CN108499556A - A kind of low-temperature denitration catalyst and preparation method thereof - Google Patents
A kind of low-temperature denitration catalyst and preparation method thereof Download PDFInfo
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- CN108499556A CN108499556A CN201810297132.3A CN201810297132A CN108499556A CN 108499556 A CN108499556 A CN 108499556A CN 201810297132 A CN201810297132 A CN 201810297132A CN 108499556 A CN108499556 A CN 108499556A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/90—Injecting reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
Include as the microporous activated Carbon Materials of carrier components and as the ZrO of active component the present invention provides a kind of low-temperature denitration catalyst and preparation method thereof2、CeO2、La2O3、Y2O3.The present invention can effectively adsorb nitre, in conjunction with fixed bed in use, better.
Description
Technical field
The invention belongs to technical field of air pollution control more particularly to a kind of low-temperature denitration catalyst and its preparation sides
Method.
Background technology
With the development of modern industrial production, the problem of atmosphere pollution becomes people's extensive concern, while nitrogen oxides
NOxAtmosphere polluting problem be gradually taken seriously since the seventies.By studying it has been found that NOxCan not only it cause photochemical
Smog is learned, and the health of the mankind can be endangered, cause high-content nitric acid rain, reduce ozone layer and some other problem, is caused
Serious atmosphere pollution.
The denitration technology of existing market mainstream is selective catalytic reduction（SCR）Technology, SCR removing nitrogen oxides is a kind of
Ripe gas denitrifying technology, the technology is because its secondary pollution is small, and purification efficiency is high, and technology maturation, denitrification rate is high by 80 ~ 90%,
It is suitble to that capacity is big, continuous emission source, becomes denitration technology most widely used in the world.Catalyst is the core of SCR denitration method
Technology.At present SCR catalyst mainly include noble metal catalyst, molecular sieve (Zeolite) catalyst, carbon-supported catalysts and
Metal oxide catalyst.Wherein, it is commonly metal oxide catalyst, such as V2O5、WO3、MoO3Deng such catalyst one
As with TiO2For carrier, there is also many defects while having the advantages that certain for such catalyst.For example, the temperature one of exhaust gas
As be 80 degree, and Ti-base catalyst denitration operating temperature is higher（300~400℃）, SCR device can only be arranged in economizer and
Between air preheater, but herein in flue gas there are a large amount of flying dusts, contain alkali metal in flying dust, the substances such as arsenic and mercury can corrode
With poison catalyst, lead to catalyst inactivation, reduce its service life, while application temperature window is relatively narrow；On the other hand, such
Vanadium component is easy to run off in catalyst, is damaged to environment and human body.
Invention content
Include the micropore as carrier components to solve the above problems, the present invention provides a kind of low-temperature denitration catalyst
Absorbent charcoal material and ZrO as active component2、CeO2、La2O3、Y2O3。
By weight percentage, CeO2Content is 1% ~ 10%, ZrO2Content is 1% ~ 5%, La2O3Content is 0.1% ~ 1%, Y2O3
Content is 0.1% ~ 1%, remaining is absorbent charcoal material.
Further, CeO2Content is 3.56% ~ 5.59%, ZrO2Content is 2.89% ~ 4.51%, La2O3Content is 0.25%
~ 0.58%, Y2O3Content is 0.28% ~ 0.61%, remaining is activated carbon.
Further, CeO2Content is that 5.51%, ZrO2 contents are 3.52%, La2O3Content is 0.58%, Y2O3Content is
0.51%, remaining is activated carbon.
Further, in activated carbon surface micropore, micropore ratio of the aperture less than 2nm is more than 80%.
The preparation method of above-mentioned low-temperature denitration catalyst, which is characterized in that include the following steps：
Step 1：Prepare activated carbon：Activated carbon is warming up to 350 ~ 500 DEG C in a furnace, N is used in temperature-rise period2Protection rises
Temperature to holding constant temperature after 350 ~ 500 DEG C for a period of time, is passed through O in thermostatic process2And CO2Mixed gas replace N2。
Step 2：Prepare catalyst component：With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O it is
Raw material is configured to cerium-zirconium-lanthanum-yttrium mixing salt solution, and H then is added into cerium-zirconium-lanthanum-yttrium mixing salt solution2O2, will be above-mentioned molten
It is stirred after constant volume after liquid mixing, i.e., prepared catalyst component solution.
