CN109201043A - A method of preparing mesoporous manganese titanium low-temperature denitration catalyst - Google Patents

A method of preparing mesoporous manganese titanium low-temperature denitration catalyst Download PDF

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Publication number
CN109201043A
CN109201043A CN201811350945.0A CN201811350945A CN109201043A CN 109201043 A CN109201043 A CN 109201043A CN 201811350945 A CN201811350945 A CN 201811350945A CN 109201043 A CN109201043 A CN 109201043A
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China
Prior art keywords
catalyst
denitration catalyst
temperature
temperature denitration
manganese titanium
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CN201811350945.0A
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Chinese (zh)
Inventor
陈建军
杨丽君
李俊华
刘海岩
王猛
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Yancheng Environmental Engineering Technology Research And Development Center Tsinghua University
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Yancheng Environmental Engineering Technology Research And Development Center Tsinghua University
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Priority to CN201811350945.0A priority Critical patent/CN109201043A/en
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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
    • 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
    • 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
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9409—Nitrogen oxides
    • B01D53/9413—Processes characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20707—Titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/2073—Manganese

Abstract

The present invention relates to a kind of methods for preparing mesoporous manganese titanium low-temperature denitration catalyst, comprising the following steps: measures acetic acid and is placed in container；Template F127, manganese acetate and butyl titanate are dissolved in the acetic acid, are sufficiently stirred to form colloidal sol；The colloidal sol of formation is transferred in culture dish and evaporation forms gel hyaline membrane under conditions of relative humidity 40%-80%；The gel hyaline membrane is transferred to aging in baking oven, to obtain meso-hole structure hybrid；The meso-hole structure hybrid is transferred to Muffle kiln roasting, the crystalline structure of cubic phase is formed, mesoporous Mn is madexTiO2Catalyst.The present invention effectively increases the denitration performance and anti-sulfur poisonous performance of catalyst, has widened the active temperature windows of catalyst, has good denitration efficiency, and in 125-350 DEG C of wide temperature range, the net conversion ratio of nitrogen oxides is up to 90% or more.

