CN107042102A - Selective catalytic reduction low-temperature denitration catalyst and preparation method thereof - Google Patents
Selective catalytic reduction low-temperature denitration catalyst 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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
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Abstract
The invention relates to a selective catalytic reduction low-temperature denitration catalyst and a preparation method thereof, and is characterized in that the method comprises the following steps: step 1: adding high-purity attapulgite into distilled water, and stirring to form attapulgite suspension; step 2: sequentially adding ammonium metavanadate and soluble salt of cerium into the attapulgite suspension, and heating in a water bath to fully mix and dissolve the ammonium metavanadate and the soluble salt of cerium; and step 3: dropwise adding ammonia water into the mixture, and adjusting the pH value to 9-14; and 4, step 4: transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction; and 5: after hydrothermal reaction, performing suction filtration to obtain a mixture precipitate, washing the mixture precipitate with distilled water to be neutral, and performing a step 6: and drying and grinding the obtained sample to obtain the required low-temperature selective catalytic reduction denitration catalyst.
Description
Technical field
The present invention relates to a kind of preparation method, and in particular to a kind of SCR low-temperature denitration catalyst and its system
Preparation Method, belongs to industrial smoke Air Pollutants nitrogen oxides and administers field.
Background technology
Early in the 1970s, the Industrial Boiler and coal fired power plant of Japan are just had begun to extensively using selective catalysis
Reduction（SCR）Denitration technology；Afterwards in 1985, Europe introduces SCR denitration technology from Japan, and the denitration technology is obtained not thereafter
Disconnected development improves and has gradually obtained global be widely applied；China introduces technology dress at first by Fujian Hou Shi thermal power plants
Put, the country there are other coal-burning power plants to start trial operation SCR denitration device successively thereafter.Because it can obtain higher NOx removal
Efficiency and easy to operate, operating cost is low, thus turned into the focus that whole world research denitration Study on Problems person competitively studies, and
And within following a period of time, SCR denitration technology will be more widely used development.
Selective-catalytic-reduction denitrified method refers within the scope of certain temperature, and reducing agent is added into flue gas（It is conventional
Have HN3, CO, urea or hydrocarbon etc.）, under conditions of SCR catalyst catalysis, nitrogen oxides in effluent and oxygen
Redox reaction occurs for gas, reducing agent to remove, so as to reach the purpose of purifying smoke.Research is found, typically with NH3As
Higher removal of nitrogen oxide efficiency can be obtained during reducing agent, so research is all unanimously thought with NH now3It is used as reducing agent
Reaction be typical selective catalytic reduction reaction.
SCR denitration can substantially be divided into three classes according to development course：（1）Noble metal type catalyst, the SCR of early stage
Denitrating technique is all to use such catalyst, and it has higher denitration performance, but using noble metals such as Pt, Rh, Pd as activity
The catalyst of catalytic center involves great expense, and to reducing agent NH3There is certain oxidation, economically seeing will necessarily be by
Eliminate；（2）Zeolite molecular sieve catalyst, progressively replaces noble metal type catalyst in the nineties in last century, its mainly by from
The zeolite molecular sieve of metal ion exchanged is made in the mode that son is exchanged, and the active temperature windows requirement of this kind of catalyst is commonly reached
600 DEG C or so, generally with C3H6As reducing agent, but it is due to that its higher active temperature interval is required, to process equipment requirement
Also relative requirement is improved, is unfavorable for commercial Application；（3）Metal oxide catalyst, this is current most study also latest model
Catalyst, active temperature windows are lower slightly, and it turns into current most widely used SCR denitration by constantly improving and developing
Catalyst, conventional scr reaction temperature general control is between 300-400 DEG C, and the most frequently used commercial SCR catalyst is with anatase
Type TiO2For carrier, with V2O5、V2O5-WO3、V2O5-MoO3Or V2O5-WO3-MoO3It is active catalyst component Deng metal oxide.
Conventional selective catalytic-reduction denitrified catalyst inevitably exist production cost do, high energy consumption, pollution it is big, raw
The problems such as operation difficulty is big is produced, simultaneous reactions temperature is too high, be easily caused catalyst poisoning inactivation.Therefore, seek in low temperature bar
Extremely urgent by the efficient catalyst of the clean and safe simply prepared under part, those skilled in the art has attempted to new
Scheme, but effect is undesirable.
