CN109317145B - Manganese oxide noble metal composite catalyst, preparation method and application thereof - Google Patents

Manganese oxide noble metal composite catalyst, preparation method and application thereof Download PDF

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CN109317145B
CN109317145B CN201811346739.2A CN201811346739A CN109317145B CN 109317145 B CN109317145 B CN 109317145B CN 201811346739 A CN201811346739 A CN 201811346739A CN 109317145 B CN109317145 B CN 109317145B
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manganese oxide
noble metal
metal composite
palladium
composite catalyst
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CN109317145A (en
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李永峰
刘芳芳
许泽华
程高
周俊丽
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Guangdong University of Technology
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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
    • 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
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/656—Manganese, technetium or rhenium
    • B01J23/6562—Manganese
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00—Specific waste
    • F23G2209/14—Gaseous waste or fumes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • 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

Abstract

The invention belongs to the field of air purification, and relates to a manganese oxide and precious metal composite catalyst, a preparation method and application thereof. The invention provides a preparation method of a manganese oxide noble metal composite catalyst, which comprises the following steps: step 1: soaking a noble metal catalyst carrier in a stannous chloride solution, and then soaking in a palladium chloride solution; step 2: putting the noble metal catalyst carrier obtained in the step 1 into a manganese oxide precursor solution for hydrothermal reaction; and step 3: putting the noble metal catalyst carrier after the hydrothermal reaction into a palladium precursor solution, heating in a water bath, and drying; the manganese oxide precursor solution comprises potassium permanganate; the palladium precursor solution comprises a palladium chloride solution. The invention also provides a manganese oxide noble metal composite catalyst and application thereof, and solves the technical problem that the prior art can not effectively reduce the use amount of noble metals and simultaneously keep the excellent low-temperature purification activity of VOCs (volatile organic compounds) of the catalyst.

