CN106540693A - A kind of catalyst of low temperature Synergistic degradation bioxin and NOx and preparation method thereof - Google Patents
A kind of catalyst of low temperature Synergistic degradation bioxin and NOx and preparation method thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- 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
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
The invention discloses catalyst of a kind of low temperature Synergistic degradation bioxin and NOx and preparation method thereof, belongs to garbage incinerating tail gas Treatment process field.The catalyst carrier is titania nanoparticles and titanium nanotube, and main active component is cerium oxide, vanadic anhydride and Pt.Catalyst aims temperature of the present invention is 140～300 DEG C, SO2Content is higher than 500mg/Nm3And the garbage incinerating tail gas containing dust, more than 95% bioxin purification efficiency and more than 80% NOx purification efficiencies can be reached, energy Shi dioxin emissions are less than 0.1ng I TEQ/Nm3, NOx emission can be made to be less than 150mg/Nm3。
Description
Technical field
The invention belongs to garbage incinerating tail gas Treatment process field, is related to a kind of for low temperature synergistic purification waste incineration tail
The catalyst of gas Zhong bioxin and NOx.
Background technology
With the fast development of social economy, China city and residents in rural community yield rapid growth.At house refuse
Reason method mainly has landfill, compost, burning etc..Burning disposal has that floor space is little, volume reduction weight-loss ratio high, processing speed is fast,
It is innoxious it is thorough, applied widely, can heat supply various advantages such as generate electricity, be at home and abroad widely used, and accounting more and more higher.It is raw
Inevitably result from containing NOx, SO in Refuse Incineration Process living2Various dirts such as, bioxin, heavy metal, HCl, particulate matter
The tail gas of dye thing.In order to control garbage incinerating tail gas pollutant emission, China formulates《Consumer waste incineration Environmental capacity mark
It is accurate》(GB 18485-2014), the emission limit of the wherein multiple pollutant such as bioxin, NOx are extremely low, it is necessary to using efficient end
End control technology.Country's external enwergy makes bioxin reach 0.1ng I-TEQ/Nm at present3The technology of discharge standard has two classes, and a class is
Active carbon adsorption technology, is sprayed by active carbon powder or adsorbent bed filters bioxin, and another kind of is catalytic oxidation technologies,
Bioxin is decomposed into into CO in the presence of catalyst2、H2The inorganic non-toxic products such as O, HCl.The most NOx of current domestic and international application
Purification techniques has two classes, and a class is SCR technology, in the presence of catalyst, is reduced using ammonia (or urea)
Agent is by NOxSelective reduction is harmless N2And H2O, another kind of is SNCR technology, in the position of suitable temperature
Reducing agent is sprayed into, without the need for catalyst, the NH discharged using reducing agent at 800～1100 DEG C3Optionally by NOxIt is reduced to nothing
Harmful N2。
The core of catalysis technique is catalyst development.Patent 200310118979.4 discloses a kind of removing incinerator
The catalyst of dioxin in discharge waste gas, the component and percetage by weight of the catalyst are:V2O51-5%, WO31-8%,
MoO30.5-1.5%, SiO21-5%, remaining be TiO2.The catalyst can have under lower temperature and higher gas air speed well
Activity, and Jing long-time using remain to activity it is constant.Patent 200910068963.4 is disclosed for removing waste incineration
Catalyst of dioxin and preparation method thereof in kiln gas, catalyst with volcanic rock as carrier, first back loading two on this carrier
Titanium oxide and V2O5, wherein catalyst component is V2O5, TiO2For supported V2O5Carrier.Initially with sol-gel process or
The even precipitation method are by TiO2It is supported on volcanic rock, then using infusion process by V2O5It is supported on TiO2On carrier.Patent
200910097149.5 disclose a kind of catalyst and its preparation side of the nitrogen oxides and organic pollution for removing discharged in burning
Method, with CNT and aluminum oxide as carrier, the catalyst with the oxide of manganese as active component is active in catalyst for catalyst
Component accounts for the 1～10% of catalyst gross mass, is prepared using solvent-thermal method.Patent CN201310751629.5 discloses a kind of whole
Body Shi bioxin Removal of catalyst and preparation method thereof, the catalyst are vanadium-tungsten-titanium System Catalyst, in 160～180 DEG C of bars
The conversion ratio for decomposing bioxin under part reaches more than 95%.Patent 201510053040.7 discloses a kind of catalytic decomposition rubbish and burns
Burn tail gas in bioxin catalyst preparation method, the catalyst with CNT as main carriers, with VOx, WOx, MnOx,
TiO2For main active catalytic component, it is vanadium-tungsten-manganese-titanium catalyst system.Patent application CN201510290287.0 is disclosed
A kind of rare earth base complex multi-component denitration, Tuo bioxin catalyst and preparation method thereof, the catalyst with titanium dioxide, silica flour is
Carrier, the compound with the compound of tungsten, the compound of vanadium, the compound of cerium and lanthanum is as active component, but the catalyst pair
The clean-up effect of bioxin and NOx and using temperature range and do not specify.
