CN113145129A - Low-temperature complete oxidation reaction method for carbon monoxide - Google Patents
Low-temperature complete oxidation reaction method for carbon monoxide Download PDFInfo
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 34
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 29
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 92
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910015189 FeOx Inorganic materials 0.000 claims abstract description 39
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 30
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 30
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 30
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002086 nanomaterial Substances 0.000 claims abstract description 9
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims abstract description 5
- 238000004873 anchoring Methods 0.000 claims abstract description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- 230000003647 oxidation Effects 0.000 claims description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 8
- 239000012716 precipitator Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229960005191 ferric oxide Drugs 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 235000013980 iron oxide Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 44
- 239000000243 solution Substances 0.000 description 18
- 229910052697 platinum Inorganic materials 0.000 description 16
- 229910000510 noble metal Inorganic materials 0.000 description 12
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 102000001554 Hemoglobins Human genes 0.000 description 2
- 108010054147 Hemoglobins Proteins 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 239000010970 precious metal Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 208000001408 Carbon monoxide poisoning Diseases 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 239000002803 fossil fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
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- 239000010948 rhodium Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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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
- B01J23/70—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
- B01J23/8906—Iron and noble metals
-
- 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
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
-
- 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
-
- B01J35/393—
-
- 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
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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
- B01J37/16—Reducing
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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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/502—Carbon monoxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention provides a low-temperature complete oxidation reaction method of carbon monoxide, which comprises the step of using a catalyst, wherein the catalyst is a hybrid nano-structure Pt catalyst, Pt is used as an active component of the catalyst, and FeO is used as the active component of the catalystxCoated or supported on SiO in a single or multiple layers2Above is a composite carrier, FeOxThe catalyst comprises a composite carrier, an active component Pt and a catalyst, wherein the composite carrier accounts for 5-20 wt% of the total mass of the composite carrier, and the active component Pt accounts for 0.5-2 wt% of the total mass of the catalyst; the preparation method of the catalyst comprises the steps of firstly adopting a deposition precipitation method to prepare FeOxCoated or supported on SiO2Thus obtaining the composite carrier; and then, anchoring or loading the Pt nano particles serving as the active component on the composite carrier by using an ultraviolet light and photocatalytic reduction method. The method of the invention can lead the CO to reach 100 percent conversion rate at 120 ℃. The catalyst of the invention has the advantages of simple preparation method, short production period, good catalyst dispersibility, high catalytic activity, higher stability and good industrial application prospect.
Description
Technical Field
The invention relates to the field of CO low-temperature oxidation processes and catalysts, in particular to a carbon monoxide low-temperature complete oxidation reaction method.
Background
Carbon monoxide is a toxic and harmful gas, is part of air pollution, and is increasingly used along with the development of industrialization and urbanization. Carbon monoxide is the pollutant with the highest content in the atmosphere, and causes great harm to human health and living environment. Carbon monoxide is colorless and tasteless, is not easy to be perceived after being inhaled into a human body, and is very easy to combine with hemoglobin in the human body, so that the hemoglobin loses the capability of transporting oxygen, and the nerve center of the human body is damaged, thereby causing carbon monoxide poisoning of the human body. In some processing enterprises, operators are equipped with specialized carbon monoxide respirators to eliminate or sequester carbon monoxide from the atmosphere for safety reasons. It is well known that the source of atmospheric carbon monoxide today is primarily incomplete combustion of hydrocarbon materials, the most significant of which is motor vehicle exhaust emissions, and the second is combustion of fossil fuels in boilers. After the 21 st century, the global automobile keeping quantity is increased sharply, the automobile using quantity is further increased in the coming years, and the air pollution caused by the automobile tail gas is increasingly serious.
Low temperature oxidation of CO means using O at a lower temperature2CO with lower concentration (0.5% -2%) is completely catalyzed and oxidized, and the CO low-temperature oxidation reaction can be applied to CO gas masks, carbon monoxide detectors, motor vehicle tail gas treatment and air purifiers. In addition, due to the proton fuel membrane cell H of today2The fuel source is mainly reformed, H2The trace amount of CO in the fuel will affect the electrode catalyst in the proton fuel membrane cell andthe Pt electrode has great poisoning effect, so the low-temperature oxidation reaction of CO has great application prospect in the field of CO removal in hydrogen-rich gas.