Description

Manganese oxide noble metal composite catalyst, preparation method and application thereof
Technical Field
The invention belongs to the field of air purification, and relates to a manganese oxide and precious metal composite catalyst, a preparation method and application thereof.
Background
Among the methods for effectively treating Volatile Organic Compounds (VOCs), catalytic oxidation combustion has attracted much attention, which has advantages of wide VOCs treatment types, high purification rate, high treatment efficiency, and the like, and the final product is CO2And water, so that secondary pollution can not be caused. The core of the method is a catalyst, wherein the honeycomb monolithic combustion catalyst is most widely applied at present due to the characteristics of pressure reduction, large treatment capacity, high mechanical and thermal stability and the like. The monolithic catalyst is mainly divided into a noble metal monolithic catalyst and a non-noble metal monolithic catalyst according to different types of active components. Noble metal monolithic catalysts have the advantages of low light-off temperature and high efficiency of low-temperature catalytic oxidation, but are expensive, how to keep the catalysisThe reduction of the consumption of noble metals on the basis of chemical activity is always the focus of research on the catalysts. The non-noble metal monolithic catalyst has the advantages of low price and good thermodynamic property, and particularly, the manganese oxide catalyst has excellent oxygen absorption and oxygen supply characteristics because a large number of variable valence state manganese ions are arranged in the crystal lattice of the manganese oxide catalyst. However, the low-temperature catalytic oxidation activity of the non-noble metal monolithic catalyst is poor, and the popularization and application of the non-noble metal monolithic catalyst in the field of VOCs purification are limited. Therefore, the inability of the prior art to effectively reduce the amount of noble metals while maintaining the superior low-temperature purification activity of VOCs in catalysts has become an urgent technical problem to be solved by those skilled in the art.
Disclosure of Invention
The invention provides a manganese oxide noble metal composite catalyst, a preparation method and application thereof, and solves the technical problem that the prior art can not effectively reduce the use amount of noble metals and simultaneously keep the excellent low-temperature purification activity of VOCs (volatile organic compounds) of the catalyst.
The invention provides a preparation method of a manganese oxide noble metal composite catalyst, which comprises the following steps:
step 1: firstly, dipping a catalyst carrier in a stannous chloride solution, and then dipping in a palladium chloride solution;
step 2: putting the catalyst carrier obtained in the step 1 into a manganese oxide precursor solution for hydrothermal reaction;
and step 3: putting the catalyst carrier after the hydrothermal reaction into a palladium precursor solution, heating in a water bath, and drying;
the manganese oxide precursor solution comprises potassium permanganate;
the palladium precursor solution comprises a palladium chloride solution.
The solvents of the manganese oxide precursor solution and the palladium precursor solution are both water.
Preferably, the catalyst carrier is honeycomb ceramic or honeycomb activated carbon.
Preferably, the concentration of the stannous chloride solution is 8-12 g/L.
More preferably, the time for immersion in the stannous chloride solution is 5-15 min.
Preferably, the concentration of the palladium chloride solution in the step 1 is 0.02-0.05 g/L.
More preferably, the time for immersion in the palladium chloride solution in step 1 is 5-15 min.
Preferably, the temperature of the hydrothermal reaction in step 2 is 90-120 ℃.
More preferably, the hydrothermal reaction time in step 2 is 12-24 h.
More preferably, the temperature of the water bath heating in step 3 is 50-80 ℃.
More preferably, the heating time of the water bath in the step 3 is 2-4 h.
Preferably, the concentration of the potassium permanganate solution is 0.05-0.15 mol/L.
More preferably, the manganese oxide precursor solution further includes acetic acid.
More preferably, the concentration of the acetic acid solution is 0-0.3 mol/L.
Preferably, the concentration of the palladium chloride solution in the step 3 is 0.02-0.04 g/L.
More preferably, the palladium precursor solution further comprises sodium hypophosphite, ammonium chloride and ammonia water.
More preferably, the concentration of the sodium hypophosphite solution is 5.0g/L, and the concentration of the ammonium chloride solution is 13.5 g/L.
The invention also provides a manganese oxide and precious metal composite catalyst, which is prepared by the preparation method of the manganese oxide and precious metal composite catalyst.
The invention also provides application of the manganese oxide noble metal composite catalyst as a purifying agent of volatile organic pollutants.
The catalyst prepared by the preparation method of the manganese oxide noble metal composite catalyst provided by the invention can ensure that two active components of noble metal palladium and manganese oxide are uniformly distributed on the surface of a honeycomb structured carrier in a staggered manner, and the catalyst shows excellent VOCs low-temperature catalytic combustion purification performance under the condition of very low palladium content (0.06-0.10 wt.%) in the catalyst by utilizing the synergistic catalytic action of the two components: the ignition is carried out at the temperature of 160 ℃ and 226 ℃ and the complete purification is achieved at the temperature of 236 ℃ and 270 ℃. The preparation method provided by the invention is simple to operate, and the obtained catalyst product is low in price and high in catalytic purification activity, and has good market application value and popularization prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a chart of surface elemental analysis (EDS) of a catalyst sample obtained in example 1 of the present invention;
FIG. 2 is an SEM surface topography of a catalyst sample obtained in example 1 of the present invention;
FIG. 3 is an EDS surface elemental analysis chart of a catalyst sample obtained in example 4 of the present invention;
FIG. 4 is an SEM surface topography of a catalyst sample obtained in example 4 of the present invention.
Detailed Description
The embodiment of the invention provides a manganese oxide noble metal composite catalyst, a preparation method and application thereof, and solves the technical problem that the prior art can not effectively reduce the use amount of noble metals and simultaneously keep the excellent low-temperature purification activity of VOCs (volatile organic compounds) of the catalyst.
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the embodiments described below are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To further illustrate the invention, the following examples are set forth without limiting the scope of the invention.
Example 1
Soaking 0.37g of 5 × 5 × 24mm honeycomb ceramic regular substrate in 10g/L stannous chloride solution at room temperature for 10min, then soaking in 0.03g/L palladium chloride solution at room temperature for 10min, and then taking out and washing with water; putting the pretreated regular substrate into a manganese oxide precursor solution (prepared by 0.10mol/L potassium permanganate, 0.1mol/L acetic acid and water), transferring the regular substrate and the solution into a hydrothermal reaction kettle, and continuously reacting for 20 hours at 100 ℃; and (2) putting the regular substrate after the hydrothermal reaction into a palladium precursor solution (prepared from 0.02g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100 mL/L25% ammonia water and water), continuously reacting for 3 hours at the water bath temperature of 60 ℃, finally taking out, washing with water, and drying at 120 ℃ to constant weight.