The content of the invention
It is an object of the invention to provide the catalyst of a kind of low temperature Synergistic degradation bioxin and NOx, with existing patent skill
The component of art is different, lower, wider using temperature range, higher to the adaptability of actual exhaust gas situation.
The catalyst of a kind of low temperature Synergistic degradation bioxin and NOx, is made up of the following raw material by percentage to the quality：
Titania nanoparticles, 20～95wt%；
Titanium nanotube, 1～50%wt%；
The compound of cerium, 1～44wt%；
The compound of vanadium, 0.5～8wt%；
The compound of Pt, 0.02～0.5wt%.
On the premise of raw material summation is 100%, the consumption of the titanium nanotube is preferably 20～50%.
The compound of Pt is preferably 0.05～0.25%.
The compound amount of cerium is preferably 15～25wt%.It is further preferred that by percentage to the quality by following original
Material is made：
Titania nanoparticles, 45～55wt%；
Titanium nanotube, 20～30%wt%；
The compound of cerium, 15～25wt%；
The compound of vanadium, 2～3wt%；
The compound of Pt, 0.05～0.25wt%.
Under above-mentioned further preferred raw material proportioning, the catalyst various aspects of performance for preparing is more preferable.
Most preferably, measure percentages to be made up of the following raw material：
Titania nanoparticles, 51.65wt%；
Titanium nanotube, 26.26%wt%；
The compound of cerium, 19.65wt%；
The compound of vanadium, 2.25wt%；
The compound of Pt, 0.19wt%.
The catalyst of the present invention is made up of carrier and active component, and carrier is titania nanoparticles and titanium nanotube
Mixture, active component are cerium oxide, vanadic anhydride and Pt.Titania nanoparticles particle diameter be 5～50nm, specific surface area
For 40～300cm2/g.Titanium nanometer bore be 1～15nm, wall thickness be 0.5～5nm, length be 30～200nm, specific surface area
For 150～700cm2/g。
The addition of the titanium nanotube in carrier is according to SO in tail gas2Concentration Huo bioxin concentration is adjusted, used as excellent
Choosing, SO in tail gas2When the higher Huo bioxin concentration of concentration is higher, the mass fraction of titanium nanotube is not less than 20%.
The present invention also provides a kind of preparation method of the catalyst of low temperature Synergistic degradation bioxin and NOx, including following step
Suddenly：
(1) titania nanoparticles and titanium nanotube are weighed by proportioning, add excessive water retting, be uniformly mixed,
Obtain catalyst carrier；
(2) compound of the compound of cerium, the compound of vanadium, platinum is dissolved in by proportioning in 60-80 DEG C of deionized water and is matched somebody with somebody
Solution is set to, catalyst carrier is added under vigorous stirring, stirring is further continued for 4～12 hours, is then dried, last 350～600
DEG C roasting 3～6 hours.