Description

A method of preparing mesoporous manganese titanium low-temperature denitration catalyst
Technical field
The present invention relates to a kind of catalyst more particularly to a kind of methods for preparing mesoporous manganese titanium low-temperature denitration catalyst.
Background technique
Nitrogen oxides is one of main atmosphere pollution, and causes the rings such as China various regions acid rain, haze, ozone layer destroying The big factors of border problem.Its emission control has become the research hotspot in environmental catalysis and Atmosphere control field.Ammonia selection Property catalysis reduction (Selective catalytic reduction, SCR) nitrogen oxides be most widely used at present The key of removal of nitrogen oxide technology, SCR technology is the catalyst of efficient stable.Currently, industrially using more mature NH3SCR catalyst is V2O5/TiO2Or in V2O5/TiO2On the basis of the catalyst that is modified, but V-W- used at present Ti catalyst series, required reaction temperature window narrows, temperature are higher, have preferable catalysis usually within the scope of 320-400 DEG C Performance, and the SO in flue gas2In the higher situation of dust concentration, different degrees of catalyst inactivation phenomenon can be generated significantly Shorten catalyst life；If to economizer, deduster and must just be taken off by the SCR process Installation on the boiler to have come into operation Sulphur device carries out biggish scrap build, greatly increases investment cost.If SCR is placed in order to extend the service life of catalyst After desulfation dust-extraction device, since flue-gas temperature is generally lower than 433 K after desulfurization and dedusting, it is necessary to carry out repeating to add to flue gas Heat, this will greatly increase denitration cost.Therefore, it develops low-temperature SCR catalyst and technique is very necessary.
Summary of the invention
The mesoporous manganese titanium that the purpose of the present invention is to provide a kind of with good removing NOx performance in low temperature range is urged Agent.The present invention passes through sol-gal process to achieve the goals above and is prepared for mesoporous MnxTiO2Catalyst, the catalyst have Good denitration efficiency, in 125-350 DEG C of wide temperature range, the net conversion ratio of nitrogen oxides is up to 90% or more.
The technical solution used in the present invention are as follows: a method of prepare mesoporous manganese titanium low-temperature denitration catalyst, including with Lower step
S01 measures acetic acid and is placed in container；
S02 is by template F127(molecular formula: EO106PO70EO106), manganese acetate and butyl titanate be dissolved in the acetic acid, It is sufficiently stirred to form colloidal sol；
The colloidal sol of formation is transferred in culture dish by S03 and to form gel saturating for evaporation under conditions of relative humidity 40%-80% Bright film；
The gel hyaline membrane is transferred to aging in baking oven by S04, to obtain meso-hole structure hybrid；
The meso-hole structure hybrid is transferred to Muffle kiln roasting by S05, forms the crystalline structure of cubic phase, is made mesoporous MnxTiO2Catalyst.
Further, the mesoporous MnxTiO20≤x≤1 in catalyst.
Further, the mesoporous MnxTiO2The molar ratio of Mn and Ti is 0.2 ~ 1 in catalyst.
Further, in the step S03 evaporating temperature be 20 DEG C -40 DEG C, be in order to allow acetic acid slow evaporation while Original structure of matter in colloidal sol will not be destroyed again and forms gel.
Further, aging temperature is 50 DEG C -70 DEG C in the step S04, is formed and is situated between to allow the slow aging of gel Pore structure hybrid.
Further, maturing temperature is 350-450 DEG C, calcining time 4-5h in the step S05, is to not break Under the premise of bad meso-hole structure, the lattice body with ordered mesopore structure is formed, enhances the interaction between manganese titanium, improves and lives Property.
Further, the amount of the acetic acid be 30-50ml, acetic acid is solvent, sufficiently dissolve template F127, manganese acetate and Butyl titanate.
Further, the molar ratio of the template F127 and manganese acetate and butyl titanate is 0.15-0.2:2-10: 10-20, template F127 are to increase the specific surface area of catalyst to form meso-hole structure, enhance the phase interaction between manganese titanium Best ratio when being to find out activity preferably with, the manganese acetate and butyl titanate that different proportion is added between manganese and titanium.
The utility model has the advantages that catalyst produced by the present invention can be used for coal-burning power plant, Industrial Boiler, building materials caused by of the invention The removing of the stationary sources such as stove and the mobile source emission nitrogen oxides of diesel vehicle.
F127 is a kind of surfactant of both sexes triblock polymer, be added in water it is a certain amount of after can form glue Beam is since the hydrophily of EO block is better than PO block, so forming micella in water using PO as kernel, EO is shell.It is added to After a greater amount of, micella can also further be assembled, and form the mesoporous molecular sieve of cubic phase.In the present invention, we give full play to mould The cubic phase processability of plate agent F127 prepares the cubic-phase mesoporous manganese titanium catalyst with large specific surface area and aperture, Biggish specific surface area and aperture can expose more active sites, form more B acid position and L acid position, absorption and activation More amino and nitro species realize nitrogen oxides to make it have better low temperature active in temperature range Efficient catalytic removing.
Pass through sol-gal process and be added to the synthetic method of template F127, MnOx can be promoted to be well dispersed in two On titanium oxide, and the specific surface area of catalyst is increased, titanium dioxide is mainly to be conducive to the Detitanium-ore-type two of denitration reaction The form of titanium oxide exists；Meanwhile the addition of template F127, the manganese titanium catalyst with cube phase structure is formd, is promoted Transmitting of the electronics between active component, catalyst surface oxygen content improve, promote the absorption and activation of reactant molecule, have Effect improves the denitration performance and anti-sulfur poisonous performance of catalyst, has widened the active temperature windows of catalyst, has good Denitration efficiency, in 125-350 DEG C of wide temperature range, the net conversion ratio of nitrogen oxides is up to 90% or more.
Detailed description of the invention
Fig. 1 activity rating temperature range is 50-350 DEG C, different temperatures, under different manganese titanium ratios, the reduction of manganese titanium catalyst The conversion ratio of NOx.
Specific embodiment
Further details of explanation is done to the present invention combined with specific embodiments below, it should be appreciated that of the invention Protection scope is not limited by the specific implementation.
Embodiment 1
Mesoporous Mn0.2TiO2The preparation of composite oxide catalysts
A) 30mL acetic acid is measured in beaker, is continuously stirred.
B) 0.2mmol template F127,4mmol manganese acetate and 20mmol butyl titanate is taken to be dissolved in (a).It is vigorously stirred 1h forms colloidal sol.
C) (b) is transferred in the Petri dish that diameter is 125mm.
D) (c) is evaporated under conditions of 20 DEG C of temperature, relative humidity 40%-80% 12h, forms hyaline membrane, then by its turn It moves on to aging in 50 DEG C of baking oven and for 24 hours, obtains meso-hole structure hybrid.
E) by (d) in Muffle furnace, 4h is roasted at 350 DEG C.Mesoporous Mn is made0.2TiO2Catalyst.
Embodiment 2
Mesoporous Mn0.4TiO2The preparation of composite oxide catalysts
A) 50mL acetic acid is measured in beaker, is continuously stirred.
B) 0.2mmol template F127,8mmol manganese acetate and 20mmol butyl titanate is taken to be dissolved in (a).It is vigorously stirred 1h forms colloidal sol.
C) (b) is transferred in the Petri dish that diameter is 125mm.
D) (c) is evaporated under conditions of 30 DEG C of temperature, relative humidity 40%-80% 12h, forms hyaline membrane, then by its turn It moves on to aging in 60 DEG C of baking oven and for 24 hours, obtains meso-hole structure hybrid.
E) by (d) in Muffle furnace, 4h is roasted at 400 DEG C.Mesoporous Mn is made0.4TiO2Catalyst.
Embodiment 3
Mesoporous Mn0.6TiO2The preparation of composite oxide catalysts
A) 40mL acetic acid is measured in beaker, is continuously stirred.
B) 0.15mmol template F127,6mmol manganese acetate and 10mmol butyl titanate is taken to be dissolved in (a).Acutely stir 1h is mixed, colloidal sol is formed.
C) (b) is transferred in the Petri dish that diameter is 125mm.
D) (c) is evaporated under conditions of 40 DEG C of temperature, relative humidity 40%-80% 12h, forms hyaline membrane, then by its turn It moves on to aging in 65 DEG C of baking oven and for 24 hours, obtains meso-hole structure hybrid.
E) by (d) in Muffle furnace, 5h is roasted at 350 DEG C.Mesoporous Mn is made0.6TiO2Catalyst.
Embodiment 4
Mesoporous Mn0.8TiO2The preparation of composite oxide catalysts
A) 50mL acetic acid is measured in beaker, is continuously stirred.
B) 0.15mmol template F127,8mmol manganese acetate and 10mmol butyl titanate is taken to be dissolved in (a).Acutely stir 1h is mixed, colloidal sol is formed.
C) (b) is transferred in the Petri dish that diameter is 125mm.
D) (c) is evaporated under conditions of 40 DEG C of temperature, relative humidity 40%-80% 12h, forms hyaline membrane, then by its turn It moves on to aging in 70 DEG C of baking oven and for 24 hours, obtains meso-hole structure hybrid.
E) by (d) in Muffle furnace, 5h is roasted at 450 DEG C.Mesoporous Mn is made0.8TiO2Catalyst.
Embodiment 5
Preparing for catalyst is same as Example 2, and 0.12g catalyst is taken to be placed in the fixed bed reactors continuously flowed, reaction Gas group becomes 0 .05%NO, 0 .05%NH3, 5%O2, Balance Air is done with nitrogen, the flow velocity of reaction gas is 300mL/min, and air speed is 127,000h-1.Activity rating temperature range is 50-350 DEG C, under different temperatures, the manganese titanium catalyst reduction NOx's of different proportion Conversion ratio is as shown in Figure 1.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (8)

