CN116328765A - Multielement doped nanorod catalyst and preparation method thereof - Google Patents
Multielement doped nanorod catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 86
- 239000002073 nanorod Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
- 239000002184 metal Substances 0.000 claims abstract description 23
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 9
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 9
- 150000003624 transition metals Chemical group 0.000 claims abstract description 9
- 239000002019 doping agent Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 107
- 239000007787 solid Substances 0.000 claims description 50
- 238000001354 calcination Methods 0.000 claims description 34
- 238000001035 drying Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 14
- 229910000510 noble metal Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 101150003085 Pdcl gene Proteins 0.000 claims 1
- 239000012716 precipitator Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 88
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 35
- 238000006243 chemical reaction Methods 0.000 description 33
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 239000011521 glass Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 230000007935 neutral effect Effects 0.000 description 14
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- 239000004810 polytetrafluoroethylene Substances 0.000 description 14
- 239000012265 solid product Substances 0.000 description 14
- 229910001220 stainless steel Inorganic materials 0.000 description 14
- 239000010935 stainless steel Substances 0.000 description 14
- 238000000967 suction filtration Methods 0.000 description 14
- 239000012696 Pd precursors Substances 0.000 description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 5
- 229910002828 Pr(NO3)3·6H2O Inorganic materials 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 102000001554 Hemoglobins Human genes 0.000 description 2
- 108010054147 Hemoglobins Proteins 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000011278 co-treatment Methods 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
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- 159000000011 group IA salts Chemical group 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910002422 La(NO3)3·6H2O Inorganic materials 0.000 description 1
- 229910003205 Nd(NO3)3·6H2O Inorganic materials 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
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- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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- 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
- B01D53/864—Removing carbon monoxide or hydrocarbons
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- 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
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Abstract
The invention provides a multielement doped nano rod catalyst and a preparation method thereof, which mainly relate to the technical field of metal catalysts and comprise a carrier, a supported active metal and a doping agent; the carrier is CeO 2 The active metal loaded on the nanorod is single metal Pd or Pt, and the dopant is transition metal or rare earth metal. By using transition metal and rare earth metal, the atomic arrangement and electronic structure of the catalyst surface can be optimized, and the catalyst performance and water resistance can be improved. By using single metal Pd or Pt, the catalyst has better low-temperature oxidation performance on CO.
Description
Technical Field
The invention mainly relates to the technical field of metal catalysts, in particular to a multi-element doped nanorod catalyst and a preparation method thereof.
Background
Carbon monoxide (CO) is one of the major common toxic air pollutants, mainly derived from industrial fumes and automobile exhaust. Can be combined with human hemoglobin, weaken the oxygen supply capacity of the hemoglobin, damage the central nervous system and have great harm to human health.
CO treatment technologies currently employed in the industry include recovery and destruction technologies. Among them, catalytic oxidation is a technique with obvious effect and development prospect. The core of the CO catalytic oxidation technology is the design and preparation of a catalyst, and different noble metals (such as Pt, au, pd, ru and the like) are often used as active sites of the catalyst. However, the prior art suffers from the following disadvantages: 1) The catalyst is high in use price due to the scarcity of noble metals; 2) The catalyst has high ignition temperature and needs the assistance of a heating furnace when in use; 3) The catalyst is deactivated because water in the environment can compete with CO for adsorption on the catalyst surface. 4) In addition, part of industrial tail gas still contains trace SO after desulfurization and purification 2 (ultra-low emission standard in China requires SO) 2 ≤35mg/m 3 )，SO 2 Can inhibit catalyst activity and lead to catalytic deactivation.
Disclosure of Invention
The invention aims to provide a multielement doped nano rod catalyst and a preparation method thereof, which solve the problems of high price, high ignition temperature and competitive adsorption or trace SO with water in the environment in CO treatment in the prior art 2 Leading to the technical problems of catalytic deactivation and the like.
The invention discloses a multielement doped nano rod catalyst, which comprises a carrier, a supported active metal and a doping agent; the carrier is CeO 2 The active metal is Pd or Pt, and the dopant is transition metal and/or rare earth metal.
By using transition metal and rare earth metal, the atomic arrangement and electronic structure of the catalyst surface can be optimized, and the catalyst performance and water resistance can be improved.
By using single metal Pd or Pt, the catalyst has better low-temperature oxidation performance on CO.
Advancing oneFurther, the CeO 2 The nanorods are synthesized by a coprecipitation-hydrothermal method.
CeO synthesized by using co-precipitation-hydrothermal method 2 Nanorods, mainly exposing CeO 2 The (110) crystal face has excellent oxidation-reduction performance and excellent oxygen storage and release capacity.