For the oxidation of CO catalyst, because noble metals have good catalytic activity at low temperature, the catalytic oxidation of CO at low temperature and low concentration mostly adopts supported noble metal type catalysts like Pt, Pd, Au, Ag, etc. Meanwhile, because the precious metal has low reserve and high price, is easy to agglomerate and deactivate in the reaction process, and because active components are easy to lose under the operating condition of high space velocity, some researchers seek cheap metal catalysts to replace the position of the precious metal in the CO catalytic oxidation reaction, such as CuO-CeO2And perovskite have been used for CO oxidation studies. In terms of catalytic performance, the low-temperature catalytic performance and catalytic effect of the cheap metal are far inferior to those of the noble metal-supported catalyst. Therefore, the noble metal loading is greatly reduced, and simultaneously, the catalytic activity and the stability of the noble metal-loaded catalyst are still the only way for the research of the noble metal catalyst.
Chinese patent CN1548368A provides a selective oxidation catalyst for carbon monoxide under hydrogen-rich conditions, which uses a small amount of noble metal to obtain higher oxidation activity and selectivity of carbon monoxide at low temperature. The catalyst is composed of a noble metal component and other metal components supported on a porous inorganic carrier. The noble metal component may be at least one of the following noble metal groups, and the other metal component may be at least one of the following other metal groups. Noble metal group: platinum, ruthenium, gold, rhodium, palladium; other metal groups: iron, titanium, zirconium, barium, tin, tungsten, zinc, molybdenum, cerium, lanthanum. The catalyst of the invention has low content of noble metal and can be effectively applied to the selective oxidation of carbon monoxide under hydrogen-rich atmosphere. The catalyst of the present invention has low initial activity temperature, wide use temperature range and effective work at 80-180 deg.c. The catalyst of the invention has oxygen selectivity as high as 80-90% in an effective working temperature range, namely, the catalyst can effectively remove carbon monoxide and simultaneously has extremely low consumption of hydrogen. In the patent, the noble metal component and other metal components of the catalyst are simultaneously impregnated or sequentially impregnated on the catalyst carrier, and the obtained catalyst has certain activity when used for catalyzing the oxidation of carbon monoxide. However, when the catalyst of the patent is used for catalyzing the oxidation of carbon monoxide, the carbon monoxide cannot achieve 100 percent conversion.
Therefore, the catalyst which has high catalytic activity, good low-temperature effect, good high-temperature stability and long service life and is used for the low-temperature complete oxidation of CO is still a challenging problem.
Disclosure of Invention
The invention aims to provide a preparation method of a composite nano catalyst suitable for CO low-temperature oxidation reaction and a corresponding carbon monoxide low-temperature complete oxidation reaction method.
Therefore, the invention provides a carbon monoxide low-temperature complete oxidation reaction method, which comprises the step of catalyzing carbon monoxide to be completely oxidized at the temperature of 100-180 ℃ by using a catalyst, wherein the catalyst is a hybrid nano-structure Pt catalyst which is marked as Pt/@ -FeOx/SiO2The catalyst takes Pt as an active component and FeOxCoated or supported on SiO in a single or multiple layers2A composite carrier in which Fe is used2O3Calculated FeOxOccupying the composite carrier FeOx/SiO25-20 wt% of the total mass, and the active component Pt accounts for 0.5-2 wt% of the total mass of the catalyst; the preparation method of the hybrid nano-structure Pt catalyst comprises the steps of firstly adopting a precipitator and a deposition precipitation method to prepare FeOxCoated or supported on SiO2Obtaining the composite carrier; and under the irradiation of ultraviolet light, anchoring or loading the active component Pt nano particles on the composite carrier by using a photocatalytic reduction method to prepare the catalyst.
In a specific embodiment, the precipitant used in the catalyst preparation method is one or more of ammonia, ammonium carbonate and sodium carbonate.
In a specific embodiment, the catalyst is pretreated and then used for completely oxidizing the carbon monoxide, wherein the pretreatment of the catalyst is carried out in inert gas with the hydrogen content of 10-50 vol%, the pretreatment temperature is 150-230 ℃, the pretreatment time is 30-120 min, and the inert gas is preferably argon.
In a specific embodiment, after the catalyst is pretreated, the pretreated catalyst is cooled to room temperature, and then the catalyst is used for catalyzing the complete oxidation of carbon monoxide.
In one embodiment, the catalyst comprises Fe2O3Calculated FeOxOccupying the composite carrier FeOx/SiO27.5-15 wt% of the total mass.
In a specific embodiment, the active component Pt accounts for 0.5-1.5 wt% of the total mass of the catalyst.
