CN114452983B - Perovskite and spinel composite type ozone decomposition catalyst - Google Patents

Perovskite and spinel composite type ozone decomposition catalyst Download PDF

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CN114452983B
CN114452983B CN202111366738.6A CN202111366738A CN114452983B CN 114452983 B CN114452983 B CN 114452983B CN 202111366738 A CN202111366738 A CN 202111366738A CN 114452983 B CN114452983 B CN 114452983B
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左同梅
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Hangzhou Tongchen Environmental Protection Technology Co ltd
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    • 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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    • 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
    • B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
    • B01D53/8675—Ozone
    • 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
    • B01J23/005—Spinels
    • 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
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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Abstract

The invention provides a perovskite and spinel composite type ozone decomposition catalyst and a preparation method thereof, wherein a composite structure is formed by taking honeycomb cordierite as a supporting structure, taking perovskite type TiNbO 5 as an adhesive layer and a dispersing agent and taking spinel type Mn 0.8Cu0.2Fe2O4 as an active component. Unlike the conventional titanium, silicon and aluminum sol, the TiNbO 5 two-dimensional nano flake colloid with a perovskite structure is used as a particle adhesive and a dispersing agent, has small high-temperature calcination shrinkage, and has a certain ozonolysis effect; unlike the conventional Cu, mn, fe and other composite oxides, the spinel Mn 0.8Cu0.2Fe2O4 has stable structure and is not easy to aggregate during heat treatment.

Description

Perovskite and spinel composite type ozone decomposition catalyst
Technical Field
The invention relates to the field of air purification, in particular to a novel perovskite-like and spinel composite type room-temperature ozone decomposition catalyst and a preparation method thereof.
Background
Ozone has extremely strong oxidizing power and is widely used in fields such as deodorization, air sterilization, aromatic hydrocarbon organic matter degradation, disinfection of medical equipment, advanced water treatment technology and the like. However, the ozone concentration is 0.1 to 1ppm, so that symptoms of dizziness, eye discomfort and sore throat can be caused, the limit concentration of acceptable ozone in 1 hour is 0.26ppmv, the ozone can cause cough, dyspnea and lung function reduction after long-term exposure to ozone environment, and the probability of emphysema can be greatly improved, so that the maximum allowable concentration in the working environment of 8 hours is less than 0.016ppm according to the ozone safety standard formulated by the world health organization; ozone can also inhibit plant growth, so that plant leaves turn yellow and even wither, and great loss is brought to agricultural production; ozone is also a greenhouse gas and photochemical contaminant, and ozone emitted into the air can cause environmental pollution. Therefore, how to eliminate ozone pollution becomes a hot spot and an important point of research.
For ozonolysis, research by researchers mainly adopts activated carbon or oxide molecular sieve to load metal oxide for treatment, wherein the oxide is mainly manganese oxide, ferric oxide, cobalt oxide, copper oxide, nickel oxide, cerium oxide and the like, such as patent CN102513106A, CN101402047A, CN101757933A and the like. Such catalysts typically support a variety of oxides on a support and during calcination and subsequent use, aggregation and migration of the active components occurs. Therefore, it is required to study a multi-metal composite oxide having a stable crystal form structure and special physicochemical properties, which are not easily aggregated, such as a perovskite structure (ABO 3) and a spinel structure (AB 2O4), and the like, as the first choice.
In recent years, patent CN 107376926A reports pure phase or transition metal doped perovskite type lanthanum ferrite (LaM xFe(1-x)O3, x is more than or equal to 0 and less than or equal to 0.2, M is transition metal), porous ceramic is directly immersed in aqueous solution of lanthanum ferrite, and the prepared and molded catalyst can be used for decomposing ozone at room temperature, but the specific surface area of the ceramic carrier is not large, and the perovskite type direct immersion has inherent defects of small load, easy falling and the like; patent CN200680015614.0 reports a mixed catalyst composed of an iron-containing compound (at least one of Fe 2O3、FeO(OH)、Fe(OH)3) and a pure spinel-structured ferrite compound (at least one of MnFe 2O4、ZnFe2O4、NiFe2O4、CuFe2O4), the state of which is controlled by temperature, and the pure spinel-structured ferrite compound is formed by coprecipitation, but the blending type [ a 1-xMx]B2O4 cannot be realized in its coprecipitation preparation method.
