CN113649019A - Catalytic material for automobile exhaust treatment and preparation method thereof - Google Patents
Catalytic material for automobile exhaust treatment and preparation method thereof Download PDFInfo
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- CN113649019A CN113649019A CN202111010191.6A CN202111010191A CN113649019A CN 113649019 A CN113649019 A CN 113649019A CN 202111010191 A CN202111010191 A CN 202111010191A CN 113649019 A CN113649019 A CN 113649019A
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- automobile exhaust
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910003122 ZnTiO3 Inorganic materials 0.000 claims abstract description 14
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000002121 nanofiber Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000004729 solvothermal method Methods 0.000 claims abstract description 8
- 229910018864 CoMoO4 Inorganic materials 0.000 claims abstract description 7
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 7
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 7
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 5
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 5
- 239000012046 mixed solvent Substances 0.000 claims abstract description 5
- 239000001509 sodium citrate Substances 0.000 claims abstract description 5
- 238000009987 spinning Methods 0.000 claims abstract description 5
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 5
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 description 17
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical group 0.000 description 1
- 150000001341 alkaline earth metal compounds Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
- B01J23/76—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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The application discloses an automobile exhaust treatment catalytic material, which is prepared by the following method: adding zinc nitrate and tetrabutyl titanate into a mixed solvent of DMF/ethanol, then adding PVP and ammonium bicarbonate, stirring and mixing uniformly, and carrying out electrostatic spinning by taking the mixture as spinning solution to form PVP-ZnTiO3Then heat treatment is carried out in air at 350-450 ℃ to obtain hollow porous ZnTiO3A nanofiber; dissolving sodium molybdate and cobalt nitrate into mixed solution of ethanol and glycerol, adding trisodium citrate, and mixing hollow porous ZnTiO3Placing the nano-fiber in the mixed solution, carrying out solvothermal reaction at the temperature of 180 ℃ plus 200 ℃, and then carrying out heat treatment at the temperature of 300 ℃ plus 400 ℃ to obtain a hollow fiberPorous ZnTiO3‑CoMoO4。
Description
Technical Field
The application relates to the technical field of environmental protection, in particular to a composite material for efficiently catalyzing nitrogen oxides in automobile exhaust and a preparation method thereof.
Background
With the rapid development of society, the number of global motor vehicles is increasing continuously, and the pollutants of automobile exhaust become one of the main sources of urban air pollution, which not only seriously threatens human health, but also has huge damage to the environment. Therefore, countries have developed more and more stringent automobile exhaust emission regulations to limit the emission of pollutants in automobile exhaust. Currently, one of the effective methods for treating nitrogen oxides in automobile exhaust is catalytic reduction (SCR), and the most core part of the SCR system is catalyst, the performance of which directly determines the exhaust removal efficiency, and the cost of which usually accounts for 30% -50% of the total price of the denitration device.
CN106268793A discloses an automobile exhaust purification catalyst and a preparation method thereof, in particular to a catalyst with NOxAn automobile exhaust purification catalyst with storage-reduction function and a preparation method thereof. The catalyst comprises a bentonite support and at least one precious metal active component selected from the group consisting of Pt, Pd and Rh loaded on the support. The content of the noble metal is 0.01-1.0 wt% of the total weight of the catalyst. The catalyst may further contain at least one transition metal selected from the group consisting of Ti, Mn, Fe, Co, Ni, Cu, Zn, Zr as an auxiliary active ingredient, the content of the transition metal being 0 to 5 wt% based on the total weight of the catalyst. The bentonite may be modified with alkali metal and/or alkaline earth metal compounds. However, the catalyst contains noble metals, and is high in price, so that the practical application of the catalyst is directly limited.