The present invention also provides another kind of preparation method of the catalyst of low temperature Synergistic degradation bioxin and NOx, including as follows
Step：
(1) titania nanoparticles and titanium nanotube are weighed by proportioning, add excessive water retting, be uniformly mixed,
Obtain catalyst carrier；
(2) compound of cerium is dissolved in deionized water by proportioning, adds catalyst carrier under vigorous stirring, continue to stir
Mix 4～12 hours, dry, 350～600 DEG C of roastings 3～6 hours, grind into powder；
(3) compound of vanadium is dissolved in saturated oxalic acid solution by proportioning, is stirred 1 hour, be subsequently adding step (2) described
Powder, continue stirring 4～12 hours, drying, 350～600 DEG C of roastings 3～6 hours, grind to form particle diameter less than 0.45mm
Grain；
(4) compound of platinum is dissolved in deionized water by proportioning, is subsequently adding step (3) particle, continue stirring 4
～12 hours, drying, 350～600 DEG C of roastings 3～6 hours.
Preferably, preparing titanium nanotube using highly basic hydro-thermal method, comprise the steps：5 are made by NaOH soluble in water
The strong base solution of～15mol/L, adds TiO in strong base solution2Particle, stirring are obtained suspension, TiO2Particle and strong base solution
Ratio control in 10～50g/L.Hydro-thermal process is carried out to suspension, the hydro-thermal time is 18～36 hours, and hydrothermal temperature is 120
～180 DEG C.Sample after hydro-thermal is washed to acidity with 0.1mol/L watery hydrochloric acid.Finally drying obtains titanium nanotube.
It is further preferred that the concentration of strong base solution is 10mol/L, TiO2Particle with the mass volume ratio of strong base solution is
30g/L, the hydro-thermal reaction time are 28 hours, and temperature is 150 DEG C.
Preferably, the compound of cerium is the one kind in cerium oxide, cerous nitrate, cerium oxalate and ammonium ceric nitrate
Preferably, the compound of vanadium is the one kind in ammonium metavanadate and vanadic anhydride.
Preferably, the compound of platinum is chloroplatinic acid.
In order to prepare integral catalyzer needs, stearic acid, glass can be added on the basis of catalyst main component
The auxiliary agents such as fiber, lactic acid, glycerine.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) catalyst carrier of the present invention has larger specific surface area, is conducive to being uniformly distributed for active material.Conventional business
With titania support specific surface area about 40～60cm2/ g, catalyst carrier specific surface area of the present invention are 40～280cm2/g。
(2) catalyst Dui bioxin of the present invention has a stronger adsorption capacity, and the capillary absorption characteristic of titanium nanotube can be by
Bioxin is adsorbed in catalyst, is conducive to quickly carrying out for catalytic oxidation.
(3) catalyst carrier of the present invention has stronger to the material that dust, sulphur ammonium salt etc. may reduce catalyst performance
Isolating power, can avoid these materials from entering catalytic inner, thus catalyst stability and the life-span it is excellent.