In view of the above, the present invention aims to load a catalyst with perovskite and spinel structures on honeycomb ceramics by adopting a proper adhesive and a dispersant, namely, to prepare an ozonolysis catalyst by adopting layered potassium titanate (KTiNbO 5) with perovskite structures and Mn 0.8Cu0.2Fe2O4 with doped spinel A 1- xMxB2O4 structures, wherein nano-sheets formed by the layered titanic niobate are mainly used as an adhesive and a dispersant of spinel active components, and simultaneously have a certain ozonolysis function, so that the forming of the ozonolysis catalyst and the synergistic effect of decomposing ozone by the perovskite and the spinel are realized.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a perovskite and spinel composite type ozonolysis catalyst.
The perovskite and spinel composite type ozone decomposition catalyst is characterized by comprising the following components: a honeycomb cordierite support structure, a perovskite TiNbO 5 and spinel type Mn 0.8Cu0.2Fe2O4 composite structure; the honeycomb cordierite supporting structure is a honeycomb carrier with a certain mesh number and a certain length, the perovskite TiNbO 5 structure is a two-dimensional nano sheet formed by acidizing and delamination of a layered KTiNbO 5, and the spinel Mn 0.8Cu0.2Fe2O4 structure is composite oxide powder formed by manganese, iron and copper at a high temperature.
A preparation method of a perovskite and spinel composite type ozone decomposition catalyst, which comprises the following steps:
Step 1, dispersing K 2CO3、TiO2、Nb2O5 in ethanol and aqueous solution according to the mass ratio of 1:2:1, slowly evaporating water and ethanol under stirring, and calcining the obtained solid at 1100 ℃ for 24 hours to obtain KTiNbO 5; dispersing 1gKTiNbO 5 into 100ml of 2mol/L nitric acid aqueous solution, stirring at room temperature for 7 days, and filtering, washing and drying to obtain HTiNbO 5; dispersing 1g of HTiNbO 5 into 100ml of deionized water, adding a tetrabutylammonium hydroxide solution with the mass fraction of 25%, adjusting to a certain pH value, stirring for a period of time at room temperature, and centrifuging at a certain rotating speed to obtain an upper colloidal liquid to obtain perovskite type TiNbO 5 nano lamellar sol;
and 2, adding manganese acetate, copper nitrate and ferric nitrate into a 2mol/L citric acid aqueous solution according to the metal ion ratio of 4:1:10, fully stirring, evaporating at a certain temperature, and calcining at a high temperature for a certain time to obtain spinel type Mn 0.8Cu0.2Fe2O4 powder.
And step 3, taking a cordierite carrier with a certain mesh number and a certain length, adding the cordierite carrier into a dilute nitric acid solution with a certain concentration, heating and boiling for a certain time, washing with water, and drying at a certain temperature to obtain the cordierite with the pretreated surface.
And 4, adding a certain amount of spinel Mn 0.8Cu0.2Fe2O4 powder into the perovskite TiNbO 5 sheet-like nano sol, adding a certain amount of pore-expanding agent, auxiliary dispersing agent and defoaming agent, and performing secondary slurry mixing to finally prepare the coating slurry with a certain pH value and particle size. And coating the slurry on the cordierite subjected to surface pretreatment by using a coating machine, and drying and calcining at a certain temperature to obtain the perovskite and spinel composite type ozonolysis catalyst.
Preferably, the pH value is 10 after tetrabutylammonium hydroxide is added in the step 1, the stirring time is 3 days, and the centrifugal speed is 10000rpm.
Preferably, the evaporating temperature in the step 2 is 70 ℃, the calcining temperature is 800 ℃ and the calcining time is 3 hours.
Preferably, the cordierite mesh number in the step 3 is 200 mesh, the length is 150mm, the dilute nitric acid concentration is 0.5mol/L, the boiling time is 0.5h, and the drying temperature is 105 ℃.