Step 3：Dipping：Catalyst component solution obtained by step 2 is impregnated into the activated carbon obtained by step 1 will mixing
Solution is stood after being stirred with activated carbon.
Step 4：It is dry：By the impregnated material obtained by step 3, drying obtains dry SCR low-temperature denitration catalyst forerunners
Body.
Step 5：Calcining：By dry SCR low-temperature denitration catalysts presoma obtained by step 4 under conditions of starvation
Calcining obtains final removing nitre material.
Further, in step 2, Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2The weight of O
Percentage is 65%：33%：0.9%：1.1%.
Further, the weight percent that mixed solution accounts for activated carbon is 40% ~ 65%.
Further, in step 2, PVA solution is additionally added into cerium-zirconium-lanthanum-yttrium mixing salt solution.
Further, in step 5, dry SCR low-temperature denitration catalysts presoma under conditions of starvation in 350 ~
600 DEG C of 1 ~ 3h of calcining.
Beneficial effects of the present invention are：
The present invention can be achieved denitration material and carry out boiler waste gas denitration in the middle low temperature of 80-240 degree, and most of boiler is useless
The temperature of gas itself can reach at least 80 degree, therefore, there is no need to install air preheater, reduce consumption caused by being heated to exhaust gas
Energy.Catalyst operating environment is also purified, and service life is long, and heavy metal of the catalyst without containing pollution environment itself, is kept away
Exempt to cause secondary pollution.
Specific implementation mode
The present invention includes as the microporous activated Carbon Materials of carrier components and as the ZrO of active component2、CeO2With
La2O3、Y2O3.Wherein, by weight percentage, CeO2Content is 1% ~ 10%, ZrO2Content is 1% ~ 5%, La2O3Content be 0.1% ~
1%, Y2O3Content is 0.1% ~ 1%.Remaining is absorbent charcoal material.The advantages of activated carbon is support material is environment friendly and pollution-free preparation work
Skill and relatively low with cost.
Preferably, CeO2Content is 3.56% ~ 5.59%, ZrO2Content is 2.89% ~ 4.51%, La2O3Content be 0.25% ~
0.58%, Y2O3Content is 0.28% ~ 0.61%, remaining is activated carbon.It is furthermore preferred that CeO2Content is 5.51%, ZrO2Content is
3.52%, La2O3Content is 0.58%, Y2O3Content is 0.51%, remaining is activated carbon.
Absorbent charcoal material of the present invention includes wood activated charcoal, activated carbon from bamboo, active fruit shell carbon, coaly activated carbon
And one or more of activated carbon fibre etc..
Activated carbon face shaping of the present invention can be column-shaped active carbon, hollow activated carbon, spherical activated charcoal, bee
One or more of nest activated carbon or fibrous activated carbon.
Absorbent charcoal material of the present invention is mainly with aperture<2nm is based on micropore（<The micropore ratio of 2nm >=
80%）, specific surface area>850m2/g.Activated carbon under the index can effectively adsorb NOXMolecule provides more reaction interfaces and anti-
Between seasonable.
SCR low-temperature denitration catalysts of the present invention, using absorbent charcoal material as carrier, CeO2For dominant catalyst, ZrO2、
La2O3、Y2O3For auxiliary agent.
Activated carbon can improve reaction interface as carrier, increase removal efficiency.Using CeO2 as dominant catalyst,
Reaction temperature can be effectively reduced, low-temperature catalytic activity is increased.Catalyst can be improved using ZrO2 as cocatalyst to live
Property, while improving catalyst thermal stability.Using La2O3And Y2O3Two kinds of auxiliary agents, can effectively improve the thermostabilization of catalyst
Property, storage oxygen interface is provided, while making up the defect of single atomic radius fixed value, to further increase catalyst activity.
