CN112892526A - Catalyst for eliminating tail gas pollutants of diesel vehicles and preparation method thereof - Google Patents
Catalyst for eliminating tail gas pollutants of diesel vehicles and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000003344 environmental pollutant Substances 0.000 title claims abstract description 22
- 231100000719 pollutant Toxicity 0.000 title claims abstract description 21
- 239000004793 Polystyrene Substances 0.000 claims description 36
- 229920002223 polystyrene Polymers 0.000 claims description 36
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 32
- 239000004005 microsphere Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 29
- 239000000839 emulsion Substances 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 19
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- 238000001035 drying Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 14
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 11
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- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 229910019029 PtCl4 Inorganic materials 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 2
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 2
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 26
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000779 smoke Substances 0.000 abstract description 5
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000002485 combustion reaction Methods 0.000 description 11
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- 238000006243 chemical reaction Methods 0.000 description 10
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- 239000011148 porous material Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- 238000009792 diffusion process Methods 0.000 description 3
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- 150000003624 transition metals Chemical class 0.000 description 3
- 229910002451 CoOx Inorganic materials 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
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- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
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- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
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- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
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Classifications
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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
- B01J23/40—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
- 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
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- B01J35/60—
-
- 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
Abstract
The invention relates to a catalyst for eliminating diesel vehicle tail gas pollutants and a preparation method thereof. The carbon smoke particle catalyst provided by the invention has the advantages of simple preparation method, easy operation of steps, low cost, suitability for large-scale production, high catalytic activity and good stability, and has important significance for eliminating carbon smoke particles of diesel vehicles, protecting environment and protecting human health.
Description
Technical Field
The invention relates to the technical field of catalytic combustion, in particular to a catalyst for eliminating tail gas pollutants of diesel vehicles and a preparation method thereof.
Background
Since the new century, the number of global vehicles is rapidly increasing with the rapid development of economic society and the continuous progress of human civilization. Diesel engines have become the main power source for heavy machinery such as automobiles and heavy goods vehicles due to their characteristics of high power, low oil consumption, high thermal efficiency, stable operation, etc. However, the particulate matter (mainly soot particles) in the tail gas of diesel vehicles is a major environmental pollutant, which poses serious hazards to the global ecological environment and human health.
The soot particles (Particulate materials, PM) are caused by the fact that when a diesel engine is combusted at high pressure, local temperature is too high, oxygen content is relatively small, the diesel engine is not favorable for full combustion of diesel oil, and soot particles are formed by cracking and dehydrogenation, and the diesel engine belongs to heterogeneous combustion and is determined by characteristics of heterogeneous combustion mode and heterogeneous combustion mode, so that the diesel engine cannot avoid formation of soot, the soot particles are small in size, generally 0.1-10 mu m, can be retained in the atmosphere for a long time, and are easy to adsorb toxic organic matter particles on the surface, so that once a human body inhales too many soot particles, the human body can generate heavy damage to the internal channels of the lung, and even lung cancer or other serious diseases are caused.
In the diesel exhaust gas aftertreatment technology, a catalyzed particulate filter (CDPF) obtained by attaching a catalyst to the pore channels of a particulate filter (DPF) through a substance having a high specific surface area is one of the most widely used technologies, and the development and optimization of a soot oxidation catalyst are the core of the technology.
The catalytic performance of soot combustion depends on two factors: the efficiency of the contact between the soot particles and the catalyst and the inherent activity of the catalyst. For conventional catalysts with smaller or non-porous pore sizes, it is difficult for soot particles to enter the interior of the catalyst and react only at the outer surface, and poor contact and/or limited contact of the soot particles with the catalyst active sites can limit the catalytic activity of soot combustion.
Therefore, it is very important to research a soot particle catalyst with high catalytic performance, which has a large number of active sites and high contact efficiency with soot particles.
Disclosure of Invention
Aiming at the problems, the invention provides a catalyst for eliminating tail gas pollutants of diesel vehicles and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants is characterized by comprising the following steps:
s1 synthesis of a carrier;
s2 catalyst preparation.