CN101972661A discloses a sulfur-resistant nitrogen oxide-removing composite metal oxide SCR catalyst, and preparation and application thereof. The catalyst comprises a structural auxiliary element M, a chromium element and a manganese element with the molar ratio of 0.2-2: 2-4: 5-8. The preparation method comprises the following steps: (1) respectively dissolving the metal precursors in citric acid, uniformly stirring, standing for 1-5 hours to respectively obtain an M metal citric acid solution, a chromium metal citric acid solution and a manganese metal citric acid solution; (2) uniformly dripping each metal citric acid solution into the container at the same time, continuously stirring, and continuously stirring for 0.5-3 hours after dripping is finished; (3) drying the mixture in an oven at 90-150 ℃ for 8-15 hours, and calcining the dried mixture in a muffle furnace for 100-350 minutes; (4) and tabletting the calcined product, grinding and sieving. However, the catalyst is easily agglomerated, resulting in a low specific surface area and severely reducing its catalytic activity.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide a composite SCR catalyst with high specific surface area and high adsorption performance, and the composite SCR catalyst still has high removal rate of nitrogen oxides under low temperature.
The catalytic material for treating the automobile exhaust is characterized by being prepared by the following method:
adding zinc nitrate and tetrabutyl titanate into a mixed solvent of DMF/ethanol, then adding PVP and ammonium bicarbonate, stirring and mixing uniformly, and carrying out electrostatic spinning by taking the mixture as spinning solution to form PVP-ZnTiO3Then heat treatment is carried out in air at 350-450 ℃ to obtain hollow porous ZnTiO3A nanofiber;
dissolving sodium molybdate and cobalt nitrate into mixed solution of ethanol and glycerol, adding trisodium citrate, and mixing hollow porous ZnTiO3Placing the nano-fiber in the mixed solution, carrying out solvothermal reaction at the temperature of 180-3-CoMoO4。
Preferably, the molar ratio of zinc nitrate to tetrabutyl titanate is 1: (1-1.3);
preferably, the volume ratio of DMF/ethanol is 1: (0.5-1);
preferably, the molar ratio of the sodium molybdate to the cobalt nitrate is 1: 1;
preferably, the solvothermal reaction time is 12-23 h;
preferably, the electrostatic spinning process parameters are as follows: the flow rate is 0.1-0.2 mm/min, the voltage is 15-25 kV, and the receiving distance is 10-20 cm.
Has the advantages that:
formation of PVP-ZnTiO by electrospinning3In the heat treatment process, PVP is taken as a template and is removed through heat treatment to form a hollow tubular structure, ammonium bicarbonate forms a plurality of gases in the high-temperature heat treatment process to escape from the fibers, so that a large number of pore structures are formed on the hollow tubular structure, and ZnTiO with high specific surface area is finally obtained3Nanofibers having excellent physical adsorptivity for contaminating source gases; using a solvothermal method as a carrier to load CoMoO4Greatly improve the CoMoO4The dispersibility and the denitration catalytic efficiency are synergistically improved, and the denitration catalytic efficiency can be used for removing nitric oxides in automobile exhaust.
Detailed Description
Example 1
Adding 5mmol of nitreAdding 3ml of zinc and 5mmol of tetrabutyl titanate, wherein the volume ratio is 1: 0.5 DMF/ethanol mixed solvent, then 8mg PVP and 3mg ammonium bicarbonate are added, stirred for 3 hours and uniformly mixed, and the mixture is taken as spinning solution to carry out electrostatic spinning to form PVP-ZnTiO3The technological parameters of electrostatic spinning are as follows: the flow rate is 0.1mm/min, the voltage is 15kV, and the receiving distance is 10 cm; then heat treatment is carried out for 1h at 350 ℃ in the air to obtain hollow porous ZnTiO3A nanofiber;
dissolving 2mmol of sodium molybdate and 2mmol of cobalt nitrate in 20ml of mixed solution of ethanol and glycerol with the volume ratio of 1:1, adding 4mmol of trisodium citrate, and mixing the hollow porous ZnTiO3Placing the nano-fiber in the mixed solution, carrying out solvothermal reaction at 180 ℃, and then carrying out heat treatment at 300 ℃ for 1h to obtain hollow porous ZnTiO3-CoMoO4。
Comparative example 1
Adding 5mmol of zinc nitrate and 5mmol of tetrabutyl titanate into 3ml of the solution, wherein the volume ratio is 1: 0.5 DMF/ethanol mixed solvent, then 8mg PVP and 3mg ammonium bicarbonate are added, stirred for 3 hours and uniformly mixed, and the mixture is taken as spinning solution to carry out electrostatic spinning to form PVP-ZnTiO3The technological parameters of electrostatic spinning are as follows: the flow rate is 0.1mm/min, the voltage is 15kV, and the receiving distance is 10 cm; then heat treatment is carried out for 1h at 350 ℃ in the air to obtain hollow porous ZnTiO3And (3) nano fibers.