1. a kind of method for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: include the following steps
S01 measures acetic acid and is placed in container；
Template F127, manganese acetate and butyl titanate are dissolved in the acetic acid by S02, are sufficiently stirred to form colloidal sol；
The colloidal sol of formation is transferred in culture dish by S03 and to form gel saturating for evaporation under conditions of relative humidity 40%-80% Bright film；
The gel hyaline membrane is transferred to aging in baking oven by S04, to obtain meso-hole structure hybrid；
The meso-hole structure hybrid is transferred to Muffle kiln roasting by S05, forms the crystalline structure of cubic phase, is made mesoporous MnxTiO2Catalyst.
2. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: described mesoporous MnxTiO20≤x≤1 in catalyst.
3. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: described mesoporous MnxTiO2The molar ratio of Mn and Ti is 0.2 ~ 1 in catalyst.
4. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: the step Evaporating temperature is 20-40 DEG C in S03.
5. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: the step Aging temperature is 50-70 DEG C in S04.
6. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: the step Maturing temperature is 350-450 DEG C in S05, calcining time 4-5h.
7. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: the acetic acid Amount be 30-50ml.
8. the method according to claim 1 for preparing mesoporous manganese titanium low-temperature denitration catalyst, it is characterised in that: the template The molar ratio of agent F127 and manganese acetate and butyl titanate is 0.15-0.2:2-10:10-20.
CN201811350945.0A 2018-11-14 2018-11-14 A method of preparing mesoporous manganese titanium low-temperature denitration catalyst Pending CN109201043A (en)

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