CN114405504A - Low-load noble metal catalyst and preparation method and application thereof - Google Patents
Low-load noble metal catalyst and preparation method and application thereof Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 113
- 239000003054 catalyst Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 25
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 111
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 34
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 34
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 238000011068 loading method Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 62
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000011734 sodium Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 31
- 229910052697 platinum Inorganic materials 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 229910002651 NO3 Inorganic materials 0.000 claims description 10
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 6
- 239000002671 adjuvant Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 23
- 229910052708 sodium Inorganic materials 0.000 description 15
- 230000003197 catalytic effect Effects 0.000 description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WMVRXDZNYVJBAH-UHFFFAOYSA-N dioxoiron Chemical compound O=[Fe]=O WMVRXDZNYVJBAH-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas 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
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- GNHOJBNSNUXZQA-UHFFFAOYSA-J potassium aluminium sulfate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GNHOJBNSNUXZQA-UHFFFAOYSA-J 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 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
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Images
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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
Abstract
The invention provides a low-load noble metal catalyst and a preparation method and application thereof, wherein the noble metal catalyst comprises noble metal, an auxiliary agent component and a carrier; the content of the noble metal is 0.05-0.2 wt%; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier; the noble metal catalyst has low noble metal loading capacity, still has good formaldehyde removal effect and is low in production cost; and the preparation method has simple flow and is easy for industrialization.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a low-load precious metal catalyst and a preparation method and application thereof.
Background
In recent years, with the progress of society, the living standard of substances is continuously improved, the air pollution problem is increased, and the formaldehyde is greatly harmful to the environment and the human health, wherein the formaldehyde is one of the most serious pollutants of indoor air, and is mainly generated by the release of some building materials and indoor decoration materials. Therefore, the research on the formaldehyde purification technology in the air and the improvement of the indoor air quality have very important significance.
At present, methods for removing formaldehyde from air include an adsorption method, a catalytic oxidation method, a photocatalytic technology, a plasma technology and the like, wherein the adsorption method is most commonly used, but the removal and purification period of the adsorption method is long, and an adsorbent needs to be replaced periodically, so that formaldehyde pollution cannot be eliminated fundamentally. The catalytic oxidation method can oxidize formaldehyde into nontoxic carbon dioxide and water at a lower temperature, has the characteristics of environmental protection and high efficiency, can fundamentally eliminate formaldehyde, is a formaldehyde removal technology with a good application prospect, and is attracted more and more attention and research.
The key to the formaldehyde degradation by the catalytic oxidation method is the performance of the catalyst, and generally speaking, the noble metal-supported catalyst shows excellent formaldehyde degradation performance at room temperature.
CN107096527A discloses a high-efficiency catalyst for indoor formaldehyde purification under normal temperature conditions, which comprises a carrier, a precious metal active component and an auxiliary agent; the carrier of the catalyst is mesoporous oxide and comprises at least one of aluminum oxide, iron dioxide, silicon dioxide and manganese oxide; the active component is at least one of a small amount of noble metals Pd, Pt, Au and Ag; the auxiliary agent is at least one of Na, K, Fe, Co, Ce and Ni; the catalyst of the method can completely convert formaldehyde into carbon dioxide and water at normal temperature and relative humidity of 50-90%.
CN104162425A discloses a catalyst for complete catalytic oxidation of indoor low-concentration formaldehyde at room temperature, which comprises a nano metal oxide, a noble metal component and an auxiliary agent component, wherein the nano metal oxide is used as a carrier, and the noble metal component is at least one of platinum, palladium, ruthenium, rhodium, gold and silver; the auxiliary agent is one or more of rare earth elements of praseodymium, samarium, lanthanum, cerium, yttrium and neodymium. The method adopts one or two rare earth modified inorganic nano oxide carriers, which is beneficial to improving the dispersion degree of metal nano particles and the activity of catalytic oxidation of formaldehyde.
However, in the prior art, the catalyst has the problems of high cost of supported metal, poor dispersibility, incapability of participating in reaction of most active sites, serious material waste and the like, so that the research on the catalyst for degrading formaldehyde still needs to further reduce the cost and improve the dispersibility of the supported metal.
Disclosure of Invention
The invention aims to provide a low-load noble metal catalyst and a preparation method and application thereof, wherein the noble metal catalyst comprises noble metal, an auxiliary component and a carrier; the content of the noble metal is 0.05-0.2 wt%; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier; the noble metal catalyst has low noble metal loading capacity, still has good formaldehyde removal effect and is low in production cost; and the preparation method has simple flow and is easy for industrialization.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the objects of the present invention is to provide a low-loading amount of a noble metal catalyst comprising a noble metal, an auxiliary component and a carrier; the content of the noble metal is 0.05-0.2 wt%; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3And (3) a carrier.
