CN105148954B - A kind of efficient cryogenic SCR denitration and preparation method thereof - Google Patents
A kind of efficient cryogenic SCR denitration and preparation method thereof Download PDFInfo
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- CN105148954B CN105148954B CN201510601870.9A CN201510601870A CN105148954B CN 105148954 B CN105148954 B CN 105148954B CN 201510601870 A CN201510601870 A CN 201510601870A CN 105148954 B CN105148954 B CN 105148954B
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Abstract
The invention discloses a kind of efficient cryogenic SCR denitration and preparation method thereof, the catalyst is prepared by following raw materials：Attapulgite, butyl titanate, acetylacetone,2,4-pentanedione, absolute ethyl alcohol, hydrochloric acid, ammonium fluoride, ammoniacal liquor, prepare by including following steps：1st, attapulgite is ultrasonically treated is purified with acid treatment；2nd, attapulgite, butyl titanate, acetylacetone,2,4-pentanedione and absolute ethyl alcohol mix compound by sol-gal process attapulgite and titanium dioxide progress；3rd, the certain temperature water-bath impregnation in ammonium fluoride solution by attapulgite and titanium dioxide compound；4th, the composite catalyst after dipping is calcined is made required catalyst in Muffle furnace after calcining.The catalyst can be used for the conversion of nitrogen oxides in catalysis coal-burning power plant's flue gas, and production cost is low, simple to operate, and effect is high, has larger application value and market prospects.
Description
Technical field
The present invention relates to the technical field of Air Pollutants removal of nitrogen oxide, more particularly to a kind of low-temperature SCR
The preparation method of catalyst for denitrating flue gas, suitable for the processing of the coal-burning boiler low-temperature flue gas such as thermal power plant, cement plant.
Background technology
In recent years, as the rapid development of industrial technology make it that the mankind are also gradual to the demand of fire coal, oil, natural gas
Year increase, plus the surge of vehicles number, inevitably causes serious pollution to atmospheric environment.Nitrogen oxides
(NOx) it is to cause one of main chief culprit of air environmental pollution, acid rain, photochemical fog, gray haze can be caused and the mankind are good for
Health and animal and plant growth cause greatly to endanger, and the flue gas of wherein discharged from coal-fired boiler is that NO_x in Air Environment mainly obtains source
One of, account for 46%.
At present, SCR（SCR）Method is most widely used maximally effective denitration technology, mainly by reducing agent
NH3Mixed in injection flue gas with flue gas, under catalyst action, NH3Selectively and NO at a certain temperaturexGeneration oxygen
Change reduction reaction generation N2And H2O, it is as follows to relate generally to reaction：
The selection of catalyst is link important in SCR denitration method, and most popular at present is metal oxidation
Thing denitrating catalyst, mainly there is V2O5/TiO2、V2O5-WO3/TiO2、V2O5-MoO3/TiO2Will Deng, this kind of catalyst activity temperature
Ask higher at 400 DEG C or so, and production cost is expensive, in addition, catalyst activity is also easily by vapor, SO2Deng influence, therefore
Unaffected SCR catalyst under exploitation low temperature environment obviously has realistic meaning.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of efficient cryogenic SCR denitration
Preparation method, low temperature SCR denitration catalyst prepared by this method have good low-temperature denitration performance.
A kind of efficient cryogenic SCR denitration of the present invention, it is characterised in that：The catalyst body material is bumps
Rod soil and titanium dioxide compound, helper component are fluorine.
The present invention also provides the efficient cryogenic SCR denitration preparation method, comprises the following steps：
It step 1, will be distributed under 20g attapulgite Ultrasonic Conditions in 200ml deionized waters, then add quality thereto
Fraction is 37% hydrochloric acid solution 20ml, and filtration washing is to neutral and dry after certain temperature water-bath back flow reaction, after obtaining purification
Attapulgite it is standby；
Step 2, the 1g attapulgites purified are added in 50ml beakers, then add butyl titanate, anhydrous thereto
Ethanol, acetylacetone,2,4-pentanedione and deionized water, stirring reaction obtains colloidal sol and is changed into gel again in room temperature, will be calcined after the drying of gained gel
It is standby with titanium dioxide compound that grinding obtains attapulgite；
Step 3, a certain amount of ammonium fluoride is dissolved in 20ml deionized waters, adds the attapulgite and two of preparation thereto
Titanium oxide compound, ammoniacal liquor regulation pH=10, the impregnation under certain temperature；
After step 4, impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, then move into
The SCR denitration of Fluorin doped attapulgite and titanium dioxide is made to calcine in Muffle furnace.