(4) there is between two kinds of carriers of catalyst of the present invention, various active material strong interaction, active material and load
Also there is between body strong interaction, the redox ability of catalyst is improved.Titania nanoparticles have preferable
Resistance to SO_2 and mechanical strength, but specific surface area is less, gas sorption ability is weaker；Titanium nanotube specific surface area is larger, surface acid
Property intensity is high, gas sorption ability is very strong, but mechanical strength is not high.Titania nanoparticles and titanium nanotube are simultaneously as load
During body, the two is spatially mutually embedded in interdependent (see accompanying drawing 1), is not only provided with the carriers such as high mechanical properties, high-specific surface area
Indispensable performance, and it has been also equipped with the speciality such as strong adsorption capacity, highly acid.These carrier characteristics cause active component to obtain height
Dispersion so that NOx, NH3、O2The material such as, dioxins quick adsorption, to catalyst surface, is the redox of active material
Journey creates favourable prerequisite.Vanadic anhydride is conventional NOx He bioxin cleaning catalyst active component, but its storage
Oxygen is indifferent, and has toxicity.NOx catalytic purifications reaction Ji bioxin oxidation reaction process is required to O2With chemical adsorption states
Participate in, cerium oxide has very strong oxygen storage capacity, is conducive to O2Chemisorbed, but the sulfur resistance of cerium oxide is slightly worse, SO2Meeting
Cause its activity decrease.The electron transfer rate of precious metals pt is exceedingly fast, and oxidation-reduction process is quickly carried out when being conducive to low temperature,
But expensive, active temperature windows are narrower.Therefore, cerium oxide, vanadic anhydride, Pt be combined with each other in catalyst surface, group
Into active material can preferably adapt to the requirement of low temperature Synergistic degradation bioxin and NOx, catalytic during practical application
It can be higher than one-component.
(5) present invention is 140～300 DEG C, SO for temperature2Content is higher than 500mg/Nm3And contain dust and sulphur ammonium salt etc.
The garbage incinerating tail gas of material, can reach more than 95% bioxin purification efficiency and more than 80% NOx purification efficiencies, can make
Dioxin emission is less than 0.1ng I-TEQ/Nm3, NOx emission can be made to be less than 150mg/m3。
(6) the fume treatment effect of catalyst of the invention especially to temperature less than 180 DEG C is especially good, remains to Shi bioxin
Discharge is less than 0.1ng I-TEQ/Nm3, NOx emission can be made to be less than 150mg/m3。
Description of the drawings
Fig. 1 is the transmission electron microscope picture of the catalyst that embodiment 1 is prepared.
Fig. 2 is the XRD spectra of the catalyst carrier that embodiment 1 is prepared.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
In following examples, the preparation method of titanium nanotube used is as follows：
By the strong base solution for making 10mol/L NaOH soluble in water, TiO is added in strong base solution2Particle, stirring are obtained
Suspension, TiO2The ratio of particle and strong base solution is controlled in 30g/L.Hydro-thermal process is carried out to suspension, the hydro-thermal time is 28
Hour, hydrothermal temperature is 160 DEG C, and the sample after hydro-thermal is washed to acidity with 0.1mol/L watery hydrochloric acid.
Other raw materials are commercial goods.
Embodiment 1
59 grams of titania nanoparticles, 30 grams of titanium nanotubes are weighed, excessive water retting is added, is uniformly mixed, obtains
To catalyst carrier；22.45 grams of cerous nitrates, 2.57 grams of ammonium metavanadates, 0.21 gram of chloroplatinic acid are dissolved in 80 DEG C of deionized water afterwards
In be configured to solution, add said catalyst carrier under vigorous stirring, be further continued for stirring 12 hours, then dry, last 400
DEG C roasting 3 hours.
The transmission electron microscope picture that embodiment 1 is obtained catalyst is as shown in Figure 1.
The XRD spectra that embodiment 1 is obtained catalyst carrier is as shown in Figure 2.
Embodiment 2
22 grams of titania nanoparticles and 50 grams of titanium nanotubes are weighed, excessive water retting is added, is uniformly mixed, obtains
To catalyst carrier；Afterwards 20 grams of cerium oxide, 8 grams of vanadic anhydrides, 0.1 gram of chloroplatinic acid are dissolved in 60 DEG C of deionized water and being configured
Into solution, said catalyst carrier is added under vigorous stirring, be further continued for stirring 4 hours, then dry, last 350 DEG C of roastings 3
Hour.
Embodiment 3
98 grams of titania nanoparticles and 2 grams of titanium nanotubes are weighed, excessive water retting is added, is uniformly mixed, obtains
To catalyst carrier；To match somebody with somebody in 2.52 grams of cerous nitrates, 0.63 gram of ammonium metavanadate, the deionized water of molten 80 DEG C of 0.25 gram of chloroplatinic acid afterwards
Solution is set to, said catalyst carrier is added under vigorous stirring, stirring 12 hours is further continued for, is then dried, last 600 DEG C of roastings
Burn 6 hours.
