CN112691660B - Method for preparing ammonia oxidation catalyst based on deposition precipitation method - Google Patents

Method for preparing ammonia oxidation catalyst based on deposition precipitation method Download PDF

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CN112691660B
CN112691660B CN202011575836.6A CN202011575836A CN112691660B CN 112691660 B CN112691660 B CN 112691660B CN 202011575836 A CN202011575836 A CN 202011575836A CN 112691660 B CN112691660 B CN 112691660B
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ammonia oxidation
oxidation catalyst
placing
diesel vehicle
mixed solution
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CN112691660A (en
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刘彩霞
王慧君
张子印
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Langfang Beechen Business Establishing Resin Material Co ltd
Tianjin University
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Tianjin 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
    • 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
    • B01J37/031—Precipitation
    • B01J37/035—Precipitation on carriers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9436—Ammonia
    • 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
    • B01J23/42—Platinum
    • 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
    • B01J23/54—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
    • B01J23/66—Silver or gold
    • 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
    • B01J23/66—Silver or gold
    • B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/681—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with arsenic, antimony or bismuth
    • 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

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Abstract

The invention discloses a method for preparing an ammonia oxidation catalyst based on a deposition precipitation method. The method comprises the following steps: firstly, placing a metal oxide carrier in a tubular furnace, carrying out heat treatment for 2-4h in a reducing atmosphere to obtain a defect carrier, and dispersing the defect carrier into deionized water; then adding ammonium carbonate solution for alkalization; dissolving a noble metal precursor in deionized water, and dripping the solution into the mixed solution; aging the mixed solution at room temperature for 1-2h, and then performing centrifugal washing; then placing the mixture in an oven for continuous drying for 10-12 h; and finally, placing the dried catalyst in a tubular furnace, and carrying out heat treatment for 2-4h in a reducing atmosphere to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method. The ammoxidation catalyst prepared by the invention can reach over 90 percent of catalytic efficiency within 350-400 ℃, and shows relatively good N 2 And selectivity, can be used for ammoxidation of diesel vehicle tail gas.