As preferable preparation method, the back flow reaction described in step 1 is to be flowed back 12 hours in 60 DEG C of water-baths.
As preferable preparation method, butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and deionized water described in step 2
Dosage be respectively 8.8ml, 15ml, 10ml and 10ml.
As preferable preparation method, the calcining heat described in step 2 is 400 DEG C, and heating rate is 10-15 DEG C/min,
Calcination time is 8 hours.
As preferable preparation method, the ammonium fluoride dosage described in step 3 is the mol ratio of butyl titanate and ammonium fluoride
For 10 ~ 1:1.
As preferable preparation method, the certain temperature described in step 3 is 25 DEG C of room temperature, and dip time is 24 hours.
As preferable preparation method, the calcining heat described in step 4 is 300 DEG C, and heating rate is 10-15 DEG C/min,
Calcination time is 6 hours.
Above-mentioned catalyst can be used for coal-fired power plant to be catalyzed the reaction that nitrogen oxides in flue gas is reduced to nitrogen.
Present invention selection attapulgite is compound instead of vanadium base class oxide and titanium dioxide progress, and attapulgite is inexpensively easy
, cost substantially reduces for vanadium base class oxide, and attapulgite is a kind of layer chain richness magnesium silicate clay pit
Thing, in needle-like or threadiness, there is larger specific surface area, there are-OH the tissues that can be reacted, special layer chain structure in surface
The zeolites duct of prosperity can be produced, and with soil characteristics is typically glued, is commonly used for the load of adsorbent, catalyst and catalyst
Body.
Compared with existing SCR denitration technology of preparing, the invention has the advantages that：
（1）Select attapulgite cheap and easy to get compound with titanium dioxide, substantially reduce the preparation cost of catalyst, prepare
Technique is simple, avoids loss of the resource in preparation process to greatest extent, the ratio table of the attapulgite after hydrochloric acid purifies
Area and pore volume greatly increase（It is shown in Table 1）, so as to add catalyst surface active site；
The specific surface area and pore-size distribution of the attapulgite of table 1, hydrochloric acid-attapulgite
（2）Using butyl titanate as the presoma of titanium dioxide, metatitanic acid four is caused using acetylacetone,2,4-pentanedione as organic solvent
Butyl ester can be sufficiently mixed therewith, be hydrolyzed in the presence of ethanol and distilled water with attapulgite, fluorine, condensation reaction, shape
Into colloidal sol, slowly polymerization forms gel between micelle is made by ageing, then prepares gained catalyst by calcining, drying；
（3）Using ammonium fluoride as the presoma of fluorine, the doping of fluorine element can increase the acid active sites of catalyst surface
Point, so as to produce a large amount of Lacking oxygens, further increase the catalytic performance of catalyst；
（4）Gained catalyst is prepared relative to extensive SCR catalyst is used at present, active catalytic temperature window reduces,
Easily failed so as to avoid catalyst by high-temperature dust covering, extend the service life of catalyst；
（5）Because temperature is more than 100 DEG C in flue gas caused by coal-burning boiler, wherein can be mingled with vapor, vapor is deposited
It can stop during the course of the reaction on a catalyst, the performance of conventional catalyst can should be the stop of vapor and substantially reduce,
The catalyst of the present invention can have preferable resistance by experimental verification to vapor.
Embodiment
With reference to embodiment, the present invention is described in more detail, but embodiments of the present invention are not limited only to this.
Purification processes are carried out to attapulgite first in following implementation, by following processing step：By 20g concave convex rods
It is distributed under native Ultrasonic Conditions in 200ml deionized waters, then adds the hydrochloric acid solution 20ml that mass fraction is 37% thereto,
Filtration washing to neutrality and is dried after certain temperature water-bath back flow reaction, and the attapulgite after being purified is standby.