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) mixing 40-60 parts by weight of Al (NO)3)3·9H2Dissolving O and 30-50 parts by weight of citric acid in 90-120 parts by weight of 95 wt% ethanol, adding 15-30 parts by weight of 3mol/L ammonia water solution, stirring at the rotation speed of 600 plus 1000rpm for 6-10h, centrifuging at the rotation speed of 6000 plus 10000rpm after the completion, and drying the obtained solid in an oven at 60 ℃ for 10-15h to obtain a precursor; (2) putting the precursor obtained in the step (1) into a muffle furnace, heating to 650 ℃ at the heating rate of 2-3 ℃/min, and calcining for 3-6h at 650 ℃ to obtain the alumina carrier Al2O3；
Preparation of S2 catalyst: (a) 20 to 30 parts by weight of Al obtained in S12O3Dispersing in 80-120 parts by weight of deionized water to obtain a dispersion A, and dissolving 20-40 parts by weight of a metal salt M in 40-60 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring at the rotating speed of 800rpm of 300-60-; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 4-7h to obtain the catalyst M/Al2O3。
Further, a preparation method of the catalyst for eliminating the diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) centrifuging 80-120 parts by weight of microsphere emulsion at the rotating speed of 3000-; (2) mixing 40-60 parts by weight of Al (NO)3)3·9H2Dissolving O and 30-50 parts by weight of citric acid in 90-120 parts by weight of 95 wt% ethanol, adding 40-60 parts by weight of the template obtained in the step (1) and 15-30 parts by weight of 3mol/L ammonia water solution, stirring at the rotation speed of 600-10000 rpm for 6-10h, centrifuging at the rotation speed of 6000-10000rpm after the stirring is finished, and performing solid centrifugation at 60 DEG CDrying in an oven for 10-15h to obtain a precursor/template compound; (3) putting the precursor/template compound obtained in the step (2) into a muffle furnace, heating to 650 ℃ at the heating rate of 2-3 ℃/min, and calcining for 3-6h at 650 ℃ to obtain the three-dimensional alumina carrier 3D-Al2O3；
Preparation of S2 catalyst: (a) 20 to 30 parts by weight of 3D-Al obtained from S12O3Dispersing in 80-120 parts by weight of deionized water to obtain a dispersion A, and dissolving 20-40 parts by weight of a metal salt M in 40-60 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring at the rotating speed of 800rpm of 300-60-; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 4-7h to obtain the catalyst M/3D-Al2O3。
The microsphere emulsion is one or a mixture of more than two of polystyrene microsphere emulsion and polymethyl methacrylate microsphere emulsion.
Preferably, the microsphere emulsion is polystyrene microsphere emulsion, and the preparation method of the polystyrene microsphere emulsion comprises the following steps: firstly, under the protection of nitrogen, 15-30 parts by weight of styrene, 2-8 parts by weight of divinylbenzene, 1-5 parts by weight of potassium persulfate, 0.5-1.5 parts by weight of azodiisobutyronitrile, 3-7 parts by weight of polyvinylpyrrolidone and 160 parts by weight of isopropanol are mixed, and then the mixture is stirred and reacted for 10-15 hours at the temperature of 70-80 ℃ and the rotating speed of 1200-1600rpm, so as to obtain the polystyrene microsphere emulsion.
The metal salt M is (NH)3)4·Pt(NO3)2、PtCl4、Co(NO3)2·6H2O、Ni(NO3)2·6H2O、Cu(NO3)2·6H2O、CoCl2One or a mixture of two or more of them.
Preferably, the metal salt is PtCl4And CoCl2Mixture of (1), said PtCl4And CoCl2The mass ratio of (1): (1-3).
The invention adopts polystyrene microspheres with uniform size and definite structure as a template, loads alumina, and removes the template through high-temperature calcination to obtain the alumina carrier with the three-dimensional ordered macroporous structure. On one hand, the macroporous structure obtained by using polystyrene as a template not only allows the soot particles to directly enter the inner pores of the macroporous structure, but also allows the soot particles to be easily transferred through the macroporous structure, and has smaller diffusion resistance to contact with active sites; the contact efficiency between soot and catalyst is significantly improved compared to the disordered macroporous sample and other nanoparticle samples. On the other hand, the surface of alumina contains a large number of Lewis acid sites capable of attenuating SO2Adsorption and oxidation of (B) and suppression of sulfate formation, increasing SO of the catalyst2The tolerance, and further the stability of the catalyst is improved.