Example 2
Soaking 0.37g of honeycomb ceramic regular substrate with the size of 5 multiplied by 24mm in stannous chloride solution of 8g/L at room temperature for 15min, then soaking in palladium chloride solution of 0.02/L at room temperature for 15min, and then taking out and washing with water; putting the pretreated regular substrate into a manganese oxide precursor solution (prepared by 0.05mol/L potassium permanganate and water), transferring the manganese oxide precursor solution and the potassium permanganate solution into a hydrothermal reaction kettle together, and continuously reacting for 24 hours at 90 ℃; and (2) putting the regular substrate after the hydrothermal reaction into a palladium precursor solution (prepared from 0.04g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100 mL/L25% ammonia water and water), continuously reacting for 2 hours at the water bath temperature of 80 ℃, finally taking out, washing with water, and drying at 120 ℃ to constant weight.
Example 3
Soaking 0.37g of honeycomb ceramic regular substrate with the size of 5 multiplied by 24mm in 12g/L stannous chloride solution at room temperature for 5min, then soaking in 0.05/L palladium chloride solution at room temperature for 5min, and then taking out and washing with water; putting the pretreated regular substrate into a manganese oxide precursor solution (prepared by 0.15mol/L potassium permanganate, 0.3mol/L acetic acid and water), transferring the solution into a hydrothermal reaction kettle together, and continuously reacting for 12 hours at 120 ℃; and (2) putting the regular substrate after the hydrothermal reaction into a palladium precursor solution (prepared from 0.03g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100 mL/L25% ammonia water and water), continuously reacting for 4 hours at the water bath temperature of 50 ℃, finally taking out, washing with water, and drying at 120 ℃ to constant weight.
Example 4
Soaking 0.42g of honeycomb activated carbon regular substrate with the size of 5 multiplied by 24mm in 10g/L stannous chloride solution at room temperature for 10min, then soaking in 0.03/L palladium chloride solution at room temperature for 10min, and then taking out and washing with water; putting the pretreated regular substrate into a manganese oxide precursor solution (prepared by 0.1mol/L potassium permanganate, 0.1mol/L acetic acid and water), transferring the regular substrate and the solution into a hydrothermal reaction kettle, and continuously reacting for 18 hours at 100 ℃; and (2) putting the regular substrate after the hydrothermal reaction into a palladium precursor solution (prepared from 0.03g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100 mL/L25% ammonia water and water), continuously reacting for 2 hours at the water bath temperature of 70 ℃, finally taking out, washing with water, and drying at 120 ℃ to constant weight.
Example 5
Soaking 0.42g of honeycomb activated carbon regular substrate with the size of 5 multiplied by 24mm in stannous chloride solution of 8g/L at room temperature for 15min, then soaking in palladium chloride solution of 0.03/L at room temperature for 10min, and then taking out and washing with water; putting the pretreated regular substrate into a manganese oxide precursor solution (prepared by 0.05mol/L potassium permanganate and water), transferring the manganese oxide precursor solution and the potassium permanganate solution into a hydrothermal reaction kettle together, and continuously reacting for 24 hours at 90 ℃; and (2) putting the regular substrate after the hydrothermal reaction into a palladium precursor solution (prepared from 0.04g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100 mL/L25% ammonia water and water), continuously reacting for 2 hours at the water bath temperature of 80 ℃, finally taking out, washing with water, and drying at 120 ℃ to constant weight.
In summary, the surface element analysis of the catalyst prepared in example 1 is performed by using EDS characterization technique, fig. 1 is an EDS surface element analysis diagram of the catalyst sample obtained in example 1, and as shown in fig. 1, in addition to four ceramic substrate elements of Si, Mg, Al and O, the existence of Mn and Pd elements can be observed, thereby proving that two active components of manganese oxide and palladium can be supported on the surface of the honeycomb ceramic substrate by using the method of compounding the in-situ self-grown manganese oxide and in-situ self-deposited noble metal palladium techniques provided in the present invention. FIG. 2 is an SEM surface topography of the catalyst prepared in example 1, and it can be seen from FIG. 2 that the manganese oxide and the noble metal palladium active component are uniformly distributed in the form of spheroidal particles on the surface of the honeycomb ceramic substrate. The catalyst samples obtained in examples 2 and 3 were subjected to EDS elemental analysis and SEM surface morphology analysis, and the results obtained were similar to those of the catalyst sample obtained in example 1.
EDS surface element analysis of the catalyst prepared in example 4 showed that in addition to the activated carbon substrate elements C, Si, Al and O, the presence of Mn and Pd was observed as shown in FIG. 3, thus confirming that the preparation method of this patent can indeed support both manganese oxide and palladium active components on the surface of the honeycomb activated carbon substrate. FIG. 4 is a SEM surface morphology of the catalyst prepared in example 4, wherein the manganese oxide and the noble metal palladium active components are uniformly distributed on the surface of the honeycomb activated carbon substrate in the form of spheroidal particles. The catalyst sample obtained in example 5 was selected for EDS elemental analysis and SEM surface morphology analysis and the results were similar to those obtained for the catalyst sample obtained in example 4.
From the results of the surface elemental analysis by EDS of the catalyst samples obtained in examples 1 to 5, the mass content of the noble metal palladium in each catalyst sample can be calculated, as shown in table 1.
The catalyst samples prepared in examples 1 to 5 were subjected to a probe reaction using toluene catalytic combustion purification at a toluene injection concentration of 1.0g/m3And volume space velocity of 10000h-1The catalyst activity was evaluated under the conditions and the results are shown in Table 1. The catalyst activity is measured as the reaction temperature T at which the toluene conversion is 10%, 50% and 90%, respectively10、T50And T90As an evaluation criterion, a lower temperature value indicates a better catalyst purification activity. As shown in Table 1, the catalyst can be ignited at a low temperature of 160-226 ℃ and completely purified at 236-270 ℃ under the condition of very low palladium content (0.06-0.10 wt.%), and shows excellent toluene catalytic combustion purification performance. This is due to the oxidation of the noble metal palladium and manganese in the composite monolithic combustion catalyst prepared by the preparation method of the patentThe two active components can be uniformly and alternately distributed on the surface of the honeycomb structured carrier, so that the oxygen absorption and oxygen supply characteristics of the manganese oxide can be better exerted, and the low-temperature oxidation activity of the noble metal palladium can be effectively improved through the synergetic catalysis.
TABLE 1 toluene Combustion cleaning Activity of catalysts prepared in examples 1-5
Figure BDA0001863942550000061
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (7)

