CN113275017A - Preparation method and application of composite pyrochlore catalyst - Google Patents

Preparation method and application of composite pyrochlore catalyst Download PDF

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CN113275017A
CN113275017A CN202110591540.1A CN202110591540A CN113275017A CN 113275017 A CN113275017 A CN 113275017A CN 202110591540 A CN202110591540 A CN 202110591540A CN 113275017 A CN113275017 A CN 113275017A
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composite
catalyst
pyrochlore
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preparing
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胡瑞生
徐畅
程天娇
胡佳楠
高小娇
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Inner Mongolia University
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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
    • B01J23/70—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
    • B01J23/83—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 rare earths or actinides
    • 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
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
    • 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
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    • 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
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
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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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2257/7022—Aliphatic hydrocarbons
    • B01D2257/7025—Methane
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    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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    • Y02C20/20—Capture or disposal of greenhouse gases of methane

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Abstract

The invention belongs to the technical field of catalyst preparation, and provides a composite pyrochlore La prepared by a sol-gel coexistence method2Zr2O7/70％Co3O4The catalyst and the preparation method have simple process and low cost, and the prepared composite pyrochlore La2Zr2O7/70％Co3O4The catalyst is applied to the catalytic oxidation reaction of the air exhaust gas of the fixed bed reactor and has good catalysisChemical activity and stability, T thereof10、T50、T90335.9 deg.C, 428.3 deg.C, 544.9 deg.C, respectively.