Further, the invention deposits the noble metal Pt nano particles on the 3D-Al under the action of the precipitator2O3In the framework, the transition metal Co is then introduced on the surface of the Pt nanoparticles by high-temperature calcination, and the Co exists in the form of oxide. The strong Pt-CoOx interaction increases the site density of the induced coordinated unsaturated metal cation and improves NO and O as compared to Pt or Co alone2Can promote NO and O2And oxygen species migrate from the crystal lattice to the surface.
The working principle of the catalyst prepared by the invention is as follows: Pt-Co/3D-Al2O3The active oxygen in (1) firstly reacts NO and SO2Oxidized into nitrate and bisulfate to be attached to the surface of the catalyst, the nitrate species change to generate nitrite after the temperature rises, and NO is released to the gas phase2，NO2Reacts with soot particles to produce CO2To realize the oxidation of soot particles; and the bisulfate as an activity inhibitor is in 3D-Al2O3Is decomposed under the action of the Lewis acid sites.
The invention has the advantages that:
1. the invention uses the template method to prepare the polystyrene microspheres with the three-dimensional ordered macroporous structure, thereby not only reducing the diffusion resistance of the carbon smoke particles, but also increasing the number of active sites and improving the contact efficiency between the carbon smoke particles and the catalyst.
2. The invention compounds alumina on the polystyrene microsphere, can provide a large amount of Lewis acid sites, and further improves the SO of the catalyst2The tolerance is improved, and the stability of the catalyst is improved.
3. According to the invention, the noble metal and the transition metal are simultaneously introduced onto the carrier, so that on one hand, the raw material cost of the catalyst is effectively reduced, and on the other hand, the catalytic activity of the catalyst can be effectively improved through the synergistic effect between the noble metal and the transition metal.
4. The preparation method is simple, the steps are easy to operate, the cost is low, and the preparation method is suitable for large-scale production. In addition, the catalyst prepared by the method has important significance for eliminating soot particles of diesel vehicles, protecting environment and protecting human health.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Polyvinylpyrrolidone, CAS No.: 9003-39-8, molecular weight: 40000, available from Bo ai New York medical science and technology group, Inc.
γ-Al2O3CAS number: 1344-28-1, type: ZTL-HAO, available from New materials, Inc. of Zhongtianli, Yangzhou.
Carbon black, degussa black U carbon, available from chang xu specialty carbon black limited.
Example 1
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) 50 parts by weight of Al(NO3)3·9H2Dissolving O and 40 parts by weight of citric acid in 100 parts by weight of 95 wt% ethanol, adding 20 parts by weight of 3mol/L ammonia water solution, stirring at 800rpm for 8 hours, centrifuging at 8000rpm, and drying the obtained solid in an oven at 60 ℃ for 12 hours to obtain a precursor; (2) putting the precursor obtained in the step (1) into a muffle furnace, heating to 650 ℃ at the heating rate of 2 ℃/min, and calcining for 4h at 650 ℃ to obtain the alumina carrier Al2O3；
Preparation of S2 catalyst: (a) 25 parts by weight of Al obtained in S12O3Dispersing in 100 parts by weight of deionized water to give a dispersion A, and adding 30 parts by weight of PtCl4Dissolving in 50 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring for 2 hours at the rotating speed of 500rpm, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5 hours, after the reaction is finished, centrifuging at the rotating speed of 8000rpm, washing the solid with deionized water for three times, and drying in an oven at the temperature of 60 ℃ for 12 hours to obtain a sample; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 5 hours to obtain the catalyst Pt/Al2O3。
Example 2
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) centrifuging 100 parts by weight of polystyrene microsphere emulsion at the rotating speed of 5000rpm for 4h, pouring out supernatant, and drying at 80 ℃ for 24h to obtain a polystyrene template; (2) placing the polystyrene template obtained in the step (1) in a muffle furnace, heating to 650 ℃ at a heating rate of 2 ℃/min, and calcining for 4h at 650 ℃ to obtain a polystyrene carrier;
preparation of S2 catalyst: (a) 25 parts by weight of the polystyrene carrier obtained in S1 was dispersed in 100 parts by weight of deionized water to obtain dispersion A, and 30 parts by weight of PtCl was added4Dissolving in 50 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion A, stirring at 500rpm for 2h, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5h, centrifuging at 8000rpm after the reaction is finished, and washing the solid with deionized water for three timesThen drying the sample in a 60 ℃ oven for 12 hours to obtain a sample; (c) and (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 5 hours to obtain the catalyst Pt/polystyrene.