Preferably, the pore-expanding agent in the step 4 is polyethylene glycol with a molecular weight of 4000, and Mn 0.8Cu0.2Fe2O4 powder: perovskite type TiNbO 5 flake nano sol: hole expanding agent: and (3) auxiliary dispersing agent: defoamer = 30g:100ml:5g:2.5g:0.1g, the pH value of the slurry after secondary slurry mixing is 8-9, the particle size is less than or equal to 5 mu m, the drying temperature of the coated honeycomb catalyst is 105 ℃, the calcining temperature is 450 ℃, and the calcining time is 3h.
The invention has the beneficial effects that: firstly, unlike the conventional TiO 2、SiO2、Al2O3 sol, the perovskite structure KTiNbO 5 is easy to form stable colloid solution containing two-dimensional nano lamellar structures under mild conditions, and the lamellar colloid structure is used as a particle adhesive and a dispersing agent, has small high-temperature calcination shrinkage and has certain catalytic activity; secondly, the active components of the conventional composite catalyst among oxides of Cu, mn, fe and the like are easy to migrate and aggregate, and the oxides of Cu, mn and Fe in Mn 0.8Cu0.2Fe2O4 forming a spinel stable structure exist as a whole and are not easy to aggregate during heat treatment. The invention realizes the forming of the ozonolysis catalyst and the synergistic effect of decomposing ozone by perovskite and spinel.
Drawings
FIG. 1A process for preparing a perovskite and spinel composite ozonolysis catalyst. In the figure, 1 is a layered perovskite KTiNbO 5, 2 is a two-dimensional nano lamellar structure formed by delamination of KTiNbO 5 under mild conditions, 3 is Mn, cu and Fe ions, 4 is spinel Mn 0.8Cu0.2Fe2O4 formed by Cu, mn and Fe at high temperature, 5 is a cordierite support carrier, 6 is a cordierite support carrier surface subjected to dilute acid treatment, and 7 is a cordierite, perovskite and spinel composite ozonolysis catalyst.
XRD pattern of FIG. 2KTiNbO 5
FIG. 3KTiNbO 5 SEM of two-dimensional nanoplatelets formed by acidizing delamination
FIG. 4 XRD pattern of Mn 0.8Cu0.2Fe2O4
Detailed Description
The invention is further described below with reference to examples. The following examples are presented only to aid in the understanding of the invention. It should be noted that it will be apparent to those skilled in the art that modifications can be made to the present invention without departing from the principles of the invention, and such modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The perovskite and spinel composite type ozone decomposition catalyst comprises a honeycomb cordierite supporting structure, a perovskite type TiNbO 5 and spinel type Mn 0.8Cu0.2Fe2O4 composite structure; the honeycomb cordierite support structure is a honeycomb carrier with a certain mesh number and a certain length, the perovskite TiNbO 5 structure is a two-dimensional nano sheet formed by acidizing and delamination of a layered KTiNbO 5, and the spinel Mn 0.8Cu0.2Fe2O4 structure is composite oxide powder formed by manganese, iron and copper at high temperature; besides certain activity, the perovskite TiNbO 5 mainly plays roles in gluing and dispersing main active components, and spinel Mn 0.8Cu0.2Fe2O4 is the main active component.
The preparation method comprises the following steps: the perovskite TiNbO 5 nano-sheet sol with certain activity is used as an adhesive and a dispersing agent, a pore-enlarging agent, a dispersing aid and a defoaming agent with a certain proportion are added, spinel Mn 0.8Cu0.2Fe2O4 serving as a main active component is fully dispersed, and then the mixture is coated on pretreated honeycomb cordierite.
Example 1:
Weighing 13.821g K 2CO3、16.000g TiO2、26.581g Nb2O5, adding into 200ml of water and ethanol solution, slowly evaporating the water and the ethanol under stirring, transferring the obtained solid into a crucible, and calcining at 1100 ℃ for 24 hours to obtain KTiNbO 5; KTiNbO 5 is dispersed into 2mol/L nitric acid aqueous solution (solid-liquid ratio 1g:100 ml), stirred for 7 days at room temperature, filtered, washed and dried to obtain HTiNbO 5; dispersing HTiNbO 5 into deionized water (solid-to-liquid ratio 1g:100 ml), dropwise adding tetrabutylammonium hydroxide solution with mass fraction of 25% to pH value of about 10, continuously stirring for 3 days, centrifuging at 10000rpm, and taking upper-layer cementing liquid to obtain perovskite type TiNbO 5 nanometer flake sol.
