CN108452796A - A kind of preparation method of the modified montmorillonite used base SCR denitration of Supported Manganese and cerium - Google Patents
A kind of preparation method of the modified montmorillonite used base SCR denitration of Supported Manganese and cerium Download PDFInfo
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- CN108452796A CN108452796A CN201810200152.4A CN201810200152A CN108452796A CN 108452796 A CN108452796 A CN 108452796A CN 201810200152 A CN201810200152 A CN 201810200152A CN 108452796 A CN108452796 A CN 108452796A
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/30—Ion-exchange
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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
- B01J23/16—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
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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Abstract
The present invention relates to the preparation methods of a kind of Supported Manganese and the modified montmorillonite used base catalyst of cerium, belong to catalysis material preparation field.The deficiencies of present invention is directed to prior art carrier higher price, reactivity is relatively low, temperature window is relatively narrow, provides a kind of preparation method for the modified montmorillonite used base catalyst having loaded manganese and cerium.Montmorillonite is modified using titanium tetrachloride solution, ion-exchange is reapplied and loads to active metal on carrier, active metal is made to be evenly distributed on carrier, then SCR denitration is made by calcining.The catalyst denitration efficiency is higher, and reaction temperature window is wider, there is the application prospect as industrial denitrating catalyst.
Description
Technical field
The present invention relates to the preparation methods of a kind of Supported Manganese and the modified montmorillonite used base catalyst of cerium, belong to catalysis material system
Standby field.
Background technology
Denitrating flue gas refers to the process of that denitrification is removed in combustion product gases, is antipollution important measure.
Nitrogen oxides is one of primary pollution source of atmosphere pollution, has the harm of intoxicating to humans and animals.What it or acid rain generated
Main arch-criminal meets water and generates nitric acid and nitrous acid to form acid rain and acid mist, and in addition to this, it also results in photochemistry cigarette
Mist and Ozone hole, seriously pollute environment, and the damage for being difficult to repair is generated to the environment that we depend on for existence.Flue gas is de- at this stage
Nitre main method is selective catalytic reduction (SCR) and selective non-catalytic reduction method (SNCR), wherein SCR denitrating flue gas skill
Art is since its denitration efficiency is high, influences denitration technology that is small and becoming research and be most widely used to boiler system.Catalyst
It is the core product of SCR denitrating flue gas, its quality directly determines the height of transformation efficiency of the oxides of nitrogen, in entire SCR denitration
It is played a crucial role in technology.
Manganese dioxide is to study relatively broad catalyst at this stage, there is catalysis effect more outstanding in many reactions
Fruit is widely used to the fields such as hydrogen peroxide decomposition, Oxidation of Carbon Monoxide.The result of study table of some SCR denitrations
Bright manganese dioxide has very high catalytic activity, by most conversion of nitrogen oxides is nitrogen under the conditions of can be existing for ammonia
Gas, denitration efficiency is very high and reaction temperature is relatively low, meets the requirement of denitrating catalyst at this stage.
Ceria is cheap as one kind, thermostabilization is good, active higher, with long service life rare earth material, is urging
Being widely used for change field is general, is either used as individual catalyst, or be all fairly obvious as carrier builder activity.
Main cause is the property because of ceria release oxygen with storage and largely, and this property is mainly by titanium dioxide
What the Lattice oxygen defect of cerium determined.The experimental results showed that the catalyzed conversion that the introducing of ceria significantly improves nitrogen oxides is lived
Property has widened reflection temperature window.
Montmorillonite is a kind of alumino-silicate, is bentonitic main component.Montmorillonite is the clay mine of three-layer tablet shape structure
Object, centre are alumina octahedral, are up and down oxygen-octahedron.Montmorillonite particle is tiny, about 0.2~1 micron, has colloidal dispersions
Characteristic contains the crystallization water and some exchange cations in crystal structure interlayer, has higher ion exchange capacity, have very strong sun
Ion-exchange capacity can use K under certain physical and chemical condition+、Ti4+、Mg2+、Fe3+、Cu2+Ion friendship is carried out Deng cation
It changes.Montmorillonite is high in China's reserves, cheap, is good catalyst carrier.
Invention content
The purpose of the present invention is overcoming prior art carrier higher price, reactivity is relatively low, temperature window is relatively narrow etc. no
Foot, provide a kind of modified montmorillonite used base Supported Manganese, cerium catalyst preparation method.