Description

Preparation method and application of composite pyrochlore catalyst
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a preparation method and application of a composite pyrochlore catalyst.
Background
During coal mining, a large amount of air (about 100-300 m) is required3/s) dilution of CH released from working face of underground coal seam4Containing CH discharged in the large ventilation air stream of an underground coal mine4To ensure CH4The concentration is below the lower explosive limit of 5%, which is usually less than 2%, and this gas is referred to as the exhaust gas.
Over the past 250 years, the concentration of methane in the atmosphere has increased by 151%, with methane mainly coming from the agricultural, energy, industrial and waste disposal industries. The amount of methane emitted in coal mining accounts for 22% of the amount of methane emitted in the energy industry, and the amount of methane emitted to the atmosphere is about 190 billionths of cubic meters each year, and is increasing each year. Methane, a greenhouse gas, destroys the ozone layer and deteriorates the atmospheric environment, and the Global Warming Potential (GWP) is 25 times higher than that of carbon dioxide, so that the exhaust gas released to the atmosphere during coal mining has a serious negative effect on global warming, and although the concentration of methane is low, the methane is considered as a potential energy source and has not been well utilized. However, due to the low concentration and high flow rate of methane in the exhaust gas, the oxidation of methane is difficult and difficult to utilize by conventional techniques.
At present, the utilization of the wind exhaust gas mainly comprises a thermal oxidation technology and a catalytic combustion technology, wherein the thermal oxidation technology is realized by high temperature (C)>1000 ℃ to cause spontaneous combustion, the main drawback being the high working temperature: (>1000 ℃) and thus the associated safety problems of high mining temperatures, the catalytic combustion technology not only allows catalytic combustion at lower reaction temperatures, but also avoids N at high temperatures2And O2NOx harmful to the atmosphere is generated by reaction, and the pyrochlore type catalyst has good thermal stability and high-temperature catalytic activity, but no report of the technology of applying the pyrochlore type catalyst to catalytic combustion of air-exhaust gas exists at present.
Therefore, how to provide a catalyst which has excellent activity and high heat resistance and can be used for catalytic reaction of combustion of exhaust gas is a problem that needs to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a composite pyrochlore catalyst with good catalytic combustion performance for air exhaust gas, and the catalyst is applied to the catalytic combustion reaction for air exhaust gas and has a lower complete conversion temperature for air exhaust gas.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of the composite pyrochlore catalyst comprises the following steps:
(1) weighing La (NO)3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2Fully dissolving O and citric acid in deionized water to obtain a mixed solution;
(2) heating the mixed solution in a water bath kettle in a constant-temperature water bath, and fully stirring to form a wet gel precursor;
(3) putting the wet gel precursor into a spot-heating oven to be dried to form dry gel;
(4) grinding the xerogel, then placing the ground xerogel in a muffle furnace for roasting, cooling to room temperature, taking out and grinding the xerogel into powder to obtain the composite pyrochlore La2Zr2O7/70％Co3O4A catalyst.
Preferably, in the above method for preparing a composite pyrochlore catalyst, the La (NO) in the step (1)3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2The molar ratio of O is 1:1:8.5, and the molar ratio of citric acid to total metal ions is 1: 1.2.
Preferably, in the above method for preparing a composite pyrochlore catalyst, La (NO)3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2The proportion relation of the total mass of the O and the citric acid to the deionized water is 1: 15-25.
Preferably, in the above preparation method of the composite pyrochlore catalyst, the temperature of the constant-temperature water bath heating in the step (2) is 66 ℃ and the time is 7.5 h.
The beneficial effects of the above technical scheme are: the heating process can evaporate water, enhance the polymerization energy among solid particles in the sol, hydrolyze metal salts to form chain or net-shaped cross-linked polymers and promote the formation of gel.
Preferably, in the above preparation method of the composite pyrochlore catalyst, in the step (3), the drying temperature is 95 ℃ and the drying time is 24 hours.
The beneficial effects of the above technical scheme are: after the gel is formed by aging, hydrolysis and polycondensation reaction are carried out, and water or other liquid needs to be removed by drying at a certain temperature, so that the hydrolysis is completely finished, and the xerogel is formed.
Preferably, in the above method for preparing a composite pyrochlore catalyst, the calcination in step (4) is: heating to 500 deg.C at a rate of 10 deg.C/min, decomposing for 3h to obtain oxide raw powder, taking out, grinding, heating to 900 deg.C at a rate of 5 deg.C/min, and calcining for 3 h.
The beneficial effects of the above technical scheme are: the roasting process can remove organic components in the sample, eliminate air holes in the xerogel and determine the phase composition, the microstructure and the required exposed crystal faces of the sample.
The invention also provides the composite pyrochlore La prepared by the method2Zr2O7/70％Co3O4A catalyst.
And the composite pyrochlore La prepared by the method2Zr2O7/70％Co3O4Application of catalyst, and preparation method of composite pyrochlore La2Zr2O7/70％Co3O4The catalyst is used for catalytic oxidation reaction of air exhaust gas of the fixed bed reactor.
According to the technical scheme, compared with the prior art, the composite pyrochlore La prepared by the method2Zr2O7/70％Co3O4The catalyst is prepared by taking common organic compound citric acid as a complexing agent and adopting a sol-gel symbiotic method, and has the advantages of simple preparation method and low cost; the prepared catalyst is applied to air-exhaust gas, and has the advantages of low ignition temperature, low complete conversion temperature, good thermal stability, hydrothermal stability and sulfur resistance, and T of the catalyst10、T50、T90335.9 deg.C, 428.3 deg.C, 544.9 deg.C, respectively.
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, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a composite pyrochlore type La2Zr2O7/70％Co3O4Catalyst and comparative phase La2Zr2O7XRD pattern of (a);
FIG. 2 shows a composite pyrochlore type La2Zr2O7/70％Co3O4Catalyst and comparative phase La2Zr2O7(ii) activity profile of (a);
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
Preparation of 5g of composite pyrochlore type La2Zr2O7/70％Co3O4The catalyst comprises the following steps: 2.270g of La (NO) was weighed out3)3·6H2O (analytically pure), 2.345g of Zr (NO)3)2·6H2O (analytically pure), 12.690g of Co (NO)3)2·6H2Dissolving O (analytically pure) and 5.508g of citric acid (analytically pure) in 200ml of deionized water, heating in a constant-temperature water bath at 66 ℃ after fully dissolving, fully stirring for 7.5h to form a wet gel precursor, placing the obtained wet gel precursor in an electrothermal oven, and drying for 24h at 95 ℃ to form dry gel; grinding the obtained dry gel to 40-60 meshes, placing the dry gel in a muffle furnace, heating to 500 ℃ at the speed of 10 ℃/min, decomposing for 3h to obtain oxide raw powder, taking out, fully grinding, placing the oxide raw powder in the muffle furnace again, heating to 900 ℃ at the speed of 5 ℃/min, roasting for 3h, cooling to room temperature, taking out, further grinding into powder to obtain the target product La2Zr2O7/70％Co3O4A sample of the catalyst.
Comparative example 1
Preparation of 5g of composite pyrochlore type La2Zr2O7The catalyst comprises the following steps: 7.567g of La (NO) were weighed out3)3·6H2O (analytically pure), 6.208g of Zr (NO)3)2·6H2Dissolving O (analytically pure) and 18.360g of citric acid (analytically pure) in 200ml of deionized water, heating in a constant-temperature water bath at 66 ℃ after fully dissolving, fully stirring for 7.5h to form a wet gel precursor, placing the obtained wet gel precursor in an electrothermal oven, and drying for 24h at 95 ℃ to form dry gel; grinding the obtained dry gel to 40-60 meshes, placing the dry gel in a muffle furnace, heating to 500 ℃ at the speed of 10 ℃/min, decomposing for 3h to obtain oxide raw powder, taking out, fully grinding, placing the oxide raw powder in the muffle furnace again, heating to 900 ℃ at the speed of 5 ℃/min, roasting for 3h, cooling to room temperature, taking out, further grinding into powder to obtain the target product La2Zr2O7A sample of the catalyst.
The catalyst obtained was tested for catalytic activity according to the following procedure:
general activity test: activity test reaction temperature is controlled by a program temperature rising instrument, and 0.20g of catalyst particle sample with 40-60 meshes is loaded in a reactorBefore the reaction, the reactor was purged with 20ml/min of nitrogen gas for 15min to remove water and air from the reaction system, and the mixed reaction gas of 20ml/min was introduced into the reactor for 20min, and then the reactor was heated to test the catalyst activity by CH4The gas infrared analyzer monitors the methane conversion rate at different temperatures.
Sulfur resistance activity test: subjecting the prepared test sample to 0.001 wt% of H2SO4Soaking, standing for 2h, transferring the sample to a constant-temperature drying oven at 100 ℃ for drying, screening the sample after the treatment, taking 0.2g of catalyst with 40-60 meshes, loading into a fixed bed reactor for activity test, and testing according to the common activity test operation.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the scheme disclosed by the embodiment, the scheme corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (8)