The present invention also provides a kind of preparation methods preparing above-mentioned denitration material, include the following steps：
Step 1：Prepare activated carbon.In a furnace by activated carbon（The present embodiment electric tube furnace）In with the speed of 3 ~ 10 DEG C/min
Rate is warming up to 350 ~ 500 DEG C, and N is used in temperature-rise period2Protection, is warming up to 350 ~ 500 DEG C of 1 ~ 2h of constant temperature, is passed through in thermostatic process
O2And CO2Mixed gas replace N2, wherein O2Content is 5% ~ 25%, CO2Content is 75% ~ 95%.
The step is using clean pollution-free oxygen and CO2Carrier material is modified, modifying process is environment friendly and pollution-free, leads to
Cross O2And CO2Synergistic effect, adjustment is advanced optimized to the pore structure of carrier, to increase its oxygen-containing functional group and reaction interface,
Obtain the low-temperature denitration catalyst carrier haveing excellent performance.
Step 2：Prepare catalyst component.With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O is
Raw material, by said components not according to weight percent 65%：33%：0.9%：1.1% is configured to cerium-zirconium-lanthanum-of 10% mass fraction
Then 30% H is added in yttrium mixing salt solution into mixed solution2O2With 10% PVA solution, addition and Ce (NO3)2.6H2O
Molar ratio be 1：1, it is settled to 1.5L after above-mentioned solution is mixed.After constant volume, 0.5h is stirred, i.e., prepared catalyst component is molten
Liquid.
The step uses non-heavy metal elemental cerium-zirconium-lanthanum-yttrium as catalyst component in active component preparation, will not shape
At dangerous waste, secondary pollution is caused, while interacting between each component, promotes catalyst performance.It should be noted that molten
It is preferred embodiment that PVA is added in liquid, is to improve solution in order to further enhance the dispersibility of metallic in mixed solution
Uniformity, while increasing the specific surface of active component, improve catalytic performance.
Step 3：Dipping.Catalyst component solution obtained by step 2 is impregnated into the modified activated carbon of step 1, is mixed
The weight percent that solution accounts for activated carbon is 40% ~ 65%, and mixed solution is proportionally added separately to reaction kettle and is stirred evenly
Afterwards, 30min is stood.
Step 4：It is dry.By the impregnated material obtained by step 3,2-4h is dried at 80 ~ 110 DEG C, it is low to obtain dry SCR
Warm denitrating catalyst presoma.
Step 5：Calcining.By dry SCR low-temperature denitration catalysts presoma obtained by step 4 under conditions of starvation
In 350 ~ 600 DEG C（5 ~ 10 DEG C/min of heating rate）Calcine 1 ~ 3h.
The specific embodiment of preparation method is illustrated below.
Specific embodiment 1：
Step 1：Prepare activated carbon.By activated carbon in a furnace in the rate of 3 DEG C/min be warming up to 350 DEG C, in temperature-rise period
Using N2Protection, is warming up to 350 DEG C of constant temperature 1h, O is passed through in thermostatic process2And CO2Mixed gas replace N2, wherein O2Content is
5% and CO2Content is 95%.
Step 2：Prepare catalyst component.With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O is
Raw material, by said components not according to weight percent 65%：33%：0.9%：1.1% is configured to cerium-zirconium-lanthanum-of 10% mass fraction
Then 30% H is added in yttrium mixing salt solution into mixed solution2O2With 10% PVA solution, addition and Ce (NO3)2.6H2O
Molar ratio be 1：1, it is settled to 1.5L after above-mentioned solution is mixed.After constant volume, 0.5h is stirred, i.e., prepared catalyst component is molten
Liquid.
Step 3：Dipping.Catalyst component solution obtained by step 2 is impregnated into the modified activated carbon of step 1, is mixed
The weight percent that solution accounts for activated carbon is 40%, mixed solution is proportionally added separately to after reaction kettle stirs evenly, quiet
Set 30min.