In the invention, the noble metal loading in the noble metal catalyst is low and is only 0.05-0.2 wt%, and the gamma-phase nano Al2O3Support and/or delta phase nano Al2O3The surface of the carrier is provided with rich loading sites, and the noble metal catalyst still has good formaldehyde removal effect under the condition of lower noble metal loading capacity through the selection of the carrier; the noble metal species with dispersed monoatomic atoms has strong hydroxyl activation capability, and the high-activity hydroxyl not only provides adsorption sites for formaldehyde species, but also can directly react with formate to generate carbon dioxide.
It is to be noted that the noble metal is contained in an amount of 0.05 to 0.2 wt%, and may be, for example, 0.05 wt%, 0.06 wt%, 0.07 wt%, 0.08 wt%, 0.09 wt%, 0.1 wt%, 0.11 wt%, 0.12 wt%, 0.13 wt%, 0.14 wt%, 0.15 wt%, 0.16 wt%, 0.17 wt%, 0.18 wt%, 0.19 wt%, 0.2 wt%, etc.; if the content of the noble metal is less than 0.05 wt%, the number of the noble metal active sites is insufficient, the activity and the stability of the catalyst are poor, and the long-time efficient oxidative decomposition of formaldehyde is difficult to realize; if the content of the noble metal is higher than 0.2 wt%, most of the noble metal does not play a catalytic role, so that the noble metal resource is wasted, and the production cost is increased.
In a preferred embodiment of the present invention, the content of the auxiliary component is 1 to 2 wt%, and may be, for example, 1 wt%, 1.1 wt%, 1.2 wt%, 1.3 wt%, 1.4 wt%, 1.5 wt%, 1.6 wt%, 1.7 wt%, 1.8 wt%, 1.9 wt%, 2 wt%, etc., but not limited to the recited values, and other values not recited in the above-mentioned range of values are also applicable.
The content of the adjuvant component of the present invention is 1 to 2 wt%, and if the content of the adjuvant component is less than 1 wt% or more than 2 wt%, the activity is lowered.
Preferably, the noble metal comprises Pt.
Preferably, the adjuvant component comprises an alkali metal element, further preferably Na.
The second object of the present invention is to provide a method for preparing the noble metal catalyst, which comprises the following steps:
(1) mixing a carrier and a solvent at one time to obtain a suspension; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier;
(2) and (2) adding a noble metal salt and an auxiliary agent into the suspension obtained in the step (1) for secondary mixing, and sequentially drying, roasting and reducing to obtain the noble metal catalyst.
It is worth to say that the gamma-phase nano Al obtained by direct purchase2O3The vector is recorded as nAl-gamma; the delta-phase nano Al obtained by direct purchase2O3The vector is recorded as nAl-delta; gamma phase nano Al2O3The carrier can also be prepared by experiment, and gamma-phase nano Al is obtained by roasting purchased pseudo-boehmite for 5 hours at 600 DEG C2O3A carrier, noted aAl-gamma; delta obtained by roasting purchased pseudoboehmite for 5 hours at 900 DEG CPhase nano Al2O3Support, designated aAl-delta.
As a preferred technical scheme of the invention, the solvent in the step (1) comprises deionized water.
Preferably, the carrier is contained in the suspension of step (1) in an amount of 1 to 20 wt%, and may be, for example, 1 wt%, 2 wt%, 3 wt%, 4 wt%, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt%, 20 wt%, etc., but is not limited to the enumerated values, and other unrecited values within the above-mentioned range of values are also applicable.
As a preferable technical scheme of the invention, the noble metal salt in the step (2) comprises platinum tetraammine nitrate.
Preferably, the auxiliary agent in step (2) comprises sodium hydroxide.
As a preferable embodiment of the present invention, the mass ratio of the noble metal salt in the step (2) to the carrier in the step (1) is (1-4):1000, and may be, for example, 1:1000, 1.2:1000, 1.5:1000, 1.7:1000, 2:1000, 2.3:1000, 2.5:1000, 2.8:1000, 3:1000, 3.2:1000, 3.5:1000, 3.7:1000, 4:1000, etc., but not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical range are also applicable.
Preferably, the mass ratio of the auxiliary agent in step (2) to the carrier in step (1) is (2-5):100, and may be, for example, 2:100, 2.2:100, 2.5:100, 2.8:100, 3:100, 3.2:100, 3.5:100, 3.7:100, 4:100, 4.2:100, 4.5:100, 4.7:100, 5:100, etc., but is not limited to the enumerated values, and other unrecited values within the above-mentioned range of values are equally applicable.
In a preferred embodiment of the present invention, the time for the secondary mixing in step (2) is 1 to 6 hours, and may be, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, etc., but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable.