Embodiment 4
98 grams of titania nanoparticles are weighed, excessive water retting is added, is uniformly mixed, obtains catalyst carrier；
3.16 grams of cerium oxalates are dissolved in deionized water, said catalyst carrier is added under vigorous stirring, continue stirring 4 hours, dried
It is dry, 350 DEG C of roastings 3 hours, grind into powder；0.5 gram of vanadic anhydride is dissolved in saturated oxalic acid solution, stirring 1 hour, so
The powder described in step (2) being added afterwards, continuing stirring 4 hours, drying, 350 DEG C of roastings 3 hours grind to form particle diameter and be less than
The particle of 0.45mm；0.65 gram of chloroplatinic acid is dissolved in deionized water, step (3) particle is subsequently adding, continues stirring 4 little
When, drying, 350 DEG C of roastings 3 hours.
Embodiment 5
22 grams of titania nanoparticles, 50 grams of titanium nanotubes are weighed, excessive water retting is added, is uniformly mixed, obtains
To catalyst carrier；63.71 grams of ammonium ceric nitrates, 0.1 gram of chloroplatinic acid are dissolved in deionized water, catalysis is added under vigorous stirring
Agent carrier, continues stirring 12 hours, drying, 600 DEG C of roastings 6 hours, grind into powder；9.71 grams of ammonium metavanadates are dissolved in into saturation
In oxalic acid solution, stir 1 hour, the powder being subsequently adding described in step (2), continue stirring 12 hours, drying, 500 DEG C of roastings 6
Hour.
Catalyst bioxin described in embodiment 1 and NOx purification efficiencies are as shown in table 1.
Flue gas of refuse burning is passed through into catalyst, flue-gas temperature is adjusted by distribution, sampling test catalyst imports and exports cigarette
Gas concentration of component.Catalyst is about 10000h using air speed-1.Oxygen content of smoke gas before non-purified is 12～15%, and NOx content is
200～250mg/m3, SO2Content is 400～500mg/m3， dioxins content is 10～15ng I-TEQ/Nm3。
1 catalyst bioxin of table and NOx purification efficiencies
| Exhaust temperature (DEG C) | Bioxin purification efficiency (%) | NOx purification efficiencies (%) |
| 140 | 95 | 80 |
| 160 | 98 | 92 |
| 180 | 99.5 | 100 |
| 220 | 99.9 | 100 |
| 260 | 99.9 | 100 |
| 300 | 99.9 | 100 |
The case that is embodied as of patent of the present invention is the foregoing is only, but the technical characteristic of patent of the present invention is not limited to
This, any those skilled in the relevant art in the field of the invention, all cover in the special of the present invention by the change or modification made
Among sharp scope.
Claims (8)
1. the catalyst of a kind of low temperature Synergistic degradation bioxin and NOx, it is characterised in that by percentage to the quality by the following raw material
Make：
2. the preparation method of the catalyst of a kind of low temperature Synergistic degradation bioxin as claimed in claim 1 and NOx, its feature exist
In comprising the steps：
(1) titania nanoparticles and titanium nanotube are weighed by proportioning, adds excessive water retting, be uniformly mixed, obtain
Catalyst carrier；
(2) compound of the compound of cerium, the compound of vanadium, platinum is dissolved in by proportioning in 60-80 DEG C of deionized water and is configured to
Solution, adds catalyst carrier under vigorous stirring, is further continued for stirring 4～12 hours, then dries, last 350～600 DEG C of roastings
Burn 3～6 hours.