1. The preparation method of the manganese oxide and precious metal composite catalyst is characterized by comprising the following steps:
step 1: firstly, dipping a catalyst carrier in a stannous chloride solution, and then dipping in a palladium chloride solution;
step 2: putting the catalyst carrier obtained in the step 1 into a manganese oxide precursor solution for hydrothermal reaction;
and step 3: putting the catalyst carrier after the hydrothermal reaction into a palladium precursor solution, heating in a water bath, and drying;
the manganese oxide precursor solution comprises potassium permanganate and acetic acid;
the palladium precursor solution comprises a palladium chloride solution, sodium hypophosphite and ammonium chloride;
the temperature of the hydrothermal reaction in the step 2 is 90-120 ℃;
the time of the hydrothermal reaction in the step 2 is 12-24 h;
the concentration of the potassium permanganate solution in the manganese oxide precursor solution is 0.05-0.15mol/L, and the concentration of the acetic acid solution is 0.1-0.3 mol/L.
2. The method for preparing a manganese oxide-noble metal composite catalyst according to claim 1, wherein the catalyst support is honeycomb ceramic or honeycomb activated carbon.
3. The preparation method of the manganese oxide-precious metal composite catalyst according to claim 1, wherein the concentration of the stannous chloride solution is 8-12 g/L.
4. The method for preparing a manganese oxide-noble metal composite catalyst according to claim 1, wherein the concentration of the palladium chloride solution in step 1 is 0.02 to 0.05 g/L.
5. The method for preparing a manganese oxide-noble metal composite catalyst according to claim 1, wherein the concentration of the palladium chloride solution in the palladium precursor solution is 0.02-0.04g/L, the concentration of the sodium hypophosphite solution is 5.0g/L, and the concentration of the ammonium chloride solution is 13.5 g/L.
6. A manganese oxide and precious metal composite catalyst is characterized by being prepared by the preparation method of the manganese oxide and precious metal composite catalyst according to any one of claims 1 to 5.
7. The use of the oxides of manganese noble metal composite catalyst according to claim 6 as a scavenger of volatile organic pollutants.
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