The preparation method of the polystyrene microsphere emulsion comprises the following steps: firstly, 20 parts by weight of styrene, 5 parts by weight of divinylbenzene, 3 parts by weight of potassium persulfate, 1 part by weight of azobisisobutyronitrile, 5 parts by weight of polyvinylpyrrolidone and 150 parts by weight of isopropanol were mixed under the protection of nitrogen, and then stirred at a temperature of 75 ℃ and a rotation speed of 1500rpm for 12 hours to obtain polystyrene microsphere emulsion.
Example 3
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) centrifuging 100 parts by weight of polystyrene microsphere emulsion at the rotating speed of 5000rpm for 4h, pouring out supernatant, and drying at 80 ℃ for 24h to obtain a polystyrene template; (2) 50 parts by weight of Al (NO)3)3·9H2Dissolving O and 40 parts by weight of citric acid in 100 parts by weight of 95 wt% ethanol, adding 50 parts by weight of the polystyrene template obtained in the step (1) and 20 parts by weight of 3mol/L ammonia water solution, stirring at 800rpm for 8 hours, centrifuging at 8000rpm after the stirring is finished, and drying the obtained solid in an oven at 60 ℃ for 12 hours to obtain a precursor/template compound; (3) putting the precursor/template compound obtained in the step (2) into a muffle furnace, heating to 650 ℃ at the heating rate of 2 ℃/min, and calcining for 4h at 650 ℃ to obtain the three-dimensional alumina carrier 3D-Al2O3；
Preparation of S2 catalyst: (a) 25 parts by weight of 3D-Al obtained in S12O3Dispersing in 100 parts by weight of deionized water to give a dispersion A, and adding 30 parts by weight of PtCl4Dissolving in 50 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring for 2 hours at the rotating speed of 500rpm, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5 hours, after the reaction is finished, centrifuging at the rotating speed of 8000rpm, washing the solid with deionized water for three times, and drying in an oven at the temperature of 60 ℃ for 12 hours to obtain a sample; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 5 hours to obtain the catalystPt/3D-Al2O3。
The preparation method of the polystyrene microsphere emulsion comprises the following steps: firstly, 20 parts by weight of styrene, 5 parts by weight of divinylbenzene, 3 parts by weight of potassium persulfate, 1 part by weight of azobisisobutyronitrile, 5 parts by weight of polyvinylpyrrolidone and 150 parts by weight of isopropanol are mixed under the protection of nitrogen, and then stirred and reacted at the temperature of 75 ℃ for 12 hours at the rotating speed of 1500rpm to obtain the polystyrene microsphere emulsion.
Comparative example
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
(1)25 parts by weight of gamma-Al2O3Dispersing in 100 parts by weight of deionized water to give a dispersion A, and adding 30 parts by weight of PtCl4Dissolving in 50 parts by weight of deionized water to obtain a solution B; (2) adding the solution B into the dispersion liquid A, stirring for 2 hours at the rotating speed of 500rpm, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5 hours, after the reaction is finished, centrifuging at the rotating speed of 8000rpm, washing the solid with deionized water for three times, and drying in an oven at the temperature of 60 ℃ for 12 hours to obtain a sample; (3) calcining the sample obtained in the step (2) at 550 ℃ for 5 hours to obtain the catalyst Pt/gamma-Al2O3。
Example 4
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) centrifuging 100 parts by weight of polystyrene microsphere emulsion at the rotating speed of 5000rpm for 4h, pouring out supernatant, and drying at 80 ℃ for 24h to obtain a polystyrene template; (2) 50 parts by weight of Al (NO)3)3·9H2Dissolving O and 40 parts by weight of citric acid in 100 parts by weight of 95 wt% ethanol, adding 50 parts by weight of the polystyrene template obtained in the step (1) and 20 parts by weight of 3mol/L ammonia water solution, stirring at 800rpm for 8 hours, centrifuging at 8000rpm after the stirring is finished, and drying the obtained solid in an oven at 60 ℃ for 12 hours to obtain a precursor/template compound; (3) putting the precursor/template compound obtained in the step (2) into a muffle furnace, heating to 650 ℃ at a heating rate of 2 ℃/min, and calcining for 4h at 650 DEG CObtaining the three-dimensional alumina carrier 3D-Al2O3；
Preparation of S2 catalyst: (a) 25 parts by weight of 3D-Al obtained in S12O3Dispersing in 100 parts by weight of deionized water to give a dispersion A, and adding 30 parts by weight of CoCl2Dissolving in 50 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring for 2 hours at the rotating speed of 500rpm, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5 hours, after the reaction is finished, centrifuging at the rotating speed of 8000rpm, washing the solid with deionized water for three times, and drying in an oven at the temperature of 60 ℃ for 12 hours to obtain a sample; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 5 hours to obtain the catalyst Co/3D-Al2O3。
The preparation method of the polystyrene microsphere emulsion comprises the following steps: firstly, 20 parts by weight of styrene, 5 parts by weight of divinylbenzene, 3 parts by weight of potassium persulfate, 1 part by weight of azobisisobutyronitrile, 5 parts by weight of polyvinylpyrrolidone and 150 parts by weight of isopropanol are mixed under the protection of nitrogen, and then stirred and reacted at the temperature of 75 ℃ for 12 hours at the rotating speed of 1500rpm to obtain the polystyrene microsphere emulsion.