Comparative example 2
Dissolving 2mmol of sodium molybdate and 2mmol of cobalt nitrate in 20ml of mixed solution of ethanol and glycerol in a volume ratio of 1:1, adding 4mmol of trisodium citrate, carrying out solvothermal reaction at 180 ℃, and then carrying out heat treatment at 300 ℃ for 1h to obtain CoMoO4。
Using 1g each of the catalysts of example 1 and comparative examples 1 to 2, the mixture was reacted in a reactor with a reaction gas composition ratio of NO500ppm, O210％，N2The reaction space velocity is 3000h for equilibrium gas-1The NO conversion effect of each catalyst was measured at different temperatures, and the results are shown in Table 1.
TABLE 1
| Example 1 | Comparative example 1 | Comparative example 2 | |
| 130℃ | 80.4％ | 69.8％ | 50.1％ |
| 180℃ | 89.1％ | 71.4％ | 65.6％ |
| 250℃ | 100％ | 85.1％ | 70.1％ |
| 300℃ | 100％ | 88.7％ | 78.1％ |
| 350℃ | 100％ | 90.4％ | 80.1％ |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims.
Claims (6)
1. The catalytic material for treating the automobile exhaust is characterized by being prepared by the following method:
adding zinc nitrate and tetrabutyl titanate into a mixed solvent of DMF/ethanol, then adding PVP and ammonium bicarbonate, stirring and mixing uniformly, and carrying out electrostatic spinning by taking the mixture as spinning solution to form PVP-ZnTiO3Then heat treatment is carried out in air at 350-450 ℃ to obtain hollow porous ZnTiO3A nanofiber;
dissolving sodium molybdate and cobalt nitrate into mixed solution of ethanol and glycerol, adding trisodium citrate, and mixing hollow porous ZnTiO3Placing the nano-fiber in the mixed solution, carrying out solvothermal reaction at the temperature of 180-3-CoMoO4。
2. The catalytic material for treating automobile exhaust according to claim 1, wherein the molar ratio of zinc nitrate to tetrabutyl titanate is 1: (1-1.3).
3. The catalytic material for treating automobile exhaust according to claim 1, wherein the volume ratio of DMF/ethanol is 1: (0.5-1).
4. The catalytic material for treating automobile exhaust according to claim 1, wherein the molar ratio of the sodium molybdate to the cobalt nitrate is 1: 1.
5. The catalytic material for treating the automobile exhaust according to the claims 1-2, wherein the solvothermal reaction time is 12-23 h.
6. The automobile exhaust treatment catalytic material according to claims 1-5, wherein the electrostatic spinning process parameters are as follows: the flow rate is 0.1-0.2 mm/min, the voltage is 15-25 kV, and the receiving distance is 10-20 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111010191.6A CN113649019A (en) | 2021-08-31 | 2021-08-31 | Catalytic material for automobile exhaust treatment and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111010191.6A CN113649019A (en) | 2021-08-31 | 2021-08-31 | Catalytic material for automobile exhaust treatment and preparation method thereof |
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| Publication Number | Publication Date |
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| CN113649019A true CN113649019A (en) | 2021-11-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202111010191.6A Withdrawn CN113649019A (en) | 2021-08-31 | 2021-08-31 | Catalytic material for automobile exhaust treatment and preparation method thereof |
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| CN (1) | CN113649019A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114106620A (en) * | 2021-12-13 | 2022-03-01 | 商河县天域工程技术中心 | Air purification environment-friendly coating |
| CN114160154A (en) * | 2021-12-13 | 2022-03-11 | 衡水市高新区博元新能源技术研发中心 | Catalyst for treating motor vehicle tail gas |
-
2021
- 2021-08-31 CN CN202111010191.6A patent/CN113649019A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114106620A (en) * | 2021-12-13 | 2022-03-01 | 商河县天域工程技术中心 | Air purification environment-friendly coating |
| CN114160154A (en) * | 2021-12-13 | 2022-03-11 | 衡水市高新区博元新能源技术研发中心 | Catalyst for treating motor vehicle tail gas |
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Application publication date: 20211116 |