The technical solution adopted by the present invention is to include the following steps：
1) a certain amount of montmorillonite is weighed, adds it to and 12-36h is stirred at room temperature in deionized water.According to every gram
Montmorillonite corresponds to 5-10mmolTi4+Amount, TiCl4 solution is made and (a certain amount of concentrated hydrochloric acid is added in solution as pillared solution
Prevent its hydrolysis), 6-12h, aging 12-24h is stirred at room temperature.Pillared solution after aging is added dropwise to montmorillonite to hang
In supernatant liquid, 12-36h is stirred at room temperature, centrifuges, removes supernatant, washs drying, roasting obtains the pillared of Ti modifications
Montmorillonite；
2) it is 12% according to metal total load amount mass fraction, the mixed solution of manganese nitrate and cerous nitrate, wherein manganese is made
It is 1 with the ratio between the amount of substance of cerium:10 to 10:Between 1.The Ti pillared montmorillonites being modified are added in the mixed solution,
6-36h is stirred at 60 DEG C, is centrifuged；
3) it is repeated as many times step 2), until the amount of metal of load no longer changes.Washing, drying, horse is placed in by gained sample
Not in stove, 400-550 DEG C of roasting 4-8h stops heating and is cooled to room temperature, and the manganese dioxide of the modified montmorillonite used base loads of Ti is made
And ceria catalyst.
It is an advantage of the invention that：
(1) active metal is loaded on carrier using ion-exchange, overcomes being unevenly distributed of traditional infusion process, mistake
The shortcomings of amount load, so that active metal is evenly distributed on carrier and can just reach load maximum capacity.
(2) montmorillonite is modified using titanium tetrachloride solution, in montmorillonite Intercalation reaction titanium elements, after calcining
The titanium dioxide of formation and the manganese dioxide of load, ceria form pillared altogether, and the total of catalyst is made to be rendered as three
The three-dimensional pore passage structure of dimension.
(3) use montmorillonite as carrier, montmorillonite can substantially reduce catalyst in China's rich reserves, cheap
Cost of manufacture, and the structure feature of montmorillonite itself determines its unique physicochemical property, such as prodigious specific surface area, has
It is reacted conducive to catalysis.
(4) use two kinds of metals of manganese and cerium as catalytically-active metals, total catalytic action makes conversion ratio have larger carry
It rises, and temperature window bigger.
Specific implementation mode
3 embodiments of the present invention are provided further below：
Embodiment 1
2.000g montmorillonites are weighed, are added in 200ml beakers, 98ml deionized waters are added thereto, are made 2wt%'s
Montmorillonite suspension stirs for 24 hours at room temperature, makes its water swelling.With pipette pipette the concentrated hydrochloric acid of a concentration of 6M of 1.7ml in
In 100ml beakers, 2.2mlTiCl is added thereto under vigorous stirring4, deionized water is slowly added dropwise and is diluted to solution
Then 50ml makes solution be aged at room temperature and pillared solution is made for 24 hours.Pillared solution is added dropwise to montmorillonite suspension
In, it stirs for 24 hours, then centrifuges acquired solution at room temperature, and be washed with deionized into supernatant and be free of Cl-For
Only.Obtained solid product is dried overnight at 80 DEG C, then calcines 6h at 500 DEG C in Muffle furnace.Weigh 0.500g mass point
Number for 50% manganese nitrate solution and six nitric hydrate cerium solids of 0.607g in 200ml beakers (amount of the substance of Mn and Ce it
Than being 1：1) 100ml deionized waters, are added thereto, gained Ti pillared montmorillonites will be added thereto, and be stirred at 60 DEG C before
12h is centrifuged.It is repeated 3 times the ion-exchange step, so that exchange capacity is reached maximum, is then dried overnight at 80 DEG C, and
6h is calcined at 500 DEG C in Muffle furnace, obtains Ti pillared montmorillonite bases load manganese dioxide, ceria denitrating catalyst.
Using SCR denitration evaluating apparatus, 0.65gTi pillared montmorillonite bases load manganese dioxide, titanium dioxide are weighed
Cerium denitrating catalyst by its pressing mold, pulverize, after 30-50 mesh sample sifters, place it in reaction tube.Reaction gas overall flow rate is
1080ml/min, wherein NO are 810ppm, NH3For 810ppm, O2It is 5.84%, remaining filling gas is N2, air speed is
80000h-1.At 350 DEG C, 400 DEG C, 450 DEG C, NO conversion ratios are 56.8%, 71.1%, 78.0%.