In a specific embodiment, the temperature for catalyzing the complete oxidation of the carbon monoxide is 120-150 ℃.
In a specific embodiment, the hybrid nanostructured Pt catalyst is prepared by the following steps:
step 4, cooling the solution obtained in the step 3, carrying out solid-liquid separation, washing and drying the obtained solid, roasting at 380-600 ℃, and grinding the roasted solid to obtain the composite carrier; the roasting time is more than 2 hours;
and 5, dispersing the composite carrier in deionized water, adding methanol serving as a photocatalytic reduction auxiliary agent, adding a chloroplatinic acid solution, performing ultrasonic oscillation dispersion, reacting under the irradiation of ultraviolet light, performing solid-liquid separation on the solution after reaction, washing the solid obtained by the solid-liquid separation, and drying in a vacuum drying oven at the temperature of 60-120 ℃ to obtain the hybrid nano-structure Pt catalyst.
In a specific embodiment, in the step 3, the stirring is continued for 30-120 min.
In a specific embodiment, in the step 4, the roasting temperature is 400 to 500 ℃, and the roasting time is 3 to 6 hours.
Compared with the prior art, the invention has the following advantages:
1. the catalyst disclosed by the invention is simple in preparation process and high in feasibility.
2. The catalyst has mild preparation conditions and small pollution caused by using medicaments, and accords with the green catalytic development trend.
3. The Pt/@ -FeO prepared by the method of the inventionx/SiO2Pt and FeO of catalystxAll have higher dispersibility.
4. Pt/@ -FeO prepared by the method of the inventionx/SiO2The catalyst has better CO low-temperature catalytic activity.
5. In the invention, the semiconductor metal oxide FeO is fully utilizedxThe hybrid nano-structure Pt catalyst is formed by uniformly loading Pt on a composite carrier under the irradiation of ultraviolet light.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a graph of Pt/@ -FeO values for different Pt contents prepared in examples 2, 3, 6x/SiO2The catalytic activity of the catalyst in the low-temperature CO oxidation reaction is shown.
FIG. 2 is 1% Pt/12.5% @ -FeO prepared in example 1x/SiO2XRD patterns of the catalyst and the composite carrier.
Detailed Description
The technique of the present invention will be described in detail below with reference to examples.
Example 1:
and 3, after the ultrasonic treatment is finished, placing the beaker in a water bath kettle, and raising the temperature to 60 ℃ under the magnetic stirring. When the temperature reaches 60 ℃, slowly dripping the precipitator solution prepared in the step 1, adjusting the pH to 8, covering a preservative film after completing the pH adjustment, and magnetically stirring for 1h at 60 ℃;
and 4, taking out the stirred solution, cooling at room temperature for 20min, performing suction filtration, and washing with a large amount of deionized water until the pH value is neutral. The resulting solid was dried in an oven at 80 ℃ for 10 h. Then the mixture is placed in a muffle furnace at 400 ℃ to be calcined for 3 hours, and the obtained solid particles are ground into fine powder. Is recorded as 12.5% @ -FeOx/SiO2A composite carrier;
step 5, weigh 0.4g of 12.5% @ -FeOx/SiO2Placing the composite carrier in a 500ml beaker, adding 40ml deionized water for dispersion, adding 6ml anhydrous methanol, stirring uniformly, covering with a preservative film for ultrasonic treatment for 30min, and adding 0.546ml H by a pipette after the ultrasonic treatment2PtCl6(0.0074g/ml) and continuing to perform ultrasonic treatment for 30 min. The solution after the completion of the ultrasonication was placed in a magnetic stirrer and illuminated with an ultraviolet lamp for 12 hours. After 12h, it was filtered and washed with a small amount of water. Finally, the mixture is placed in a vacuum drying oven at 80 ℃ for drying for 11 h. The resulting catalyst was reported as 1% Pt/12.5% @ -FeOx/SiO2。
Example 2:
same as example 1, except that H was added2PtCl6The amount of the solution was 1.100ml, and the mass fraction of Pt was 2 wt%, addedThe weight of ferric nitrate nonahydrate is 1.685g, FeOxIs 10% and is recorded as 2% Pt/10% FeOx/SiO2。
Example 3:
same as example 1, except that H was added2PtCl6The amount of the solution was 1.671ml, the mass fraction of Pt was 3 wt%, and the mass of ferric nitrate nonahydrate added was 1.685g, FeOxThe mass fraction of (B) is 10%, and is recorded as 3% Pt/10% FeOx/SiO2。