Further, the transition metal is Fe, co, mn, N i, cr, V or Zr.
Further, the rare earth metal is La, pr or Nd.
Further, the supported active metal is a highly dispersed noble metal Pd or Pt atom.
Further, the mass percentage of the doped nanorod-shaped supported catalyst is 100%, wherein the content of the supported noble metal is 0.01% -0.5%.
Further, the mass percentage of the doped nano rod-shaped supported catalyst is 100%, wherein the doping content of the transition metal is 0% -2.5%, and the doping content of the rare earth metal is 0% -2.5%.
The second purpose of the invention is to protect a preparation method of the multielement doped nano rod catalyst, which comprises the following steps:
s1, preparing a precursor solution and an alkali solution;
s2, mixing and stirring the precursor solution and the alkali solution, fully ageing the mixed solution, performing hydrothermal reaction at high temperature, washing, filtering and drying the reacted catalyst overnight to obtain a solid;
s3, calcining the solid prepared in the step S2 to obtain metal doped CeO 2 A nanorod carrier;
s4, gradually dropwise adding the noble metal solution into the multi-metal doped CeO prepared in the step S3 2 The nanorod carrier reacts and is stirred uniformly; drying the reacted catalyst overnight, and calcining again to obtain the final multi-element doped CeO 2 The nanorods support a noble metal catalyst.
Further, the precursor solution preparation method is to dissolve the metal precursor and cerium nitrate solid in deionized water solution at the same time to prepare the precursor solution.
Further, the preparation method of the alkali solution comprises the steps of dissolving the solid precipitant in deionized water to prepare the alkali solution.
Further, the precipitant is an alkaline salt or a strong base.
Further, the alkaline salt is Na 2 CO 3 、K 2 CO 3 Or urea.
Further, the strong base is KOH, naOH or ammonia water.
Further, the precipitant is NaOH.
Further, the aging reaction temperature in step S2 is 25 to 60 ℃, preferably 25 ℃, and the time is 1 to 3 hours, preferably 1 hour.
Further, the hydrothermal reaction temperature in step S2 is 100 to 180 ℃, preferably 100 ℃, and the time is 6 to 48 hours, preferably 12 hours.
Further, the drying temperature in step S2 is 60 to 100 ℃, preferably 60 ℃, and the time is 12 to 24 hours, preferably 12 hours.
Further, the calcination temperature in step S3 is 300 to 600 ℃, preferably 400 ℃, and the time is 1 to 8 hours, preferably 4 hours.
Further, the reaction temperature in step S4 is 80 ℃.
Further, the catalyst calcination temperature in step S4 is 300 to 600 ℃, preferably 300 ℃, for 1 to 8 hours, preferably 2 hours.
Further, the noble metal solution in step S4 is PdC l 2 ，Pd(NO 3 ) 2 ，PtC l 2 ，Pt(NO 3 ) 2 Is configured as a precursor.
Compared with the prior art, the invention has the following beneficial effects:
1. the multi-metal doped catalyst can regulate and optimize the atomic arrangement mode and the electronic structure of the catalyst surface by controlling the metal doping amount. Even if only a small amount of noble metal Pd or Pt is supported, excellent low-temperature activity can be exhibited. At the same time, the multi-metal doping is remarkableProlonging the service life of the catalyst in the presence of water or SO 2 Service life in environment.
Drawings
FIG. 1 is a schematic illustration of a catalyst performance test apparatus according to an embodiment of the present invention;
FIG. 2 shows 0.2% Pd/2.5% Fe 2.5% Pr-CeO prepared in example 6 of the present invention 2 Transmission Electron Microscopy (TEM) and energy dispersive X-ray spectroscopy (EDX) element profiles of the nanorod catalysts, (a) scale 50nm, (b) scale 2nm, (c) scale 20 (d)
nm。
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments.