Embodiment 2
2.000g montmorillonites are weighed, are added in 200ml beakers, 98ml deionized waters are added thereto, are made 2wt%'s
Montmorillonite suspension, stirs 30h at room temperature, makes its water swelling.With pipette pipette the concentrated hydrochloric acid of a concentration of 6M of 1.7ml in
In 100ml beakers, 2.2mlTiCl is added thereto under vigorous stirring4, deionized water is slowly added dropwise and is diluted to solution
50ml, is stirred at room temperature 9h, and pillared solution is made in ageing 18h.Pillared solution is added dropwise in montmorillonite suspension, in
30h is stirred at room temperature, then centrifuges acquired solution, and is washed with deionized into supernatant and is free of Cl-Until.Institute
It obtains solid product to be dried overnight at 65 DEG C, then 6h is calcined at 500 DEG C in Muffle furnace.Weighing 1.177g mass fractions is
(the ratio between the amount of substance of Mn and Ce is 50% manganese nitrate solution and six nitric hydrate cerium solids of 0.286g in 200ml beakers
5：1) 100ml deionized waters, are added thereto, gained Ti pillared montmorillonites will be added thereto, and be stirred at 60 DEG C for 24 hours before,
It centrifuges.It is repeated 3 times the ion-exchange step, so that exchange capacity is reached maximum, is then dried overnight at 80 DEG C, and in Muffle
8h is calcined at 500 DEG C in stove, obtains Ti pillared montmorillonite bases load manganese dioxide, ceria denitrating catalyst.
Using SCR denitration evaluating apparatus, 0.65gTi pillared montmorillonite bases load manganese dioxide, titanium dioxide are weighed
Cerium denitrating catalyst by its pressing mold, pulverize, after 30-50 mesh sample sifters, place it in reaction tube.Reaction gas overall flow rate is
1080ml/min, wherein NO are 810ppm, NH3For 810ppm, O2It is 5.84%, remaining filling gas is N2, air speed is
80000h-1.At 250 DEG C, 300 DEG C, 350 DEG C, NO conversion ratios are 40.1%, 69.8%, 80.5%.
Embodiment 3
2.000g montmorillonites are weighed, are added in 200ml beakers, 98ml deionized waters are added thereto, are made 2wt%'s
Montmorillonite suspension, stirs 36h at room temperature, makes its water swelling.With pipette pipette the concentrated hydrochloric acid of a concentration of 6M of 1.7ml in
In 100ml beakers, 2.2mlTiCl is added thereto under vigorous stirring4, deionized water is slowly added dropwise and is diluted to solution
50ml, is stirred at room temperature 12h, and pillared solution is made in ageing for 24 hours.Pillared solution is added dropwise in montmorillonite suspension,
36h is stirred at room temperature, then centrifuges acquired solution, and is washed with deionized into supernatant and is free of Cl-Until.
Obtained solid product is dried overnight at 65 DEG C, then calcines 8h at 500 DEG C in Muffle furnace.Weighing 1.245g mass fractions is
(the ratio between the amount of substance of Mn and Ce is 50% manganese nitrate solution and six nitric hydrate cerium solids of 0.151g in 200ml beakers
10：1) 100ml deionized waters, are added thereto, gained Ti pillared montmorillonites will be added thereto before, 36h is stirred at 60 DEG C,
It centrifuges.It is repeated 3 times the ion-exchange step, so that exchange capacity is reached maximum, is then dried overnight at 80 DEG C, and in Muffle
8h is calcined at 500 DEG C in stove, obtains Ti pillared montmorillonite bases load manganese dioxide, ceria denitrating catalyst.
Using SCR denitration evaluating apparatus, 0.65gTi pillared montmorillonite bases load manganese dioxide, titanium dioxide are weighed
Cerium denitrating catalyst by its pressing mold, pulverize, after 30-50 mesh sample sifters, place it in reaction tube.Reaction gas overall flow rate is
1080ml/min, wherein NO are 810ppm, NH3For 810ppm, O2It is 5.84%, remaining filling gas is N2, air speed is
80000h-1.At 250 DEG C, 300 DEG C, 350 DEG C, NO conversion ratios are 44.8%, 70.9%, 83.6%.
Claims (6)
1. the preparation method of the modified montmorillonite used base SCR denitration of a kind of Supported Manganese and cerium, it is characterized in that including following step
Suddenly：
1) a certain amount of montmorillonite is weighed, adds it to and 12-36h is stirred at room temperature in deionized water；TiCl is made4Solution
As pillared solution, a certain amount of concentrated hydrochloric acid is added in solution prevents its hydrolysis, and 6-12h, aging 12-24h is stirred at room temperature；It will
Pillared solution is added dropwise in montmorillonite suspension after aging, is stirred at room temperature 12-36h, is centrifuged, is removed supernatant
Liquid, washs drying, and roasting obtains the pillared montmorillonite of Ti modifications；
2) it is 12% according to metal total load amount mass fraction, the mixed solution of manganese nitrate and cerous nitrate, wherein manganese and cerium is made
The ratio between the amount of substance be 1:10 to 10:Between 1；The Ti pillared montmorillonites being modified are added in mixed solution, at 60 DEG C
6-36h is stirred, is centrifuged；
3) it is repeated as many times step 2), until the amount of metal of load no longer changes；Washing, drying, Muffle furnace is placed in by gained sample
In, 400-550 DEG C of roasting 4-8h stops heating and is cooled to room temperature, be made Ti modified montmorillonite used base loads manganese dioxide and
Ceria catalyst.