Manganese acetate, copper nitrate and ferric nitrate are weighed according to the metal ion ratio of 4:1:10, added into a slightly excessive 2mol/L citric acid aqueous solution, fully stirred, evaporated to dryness at 70 ℃, and calcined at 800 ℃ for 3 hours, so as to obtain spinel Mn 0.8Cu0.2Fe2O4 powder.
Cordierite with the mesh number of 200 meshes and the size of 150mm is added into a 0.5mol/L dilute nitric acid solution, boiling time is 0.5h, cooling, washing with water and drying to constant weight at 105 ℃.
The total slurry amount required for one whole coating is 3000ml, according to Mn 0.8Cu0.2Fe2O4 powder: perovskite type TiNbO 5 flake nano sol: hole expanding agent: and (3) auxiliary dispersing agent: defoamer = 30g:100ml:5g:2.5g: the coating slurry is prepared according to the proportion of 0.1g, wherein the pore-expanding agent is polyethylene glycol with the molecular weight of 4000, the dispersing aid agent is peregal, and the defoaming agent is high molecular modified alcohol. Coarse adjustment is carried out by adopting coarse zirconium beads, secondary fine adjustment is carried out by adopting fine zirconium beads, and the pH value of the slurry is=9, and the particle size is less than or equal to 5 mu m.
Coating the slurry on the cordierite subjected to surface pretreatment by using a coating machine, wherein the drying temperature of the coated honeycomb catalyst is 105 ℃, the calcining temperature is 450 ℃, and the calcining time is 3 hours, so as to obtain the perovskite and spinel composite ozonolysis catalyst.
Example 2:
the solid content of the perovskite type TiNbO 5 nanometer flake sol is changed by adjusting the pH value, increasing the stirring time and reducing the centrifugal rate. KTiNbO 5、HTiNbO5 preparation was carried out as in example 1; dispersing HTiNbO 5 into deionized water (solid-to-liquid ratio 1g:100 ml), dropwise adding tetrabutylammonium hydroxide solution with mass fraction of 25% to pH value of about 12, continuously stirring for 7 days, centrifuging at 9000rpm, and taking the upper layer cementing liquid to obtain perovskite type TiNbO 5 nanometer flake sol.
Spinel type Mn 0.8Cu0.2Fe2O4 powder and cordierite pretreatment were the same as in example 1.
The addition amount of spinel is changed, and the loading amount is improved. According to Mn 0.8Cu0.2Fe2O4 powder: perovskite type TiNbO 5 flake nano sol: hole expanding agent: and (3) auxiliary dispersing agent: defoamer = 40g:100ml:5g:2.5g: the coating slurry was prepared at a ratio of 0.1 g. Coarse adjustment is carried out by adopting coarse zirconium beads, secondary fine adjustment is carried out by adopting fine zirconium beads, and the pH value of the slurry is=9, and the particle size is less than or equal to 5 mu m. The slurry was coated on the surface-pretreated cordierite with a coater at a drying temperature of 105 c, a calcination temperature of 450 c and a calcination time of 3 hours.
Example 3:
The solid content of the perovskite type TiNbO 5 nanometer flake sol is changed by regulating the pH value, reducing the stirring time and improving the centrifugal rate. KTiNbO 5、HTiNbO5 preparation was carried out as in example 1; dispersing HTiNbO 5 into deionized water (solid-to-liquid ratio 1g:100 ml), dropwise adding tetrabutylammonium hydroxide solution with mass fraction of 25% to pH value of about 9, continuously stirring for 1 day, centrifuging at 12000rpm, and taking the upper layer cementing liquid to obtain perovskite type TiNbO 5 nanometer flake sol.
Spinel type Mn 0.8Cu0.2Fe2O4 powder and cordierite pretreatment were the same as in example 1.
The addition amount of spinel is reduced, and the loading amount is reduced. According to Mn 0.8Cu0.2Fe2O4 powder: perovskite type TiNbO 5 flake nano sol: hole expanding agent: and (3) auxiliary dispersing agent: defoamer = 10g:100ml:5g:2.5g: the coating slurry was prepared at a ratio of 0.1 g. Coarse adjustment is carried out by adopting coarse zirconium beads, secondary fine adjustment is carried out by adopting fine zirconium beads, and the pH value of the slurry is=9, and the particle size is less than or equal to 5 mu m. The slurry was coated on the surface-pretreated cordierite with a coater at a drying temperature of 105 c, a calcination temperature of 450 c and a calcination time of 3 hours.