Example 4:
the same as example 1, except that the amount of ferric nitrate nonahydrate added was 0.803g, FeOxIs 5 wt%, and is recorded as 1% Pt/5% FeOx/SiO2。
Example 5:
the same as example 1, except that the amount of ferric nitrate nonahydrate added was 1.235g, FeOxIs 7.5 wt%, and is recorded as 1% Pt/7.5% FeOx/SiO2。
Example 6:
similar to example 1, except that 1.685g of ferric nitrate nonahydrate was added, the mass of FeOxIs 10 wt%, and is recorded as 1% Pt/10% FeOx/SiO2。
Example 7:
the same as example 1, except that the amount of ferric nitrate nonahydrate added was 2.675g in mass, FeOxIs 15 wt%, and is recorded as 1% Pt/15% FeOx/SiO2。
Example 8:
the same as example 1, except that 3.791g of ferric nitrate nonahydrate were added in mass, FeOxIs 20 wt%, and is recorded as 1% Pt/20% FeOx/SiO2。
Evaluation of catalyst Activity
In this example, different FeO's in the catalysts of the examples are consideredxThe effect of loading and different Pt loadings on the catalytic oxidation performance of CO. The catalysts prepared in examples 1-8 were used for CO oxidation. All reaction examples were carried out in a miniature fixed bed reactorFirstly, the temperature of the pretreated catalyst is reduced, and then the pretreated catalyst is switched to the reaction gas. Standard mixed reaction gas (0.998% vol CO, 1.05% volO)2And the balance gas Ar) controls the air inflow flow rate through a mass flow controller and then enters the tubular reactor. The tubular resistance furnace heats the tubular reaction tube through a programmed heating program, the temperature is controlled by a temperature control thermocouple tightly attached to the outer wall of the reactor, and the temperature inside the catalyst during the reaction is measured by a movable thermocouple. The product analysis adopts a manual sample injection mode, the tail gas of the reactor is extracted by a gas sample injection needle, and 200 mu L of sample is injected into the chromatogram for analysis. The sample gas was analyzed using an Agilent 6890N gas chromatograph equipped with a TDX-01 carbon molecular sieve packed column and Thermal Conductivity Detector (TCD), hydrogen as carrier gas.
And taking 150mg of catalyst to perform CO catalytic oxidation reaction performance test on a miniature fixed bed reactor. The space velocity of the reaction gas is 19151 ml/(g)catH). Before the reaction performance of the sample is tested, the catalyst: the silica sand was diluted 1:4 and then placed in a silica tube. Then the catalyst is firstly used with 30 vol% H2and/Ar is pretreated for 40min at the temperature of 200 ℃, then the temperature is reduced to the room temperature, and the reaction is started by switching to the standard mixed reaction gas. The activity test conditions were: the test temperature is 30-150 ℃ under normal pressure. Temperature programming control is adopted in the reaction.
Catalyst activity is expressed as percent CO conversion:
wherein
Xco: indicating the percent conversion of CO;
Aco,in: the peak area of CO before reaction;
Aco,out: refers to the peak area of CO after the reaction.
Table 1 lists the Pt/FeOx/SiO powders prepared in examples 1-82The catalytic activity of the catalyst in the low-temperature oxidation reaction of CO.
TABLE 1
As can be seen from Table 1, the catalyst was 1% Pt/12.5@ -FeOx/SiO2At 120 ℃, the CO conversion rate reaches 100 percent. As can be seen from FIG. 2, FeOxWhen the load is 10%, the load is within 1% to 3%, the CO low-temperature oxidation performance of the catalyst is rapidly reduced along with the increase of the Pt load, and the 1% Pt/10% FeOx/SiO2The catalyst exhibited 100% CO conversion at 120 ℃ while 2% Pt/10% FeOx/SiO2、3％Pt/10％FeOx/SiO2The conversion at 120 ℃ was only 55% and 32%, respectively. The content of Pt in the catalyst is increased, and the CO low-temperature conversion rate of the catalyst is reduced, which shows that the Pt in the catalyst is agglomerated and has large size, thereby being not beneficial to the low-temperature oxidation reaction of CO. When FeO is presentxWhen the load is between 7.5 and 20 percent, the CO catalyst activity of the catalyst is better, and FeO is preferredxThe loading amount is 10-12.5%. As can be seen from FIG. 2, FeO at a load of 12.5%xAnd 1% Pt, FeO is still not visible in the XRD patternxAnd peaks of Pt due to FeO in the catalystxAnd Pt has good dispersibility.