2. the preparation method of the modified montmorillonite used base SCR denitration of a kind of Supported Manganese according to claim 1 and cerium,
It is characterized in that：Obtained catalyst matrix is Ti pillared montmorillonites.
3. the preparation method of the modified montmorillonite used base catalyst of a kind of Supported Manganese according to claim 1 and cerium, feature
It is：The active metal of obtained catalyst load is manganese and cerium.
4. the preparation method of the modified montmorillonite used base catalyst of a kind of Supported Manganese according to claim 1 and cerium, feature
It is：The method for synthesizing pillared montmorillonite is infusion process, and the pillared liquid used is the TiCl of aging4Hydrochloric acid solution.
5. the preparation method of the modified montmorillonite used base catalyst of a kind of Supported Manganese according to claim 1 and cerium, feature
It is：When on supported active metals to matrix, the carrying method used is ion-exchange.
6. the preparation method of the modified montmorillonite used base catalyst of a kind of Supported Manganese according to claim 1 and cerium, feature
It is：The total mass fraction of supported active metals is 12%, and the dosage of pillared metal Ti is every gram of montmorillonite 5-10mmolTi4+。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126817A (en) * | 2018-11-07 | 2019-01-04 | 东北大学 | A kind of iron, tungsten, zinc improvement cerium oxide/manganese oxide SCR denitration and preparation method thereof |
| CN109589970A (en) * | 2018-12-22 | 2019-04-09 | 北京工业大学 | Aluminium manganese is total to the preparation method and application of pillared montmorillonite load Pr-Ce composite catalyst |
| CN112844441A (en) * | 2021-01-12 | 2021-05-28 | 上海大学 | Ion exchange type montmorillonite-based denitration catalyst resistant to alkali metal and heavy metal poisoning and preparation method thereof |
| CN112973667A (en) * | 2021-03-05 | 2021-06-18 | 河南康宁特环保科技股份有限公司 | Novel titanium dioxide doped modified layer columnar clay denitration catalyst and preparation method thereof |
| CN114797841A (en) * | 2022-03-24 | 2022-07-29 | 绍兴文理学院 | Mn (manganese) 4+ And Ce 3+ Preparation method of enhanced Mn-M-Ti-O ultralow-temperature denitration catalyst |
| CN115007125A (en) * | 2022-07-08 | 2022-09-06 | 湘潭大学 | Sepiolite-loaded manganese-cerium composite catalyst and preparation method and application thereof |
| CN115301230A (en) * | 2022-08-16 | 2022-11-08 | 中国科学院赣江创新研究院 | Manganese-based double-zone denitration catalyst and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126817A (en) * | 2018-11-07 | 2019-01-04 | 东北大学 | A kind of iron, tungsten, zinc improvement cerium oxide/manganese oxide SCR denitration and preparation method thereof |
| CN109589970A (en) * | 2018-12-22 | 2019-04-09 | 北京工业大学 | Aluminium manganese is total to the preparation method and application of pillared montmorillonite load Pr-Ce composite catalyst |
| CN109589970B (en) * | 2018-12-22 | 2021-10-15 | 北京工业大学 | Preparation method and application of aluminum-manganese co-pillared montmorillonite supported Pr-Ce composite catalyst |
| CN112844441A (en) * | 2021-01-12 | 2021-05-28 | 上海大学 | Ion exchange type montmorillonite-based denitration catalyst resistant to alkali metal and heavy metal poisoning and preparation method thereof |
| CN112973667A (en) * | 2021-03-05 | 2021-06-18 | 河南康宁特环保科技股份有限公司 | Novel titanium dioxide doped modified layer columnar clay denitration catalyst and preparation method thereof |
| CN114797841A (en) * | 2022-03-24 | 2022-07-29 | 绍兴文理学院 | Mn (manganese) 4+ And Ce 3+ Preparation method of enhanced Mn-M-Ti-O ultralow-temperature denitration catalyst |
| CN114797841B (en) * | 2022-03-24 | 2024-03-22 | 绍兴文理学院 | Mn (Mn) 4+ And Ce (Ce) 3+ Preparation method of enhanced Mn-M-Ti-O ultralow temperature denitration catalyst |
| CN115007125A (en) * | 2022-07-08 | 2022-09-06 | 湘潭大学 | Sepiolite-loaded manganese-cerium composite catalyst and preparation method and application thereof |
| CN115301230A (en) * | 2022-08-16 | 2022-11-08 | 中国科学院赣江创新研究院 | Manganese-based double-zone denitration catalyst and preparation method and application thereof |
| CN115301230B (en) * | 2022-08-16 | 2023-11-07 | 中国科学院赣江创新研究院 | Manganese-based double-zone denitration catalyst and preparation method and application thereof |
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