Description

Method for preparing ammonia oxidation catalyst based on deposition precipitation method
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a method for preparing an ammonia oxidation catalyst based on a deposition precipitation method.
Background
With the continuous and rapid development of economy in China, the quantity of motor vehicles kept by people is continuously increased, and the problem of air pollution caused by moving sources is more serious. Nitrogen Oxides (NO) x ) Is one of the main atmospheric pollutants, only accounts for 9.1 percent of diesel vehicles of motor vehicles, and discharges NO x Occupying steamThe total emission of the vehicle is more than 80%. For diesel vehicle tail gas NO x Currently, NH is mostly used 3 SCR technology for abatement, which in practice requires the addition of an excess of urea to achieve a high NO conversion, NH 3 the/NO ratio is less than 1 (. apprxeq.0.90-0.95) and therefore results in unreacted ammonia (NH) 3 ) The leakage phenomenon of (1). To solve the problem of NO in the atmospheric environment x The pollution problem and the discharge standard of the tail gas of the diesel vehicles of all countries are also stricter. Data of emission limit and measurement method of pollutants for heavy-duty diesel vehicles (sixth stage of China) (national VI for short) implemented nationwide in 2021 show that heavy-duty diesel engines do not have high emission efficiency x The emission limit requirement is 70% stricter than that of the national V. To satisfy the increasingly stringent diesel vehicle NO x Emission standard using NH 3 SCR technology will add more urea to produce NH 3 To reduce NO x And thus unreacted slipped NH 3 The amount is also increasing. At the same time, the national VI standard first converts NH 3 The emission limit was included (10 ppm). Thus, control of diesel vehicle exhaust NH 3 The emission becomes an important task of winning the 'blue sky guard war'.
For heavy-duty diesel vehicles, a combined aftertreatment system of EGR + DOC + DPF + SCR is often adopted for exhaust treatment. To solve NH generated by SCR catalyst 3 The problem of leakage is that an ASC (ammonia Slip catalyst) catalytic device is generally arranged at the downstream of an SCR device, and ammonia selective catalytic oxidation technology (NH) is utilized 3 SCO) vs. NH escaped 3 The key point of the treatment lies in NH 3 SCO catalyst design. Escaped NH in tail gas of diesel vehicle 3 The lower the content, the smaller the required ASC catalyst volume, the higher the space velocity compared to the SCR catalyst. At the same time, higher concentration of O is also present in the tail gas 2 And water vapor. Tail gas temperature of diesel vehicle in cold start stage<The CDPF equipment reduces the requirement on the thermal stability of the catalyst at 200 ℃, but the passive regeneration assistance is still needed at present, and the tail gas temperature can reach over 600 ℃. At present, novel NH 3 The design of SCO catalysts faces the following challenges: 1) NH 3 Has a low ignition temperature (<At 300 ℃, external heating is not needed; 2) to reduce NH concentration 3 (<500ppm) Selectivity conversionTo N 2 (ii) a 3) Sufficient stability at high concentrations of water vapor; therefore, research and development of the catalyst has the advantages of good low-temperature activity, wide temperature window and N 2 NH having high selectivity and excellent stability 3 SCO catalysts are the direction of research for the treatment of diesel exhaust NH 3.
At present, a single noble metal component is easy to agglomerate, sinter and the like to deactivate the catalyst, and is expensive. Although the transition metal catalyst is low in price, the low-temperature activity is poor, and the temperature window is narrow. Molecular sieve based catalyst N 2 The selectivity is excellent, but the low temperature activity and hydrothermal stability need to be improved. Simultaneously satisfies the low temperature high activity and high N 2 The catalyst with excellent selectivity and hydrothermal stability is not found, so the research on the preparation method of the catalyst for the tail gas of the diesel vehicle and the ammoxidation performance of the catalyst have great application prospects.
Disclosure of Invention
The invention aims to provide a method for preparing an ammonia oxidation catalyst based on an impregnation method.
A method for preparing an ammonia oxidation catalyst based on a deposition precipitation method comprises the following steps:
(1) placing the metal oxide carrier in a tube furnace, and carrying out heat treatment for 2-4h at 400-500 ℃ in a reducing atmosphere to obtain a defect carrier with surface oxygen vacancies;
(2) dispersing the defect carrier obtained in the step (1) into deionized water to obtain a mixed solution; then adding ammonium carbonate solution for alkalization; dissolving a noble metal precursor in deionized water to prepare a precursor solution, and dripping the precursor solution into the mixed solution;
(3) aging the mixed solution prepared in the step (2) at room temperature for 1-2h, and then performing centrifugal washing; then placing the mixture in an oven to be dried continuously for 10-12h at the temperature of 100-120 ℃;
(4) and (4) placing the dried catalyst obtained in the step (3) in a tubular furnace, and carrying out heat treatment for 2-4h at the temperature of 400-500 ℃ in a reducing atmosphere to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method.
The metal oxide is CeO 2 、TiO 2 、SnO 2 、Sb 2 O 3 One or more ofAnd (4) seed selection.
The noble metal precursor is one or more of chloroplatinic acid, silver nitrate and gold chloride.
The reducing atmosphere is H 2 /N 2 。
The mass ratio of the defect carrier to the noble metal precursor is 6000: (1-6).
The mass ratio of the defect carrier to the ammonium carbonate is 300: (1-5).
An ammoxidation catalyst obtained by the above-mentioned production method.
The application of the ammoxidation catalyst is used for treating the diesel vehicle emission containing NH 3 The tail gas of (3).
The invention has the beneficial effects that: the ammonia oxidation catalyst prepared by the sedimentation method can be used for the ammonia oxidation technology of the tail gas of the diesel vehicle, and has good catalytic activity. The ammoxidation catalyst prepared by the method can reach the catalytic efficiency of more than 90% at 350-400 ℃, and shows relatively good N 2 And (4) selectivity.
Drawings
FIG. 1 shows NH of an ammoxidation catalyst prepared by precipitation in example 1 3 And (5) oxidation test results.