Step 4：It is dry.By the impregnated material obtained by step 3,2-4h is dried at 80 ~ 110 DEG C, it is low to obtain dry SCR
Warm denitrating catalyst presoma.
Step 5：Calcining.By dry SCR low-temperature denitration catalysts presoma obtained by step 4 under conditions of starvation
In 350 DEG C（5 DEG C/min of heating rate）Calcine 1h.
Specific embodiment 2：
Step 1：Prepare activated carbon.Activated carbon is warming up to 500 DEG C, in temperature-rise period with the rate of 10 DEG C/min in a furnace
Using N2Protection, is warming up to 500 DEG C of constant temperature 2h, O is passed through in thermostatic process2And CO2Mixed gas replace N2, wherein O2Content is
25%、CO2Content is 75%.
Step 2：Prepare catalyst component.With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O is
Raw material, by said components not according to weight percent 65%：33%：0.9%：1.1% is configured to cerium-zirconium-lanthanum-of 10% mass fraction
Then 30% H is added in yttrium mixing salt solution into mixed solution2O2With 10% PVA solution, addition and Ce (NO3)2.6H2O
Molar ratio be 1：1, it is settled to 1.5L after above-mentioned solution is mixed.After constant volume, 0.5h is stirred, i.e., prepared catalyst component is molten
Liquid.
Step 3：Dipping.Catalyst component solution obtained by step 2 is impregnated into the modified activated carbon of step 1, is mixed
The weight percent that solution accounts for activated carbon is 65%, mixed solution is proportionally added separately to after reaction kettle stirs evenly, quiet
Set 30min.
Step 4：It is dry.By the impregnated material obtained by step 3,4h is dried at 110 DEG C, it is de- to obtain dry SCR low temperature
Denox catalyst presoma.
Step 5：Calcining.By dry SCR low-temperature denitration catalysts presoma obtained by step 4 under conditions of starvation
In 600 DEG C（10 DEG C/min of heating rate）Calcine 3h.
Specific embodiment 3：
Step 1：Prepare activated carbon.Activated carbon is warming up to 450 DEG C with the rate of 7 DEG C/min in a furnace, is adopted in temperature-rise period
Use N2Protection, is warming up to 450 DEG C of constant temperature 1.5h, O is passed through in thermostatic process2And CO2Mixed gas replace N2, wherein O2Content is
20% and CO2Content is 80%.
Step 2：Prepare catalyst component.With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O it is
Raw material, by said components not according to weight percent 65%：33%：0.9%：1.1% is configured to cerium-zirconium-lanthanum-of 10% mass fraction
Then 30% H is added in yttrium mixing salt solution into mixed solution2O2With 10% PVA solution, addition and Ce (NO3)2.6H2O
Molar ratio be 1：1, it is settled to 1.5L after above-mentioned solution is mixed.After constant volume, 0.5h is stirred, i.e., prepared catalyst component is molten
Liquid.
Step 3：Dipping.Catalyst component solution obtained by step 2 is impregnated into the modified activated carbon of step 1, is mixed
The weight percent that solution accounts for activated carbon is 50%, mixed solution is proportionally added separately to after reaction kettle stirs evenly, quiet
Set 30min.
Step 4：It is dry.By the impregnated material obtained by step 3,2-4h is dried at 100 DEG C, obtains dry SCR low temperature
Denitrating catalyst presoma.
Step 5：Calcining.By dry SCR low-temperature denitration catalysts presoma obtained by step 4 under conditions of starvation
In 500 DEG C（7 DEG C/min of heating rate）Calcine 2h.
Claims (10)
1. a kind of low-temperature denitration catalyst, which is characterized in that include as the microporous activated Carbon Materials of carrier components and as work
The ZrO of property component2、CeO2、La2O3、Y2O3。
2. low-temperature denitration catalyst as described in claim 1, which is characterized in that by weight percentage, CeO2Content be 1% ~
10%, ZrO2Content is 1% ~ 5%, La2O3Content is 0.1% ~ 1%, Y2O3Content is 0.1% ~ 1%, remaining is absorbent charcoal material.
