CN114653367A - Preparation and application of iridium-supported catalyst with different carriers - Google Patents

Preparation and application of iridium-supported catalyst with different carriers Download PDF

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CN114653367A
CN114653367A CN202210280162.XA CN202210280162A CN114653367A CN 114653367 A CN114653367 A CN 114653367A CN 202210280162 A CN202210280162 A CN 202210280162A CN 114653367 A CN114653367 A CN 114653367A
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iridium
temperature
catalyst
tio
methane
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杨东江
段会梅
纪嘉宾
孔凡鑫
邹译慧
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Qingdao University
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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
    • B01J23/38—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
    • B01J23/63—Platinum group metals with rare earths or actinides
    • 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
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/46—Ruthenium, rhodium, osmium or iridium
    • B01J23/468—Iridium
    • 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
    • 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
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • 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
    • B01J37/08—Heat treatment
    • 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
    • B01J37/16—Reducing
    • B01J37/18—Reducing with gases containing free hydrogen
    • 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
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
    • 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

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Abstract

The invention provides a preparation method of iridium-supported catalysts with different carriers and low-concentration methane (CH) prepared by the method4The content is less than 1 percent), and the invention belongs to the field of catalytic combustion of methane and low-carbon alkane. The oxide carrier used comprisesMnO2Nanowire, TiO2、CeO2And the like. The preparation method of the iridium-supported catalyst with different carriers comprises the following steps: first MnO is added2Nanowire, TiO2、CeO2The carrier material and a certain amount of iridium salt solution are dispersed, mixed and dried by ultrasound, and then are dried for 24 to 36 hours in a freeze dryer or dried for 10 to 15 hours in an oven at the temperature of 100-120 ℃, and then are roasted for 1 to 4 hours in air at the temperature of 400-600 ℃, and finally the powder sample is subjected to 5 to 10 percent H2Reducing for 1-3h at the temperature of 300-600 ℃ under the Ar atmosphere to obtain iridium catalyst powder Ir/MO supported by different carriersx(M ═ Mn, Ti, Ce, etc.). Iridium catalysts loaded on different carriers show better low-temperature methane catalytic activity, wherein commercial anatase titanium oxide is loaded with iridium Ir/TiO2The P catalyst has the best methane catalytic combustion activity. The preparation method is simple and economic, has no harmful by-products, and has high low-temperature catalytic activity, thereby having important guiding significance in the aspects of eliminating low-concentration methane and designing the catalyst in the field of alkane combustion.