Embodiment 1
（1）The 1g attapulgites purified are added in 50ml beakers, then add thereto 8.8ml butyl titanates,
15ml absolute ethyl alcohols, 10ml acetylacetone,2,4-pentanediones and 10ml deionized waters, stirring reaction obtains colloidal sol and is changed into gel again by institute in room temperature
To obtain attapulgite standby with titanium dioxide compound for calcining and grinding after gel drying；
（2）9.54g ammonium fluorides are dissolved in 20ml deionized waters, add attapulgite/titanium dioxide of preparation thereto
Titanium compound, ammoniacal liquor regulation pH=10, the impregnation 24 hours at 25 DEG C of room temperature；
（3）After impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, be put into Muffle furnace
Calcined 6 hours with 300 DEG C, grind the SCR denitration that Fluorin doped attapulgite and titanium dioxide is made；
（4）Assigned temperature window is carried out to above-mentioned catalyst and carries out SCR denitration catalytically active assessment；
（5）0.5g catalyst samples are taken to be fitted into fixed bed quartz tube reactor, reactor is put into temperature programmed control reacting furnace
In, controlling reaction temperature scope is between 80-240 DEG C；80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C,
At 220 DEG C, 240 DEG C after stabilization, concentration data is gathered by flue gas analyzer, calculates the removal efficiency of nitrogen oxides；
（6）Evaluating catalyst condition controls：The flue gas each group of simulation turns into φ (O2)=3%, NO 500-600ppm, N2
For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（7）Study of Catalyst is controlled by water vapor conditions influence condition：The flue gas each group of simulation turns into φ (O2)=3%, NO
For 500-600ppm, φ（Vapor）=1%, N2For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（8）Evaluating catalyst result such as table 2 below, wherein at 160 DEG C, removal of nitrogen oxide efficiency is up to 91%, vapor
Catalytic efficiency can still reach 88% under existence condition.
The evaluating catalyst result of table 2
Embodiment 2
（1）The 1g attapulgites purified are added in 50ml beakers, then add thereto 8.8ml butyl titanates,
15ml absolute ethyl alcohols, 10ml acetylacetone,2,4-pentanediones and 10ml deionized waters, stirring reaction obtains colloidal sol and is changed into gel again by institute in room temperature
To obtain attapulgite standby with titanium dioxide compound for calcining and grinding after gel drying；
（2）7.63g ammonium fluorides are dissolved in 20ml deionized waters, add attapulgite/titanium dioxide of preparation thereto
Titanium compound, ammoniacal liquor regulation pH=10, the impregnation 24 hours at 25 DEG C of room temperature；
（3）After impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, be put into Muffle furnace
Calcined 6 hours with 300 DEG C, grind the SCR denitration that Fluorin doped attapulgite and titanium dioxide is made；
（4）Assigned temperature window is carried out to above-mentioned catalyst and carries out SCR denitration catalytically active assessment；
（5）0.5g catalyst samples are taken to be fitted into fixed bed quartz tube reactor, reactor is put into temperature programmed control reacting furnace
In, controlling reaction temperature scope is between 80-240 DEG C；80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C,
At 220 DEG C, 240 DEG C after stabilization, concentration data is gathered by flue gas analyzer, calculates the removal efficiency of nitrogen oxides；
（6）Evaluating catalyst condition controls：The flue gas each group of simulation turns into φ (O2)=3%, NO 500-600ppm, N2
For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（7）Study of Catalyst is controlled by water vapor conditions influence condition：The flue gas each group of simulation turns into φ (O2)=3%, NO
For 500-600ppm, φ（Vapor）=1%, N2For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（8）Evaluating catalyst result such as table 3 below, at wherein 140-160 DEG C, removal of nitrogen oxide efficiency is up to 96%, water
Catalytic efficiency can still reach 95% under presence of steam.