Example 1
Multi-element doped nano rod catalyst and preparation method thereof, 1.736g Ce (NO) 3 ) 3 ·6H 2 The O solid was dissolved in 10m L solution to prepare Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.001g Pd) was added to 1g CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.1% Pd/CeO 2 。
Example 2
1.736g Ce (NO) 3 ) 3 ·6H 2 The O solid was dissolved in 10m L solution to prepare Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.001g Pt) was added to 1g CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.1% Pt/CeO 2 。
Example 3
1.6926g Ce (NO) 3 ) 3 ·6H 2 O and 0.0435g Pr (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare Pr-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then Pr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Pr-CeO is obtained 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.001g Pd) was added to 1g Pr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.1% Pd/2.5% Pr-CeO 2 。
Example 4
1.6492g Ce (NO) 3 ) 3 ·6H 2 O and 0.1696g Co (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare Co-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then Co-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining Co-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.001g Pd) was added to 1g Co-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.1% Pd/5% Co-CeO 2 。
Example 5
1.6926g Ce (NO) 3 ) 3 ·6H 2 O and 0.0897g Mn (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare Mn-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then Mn-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining Mn-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.002g Pd) was added to 1g Mn-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.2% Pd/2.5% Mn-CeO 2 。
Example 6
1.6926g Ce (NO) 3 ) 3 ·6H 2 O and 0.1240g Fe (NO) 3 ) 3 ·9H 2 O solid was dissolved in 10m L solution to prepare 0.4 mol/L Fe-Ce (NO) 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then Fe-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining Fe-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.002g Pd) was added to 1g Fe-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.2% Pd/2.5% Fe-CeO 2 。
Example 7
1.6492g Ce (NO) 3 ) 3 ·6H 2 O、0.0435g Pr(NO 3 ) 3 ·6H 2 O and 0.1240g Fe (NO) 3 ) 3 ·9H 2 O solid was dissolved in 10m L solution to prepare 0.4 mol/L FePr-Ce (NO) 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then FePr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining FePr-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.002g Pd) was added to 1g FePr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; drying the reacted catalyst overnightAfter that, calcination was carried out at 300℃for 2 hours. The catalyst obtained is 0.2% Pd/2.5% Fe 2.5% Pr-CeO 2 。
Example 8
1.6492g Ce (NO) 3 ) 3 ·6H 2 O、0.0434g La(NO 3 ) 3 ·6H 2 O and 0.0848g Co (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare 0.4 mol/L CoLa-Ce (NO) 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then CoLa-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining CoLa-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.002g Pd) was added to 1g CoLa-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.2% Pd/2.5% Co 2.5% La-CeO 2 。
Example 9
1.5624g Ce (NO) 3 ) 3 ·6H 2 O、0.0872g Nd(NO 3 ) 3 ·6H 2 O and 0.1794g Mn (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare MnNd-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then MnNd-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining MnNd-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.002g Pd) was added to 1g MnNd-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.2% Pd/5% Mn 5% Md-CeO 2 。
Example 10
1.6926g Ce (NO) 3 ) 3 ·6H 2 O and 0.0435g Pr (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare Pr-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then Pr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Pr-CeO is obtained 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.005g Pd) was added to 1g Pr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.5% Pd/2.5% Pr-CeO 2 。
Example 11
1.736g Ce (NO) 3 ) 3 ·6H 2 The O solid was dissolved in 10m L solution to prepare Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 deg.C4 hours. Obtaining CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.0001g Pd) was added to 1g CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.01% Pd/CeO 2 。
Example 12
1.6492g Ce (NO) 3 ) 3 ·6H 2 O、0.0435g Pr(NO 3 ) 3 ·6H 2 O and 0.0897g Mn (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare MnPr-Ce (NO) at 0.4 mol/L 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then MnPr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining MnPr-CeO 2 A nanorod carrier. Preparation of aqueous palladium precursor solution 0.5mL (containing 0.005g Pt) was added to 1g MnPr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained was 0.5% Pt/2.5% Mn 2.5% Pr-CeO 2 。
Example 13
1.6492g Ce (NO) 3 ) 3 ·6H 2 O、0.0435g Pr(NO 3 ) 3 ·6H 2 O and 0.1240g Fe (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare 0.4 mol/L FePr-Ce (NO) 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Stainless steel reaction added to polytetrafluoroethylene autoclave linerIn the kettle, the treatment is carried out at 100 ℃ for 12h. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then FePr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining FePr-CeO 2 A nanorod carrier. Preparation of aqueous solution of palladium and platinum precursor 0.5mL (containing 0.002g Pt and 0.002g Pd) was added to 1g FePr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained is 0.2% Pt-0.2% Pd/2.5% Mn 2.5% Pr-CeO 2 。
Example 14
1.5624g Ce (NO) 3 ) 3 ·6H 2 O、0.0870g Pr(NO 3 ) 3 ·6H 2 O and 0.1696g Co (NO) 3 ) 3 ·6H 2 O solid was dissolved in 10m L solution to prepare 0.4 mol/L CoPr-Ce (NO) 3 ) 3 A solution. 19.2g of NaOH solid was dissolved in 70/m L solution to prepare 6.886 mol/L NaOH solution. The two solutions were thoroughly mixed in a heat resistant glass bottle and stirred continuously for 1h to thoroughly age the mixture. Added into a stainless steel reaction kettle with a polytetrafluoroethylene autoclave liner, and treated for 12 hours at 100 ℃. The solid product is centrifugally separated, washed to be neutral by suction filtration, and then CoPr-CeO 2 The solid was dried in an oven at 60 ℃ for 12 hours. Calcining in air at 400 ℃ for 4 hours. Obtaining CoPr-CeO 2 A nanorod carrier. Preparation of aqueous palladium and platinum precursor solution 0.5mL (containing 0.005g Pt and 0.005g Pd) was added to 1g CoPr-CeO 2 Stirring uniformly in a nano rod carrier, and continuously reacting at the reaction temperature of 80 ℃; after drying the reacted catalyst overnight, calcination was carried out at 300℃for 2 hours. The catalyst obtained is 0.5% Pt-0.5% Pd/5% Mn 5% Pr-CeO 2 。
Catalyst Performance test
The double doped Pd/CeO prepared in examples 1-12 were used separately 2 The nanorod catalyst is placed in a U-shaped reactor, and the catalytic performance of the nanorod catalyst is tested. Without pretreatment before testing, the feed gas is CO of 0.6 mL/min, oxygen of 12 mL/min, argon of 47.4 mL/min4.2 vol% water vapor, 100mg/m 3 Is tested at a space velocity of 70000h -1 . The catalyst amount was 50mg, the pressure was normal pressure, and the reaction apparatus was as shown in FIG. 1. The test results are shown in Table 1.