Description

Preparation and application of iridium-supported catalyst with different carriers
Technical Field
The invention belongs to the field of catalytic combustion of methane and low-carbon alkane, and particularly relates to a preparation method and application of an iridium-supported catalyst with different carriers.
Background
In recent years, with the development of the mining and exploiting technologies of shale gas and combustible ice and the strong advocated environmental policy of "coal to gas" by the chinese government, natural gas is becoming the focus of the global energy supply and demand pattern as a clean energy. Methane as the main component of natural gas has the advantages of high heat value, low cost, safety, no toxicity and the like. But methane gas has a greenhouse effect 25 times that of carbon dioxide. These problems have become more serious as the use of natural gas has increased year by year, which requires that unburned and full methane be purified before being discharged. Especially in internal combustion engines and natural gas powered vehicles, controlling methane emissions and eliminating low levels of unburned methane is of great practical significance. If methane is directly combusted, the temperature during combustion will exceed 1200 ℃. The higher the temperature, the more likely the side reactions of incomplete combustion of methane, such as carbon monoxide, soot particles and other hydrocarbons, etc., will occur. At the same time, such high temperatures also lead to NOxThe formation of contaminants. In addition, due to the high degree of structural symmetry of the nonpolar methane molecule (C-H bond energies up to 434kJ/mol), CH4Difficult to activate under mild conditions. The catalytic combustion of methane is an important means for converting and utilizing clean energy and controlling methane emission, and the development of a high-performance catalytic combustion catalyst is imminent.
Compared with other catalysts, noble metals such as Pd and Pt are the most studied at present due to their good low-temperature catalytic activityA methane-like combustion catalyst. Recently, the Weave team has theoretically demonstrated CH using a study of model surface chemistry4Can be in IrO2{110} surface formation of a strong sigma complex, CH is achieved at lower temperatures4Wherein the C-H bond is cleaved. And CH4In IrO2The activation energy of C-H fracture of the {110} surface is far lower than that of PdO {101 }. In addition, metal oxide support-metal interface interactions can greatly improve the catalytic performance of metal catalysts. Therefore, the research on the methane catalytic combustion performance of different metal oxide supported iridium catalysts and the development of high-performance methane catalytic combustion catalysts have extremely important research significance.
Disclosure of Invention
The preparation process is simple, expensive equipment is not needed, the obtained iridium nano-catalyst loaded by different carriers has good low-temperature catalytic activity in methane combustion catalysis, and has bright application prospect in the elimination of low-concentration methane.
Preparation and application of iridium nanocrystalline catalyst loaded on different carriers specifically comprise the following steps:
1. an iridium nanocrystalline catalyst loaded on different carriers uses metal oxides with different properties as carriers, and Ir with the mass fraction of 0.5-2% is loaded on the metal oxide carriers with different properties by wet impregnation.
2. The iridium nanocrystalline catalyst loaded on different carriers mainly comprises commercially available TiO2、CeO2Synthesized TiO with different morphologies2、CeO2And fibrous MnO2Nanowires, and the like.
3. The iridium nanocrystalline catalyst loaded by different carriers is prepared by the following method: respectively adding a certain amount of TiO2、CeO2、MnO2Spreading the carrier powder in a beaker, dropwise adding an iridium precursor solution (chloroiridic acid or iridium chloride and the like) with the mass fraction of 1% onto the surface of the carrier powder, and then performing ultrasonic dispersion at room temperature for 0.5-1h to obtain uniformly dispersed wet powder; drying the wet powder material in a blast drying oven at the temperature of 100-120 ℃ for 10-15h or freeze-drying in a freeze dryer24-36 h; then the powder sample is roasted in a muffle furnace for 1-4H at the temperature of 450-550 ℃ in air, and finally the powder sample is roasted in 5-10% H2Reducing for 1-3h at the temperature of 600 ℃ under the Ar atmosphere at 300-.
4. The iridium nanocrystalline catalyst loaded by different carriers is applied to methane catalytic combustion.
5. The catalytic application process comprises the steps of firstly placing 100-250mg of supported iridium nanocrystalline catalyst in a quartz tube of a micro fixed bed reactor, then introducing reaction gas at the flow rate of 50-100ml/min, and simultaneously raising the temperature to 350 ℃ at the temperature rise rate of 5 ℃/min for pretreatment for 1h under the reaction atmosphere. Then cooling to room temperature, detecting the reaction gas at intervals of 25 ℃ by an online gas chromatograph (Shimadzu GC-2014 gas chromatograph) at the temperature rise rate of 5 ℃/min and between 200 ℃ and 450 ℃, and recording the methane conversion rate. The reaction gas contained 0.2% CH4、2％O2And the balance of inert gas argon.
