can give birth to
At a large amount of solid sulfur, and since gas velocity is larger (flow of Ar is 500ml/min), it will lead to a large amount of sightless sulphur of naked eyes
Sulphur particle is blown out, if being directly connected to instrument, be will lead to a large amount of particles and is entered in instrument and damage sensor, causes data inaccurate
True even instrument failure.Therefore, it is necessary to the gas outlets in reaction system to add one layer of filter membrane, to filter out tiny drusen.
In addition, in order to guarantee that data are as accurate as possible, the measurement of each temperature section requires to reach the temperature in reaction temperature
It is measured after 30min.
The evaluation result of d- catalyst performance:
Attached drawing 2 is NO and SO of the present invention2Conversion ratio figure.From figure 2 it can be seen that in 160 DEG C -240 DEG C this temperature
In section, the conversion ratio of NO is significantly raised as the temperature rises, and SO2Conversion ratio only occur as the temperature rises it is light
Micro- decline is all close to or up to 100% in most of temperature section, is totally maintained at 90% or more.And more different match
The CeFe catalyst of ratio is it can be found that the either removal efficiency of NO or SO2Removal efficiency, in addition Fe5Ce5-AT is better than
The two, and about 95% denitration efficiency and about 85% desulfuration efficiency are realized in 220 DEG C -240 DEG C this temperature ranges.Cause
This, it is believed that Fe5Ce5-AT is appropriate two-component catalyst, can preferably realize and synchronize in some temperature range
Desulphurization denitration.
The most suitable synchronized desulfuring and denitrifying catalyst of the present invention is Fe5Ce5-AT, most suitable to urge in 220 DEG C of -240 DEG C of temperature sections
The desulfuration efficiency of agent is 95% or so, and denitration efficiency is 85% or so.
Claims (7)
1. a kind of Fe-Ce based composite catalyst suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique, it is characterised in that: be with
Al2O3-TiO2For complex carrier, load active component Fe2O3-CeO2Made of；
In the complex carrier, Al2O3With TiO2Molar ratio be 1:1；Active component Fe2O3-CeO2Load capacity be 8wt%
~12wt%；The catalytic temperature of catalyst is 160 DEG C~240 DEG C.
2. a kind of Fe-Ce based composite catalyst suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique described in claim 1
Preparation method, it is characterised in that: the following steps are included:
1) complex carrier Al is first prepared2O3-TiO2；
2) composite catalyst Fe is prepared after2O3-CeO2/Al2O3-TiO2。
It is urged 3. a kind of Fe-Ce base suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique according to claim 2 is compound
The preparation method of agent, it is characterised in that: in step 1), the Al2O3-TiO2It is solidifying by colloidal sol-with aluminium salt and titanate esters
Made of the preparation of glue method.
It is urged 4. a kind of Fe-Ce base suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique according to claim 3 is compound
The preparation method of agent, it is characterised in that: in step 1), the aluminium salt is aluminum nitrate；The titanate esters are four fourth of metatitanic acid
Ester；The molar ratio of the aluminum nitrate and butyl titanate is 2:1.
It is urged 5. a kind of Fe-Ce base suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique according to claim 2 is compound
The preparation method of agent, it is characterised in that: in step 2), the composite catalyst Fe2O3-CeO2/Al2O3-TiO2It is iron
Salt and cerium salt mixing after, then with complex carrier Al2O3-TiO2It is prepared by equi-volume impregnating.
It is urged 6. a kind of Fe-Ce base suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique according to claim 5 is compound
The preparation method of agent, it is characterised in that: in step 2), the molysite is ferric nitrate；The cerium salt is cerous nitrate.
It is urged 7. a kind of Fe-Ce base suitable for vulcanizing hydrogen catalysis reduction and desulfurization denitrating technique according to claim 6 is compound
The preparation method of agent, it is characterised in that: the active component Fe2O3With CeO2Mass ratio be (2~8): (8~2).
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| CN110252317B (en) * | 2019-07-04 | 2021-07-13 | 福州大学 | Ce-Fe-based catalyst for efficiently removing nitrogen oxides at low temperature |
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