TABLE 1 catalyst of the invention catalyzes H 2 Catalytic combustion performance test results
Note that: t (T) 10 A temperature corresponding to 10% conversion to the target.
T 99 A temperature corresponding to 99% conversion to the target.
CO is not completely converted.
As can be seen from Table 1 above, the multi-metal doping of the present invention can significantly increase the CO oxidation activity of the catalyst at low temperatures, and prolong the catalyst in the presence of water or SO 2 The service life in the environment is prolonged, and the use cost of the catalyst is reduced.
The above is an embodiment exemplified in this example, but this example is not limited to the above-described alternative embodiments, and a person skilled in the art may obtain various other embodiments by any combination of the above-described embodiments, and any person may obtain various other embodiments in the light of this example. The above detailed description should not be construed as limiting the scope of the present embodiments, which is defined in the claims and the description may be used to interpret the claims.
Claims (10)
1. A multi-element doped nanorod catalyst, characterized in that: comprises a carrier, a supported active metal and a doping agent; the carrier is CeO 2 The active metal is Pd or Pt, and the dopant is transition metal and/or rare earth metal.
2. The multi-element doped nanorod catalyst according to claim 1, wherein the transition metal is Fe, co, mn, ni, cr, V or Zr.
3. The multi-element doped nanorod catalyst according to claim 1, wherein the rare earth metal is La, pr or Nd.
4. A multi-element doped nanorod catalyst according to claim 1, wherein: the supported active metal is a highly dispersed noble metal Pd or Pt atom.
5. A multi-element doped nanorod catalyst according to claim 1, wherein: the mass percentage of the doped nano rod-shaped supported catalyst is 100%, wherein the content of the supported noble metal is 0.01% -0.5%.
6. A multi-element doped nanorod catalyst according to claim 1, wherein: the mass percentage of the doped nano rod-shaped supported catalyst is 100%, wherein the doping content of the transition metal is 0% -2.5%, and the doping content of the rare earth metal is 0% -2.5%.
7. The method for preparing the multi-element doped nanorod catalyst according to any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
s1, preparing a precursor solution and an alkali solution;
s2, mixing and stirring the precursor solution and the alkali solution, fully ageing the mixed solution, performing hydrothermal reaction at high temperature, washing, filtering and drying the reacted catalyst overnight to obtain a solid;
s3, calcining the solid prepared in the step S2 to obtain metal doped CeO 2 A nanorod carrier;
s4, gradually dropwise adding the noble metal solution into the poly-catalyst prepared in the step S3CeO doped with metal 2 The nanorod carrier reacts and is stirred uniformly; and drying the reacted catalyst overnight, and calcining again to obtain the final multi-element doped nano rod catalyst.
8. The method for preparing the multi-element doped nanorod catalyst according to claim 7, wherein the method comprises the following steps: the preparation method of the precursor solution comprises the step of simultaneously dissolving a metal precursor and cerium nitrate solid in deionized water solution to prepare the precursor solution.
9. The method for preparing the multi-element doped nanorod catalyst according to claim 7, wherein the method comprises the following steps: the preparation method of the alkali solution comprises the steps of dissolving a precipitator solid in deionized water to prepare the alkali solution.
10. The method for preparing a multi-element doped nanorod catalyst according to claim 7, wherein the noble metal solution in the step S4 is PdCl 2 ，Pd(NO 3 ) 2 ，PtCl 2 ，Pt(NO 3 ) 2 Is configured as a precursor.
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