The content of the invention
There is provided SCR under a kind of low temperature exactly for technical problem present in prior art by the present invention
The catalyst and its preparation technology of nitrogen oxides in industrial smoke, the technical scheme overcomes the deficiencies in the prior art, compared with low temperature
The lower high-efficiency denitration catalyst that safety non-toxic is prepared by simple hydrothermal synthesis method of degree.
To achieve these goals, technical scheme is as follows, a kind of SCR low-temperature denitration catalysis
Agent and preparation method thereof, it is characterised in that methods described step is as follows：Step 1：High pure attapulgite clay is added in distilled water
Stirring forms attapulgite suspension；
Step 2：The soluble-salt of ammonium metavanadate and cerium is added sequentially in attapulgite suspension, heating water bath is allowed to abundant
Mixed dissolution；
Step 3：Ammoniacal liquor is added dropwise into mixture, regulation pH value is in 9-14；
Step 4：Above-mentioned mixed liquor is moved to hydro-thermal reaction is carried out in hydrothermal reaction kettle；
Step 5：Suction filtration obtains mixture precipitation after hydro-thermal reaction, is washed with distilled water to neutrality
Step 6：Obtained sample is dried, ground, you can the low-temperature selective catalytic reduction denitration catalysis needed for obtaining
Agent.
As a modification of the present invention, the purity of the high pure attapulgite clay described in step 1 is mass fraction 99%, consumption
For 2 ~ 6 grams, distillation water consumption is 10 ~ 30 milliliters.
As a modification of the present invention, the soluble-salt of the cerium described in step 2 is six water cerous nitrates or six water cerium chlorides.
As a modification of the present invention, the water bath heating temperature described in step 2 is 60 ~ 80 DEG C, and the heating water bath time is
30 ~ 60 minutes.
As a modification of the present invention, ammonium metavanadate inventory described in step 2 is 0.002mol ~ 0.008mol, inclined vanadium
The molar ratio of sour ammonium and six water cerous nitrates is 1:1.
As a modification of the present invention, the mass concentration of ammoniacal liquor described in step 3 is 25% ~ 28%.
As a modification of the present invention, the hydrothermal temperature control described in step 4 is 150 ~ 200 DEG C, hydro-thermal reaction
Shi Changwei 8 ~ 12 hours.
As a modification of the present invention, the drying temperature control described in step 6 is 80 ~ 100 DEG C, drying time is 24 ~
28 hours.
The present invention is mainly from the presoma of ammonium metavanadate, the ammonium salt of cerium or chlorate as catalyst activity component
Because they can remove ammonia, nitrate ion and chlorine by being heated at high temperature generation nitrogen oxides or washing during the course of the reaction
The component without catalytic performance such as ion；Preparation method selects hydro-thermal reaction method, mainly due to high temperature high pressure enclosed reaction ring
Border can make each presoma component rapid-digestion react new component of the generation with catalytic activity, and uniform load is in recessed
On convex rod soil, hydro-thermal reaction method has the advantages that corrosion resistance is good, reaction unharmful substance overflows, acid and alkali-resistance, reduces pollution,
It is easy and safe to operate.
Relative to prior art, the invention has the advantages that, 1）Low, the of the invention carrier of the technical scheme production cost
Material is that high pure attapulgite clay is bar-like structure, with larger ratio surface and aperture, is conducive to various active catalytic components
Load, and it is cheap and easy to get；The oxide of vanadium has higher efficiency in terms of catalyst nox removing, but to catalysis temperature
Degree requires higher so that vanadium and cerium are formed new active catalytic components cerium vanadate by hydro-thermal reaction by energy consumption increase, the present invention,
Uniformly it is carried on bar-shaped attapulgite, the temperature needed for the SCR removing nitrogen oxides not only substantially reduced
Degree, also improves the active sites points of catalyst surface so that catalytic performance has larger lifting, and with certain anti-
SO2Poison performance；3）Preparation method is simple, and synthesis temperature is low, and raw material availability is high, is more conducive to reach that clean and effective is kept the safety in production
Purpose.