Example 5
A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants comprises the following steps:
s1 carrier synthesis: (1) centrifuging 100 parts by weight of polystyrene microsphere emulsion at the rotating speed of 5000rpm for 4h, pouring out supernatant, and drying at 80 ℃ for 24h to obtain a polystyrene template; (2) 50 parts by weight of Al (NO)3)3·9H2Dissolving O and 40 parts by weight of citric acid in 100 parts by weight of 95 wt% ethanol, adding 50 parts by weight of the polystyrene template obtained in the step (1) and 20 parts by weight of 3mol/L ammonia water solution, stirring at 800rpm for 8 hours, centrifuging at 8000rpm after the stirring is finished, and drying the obtained solid in an oven at 60 ℃ for 12 hours to obtain a precursor/template compound; (3) putting the precursor/template compound obtained in the step (2) into a muffle furnace, heating to 650 ℃ at the heating rate of 2 ℃/min, and calcining for 4h at 650 ℃ to obtain the three-dimensional alumina carrier 3D-Al2O3；
S2 catalysisPreparation of the agent: (a) 25 parts by weight of 3D-Al obtained in S12O3Dispersed in 100 parts by weight of deionized water to obtain a dispersion A, and 30 parts by weight of a metal salt (10 parts by weight of PtCl)4And 20 parts by weight of CoCl2) Dissolving in 50 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring for 2 hours at the rotating speed of 500rpm, adding 50 parts by weight of 0.1mol/L NaOH aqueous solution, continuing stirring for 5 hours, after the reaction is finished, centrifuging at the rotating speed of 8000rpm, washing the solid with deionized water for three times, and drying in an oven at the temperature of 60 ℃ for 12 hours to obtain a sample; (c) calcining the sample obtained in the step (b) at the high temperature of 650 ℃ for 5 hours to obtain the catalyst Pt-Co/3D-Al2O3。
The preparation method of the polystyrene microsphere emulsion comprises the following steps: firstly, 20 parts by weight of styrene, 5 parts by weight of divinylbenzene, 3 parts by weight of potassium persulfate, 1 part by weight of azobisisobutyronitrile, 5 parts by weight of polyvinylpyrrolidone and 150 parts by weight of isopropanol are mixed under the protection of nitrogen, and then stirred and reacted at the temperature of 75 ℃ for 12 hours at the rotating speed of 1500rpm to obtain the polystyrene microsphere emulsion.
Test example 1
Evaluation of catalytic performance: the specific test method refers to the Master thesis "Low temperature Activity and Sulfur resistance Performance research of non-noble Metal CDPF catalyst for catalytic Oxidation of soot 2.4CDPF catalyst Performance evaluation experiment
Weighing 45mg of catalyst and 5mg of standard carbon black, placing the catalyst and the standard carbon black in an agate mortar, fully stirring for 10 minutes, then placing the catalyst and the standard carbon black in a sample bottle, fully shaking and mixing for 10 minutes to simulate the loose contact state of the catalyst and the carbon black, then placing the catalyst and the carbon black in a constant temperature area of a quartz reaction tube with the inner diameter of 10mm, and fixing two ends of the quartz reaction tube by quartz cotton. And (3) testing conditions are as follows: gas composition: 6.5% O2800ppm NO, the remainder being N2Gas flow 200 mL/min-1Then the system is set at 2 ℃ min-1The rate of temperature rise was increased to 650 ℃ and CO was recorded2And the formation of CO. The catalytic activity of the catalyst prepared in the example of the present invention is expressed by the combustion temperature (T) of soot particles. The lower the temperature value, the higher the catalytic activity, passing through T10，T50，T90Evaluation of (A)Estimation of the catalytic Activity, where T10，T50And T90The values of (d) are defined as the temperature points for 10%, 50% and 90% soot conversion, respectively.