The evaluating catalyst result of table 3
Embodiment 3
（1）The 1g attapulgites purified are added in 50ml beakers, then add thereto 8.8ml butyl titanates,
15ml absolute ethyl alcohols, 10ml acetylacetone,2,4-pentanediones and 10ml deionized waters, stirring reaction obtains colloidal sol and is changed into gel again by institute in room temperature
To obtain attapulgite standby with titanium dioxide compound for calcining and grinding after gel drying；
（2）5.74g ammonium fluorides are dissolved in 20ml deionized waters, add attapulgite/titanium dioxide of preparation thereto
Titanium compound, ammoniacal liquor regulation pH=10, the impregnation 24 hours at 25 DEG C of room temperature；
（3）After impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, be put into Muffle furnace
Calcined 6 hours with 300 DEG C, grind the SCR denitration that Fluorin doped attapulgite and titanium dioxide is made；
（4）Assigned temperature window is carried out to above-mentioned catalyst and carries out SCR denitration catalytically active assessment；
（5）0.5g catalyst samples are taken to be fitted into fixed bed quartz tube reactor, reactor is put into temperature programmed control reacting furnace
In, controlling reaction temperature scope is between 80-240 DEG C；80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C,
At 220 DEG C, 240 DEG C after stabilization, concentration data is gathered by flue gas analyzer, calculates the removal efficiency of nitrogen oxides；
（6）Evaluating catalyst condition controls：The flue gas each group of simulation turns into φ (O2)=3%, NO 500-600ppm, N2
For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（7）Study of Catalyst is controlled by water vapor conditions influence condition：The flue gas each group of simulation turns into φ (O2)=3%, NO
For 500-600ppm, φ（Vapor）=1%, N2For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；（8）Evaluating catalyst result such as table 4 below, wherein at 160 DEG C, removal of nitrogen oxide efficiency is up to 96%, and vapor has bar
Catalytic efficiency can still reach 91% under part.
The evaluating catalyst result of table 4
Embodiment 4
（1）The 1g attapulgites purified are added in 50ml beakers, then add thereto 8.8ml butyl titanates,
15ml absolute ethyl alcohols, 10ml acetylacetone,2,4-pentanediones and 10ml deionized waters, stirring reaction obtains colloidal sol and is changed into gel again by institute in room temperature
To obtain attapulgite standby with titanium dioxide compound for calcining and grinding after gel drying；
（2）3.82g ammonium fluorides are dissolved in 20ml deionized waters, add attapulgite/titanium dioxide of preparation thereto
Titanium compound, ammoniacal liquor regulation pH=10, the impregnation 24 hours at 25 DEG C of room temperature；
（3）After impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, be put into Muffle furnace
Calcined 6 hours with 300 DEG C, grind the SCR denitration that Fluorin doped attapulgite and titanium dioxide is made；
（4）Assigned temperature window is carried out to above-mentioned catalyst and carries out SCR denitration catalytically active assessment；
（5）0.5g catalyst samples are taken to be fitted into fixed bed quartz tube reactor, reactor is put into temperature programmed control reacting furnace
In, controlling reaction temperature scope is between 80-240 DEG C；80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C,
At 220 DEG C, 240 DEG C after stabilization, concentration data is gathered by flue gas analyzer, calculates the removal efficiency of nitrogen oxides；
（6）Evaluating catalyst condition controls：The flue gas each group of simulation turns into φ (O2)=3%, NO 500-600ppm, N2
For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（7）Study of Catalyst is controlled by water vapor conditions influence condition：The flue gas each group of simulation turns into φ (O2)=3%, NO
For 500-600ppm, φ（Vapor）=1%, N2For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（8）Evaluating catalyst result such as table 5 below, wherein at 160 DEG C, removal of nitrogen oxide efficiency is up to 91%, vapor
Catalytic efficiency can still reach 87% under existence condition.
The evaluating catalyst result of table 5
Embodiment 5
（1）The 1g attapulgites purified are added in 50ml beakers, then add thereto 8.8ml butyl titanates,
15ml absolute ethyl alcohols, 10ml acetylacetone,2,4-pentanediones and 10ml deionized waters, stirring reaction obtains colloidal sol and is changed into gel again by institute in room temperature
To obtain attapulgite standby with titanium dioxide compound for calcining and grinding after gel drying；
（2）1.91g ammonium fluorides are dissolved in 20ml deionized waters, add attapulgite/titanium dioxide of preparation thereto
Titanium compound, ammoniacal liquor regulation pH=10, the impregnation 24 hours at 25 DEG C of room temperature；
（3）After impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, be put into Muffle furnace
Calcined 6 hours with 300 DEG C, grind the SCR denitration that Fluorin doped attapulgite and titanium dioxide is made；
（4）Assigned temperature window is carried out to above-mentioned catalyst and carries out SCR denitration catalytically active assessment；
（5）0.5g catalyst samples are taken to be fitted into fixed bed quartz tube reactor, reactor is put into temperature programmed control reacting furnace
In, controlling reaction temperature scope is between 80-240 DEG C；80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C,
At 220 DEG C, 240 DEG C after stabilization, concentration data is gathered by flue gas analyzer, calculates the removal efficiency of nitrogen oxides；
（6）Evaluating catalyst condition controls：The flue gas each group of simulation turns into φ (O2)=3%, NO 500-600ppm, N2
For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（7）Study of Catalyst is controlled by water vapor conditions influence condition：The flue gas each group of simulation turns into φ (O2)=3%, NO
For 500-600ppm, φ（Vapor）=1%, N2For Balance Air, overall flow rate 400-600ml/min, holding air speed is 25000h-1；
（8）Evaluating catalyst result such as table 6 below, at wherein 140-160 DEG C, removal of nitrogen oxide efficiency is up to 93%, water
Catalytic efficiency can still reach 88% under presence of steam.