Embodiment：
In order to deepen the understanding of the present invention, the technical program is described in detail with reference to embodiment.
Embodiment 1:
A kind of SCR low-temperature denitration catalyst and preparation method thereof, methods described step is as follows：
Step 1：High pure attapulgite clay is added to stirring in distilled water and forms attapulgite suspension；
Step 2：The soluble-salt of ammonium metavanadate and cerium is added sequentially in attapulgite suspension, heating water bath is allowed to abundant
Mixed dissolution；
Step 3：Ammoniacal liquor is added dropwise into mixture, regulation pH value is 9；
Step 4：Above-mentioned mixed liquor is moved to hydro-thermal reaction is carried out in hydrothermal reaction kettle；
Step 5：Suction filtration obtains mixture precipitation after hydro-thermal reaction, is washed with distilled water to neutrality
Step 6：Obtained sample is dried, ground, you can the low-temperature selective catalytic reduction denitration catalysis needed for obtaining
Agent；
Wherein：The purity of high pure attapulgite clay described in step 1 is mass fraction 99%, and consumption is 2 grams, and distillation water consumption is 10
Milliliter；
The soluble-salt of cerium described in step 2 is six water cerous nitrates；
Water bath heating temperature described in step 2 is 60 DEG C, and the heating water bath time is 30 minutes；
Ammonium metavanadate inventory described in step 2 is 0.002mol, and the molar ratio of ammonium metavanadate and six water cerous nitrates is 1:1；
The mass concentration of ammoniacal liquor described in step 3 is 25%；
Hydrothermal temperature control described in step 4 is 150 DEG C, a length of 8 hours during hydro-thermal reaction；
Drying temperature control described in step 6 is 80 DEG C, and drying time is 24 hours.
Embodiment 2:
A kind of SCR low-temperature denitration catalyst and preparation method thereof, methods described step is as follows：
Step 1：High pure attapulgite clay is added to stirring in distilled water and forms attapulgite suspension；
Step 2：The soluble-salt of ammonium metavanadate and cerium is added sequentially in attapulgite suspension, heating water bath is allowed to abundant
Mixed dissolution；
Step 3：Ammoniacal liquor is added dropwise into mixture, regulation pH value is 14；
Step 4：Above-mentioned mixed liquor is moved to hydro-thermal reaction is carried out in hydrothermal reaction kettle；
Step 5：Suction filtration obtains mixture precipitation after hydro-thermal reaction, is washed with distilled water to neutrality
Step 6：Obtained sample is dried, ground, you can the low-temperature selective catalytic reduction denitration catalysis needed for obtaining
Agent；
Wherein：The purity of high pure attapulgite clay described in step 1 is mass fraction 99%, and consumption is 6 grams, and distillation water consumption is 30
Milliliter；
The soluble-salt of cerium described in step 2 is six water cerium chlorides；
Water bath heating temperature described in step 2 is 80 DEG C, and the heating water bath time is 60 minutes；
Ammonium metavanadate inventory described in step 2 is 0.008mol, and the molar ratio of ammonium metavanadate and six water cerous nitrates is 1:1；
The mass concentration of ammoniacal liquor described in step 3 is 28%；
Hydrothermal temperature control described in step 4 is 200 DEG C, a length of 12 hours during hydro-thermal reaction；
Drying temperature control described in step 6 is 100 DEG C, and drying time is 28 hours.