TABLE 1 results of catalyst Performance testing
| T10/℃ | T50/℃ | T90/℃ | |
| Example 1 | 343 | 435 | 495 |
| Example 2 | 392 | 494 | 563 |
| Example 3 | 307 | 392 | 436 |
| Comparative example | 356 | 450 | 514 |
| Example 4 | 319 | 408 | 462 |
| Example 5 | 278 | 356 | 416 |
As can be seen from examples 3-5, when Pt and Co were introduced simultaneously on the support, strong Pt-CoOx interaction induced Pt2+And Pt4+Formation of Pt on the surface of the support2+And Pt4+Increased density, promoting the formation of active site-oxygen vacancy, and enhancing NO and O2The active sites of the activation character adsorb and activate oxygen atoms, further accelerating the migration rate of oxygen atoms from the lattice to the surface, thereby lowering the combustion temperature of the soot particles.
Test example 2
Evaluation of catalyst stability: collecting the catalyst used in the catalytic reaction, then weighing 45mg of catalyst and 5mg of standard carbon black, placing the catalyst and the standard carbon black in an agate mortar, fully stirring the catalyst for 10 minutes by using a medicine spoon, then placing the catalyst and the standard carbon black in a sample bottle, fully and uniformly shaking the mixture for 10 minutes to simulate the loose contact state of the catalyst and the soot, then placing the catalyst and the soot in a constant temperature area of a quartz reaction tube with the inner diameter of 10mm, and fixing two ends by using quartz cotton. And (3) testing conditions are as follows: gas composition: 6.5% O2800ppm NO, the remainder being N2Gas flow 200 mL/min-1Then the system is set at 2 ℃ min-1The rate of temperature rise was increased to 650 ℃ and CO was recorded2And the formation of CO, using a combination of [ CO ]2]outIndicating CO in the combustion process2In the amount of [ CO ]]outIndicating the amount of CO produced during combustion. CO for catalyst stabilization2Selectivity (S)CO2) To represent; CO 22Selectivity (S)CO2) Is calculated in the following manner：
Table 2 catalyst stability test results
As can be seen from examples 1-3 and comparative examples, the catalyst carrier with the three-dimensional ordered macroporous structure prepared by using the soft template method can not only reduce the combustion temperature of soot particles, but also effectively improve the stability of the catalyst. This may be due to the following reasons: on one hand, the macroporous structure obtained by using polystyrene as a template not only allows the soot particles to directly enter the inner pores of the macroporous structure, but also allows the soot particles to be easily transferred through the macroporous structure, and has smaller diffusion resistance to contact with active sites; with commercial gamma-Al2O3Compared with a sample, the contact efficiency between the carbon smoke particles and the catalyst is obviously improved; on the other hand, the surface of alumina contains a large number of Lewis acid sites capable of attenuating SO2Adsorption and oxidation of (B) and suppression of sulfate formation, increasing SO of the catalyst2The tolerance, and further the stability of the catalyst is improved.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (8)
1. A preparation method of a catalyst for eliminating diesel vehicle tail gas pollutants is characterized by comprising the following steps:
s1 synthesis of a carrier;
s2 catalyst preparation.