3. the preparation method of the catalyst of a kind of low temperature Synergistic degradation bioxin as claimed in claim 1 and NOx, its feature exist
In, it is characterised in that comprise the steps：
(1) titania nanoparticles and titanium nanotube are weighed by proportioning, adds excessive water retting, be uniformly mixed, obtain
Catalyst carrier；
(2) compound of cerium is dissolved in deionized water by proportioning, adds catalyst carrier under vigorous stirring, continue stirring 4
～12 hours, drying, 350～600 DEG C of roastings 3～6 hours, grind into powder；
(3) compound of vanadium is dissolved in saturated oxalic acid solution by proportioning, is stirred 1 hour, the powder being subsequently adding described in step (2)
End, continues stirring 4～12 hours, and drying, 350～600 DEG C of roastings 3～6 hours grind to form particle of the particle diameter less than 0.45mm；
(4) compound of platinum is dissolved in deionized water by proportioning, is subsequently adding step (3) particle, continue stirring 4～12
Hour, drying, 350～600 DEG C of roastings 3～6 hours.
4. the preparation method according to Claims 2 or 3, it is characterised in that：As SO in handled tail gas2Concentration is higher than 500mg/
Nm3Huo bioxin concentration is higher than 15ng I-TEQ/Nm3When, in carrier, the ratio of titanium nanotube is not less than 20%.
5. the preparation method according to Claims 2 or 3, it is characterised in that the titanium nanotube is prepared by the following method：
TiO is added in the NaOH strong base solutions that concentration is 5～15mol/L2Particle, stirring are obtained suspension, TiO2Particle with it is strong
The mass volume ratio example of aqueous slkali is controlled in 10～50g/L；Hydro-thermal process is carried out to suspension, the hydro-thermal time is 18～36 little
When, hydrothermal temperature is 120～180 DEG C；Sample after hydro-thermal reaction watery hydrochloric acid is washed to acidity, drying.
6. the preparation method according to Claims 2 or 3, it is characterised in that the compound of cerium is cerium oxide, cerous nitrate, oxalic acid
One kind in cerium and ammonium ceric nitrate.
7. the preparation method according to Claims 2 or 3, it is characterised in that the compound of vanadium is ammonium metavanadate or five oxidations two
Vanadium.
8. the preparation method according to Claims 2 or 3, it is characterised in that the compound of platinum is chloroplatinic acid.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107952449A (en) * | 2017-12-15 | 2018-04-24 | 江苏龙净科杰催化剂再生有限公司 | Low temperature collaboration denitration Tuo bioxin demercuration honeycombed catalysts and preparation method thereof |
| CN108295840A (en) * | 2018-01-24 | 2018-07-20 | 清华大学 | Manganese-based catalyst and its preparation and application of a kind of efficient synergistic purification nitrogen oxides He bioxin |
| CN108671917A (en) * | 2018-04-26 | 2018-10-19 | 上海羽和新材料有限公司 | A kind of catalyst and preparation method thereof of efficient cryogenic catalysis VOCs exhaust gas decompositions |
| CN108786788A (en) * | 2018-06-21 | 2018-11-13 | 上海理工大学 | A kind of removing dioxin in flue gas and NOxCatalyst and preparation method and application |
| CN109126773A (en) * | 2018-09-28 | 2019-01-04 | 航天凯天环保科技股份有限公司 | A kind of garbage-incineration smoke purifying catalyst and preparation method thereof |
| CN111871070A (en) * | 2019-11-12 | 2020-11-03 | 南京工业大学 | Integrated filter material |
| CN114588944A (en) * | 2022-03-29 | 2022-06-07 | 北京方信立华科技有限公司 | Catalyst for cooperatively treating NOx and dioxin and preparation method thereof |
| CN114797837A (en) * | 2022-03-20 | 2022-07-29 | 浙江大学 | Catalyst capable of removing secondary pollutants in flue gas by concerted catalysis under low-temperature condition |
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| CN114588944A (en) * | 2022-03-29 | 2022-06-07 | 北京方信立华科技有限公司 | Catalyst for cooperatively treating NOx and dioxin and preparation method thereof |
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