Embodiment 3:
A kind of SCR low-temperature denitration catalyst and preparation method thereof, methods described step is as follows：
Step 1：High pure attapulgite clay is added to stirring in distilled water and forms attapulgite suspension；
Step 2：The soluble-salt of ammonium metavanadate and cerium is added sequentially in attapulgite suspension, heating water bath is allowed to abundant
Mixed dissolution；
Step 3：Ammoniacal liquor is added dropwise into mixture, regulation pH value is 12；
Step 4：Above-mentioned mixed liquor is moved to hydro-thermal reaction is carried out in hydrothermal reaction kettle；
Step 5：Suction filtration obtains mixture precipitation after hydro-thermal reaction, is washed with distilled water to neutrality
Step 6：Obtained sample is dried, ground, you can the low-temperature selective catalytic reduction denitration catalysis needed for obtaining
Agent；
Wherein：The purity of high pure attapulgite clay described in step 1 is mass fraction 99%, and consumption is 4 grams, and distillation water consumption is 20
Milliliter；
The soluble-salt of cerium described in step 2 is six water cerous nitrates or six water cerium chlorides；
Water bath heating temperature described in step 2 is 70 DEG C, and the heating water bath time is 50 minutes；
Ammonium metavanadate inventory described in step 2 is 0.005mol, and the molar ratio of ammonium metavanadate and six water cerous nitrates is 1:1；
The mass concentration of ammoniacal liquor described in step 3 is 26%；
Hydrothermal temperature control described in step 4 is 180 DEG C, a length of 10 hours during hydro-thermal reaction；
Drying temperature control described in step 6 is 90 DEG C, and drying time is 25 hours.
Application Example 1：
Weigh 0.3g catalyst CeVOx(0.002)/ATP, investigates low-temperature catalytic activity window of the catalyst between 120 ~ 260 DEG C
Catalytic performance.The total flow of simulated flue gas is 1000ml/min, and air speed is 40000h-1, simulated flue gas is by 3% O2、600ppm
NO、600ppm NH3With Balance Air N2Composition.Test result shows：Between 120-180 DEG C, the denitration performance of catalyst is with temperature
The increase of degree and increase, more than 85% is reached at 160-180 DEG C, then as temperature further increases, the performance of catalyst starts
Decline.Catalyst CeVOx(0.002)/ATP optimum activity reaction temperature is 180 DEG C, and denitration efficiency is 95.61%.
Application Example 2
Weigh 0.3g catalyst CeVOx(0.004)/ATP, investigates low-temperature catalytic activity window of the catalyst between 120 ~ 260 DEG C
Catalytic performance.The total flow of simulated flue gas is 1000ml/min, and air speed is 40000h-1, simulated flue gas is by 3% O2、600ppm
NO、600ppm NH3With Balance Air N2Composition.Test result shows：Between 120-200 DEG C, the denitration performance of catalyst is with temperature
The increase of degree and increase, more than 90% is reached at 160-200 DEG C, then as temperature further increases, the performance of catalyst starts
Decline.Catalyst CeVOx(0.004)/ATP optimum activity reaction temperature is 200 DEG C, and denitration efficiency is 93.12%.
Application Example 3
Weigh 0.3g catalyst CeVOx(0.008)/ATP, investigates low-temperature catalytic activity window of the catalyst between 120 ~ 260 DEG C
Catalytic performance.The total flow of simulated flue gas is 1000ml/min, and air speed is 40000h-1, simulated flue gas is by 3% O2、600ppm
NO、600ppm NH3With Balance Air N2Composition.Test result shows：Between 120-200 DEG C, the denitration performance of catalyst is with temperature
The increase of degree and increase, more than 93% is reached at 160-200 DEG C, then as temperature further increases, the performance of catalyst starts
Decline.Catalyst CeVOx(0.008)/ATP optimum activity reaction temperature is 200 DEG C, and denitration efficiency is 96.78%.
Application Example 4
Weigh 0.3g catalyst CeVOx(0.008)/ATP, anti-SO is carried out in 200 DEG C of temperature windows2Performance test.Simulated flue gas
Total flow be 1000ml/min, air speed is 40000h-1, simulated flue gas is by 3% O2、600ppm NO、600ppm NH3、100-
300ppmSO2With Balance Air N2Composition.Anti- SO2The performance test results show：O2Under existence condition, 100ppm SO is added2, catalysis
The denitration effect of agent is unaffected or even is slightly increased, with addition SO2The increase of concentration, under the performance of catalyst starts
Drop：200ppmSO2When, catalyst CeVOx(0.008)/ATP denitration efficiency is reduced to 88.82%；300ppmSO2When, catalyst
CeVOx(0.008)/ATP denitration efficiency is reduced to 84.39%, and reaction stops only being passed through SO after three hours2, the efficiency of catalyst opens
Beginning slowly increases, and all returns to original optimal catalytic states substantially after 1h.