Overall, 100% conversion of CO was achieved at 120 ℃ using the process of the present invention. Compared with the traditional CO complete oxidation method, the catalyst Pt/@ -FeO of the inventionx/SiO2The preparation method is simple, the production period is short, and the obtained catalyst has good dispersibility, high catalytic activity, higher stability and good industrial application prospect.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. Low temperature of carbon monoxideThe complete oxidation reaction method comprises the step of catalyzing carbon monoxide to be completely oxidized at the temperature of 100-180 ℃ by using a catalyst, wherein the catalyst is a Pt catalyst with a hybrid nano structure and is marked as Pt/@ -FeOx/SiO2The catalyst takes Pt as an active component and FeOxCoated or supported on SiO in a single or multiple layers2A composite carrier in which Fe is used2O3Calculated FeOxOccupying the composite carrier FeOx/SiO25-20 wt% of the total mass, and the active component Pt accounts for 0.5-2 wt% of the total mass of the catalyst; the preparation method of the hybrid nano-structure Pt catalyst comprises the steps of firstly adopting a precipitator and a deposition precipitation method to prepare FeOxCoated or supported on SiO2Obtaining the composite carrier; and under the irradiation of ultraviolet light, anchoring or loading the active component Pt nano particles on the composite carrier by using a photocatalytic reduction method to prepare the catalyst.
2. The reaction method of claim 1, wherein the precipitant used in the preparation method of the catalyst is one or more of ammonia water, ammonium carbonate and sodium carbonate.
3. The reaction process according to claim 1, wherein the catalyst is pretreated before being used for the complete oxidation of the carbon monoxide, the pretreatment of the catalyst being carried out in an inert gas having a hydrogen content of 10 to 50 vol%, the pretreatment temperature being 150 ℃ to 230 ℃ and the pretreatment time being 30min to 120min, the inert gas being preferably argon.
4. The reaction process of claim 3, wherein the catalyst is pretreated, the pretreated catalyst is cooled to room temperature, and the catalyst is used for catalyzing the complete oxidation of carbon monoxide.
5. The reaction process of claim 1 wherein the catalyst comprises Fe2O3Calculated FeOxIs composed ofCarrier FeOx/SiO27.5-15 wt% of the total mass.
6. The reaction method according to claim 1, wherein the active component Pt accounts for 0.5-1.5 wt% of the total mass of the catalyst.
7. The reaction process according to any one of claims 1 to 5, wherein the temperature for catalyzing the complete oxidation of carbon monoxide is 120 to 150 ℃.
8. The reaction method according to any one of claims 1 to 5, wherein the hybrid nanostructure Pt catalyst is prepared by the following specific steps:
step 1, preparing a precipitator solution;
step 2, preparing a solution containing iron and silicon dioxide, specifically dissolving ferric nitrate or ferric chloride into deionized water, uniformly stirring to form an iron-containing solution, and then adding a proper amount of gas phase method SiO2Adding the mixture into an iron-containing solution, and uniformly stirring to obtain a solution containing iron and silicon dioxide; the steps 1 and 2 can be carried out in any sequence or simultaneously;
step 3, adding the precipitator solution prepared in the step 1 into the solution obtained in the step 2 at the temperature of 50-80 ℃ to ensure that the pH of the solution is 8-9, and then keeping the reaction temperature at 50-80 ℃ and continuously stirring for more than 30 min;
step 4, cooling the solution obtained in the step 3, carrying out solid-liquid separation, washing and drying the obtained solid, roasting at 380-600 ℃, and grinding the roasted solid to obtain the composite carrier; the roasting time is more than 2 hours;
and 5, dispersing the composite carrier in deionized water, adding methanol serving as a photocatalytic reduction auxiliary agent, adding a chloroplatinic acid solution, performing ultrasonic oscillation dispersion, reacting under the irradiation of ultraviolet light, performing solid-liquid separation on the solution after reaction, washing the solid obtained by the solid-liquid separation, and drying in a vacuum drying oven at the temperature of 60-120 ℃ to obtain the hybrid nano-structure Pt catalyst.
9. The reaction method according to claim 8, wherein the stirring is continued for 30 to 120min in the step 3.
10. The reaction method according to claim 8, wherein in the step 4, the calcination temperature is 400 to 500 ℃ and the calcination time is 3 to 6 hours.
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