2. The method for preparing a catalyst for eliminating pollutants from the exhaust gas of a diesel vehicle as claimed in claim 1, comprising the steps of:
s1 carrier synthesis: (1) mixing 40-60 parts by weight of Al (NO)3)3·9H2Dissolving O and 30-50 parts by weight of citric acid in 90-120 parts by weight of 95 wt% ethanol, adding 15-30 parts by weight of 3mol/L ammonia water solution, stirring at the rotation speed of 600 plus 1000rpm for 6-10h, centrifuging at the rotation speed of 6000 plus 10000rpm after the completion, and drying the obtained solid in an oven at 60 ℃ for 10-15h to obtain a precursor; (2) putting the precursor obtained in the step (1) into a muffle furnace, heating to 650 ℃ at the heating rate of 2-3 ℃/min, and calcining for 3-6h at 650 ℃ to obtain the alumina carrier Al2O3；
Preparation of S2 catalyst: (1) 20 to 30 parts by weight of Al obtained in S12O3Dispersing in 80-120 parts by weight of deionized water to obtain a dispersion A, and dissolving 20-40 parts by weight of a metal salt M in 40-60 parts by weight of deionized water to obtain a solution B; (2) adding the solution B into the dispersion liquid A, stirring at the rotating speed of 800rpm of 300-60-; (3) calcining the sample obtained in the step (2) at 650 ℃ for 4-7h to obtain M/Al2O3。
3. The method for preparing a catalyst for removing pollutants from the exhaust gas of a diesel vehicle as claimed in claim 2, comprising the steps of:
s1 carrier synthesis: (1) centrifuging 80-120 parts by weight of microsphere emulsion at the rotating speed of 3000-; (2) mixing 40-60 parts by weight of Al (NO)3)3·9H2Dissolving O and 30-50 parts by weight of citric acid in 90-120 parts by weight of 95 wt% ethanol, and then adding 40-60 parts by weight of the template obtained in the step (1) and 15-30 parts by weight of 3mol/L ammonia waterStirring the solution at the rotation speed of 600-1000rpm for 6-10h, centrifuging at the rotation speed of 6000-10000rpm after the solution is finished, and drying the obtained solid in an oven at 60 ℃ for 10-15h to obtain a precursor/template compound; (3) putting the precursor/template compound obtained in the step (2) into a muffle furnace, heating to 650 ℃ at the heating rate of 2-3 ℃/min, and calcining for 3-6h at 650 ℃ to obtain the three-dimensional alumina carrier 3D-Al2O3；
Preparation of S2 catalyst: (a) 20 to 30 parts by weight of 3D-Al obtained from S12O3Dispersing in 80-120 parts by weight of deionized water to obtain a dispersion A, and dissolving 20-40 parts by weight of a metal salt M in 40-60 parts by weight of deionized water to obtain a solution B; (b) adding the solution B into the dispersion liquid A, stirring at the rotating speed of 800rpm of 300-60-; (c) calcining the sample obtained in the step (b) at 650 ℃ for 4-7h to obtain M/3D-Al2O3。
4. The method of claim 3, wherein the microsphere emulsion is one or a mixture of more than two of polystyrene microsphere emulsion and polymethyl methacrylate microsphere emulsion.
5. The method for preparing a catalyst for eliminating pollutants from the exhaust gas of diesel vehicles according to claim 4, wherein the microsphere emulsion is polystyrene microsphere emulsion.
6. The method for preparing a catalyst for eliminating pollutants from the exhaust gas of diesel vehicles according to claim 5, wherein the polystyrene microsphere emulsion is prepared by the following steps: firstly, under the protection of nitrogen, 15-30 parts by weight of styrene, 2-8 parts by weight of divinylbenzene, 1-5 parts by weight of potassium persulfate, 0.5-1.5 parts by weight of azodiisobutyronitrile, 3-7 parts by weight of polyvinylpyrrolidone and 160 parts by weight of isopropanol are mixed, and then the mixture is stirred and reacted for 10-15 hours at the temperature of 70-80 ℃ and the rotating speed of 1200-1600rpm, so as to obtain the polystyrene microsphere emulsion.
7. The method for preparing a catalyst for removing pollutants from the exhaust gas of diesel vehicles as claimed in claim 2 or 3, wherein the metal salt M is (NH)3)4·Pt(NO3)2、PtCl4、Co(NO3)2·6H2O、Ni(NO3)2·6H2O、Cu(NO3)2·6H2O、CoCl2One or a mixture of two or more of them.
8. A catalyst for eliminating pollutants from the exhaust gas of diesel vehicles, which is prepared by the method of any one of claims 1 to 7.
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| CN114904526B (en) * | 2022-06-13 | 2023-11-14 | 湖北拓扑来微科技有限公司 | Self-buffering system Co-MOOH@M x O y Preparation method and application of integral material |
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