Preferably, the drying in the step (2) comprises rotary steaming and drying which are carried out in sequence.
Preferably, the temperature of the rotary evaporation is 40-80 ℃, for example, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like, but is not limited to the recited values, and other values not recited in the above numerical range are also applicable.
Preferably, the temperature of the drying is 60-100 ℃, such as 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃ and the like, but not limited to the recited values, and other values not recited in the above numerical range are also applicable.
Preferably, the drying time is 1 to 12 hours, for example, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, etc., but not limited to the recited values, and other values not recited in the above numerical range are also applicable.
As a preferred embodiment of the present invention, the temperature of the calcination in step (2) is 200-800 deg.C, and may be, for example, 200 deg.C, 250 deg.C, 300 deg.C, 350 deg.C, 400 deg.C, 450 deg.C, 500 deg.C, 550 deg.C, 600 deg.C, 650 deg.C, 700 deg.C, 750 deg.C, 800 deg.C, etc., but it is not limited to the values listed, and other values not listed in the above range of values are also applicable.
Preferably, the calcination time in step (2) is 1-8h, such as 1h, 2h, 3h, 4h, 5h, 6h, 7h, 8h, etc., but not limited to the recited values, and other values in the above range are also applicable.
Preferably, the reduction of step (2) is carried out in a hydrogen atmosphere.
Preferably, the temperature of the reduction in step (2) is 100-700 ℃, and may be, for example, 100 ℃, 150 ℃, 200 ℃, 250 ℃, 300 ℃, 350 ℃, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, etc., but is not limited to the recited values, and other unrecited values within the above-mentioned range of values are also applicable.
Preferably, the reduction time in step (2) is 0.5-6h, such as 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, etc., but not limited to the recited values, and other values not recited in the above range of values are also applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) mixing a carrier and deionized water at one time to obtain suspension with the carrier content of 1-20 wt%;
wherein the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier;
(2) adding noble metal salt and an auxiliary agent into the suspension obtained in the step (1) for secondary mixing for 1-6h, sequentially carrying out rotary evaporation at 40-80 ℃, drying for 1-12h at 60-100 ℃, roasting for 1-8h at 200-800 ℃, and reducing for 0.5-6h at 100-700 ℃ in a hydrogen atmosphere to obtain a noble metal catalyst;
wherein the mass ratio of the noble metal salt to the carrier in the step (1) is controlled to be (1-4):1000, and the mass ratio of the auxiliary agent to the carrier in the step (1) is controlled to be (2-5): 100.
The invention also aims to provide application of the noble metal catalyst which is one of the aims, and the noble metal catalyst is used for removing formaldehyde.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the noble metal catalyst and the preparation method thereof, the carrier is selected, so that the noble metal catalyst still has a good formaldehyde removal effect when the loading of the noble metal is low;
(2) the preparation method of the noble metal catalyst has the advantages of low production cost, simple process and easy industrialization.
Drawings
FIG. 1 is an SEM topography of a noble metal catalyst according to example 1 of the present invention;
fig. 2 is a graph showing the distribution of Pt in the noble metal catalyst according to example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
In the embodiment of the invention, the directly purchased gamma-phase nano Al2O3The vector is recorded as nAl-gamma; the delta-phase nano Al obtained by direct purchase2O3The vector is recorded as nAl-delta; the gamma-phase nano Al obtained by direct purchase is used2O3Roasting the carrier for 4 hours at 1000 ℃ to obtain theta-phase nano Al2O3Vector, denoted as nAl- θ; the gamma-phase nano Al obtained by direct purchase is used2O3Roasting the carrier at 1200 deg.c for 4 hr to obtain alpha-phase nano Al2O3Vector, denoted as nAl- α; roasting the directly purchased pseudoboehmite for 5 hours at the temperature of 600 ℃ to obtain gamma-phase nano Al2O3A carrier, noted aAl-gamma; calcining the directly purchased pseudoboehmite at 900 ℃ for 5 hours to obtain delta-phase nano Al2O3A support, designated aAl-delta; with potassium aluminum sulfate dodecahydrate (KAl (SO)4)2·12H2O), urea (CO (NH)2)2) Preparing pseudo-boehmite from raw materials by hydrothermal for 3h at 170 ℃, and roasting for 5 hours at 600 ℃ to obtain gamma-phase micron Al2O3Vector, recorded as mAl- γ.