6. The catalytic application is that under the gas flow rate of 50-100ml/min and the reaction temperature of 350 ℃, compared with iridium catalysts supported by other carriers, commercial anatase titanium oxide supports iridium Ir/TiO2The P-methane conversion rate reaches 100% of complete conversion.
The invention has the following advantages:
the preparation process is simple, expensive equipment is not needed, and the obtained supported iridium nanocrystal has excellent low-temperature catalytic activity in methane combustion catalysis, and has bright application prospect in low-concentration methane elimination.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the scope of the present invention is not limited to the implementation thereof.
Example 1
2％Ir/MnO2Preparing a nano catalyst:
adding a certain amount of fibrous MnO2Spreading the powder in a beaker, and dropwise adding an iridium precursor solution with the mass fraction of 2% into the MnO2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then the wet powder is mixedDrying in a freeze dryer for 24-36 h; then, the powder sample is roasted in a muffle furnace at the temperature of 450-2A nanocrystalline catalyst.
Example 2
1％Ir/TiO2Preparation of {100} nanocrystalline catalyst:
adding a certain amount of TiO2The {100} powder was spread in a beaker, and an iridium precursor solution of 1% mass fraction was added dropwise to the above TiO precursor solution2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then drying the wet powder in a blast drying oven at the temperature of 100-120 ℃ for 10-15 h; then the powder sample is roasted in a muffle furnace for 1-4H at the temperature of 450-550 ℃ in air, and finally the powder sample is roasted in 5-10% H2Reducing for 1-3h at the temperature of 600 ℃ under the atmosphere of/Ar to obtain 1 percent Ir/TiO2{100} nanocrystalline catalyst.
Example 3
1％Ir/TiO2Preparation of {101} nanocrystalline catalyst:
adding a certain amount of TiO2{101} powder was spread in a beaker, and an iridium precursor solution of 1% mass fraction was added dropwise to the above TiO precursor solution2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then drying the wet powder material in a blast drying oven at the temperature of 100-120 ℃ for 10-15 h; then the powder sample is roasted in a muffle furnace for 1-4H at the temperature of 450-550 ℃ in air, and finally the powder sample is roasted in 5-10% H2Reducing for 1-3h at the temperature of 600 ℃ under the atmosphere of/Ar to obtain 1 percent Ir/TiO2{101} nanocrystalline catalyst.
Example 4
1％Ir/TiO2Preparation of-B nanocrystalline catalyst:
a certain amount of B phase TiO2The nano-fiber is spread in a beaker, and the iridium precursor solution with the mass fraction of 1 percent is dripped into the TiO dropwise2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then drying the wet powder in a blast drying oven at the temperature of 100-120 ℃ for 10-15 h; then the powder sample is roasted in a muffle furnace for 1-4h at the temperature of 450-550 ℃ in air, and finally the powder sample is roasted at 5 DEG C-10％H2Reducing for 1-3h at the temperature of 600 ℃ under the atmosphere of/Ar to obtain 1 percent Ir/TiO2-B nanocrystalline catalyst.
Example 5
1％Ir/TiO2-preparation of P nanocrystalline catalyst:
mixing a certain amount of commercial anatase TiO2(TiO2-P) spreading the powder in a beaker, dropping 1% by mass of iridium precursor solution dropwise into the TiO2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then drying the wet powder in a blast drying oven at the temperature of 100-120 ℃ for 10-15 h; then baking the powder sample in a muffle furnace at the temperature of 450-550 ℃ for 1-4H, and finally baking the powder sample in 5-10% H2Reducing for 1-3h at the temperature of 300 ℃ and 600 ℃ under the Ar atmosphere to obtain 1 percent Ir/TiO2-P nanocrystalline catalyst.
Example 6
2％Ir/CeO2Preparing a nanocrystalline catalyst:
a certain amount of CeO2Spreading the powder in a beaker, and dropwise adding an iridium precursor solution with the mass fraction of 2% into the TiO2Performing ultrasonic dispersion on the surface of the powder for 0.5-1h at room temperature to obtain uniformly dispersed wet powder; then drying the wet powder in a blast drying oven at the temperature of 100-120 ℃ for 10-15 h; then the powder sample is roasted in a muffle furnace for 1-4H at the temperature of 450-550 ℃ in air, and finally the powder sample is roasted in 5-10% H2Reducing for 1-3h at the temperature of 600 ℃ under the atmosphere of/Ar to obtain 1 percent Ir/CeO2A nanocrystalline catalyst.
Example 7
Testing of catalytic performance in methane combustion reaction:
the methane catalytic combustion reaction is to place the prepared iridium nanocrystalline catalyst loaded by different carriers in a quartz reaction tube of a micro fixed bed reactor, then introduce reaction gas at the flow rate of 50-100ml/min, and simultaneously raise the temperature to 400 ℃ at the temperature rise rate of 5 ℃/min and pretreat the catalyst for 1h under the reaction atmosphere. Cooling to room temperature, maintaining at 200-450 deg.C and 25 deg.C for 30-60min, and detecting the reaction gas by on-line gas chromatographyThe assay (Shimadzu GC-2014 gas chromatograph) records the methane conversion. The reaction gas contained 0.2% CH4、2％O2And the balance of inert gas argon. Results of the catalytic combustion activity of methane for the different supported iridium catalysts are shown in table 1.
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
T50(℃) 350 320 320 352 287 353
T99(℃) 430 395 400 415 345 436