The evaluating catalyst result of table 6
Claims (7)
- A kind of 1. efficient cryogenic SCR denitration, it is characterised in that：The catalyst body material is attapulgite and dioxy Change titanium compound, helper component is fluorine；The preparation method of described efficient cryogenic SCR denitration, comprises the following steps：It step 1, will be distributed under 20g attapulgite Ultrasonic Conditions in 200ml deionized waters, then add mass fraction thereto For 37% hydrochloric acid solution 20ml, filtration washing is to neutral and dry after certain temperature water-bath back flow reaction, after being purified Attapulgite is standby；Step 2, by 1g purify attapulgite be added in 50ml beakers, then thereto add butyl titanate, absolute ethyl alcohol, Acetylacetone,2,4-pentanedione and deionized water, stirring reaction obtains colloidal sol and is changed into calcining and grinding after gel dries gained gel again obtaining in room temperature It is standby with titanium dioxide compound to attapulgite；Step 3, a certain amount of ammonium fluoride is dissolved in 20ml deionized waters, adds the attapulgite and titanium dioxide of preparation thereto Titanium compound, ammoniacal liquor regulation pH=10, the impregnation under certain temperature；After step 4, impregnation, to composite catalyst filtration washing to neutrality and move to baking oven and be dried, then move into Muffle The SCR denitration of Fluorin doped attapulgite and titanium dioxide is made to calcine in stove.
- 2. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：Back flow reaction described in step 1 To be flowed back 12 hours in 60 DEG C of water-baths.
- 3. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：The fourth of metatitanic acid four described in step 2 Ester, absolute ethyl alcohol, the dosage of acetylacetone,2,4-pentanedione and deionized water are respectively 8.8ml, 15ml, 10ml and 10ml.
- 4. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：Calcining heat described in step 2 For 400 DEG C, heating rate is 10-15 DEG C/min, and calcination time is 8 hours.
- 5. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：Ammonium fluoride described in step 3 is used The mol ratio measured as butyl titanate and ammonium fluoride is 10~1:1.
- 6. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：Certain temperature described in step 3 For 25 DEG C of room temperature, dip time is 24 hours.
- 7. efficient cryogenic SCR denitration according to claim 1, it is characterised in that：Calcining heat described in step 4 For 300 DEG C, heating rate is 10-15 DEG C/min, and calcination time is 6 hours.
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| CN106540684B (en) * | 2016-12-06 | 2019-05-10 | 北京国电龙源环保工程有限公司 | The preparation method of high activity honeycomb fashion SCR catalyst |
| CN107042102A (en) * | 2016-12-07 | 2017-08-15 | 盐城复华环保产业开发有限公司 | Selective catalytic reduction low-temperature denitration catalyst and preparation method thereof |
| CN106732541A (en) * | 2016-12-07 | 2017-05-31 | 盐城复华环保产业开发有限公司 | Method for preparing low-temperature selective catalytic reduction denitration catalyst by ultrasonic impregnation method |
| CN109111693A (en) * | 2018-06-29 | 2019-01-01 | 江苏德溢利新材料科技有限公司 | A kind of glass reinforced plastic photovoltaic bracket that high-ductility is weather-proof |
| CN109111651A (en) * | 2018-06-29 | 2019-01-01 | 江苏德溢利新材料科技有限公司 | A kind of weather-proof plastics photovoltaic bracket of high-ductility |
| CN108912608A (en) * | 2018-06-29 | 2018-11-30 | 江苏德溢利新材料科技有限公司 | A kind of the glass reinforced plastic photovoltaic bracket and its processing technology of modification |
| CN114433071A (en) * | 2021-12-29 | 2022-05-06 | 江苏世清环保科技有限公司 | Denitration catalyst prepared by taking attapulgite as carrier and preparation method thereof |
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