Claims (4)

1. A method for preparing a perovskite and spinel composite type ozone decomposition catalyst, which is characterized by comprising the following steps:
Step 1, dispersing K 2CO3、TiO2、Nb2O5 in ethanol and aqueous solution according to the mass ratio of 1:2:1, slowly evaporating water and ethanol under stirring, and calcining the obtained solid at 1100 ℃ for 24 hours to obtain KTiNbO 5; dispersing 1gKTiNbO 5 into 100ml of 2mol/L nitric acid aqueous solution, stirring at room temperature for 7 days, and filtering, washing and drying to obtain HTiNbO 5; dispersing 1g of HTiNbO 5 into 100ml of deionized water, adding a tetrabutylammonium hydroxide solution with the mass fraction of 25%, adjusting to a certain pH value, stirring for a period of time at room temperature, and centrifuging at a certain rotating speed to obtain an upper colloidal liquid to obtain perovskite type TiNbO 5 nano lamellar sol;
Step 2, adding manganese acetate, copper nitrate and ferric nitrate into a 2mol/L citric acid aqueous solution according to the metal ion ratio of 4:1:10, fully stirring, evaporating at a certain temperature, and calcining at a high temperature for a certain time to obtain spinel type Mn 0.8Cu0.2Fe2O4 powder;
Step 3, taking a cordierite carrier with a certain mesh number and a certain length, adding the cordierite carrier into a dilute nitric acid solution with a certain concentration, heating and boiling for a certain time, washing with water, and drying at a certain temperature to obtain the honeycomb cordierite with the pretreated surface;
Step 4, adding a certain amount of spinel Mn 0.8Cu0.2Fe2O4 powder into perovskite TiNbO 5 nano flaky sol, adding a certain amount of pore-enlarging agent, auxiliary dispersing agent and defoaming agent, carrying out secondary slurry mixing, finally preparing coating slurry with a certain pH value and particle size, coating the slurry on the surface-pretreated honeycomb cordierite by using a coating machine, and drying and calcining at a certain temperature to obtain the perovskite and spinel composite ozonolysis catalyst; wherein the pore-expanding agent is polyethylene glycol with the molecular weight of 4000-6000, the dispersing aid agent is peregal, and the defoaming agent is high-molecular modified alcohol; spinel type Mn 0.8Cu0.2Fe2O4 powder: perovskite type TiNbO 5 nanometer lamellar sol: hole expanding agent: and (3) auxiliary dispersing agent: defoamer= (10-40 g): 100ml:5g:2.5g:0.1g, coarse adjustment is carried out by adopting coarse zirconium beads, secondary fine adjustment is carried out by adopting fine zirconium beads, thus obtaining slurry with pH=7-9, particle size less than or equal to 5 mu m, drying temperature of the coated honeycomb catalyst is 105-120 ℃, and calcining temperature is 400-500 ℃.
2. The method for preparing the perovskite and spinel composite ozonolysis catalyst according to claim 1, characterized in that: in the step 1, solid-phase grinding is not adopted, ethanol and water are adopted for dispersion and then evaporated to dryness, so that K 2CO3、TiO2、Nb2O5 is fully mixed, and the subsequent calcination is facilitated; the pH value range is 9-12 after tetrabutylammonium hydroxide is added, the stirring time is 1-7 days, and the centrifugal rotating speed is 9000-12000rpm.
3. The method for preparing the perovskite and spinel composite ozonolysis catalyst according to claim 1, characterized in that: in the step 2, the evaporating temperature is 60-95 ℃, the calcining temperature is 600-900 ℃ and the calcining time is 2-6h.
4. The method for preparing the perovskite and spinel composite ozonolysis catalyst according to claim 1, characterized in that: in the step 3, the mesh number of the honeycomb cordierite is 50-200 meshes, the length is 50-350mm, the concentration of dilute nitric acid is 0.1-1mol/L, the boiling time is 0.5-1h, and the drying temperature is 100-120 ℃.
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