Claims (6)

1. The preparation method of the iridium nanocrystalline catalyst loaded on different carriers is characterized in that the supported iridium nanocrystalline catalyst takes metal oxides with different properties as carriers, and Ir with the mass fraction of 0.5-2% is loaded on the metal oxide carriers with different properties by wet impregnation.
2. The iridium nanocrystalline catalyst supported on a different carrier according to claim 1, wherein the carrier comprises fibrous MnO2Nanowire, commercially available TiO2、CeO2And synthesized TiO with different morphologies2、CeO2And the like.
3. The iridium nanocrystalline catalyst supported by different carriers according to claim 1, wherein the supported iridium nanocrystalline catalyst is prepared by the following method: respectively adding a certain amount of MnO2、TiO2、CeO2Spreading the carrier powder in a beaker, dropwise adding an iridium precursor solution (chloroiridic acid, iridium chloride and the like) with the mass fraction of 0.5-2% onto the surface of the carrier powder, and then performing ultrasonic dispersion at room temperature for 0.5-1h to obtain uniformly dispersed wet powder; placing the wet powder material in a freeze dryer for freeze drying for 24-36h or drying in an oven at the temperature of 100-120 ℃ for 10-15 h; then baking the powder sample in a muffle furnace at the temperature of 450-550 ℃ for 1-4H, and finally baking the powder sample in 5-10% H2Reducing for 1-3h at the temperature of 600 ℃ under the Ar atmosphere at 300-.
4. Use of a different supported iridium nanocrystalline catalyst according to claim 1 or 2 or 3 in catalytic combustion of methane.
5. The catalytic application as claimed in claim 4, wherein the catalytic application process comprises first 100-250mg of supported iridium nanocrystalsThe catalyst is placed in a quartz tube of a micro fixed bed reactor, then reaction gas is introduced at the flow rate of 50-100ml/min, and the temperature is raised to 350 ℃ at the temperature raising rate of 5 ℃/min, and the pretreatment is carried out for 1h under the reaction atmosphere. Then cooling to room temperature, detecting the reaction gas at intervals of 25 ℃ by an online gas chromatograph (Shimadzu GC-2014 gas chromatograph) at a heating rate of 5 ℃/min between 200 ℃ and 450 ℃ and recording the methane conversion rate. The reaction gas contained 0.2% CH4、2％O2And the balance of inert gas argon.
6. The catalytic application of claim 4, wherein commercial anatase titania supported iridium Ir/TiO compared to other supported iridium catalysts at gas flow rates of 50-100ml/min, reaction temperature of 350 ℃, is2The methane conversion rate of the P catalyst reaches 100 percent of complete conversion.
CN202210280162.XA 2022-03-11 2022-03-11 Preparation and application of iridium-supported catalyst with different carriers Pending CN114653367A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116272968A (en) * 2022-09-07 2023-06-23 中山大学 Carbon-supported Ir catalyst and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
JP2003170049A (en) * 2001-12-10 2003-06-17 Toyota Motor Corp Exhaust gas cleaning catalyst
CN106540754A (en) * 2015-09-18 2017-03-29 中国科学院大连化学物理研究所 A kind of catalyst for catalytic combustion and its preparation method and application
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116272968A (en) * 2022-09-07 2023-06-23 中山大学 Carbon-supported Ir catalyst and preparation method and application thereof
CN116272968B (en) * 2022-09-07 2024-01-30 中山大学 Carbon-supported Ir catalyst and preparation method and application thereof

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