1. The preparation method of the composite pyrochlore catalyst is characterized by comprising the following steps of:
(1) weighing La (NO)3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2Fully dissolving O and citric acid in deionized water to obtain a mixed solution;
(2) heating the mixed solution in a water bath kettle in a constant-temperature water bath, and fully stirring to form a wet gel precursor;
(3) putting the wet gel precursor into a spot-heating oven to be dried to form dry gel;
(4) grinding the xerogel, then placing the ground xerogel in a muffle furnace for roasting, cooling to room temperature, taking out and grinding the xerogel into powder to obtain the composite pyrochlore La2Zr2O7/70％Co3O4A catalyst.
2. The method for preparing a composite pyrochlore catalyst as claimed in claim 1 wherein in step (1) La (NO) is added3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2The molar ratio of O is 1:1:8.5, and the molar ratio of citric acid to total metal ions is 1: 1.2.
3. The method for preparing a composite pyrochlore catalyst as claimed in claim 1 wherein the La (NO) is3)3·6H2O、Zr(NO3)2·6H2O、Co(NO3)2·6H2The proportion relation between the total mass of the O and the citric acid and the deionized water is 1: 15-1: 25.
4. The method for preparing the composite pyrochlore catalyst according to claim 1, wherein the constant temperature water bath heating in the step (2) is carried out at a temperature of 66 ℃ for 7.5 hours.
5. The method for preparing a composite pyrochlore catalyst according to claim 1, wherein the drying temperature in step (3) is 95 ℃ and the drying time is 24 hours.
6. The method for preparing the composite pyrochlore catalyst according to claim 1, wherein the calcination in step (4) is: heating to 500 deg.C at a rate of 10 deg.C/min, decomposing for 3h to obtain oxide raw powder, taking out, grinding, heating to 900 deg.C at a rate of 5 deg.C/min, and calcining for 3 h.
7. A composite pyrochlore La prepared by the method of any one of claims 1 to 62Zr2O7/70％Co3O4A catalyst.
8. A composite pyrochlore La prepared by the method of any one of claims 1 to 62Zr2O7/70％Co3O4Use of a catalyst, characterized in that the composite pyrochlore La is used2Zr2O7/70％Co3O4The catalyst is used in the catalytic oxidation reaction of the air exhaust gas of the fixed bed reactor.
CN202110591540.1A 2021-05-28 2021-05-28 Preparation method and application of composite pyrochlore catalyst Pending CN113275017A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1282307A (en) * 1968-07-02 1972-07-19 Commissariat Energie Atomique Method of preparation of homogeneous oxides of two or more elements in a fineley divided form and products obtained
CN101293201A (en) * 2008-05-30 2008-10-29 内蒙古大学 Method for preparing methyl hydride combustion catalyst
CN102142564A (en) * 2011-02-24 2011-08-03 安徽工业大学 LaFeO3-base cathode material of sulfur-oxygen fuel cell
CN104084210A (en) * 2014-07-21 2014-10-08 内蒙古大学 Preparation method of double-doping composite oxide catalyst for methane combustion
CN104478464A (en) * 2014-12-16 2015-04-01 浙江大学 Method for preparing porous lanthanum zirconate block

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1282307A (en) * 1968-07-02 1972-07-19 Commissariat Energie Atomique Method of preparation of homogeneous oxides of two or more elements in a fineley divided form and products obtained
CN101293201A (en) * 2008-05-30 2008-10-29 内蒙古大学 Method for preparing methyl hydride combustion catalyst
CN102142564A (en) * 2011-02-24 2011-08-03 安徽工业大学 LaFeO3-base cathode material of sulfur-oxygen fuel cell
CN104084210A (en) * 2014-07-21 2014-10-08 内蒙古大学 Preparation method of double-doping composite oxide catalyst for methane combustion
CN104478464A (en) * 2014-12-16 2015-04-01 浙江大学 Method for preparing porous lanthanum zirconate block

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
白雪: "复合烧绿石型La2Zr2O7催化剂对风排瓦斯气催化燃烧的性能研究", 《中国优秀硕士学位论文全文数据库（工程科技Ⅰ辑）》 *

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