FIG. 2 shows N of an ammoxidation catalyst prepared by precipitation in example 1 2 And (4) selecting a test result.
FIG. 3 is an XRD pattern of an ammonia oxidation catalyst prepared by precipitation in example 1.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
12g of CeO 2 Placing in a tube furnace, heating from room temperature to 400 deg.C at a heating rate of 5 deg.C/min, and reducing in a reducing atmosphere (5% H) 2 /95％N 2 ) Pretreating for 2h to obtain a solution withA defect carrier of surface oxygen vacancies. 6g of the defect carrier was dissolved in 100mL of deionized water to obtain a mixed solution and stirred for 30min, followed by alkalinization by dropwise addition of 0.6mL of a 10% ammonium carbonate solution. Chloroplatinic acid containing crystal water is dissolved in deionized water to prepare a chloroplatinic acid solution with the concentration of 0.01 g/mL. 0.252mL of chloroplatinic acid solution is dripped into the mixed solution, and then the mixed solution is aged for 1h at room temperature and then is centrifugally washed. The mixture was then placed in an oven, dried at 120 ℃ for 12h, and cooled to room temperature. The dried catalyst obtained was placed in a tube furnace and heated from room temperature to 400 ℃ at a rate of 5 ℃/min in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 2 hours to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method.
Example 2
12g of TiO 2 Placing in a tube furnace, heating from room temperature to 400 deg.C at a heating rate of 5 deg.C/min, and reducing in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 3h to obtain a defect carrier with surface oxygen vacancies. 6g of defect carrier was dissolved in 100mL of deionized water to obtain a mixed solution and stirred for 30min, and then alkalified by dropwise addition of 0.6mL of a 10% ammonium carbonate solution. Chloroplatinic acid containing crystal water is dissolved in deionized water to prepare a chloroplatinic acid solution with the concentration of 0.01 g/mL. 0.252mL of chloroplatinic acid solution is dripped into the mixed solution, and then the mixed solution is aged for 1h at room temperature and then is centrifugally washed. The mixture was then placed in an oven, dried at 120 ℃ for 12h, and cooled to room temperature. The dried catalyst obtained was placed in a tube furnace and heated from room temperature to 450 ℃ at a rate of 5 ℃/min in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 2 hours to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method.
Example 3
12g of SnO 2 Placing in a tube furnace, heating from room temperature to 400 deg.C at a heating rate of 5 deg.C/min, and reducing in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 2h to obtain a defect carrier with surface oxygen vacancies. 6g of defect carrier was dissolved in 100mL of deionized water to obtain a mixed solution and stirred for 30min, and then alkalified by dropwise addition of 0.6mL of a 10% ammonium carbonate solution. Dissolving silver nitrate in waterIonized water to prepare 0.01g/mL silver nitrate solution. 0.252mL of silver nitrate solution is dripped into the mixed solution, and then the mixed solution is aged for 1h at room temperature and then centrifuged and washed. The mixture was then placed in an oven, dried at 120 ℃ for 12h, and cooled to room temperature. The dried catalyst obtained was placed in a tube furnace and heated from room temperature to 400 ℃ at a rate of 5 ℃/min in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 2 hours to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method.
Example 4
12g of Sb 2 O 3 Placing in a tube furnace, heating from room temperature to 400 deg.C at a heating rate of 5 deg.C/min, and reducing in a reducing atmosphere (5% H) 2 /95％N 2 ) And pretreating for 2h to obtain a defect carrier with surface oxygen vacancies. 6g of defect carrier was dissolved in 100mL of deionized water to obtain a mixed solution and stirred for 30min, and then alkalified by dropwise addition of 0.6mL of a 10% ammonium carbonate solution. Dissolving gold chloride in deionized water to prepare a gold chloride solution of 0.01 g/mL. 0.252mL of gold chloride solution was added dropwise to the above mixed solution, followed by aging at room temperature for 1 hour and centrifugal washing. The mixture was then placed in an oven, dried at 120 ℃ for 12h, and cooled to room temperature. The dried catalyst obtained was placed in a tube furnace and heated from room temperature to 400 ℃ at a rate of 5 ℃/min in a reducing atmosphere (5% H) 2 /95％N 2 ) Pretreating for 2h to obtain the ammoxidation catalyst prepared by a deposition precipitation method.
Experimental example:
the ammoxidation catalyst prepared in example 1 was pelletized and sieved (50 mesh) to prepare ammoxidation catalyst particles, which were then placed in a fixed bed gaseous reaction apparatus to conduct a catalytic activity evaluation experiment. The catalytic reactor is a quartz glass tube, the inner diameter of the quartz glass tube is 0.6cm, the solid catalyst bed layer is heated by opening a tubular resistance furnace, and the reaction temperature is controlled by a program temperature controller. The simulated smoke component is 500ppmNH 3 ,10％O 2 ,N 2 Is the balance gas. The total flow of the reaction gas is 300mL/min, and the space velocity is 100,000h -1 The reaction temperature is 150 ℃ and 400 ℃, and measuring points are arranged at intervals of 50 ℃. NH 3 Of (2) is initiatedAnd outlet concentration and NO 2 ，NO，N 2 The outlet concentration of O was analyzed on-line by fourier infrared spectroscopy. To ensure the accuracy and stability of the data, all data were recorded after the temperature point stabilized for about 30 min.
The results are shown in FIGS. 1 to 3, in which FIG. 1 shows NH of an ammoxidation catalyst prepared by a precipitation method according to the present invention 3 Oxidation test results; FIG. 2 shows N of an ammoxidation catalyst prepared by precipitation according to the present invention 2 A selective test result; FIG. 3 is an XRD pattern of an ammonia oxidation catalyst prepared by precipitation in accordance with the present invention.
As can be seen from the graphs in FIGS. 1 to 3, the ammonia oxidation catalyst prepared by the deposition precipitation method can be used for the ammonia oxidation technology of the tail gas of the diesel vehicle, has good catalytic activity, achieves the catalytic efficiency of more than 90 percent within 350 to 400 ℃, and shows relatively good N 2 And (4) selectivity.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.