3. low-temperature denitration catalyst as claimed in claim 2, which is characterized in that CeO2Content is 3.56% ~ 5.59%, ZrO2Contain
Amount is 2.89% ~ 4.51%, La2O3Content is 0.25% ~ 0.58%, Y2O3Content is 0.28% ~ 0.61%, remaining is activated carbon.
4. low-temperature denitration catalyst as claimed in claim 3, which is characterized in that by weight percentage, CeO2Content is
5.51%, ZrO2 content are 3.52%, La2O3Content is 0.58%, Y2O3Content is 0.51%, remaining is activated carbon.
5. low-temperature denitration catalyst as described in claim 1, which is characterized in that in activated carbon surface micropore, aperture is less than 2nm
Micropore ratio be more than 80%.
6. such as the preparation method of claim 1 ~ 5 any one of them low-temperature denitration catalyst, which is characterized in that including walking as follows
Suddenly：
Step 1：Prepare activated carbon：Activated carbon is warming up to 350 ~ 500 DEG C in a furnace, N is used in temperature-rise period2Protection rises
Temperature to holding constant temperature after 350 ~ 500 DEG C for a period of time, is passed through O in thermostatic process2And CO2Mixed gas replace N2；
Step 2：Prepare catalyst component：With Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2O it is raw material
It is configured to cerium-zirconium-lanthanum-yttrium mixing salt solution, H then is added into cerium-zirconium-lanthanum-yttrium mixing salt solution2O2, above-mentioned solution is mixed
It is stirred after constant volume after conjunction, i.e., prepared catalyst component solution；
Step 3：Dipping：Catalyst component solution obtained by step 2 is impregnated into mixed solution in the activated carbon obtained by step 1
It is stood after being stirred with activated carbon；
Step 4：It is dry：By the impregnated material obtained by step 3, drying obtains dry SCR low-temperature denitration catalyst presomas；
Step 5：Calcining：Dry SCR low-temperature denitration catalysts presoma obtained by step 4 is forged under conditions of starvation
It burns, obtains final removing nitre material.
7. the preparation method of low-temperature denitration catalyst as claimed in claim 6, which is characterized in that in step 2, Ce (NO3)2.6H2O、ZrOCO3、La(NO3)3.6H2O、Y(NO3)3.6H2The weight percent of O is 65%：33%：0.9%：1.1%.
8. the preparation method of low-temperature denitration catalyst as claimed in claim 6, which is characterized in that mixed solution accounts for activated carbon
Weight percent is 40% ~ 65%.
9. the preparation method of low-temperature denitration catalyst as claimed in claim 6, which is characterized in that in step 2, to cerium-zirconium-
It is additionally added PVA solution in lanthanum-yttrium mixing salt solution.
10. the preparation method of low-temperature denitration catalyst as claimed in claim 6, which is characterized in that in step 5, dry SCR
Low-temperature denitration catalyst presoma calcines 1 ~ 3h under conditions of starvation in 350 ~ 600 DEG C.
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| CN111790398A (en) * | 2020-07-03 | 2020-10-20 | 河北唯沃环境工程科技有限公司 | Low-temperature denitration catalyst and preparation method thereof |
| CN111939757A (en) * | 2020-08-10 | 2020-11-17 | 暨南大学 | Method for removing nitrogen oxides in low-temperature flue gas |
| CN114849687A (en) * | 2022-03-24 | 2022-08-05 | 山东亮剑环保新材料有限公司 | Preparation method of rare earth modified composite activated carbon-based catalyst |
| CN114931943A (en) * | 2022-05-18 | 2022-08-23 | 山东亮剑环保新材料有限公司 | SCR denitration catalyst and production method thereof |
| CN116689018A (en) * | 2023-05-25 | 2023-09-05 | 南京工业大学 | Low-temperature denitration catalyst synthesized by taking waste FCC catalyst as raw material and preparation method thereof |
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| CN116689018A (en) * | 2023-05-25 | 2023-09-05 | 南京工业大学 | Low-temperature denitration catalyst synthesized by taking waste FCC catalyst as raw material and preparation method thereof |
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