It should be noted that above-described embodiment, not for limiting protection scope of the present invention, in above-mentioned technical proposal
On the basis of made equivalents or replacement each fall within the scope that the claims in the present invention are protected.
Claims (8)
1. a kind of SCR low-temperature denitration catalyst and preparation method thereof, it is characterised in that methods described step is such as
Under：Step 1：High pure attapulgite clay is added to stirring in distilled water and forms attapulgite suspension；
Step 2：The soluble-salt of ammonium metavanadate and cerium is added sequentially in attapulgite suspension, heating water bath is allowed to abundant
Mixed dissolution；
Step 3：Ammoniacal liquor is added dropwise into mixture, regulation pH value is in 9-14；
Step 4：Above-mentioned mixed liquor is moved to hydro-thermal reaction is carried out in hydrothermal reaction kettle；
Step 5：Suction filtration obtains mixture precipitation after hydro-thermal reaction, is washed with distilled water to neutrality
Step 6：Obtained sample is dried, ground, you can the low-temperature selective catalytic reduction denitration catalysis needed for obtaining
Agent.
2. a kind of SCR low-temperature denitration catalyst according to claim 1 and preparation method thereof, its feature
It is：High pure attapulgite clay purity described in step 1 is mass fraction 99%, and consumption is 2 ~ 6 grams, and distillation water consumption is 10 ~ 30 millis
Rise.
3. a kind of SCR low-temperature denitration catalyst according to claim 2 and preparation method thereof, its feature
It is：The soluble-salt of cerium described in step 2 is six water cerous nitrates or six water cerium chlorides.
4. a kind of SCR low-temperature denitration catalyst according to Claims 2 or 3 and preparation method thereof, it is special
Levy and be：Water bath heating temperature described in step 2 is 60 ~ 80 DEG C, and the heating water bath time is 30 ~ 60 minutes.
5. a kind of SCR low-temperature denitration catalyst according to claim 4 and preparation method thereof, its feature
It is：Ammonium metavanadate inventory described in step 2 is 0.002mol ~ 0.008mol, and ammonium metavanadate and six feeding intake for water cerous nitrate are rubbed
You are than being 1:1.
6. a kind of SCR low-temperature denitration catalyst according to claim 5 and preparation method thereof, its feature
It is：Weights of ammonia concentration described in step 3 is 25% ~ 28%.
7. a kind of SCR low-temperature denitration catalyst according to claim 6 and preparation method thereof, its feature
It is：Hydrothermal temperature control described in step 4 is 150 ~ 200 DEG C, a length of 8 ~ 12 hours during hydro-thermal reaction.
8. a kind of SCR low-temperature denitration catalyst according to claim 7 and preparation method thereof, its feature
It is：Drying temperature control described in step 6 is 80 ~ 100 DEG C, and drying time is 24 ~ 28 hours.
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Cited By (3)
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|---|---|---|---|---|
| CN110773168A (en) * | 2019-11-04 | 2020-02-11 | 中国石油大学(华东) | A kind of denitration catalyst and its preparation method and a kind of denitration method |
| 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 |
| CN117696044A (en) * | 2024-01-24 | 2024-03-15 | 兰州大学 | Attapulgite-doped rare earth SCR catalyst and preparation method thereof |
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| CN105771967A (en) * | 2016-03-30 | 2016-07-20 | 盐城工学院 | Metal oxide-vanadate/attapulgite catalyst |
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| CN110773168A (en) * | 2019-11-04 | 2020-02-11 | 中国石油大学(华东) | A kind of denitration catalyst and its preparation method and a kind of denitration method |
| 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 |
| CN117696044A (en) * | 2024-01-24 | 2024-03-15 | 兰州大学 | Attapulgite-doped rare earth SCR catalyst and preparation method thereof |
| CN117696044B (en) * | 2024-01-24 | 2024-06-11 | 兰州大学 | A kind of attapulgite rare earth doped SCR catalyst and preparation method thereof |
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Application publication date: 20170815 |