Claims (5)

1. NH-containing ammonia oxidation catalyst for treating diesel vehicle emission 3 The method is characterized in that the ammonia oxidation catalyst is prepared by the following method:
(1) CeO is added 2 Placing the mixture in a tube furnace, and carrying out heat treatment for 2-4h at 400-500 ℃ in a reducing atmosphere to obtain a defect carrier with surface oxygen vacancies;
(2) dispersing the defect carrier obtained in the step (1) into deionized water to obtain a mixed solution; then adding ammonium carbonate solution for alkalization; dissolving a noble metal precursor in deionized water to prepare a precursor solution, and dripping the precursor solution into the mixed solution;
(3) aging the mixed solution prepared in the step (2) at room temperature for 1-2h, and then performing centrifugal washing; then placing the mixture in an oven to be dried continuously for 10-12h at the temperature of 100-120 ℃;
(4) and (4) placing the dried catalyst obtained in the step (3) in a tubular furnace, and carrying out heat treatment for 2-4h at the temperature of 400-500 ℃ in a reducing atmosphere to obtain the ammonia oxidation catalyst prepared by a deposition precipitation method.
2. The ammonia oxidation catalyst of claim 1 for treating diesel vehicle emissions containing NH 3 The application of the tail gas is characterized in that the noble metal precursor is one or more of chloroplatinic acid, silver nitrate and gold chloride.
3. The ammonia oxidation catalyst of claim 1 for treating diesel vehicle emissions containing NH 3 Characterized in that the reducing atmosphere is H 2 /N 2 。
4. The ammonia oxidation catalyst of claim 1 for treating diesel vehicle emissions containing NH 3 The application of the method in the tail gas is characterized in that the mass ratio of the defect carrier to the precious metal precursor is 6000: (1-6).
5. The ammonia oxidation catalyst of claim 1 for treating diesel vehicle emissions containing NH 3 The application of the tail gas is characterized in that the mass ratio of the defect carrier to ammonium carbonate is 300: (1-5).
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