Example 1
This example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.05 wt%, the Na content being 2 wt%; the preparation method comprises the following steps:
(1) mixing the nAl-gamma carrier and deionized water at one time to obtain suspension with the nAl-gamma carrier content of 10 wt%;
(2) adding platinum tetraammine nitrate and sodium hydroxide into the suspension obtained in the step (1) to carry out secondary mixing for 1h, carrying out rotary evaporation at 60 ℃, drying at 100 ℃ for 5h, roasting at 400 ℃ for 2h, and reducing at 300 ℃ for 2h in a hydrogen atmosphere to obtain a noble metal catalyst;
wherein the mass ratio of the platinum tetraammine nitrate to the nAl-gamma carrier in the step (1) is controlled to be 1:1000, and the mass ratio of the sodium hydroxide to the nAl-gamma carrier in the step (1) is controlled to be 5: 100.
The SEM topography of the noble metal catalyst obtained in this example is shown in fig. 1, and it can be seen that the nAl- γ carrier is in the shape of a nanorod; the distribution diagram of Pt in the noble metal catalyst obtained in this example is shown in fig. 2, and it can be seen that Pt atoms in the noble metal catalyst are uniformly distributed and have good dispersibility.
Example 2
This example provides a noble metal catalyst and a method of preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.1 wt%, the Na content being 1.5 wt%; the preparation method comprises the following steps:
(1) mixing the nAl-gamma carrier and deionized water at one time to obtain suspension with the nAl-gamma carrier content of 1 wt%;
(2) adding platinum tetraammine nitrate and sodium hydroxide into the suspension obtained in the step (1) to carry out secondary mixing for 6h, carrying out rotary evaporation at 80 ℃ in sequence, drying at 80 ℃ for 1h, roasting at 200 ℃ for 8h, and reducing at 100 ℃ for 6h in a hydrogen atmosphere to obtain a noble metal catalyst;
wherein the mass ratio of the platinum tetraammine nitrate to the nAl-gamma carrier in the step (1) is controlled to be 2:1000, and the mass ratio of the sodium hydroxide to the nAl-gamma carrier in the step (1) is controlled to be 3: 100.
Example 3
This example provides a noble metal catalyst and a method of preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.2 wt%, the Na content being 1 wt%; the preparation method comprises the following steps:
(1) mixing the nAl-gamma carrier and deionized water at one time to obtain a suspension with the nAl-gamma carrier content of 20 wt%;
(2) adding platinum tetraammine nitrate and sodium hydroxide into the suspension obtained in the step (1) to carry out secondary mixing for 3h, carrying out rotary evaporation at 40 ℃ in sequence, drying at 60 ℃ for 12h, roasting at 800 ℃ for 1h, and reducing at 700 ℃ for 0.5h in a hydrogen atmosphere to obtain a noble metal catalyst;
wherein the mass ratio of the platinum tetraammine nitrate to the nAl-gamma carrier in the step (1) is controlled to be 4:1000, and the mass ratio of the sodium hydroxide to the nAl-gamma carrier in the step (1) is controlled to be 2: 100.
Example 4
This example provides a noble metal catalyst and a method of preparing the same, the noble metal catalyst including Pt, Na, and a nAl- δ support, the Pt content being 0.05 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the vector in the step (1) is a nAl-delta vector.
Example 5
The present embodiment provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and al- γ support, the content of Pt being 0.05 wt%, and the content of Na being 2 wt%; the preparation is as described in example 1, with the only difference that: the carrier in the step (1) is an aAl-gamma carrier.
Example 6
This example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and an al- δ support, the Pt content being 0.05 wt%, and the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the carrier in the step (1) is an aAl-delta carrier.
Example 7
This example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.05 wt%, the Na content being 0.5 wt%; the preparation is as described in example 1, with the only difference that: the mass ratio of the sodium hydroxide in the step (2) to the nAl-gamma vector in the step (1) is 1: 100.
Example 8
This example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.05 wt%, and the Na content being 3 wt%; the preparation is as described in example 1, with the only difference that: the mass ratio of the sodium hydroxide in the step (2) to the nAl-gamma vector in the step (1) is 6: 100.
Comparative example 1
The present comparative example provides a noble metal catalyst and a method of preparing the same, the noble metal catalyst including Pt, Na, and a nAl- α carrier, the Pt content being 0.05 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the vector in the step (1) is an nAl-alpha vector.
Comparative example 2
The present comparative example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- θ carrier, the Pt content being 0.05 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the vector in the step (1) is an nAl-theta vector.
Comparative example 3
The present comparative example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and mAl- γ support, the Pt content being 0.05 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the carrier in the step (1) is an mAl-gamma carrier.
Comparative example 4
The present comparative example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst comprising Pt and a nAl- γ support, the Pt content being 0.05 wt%; the preparation is as described in example 1, with the only difference that: no sodium hydroxide is added in the step (2).
Comparative example 5
The present comparative example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.3 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the mass ratio of the platinum tetraammine nitrate in the step (2) to the nAl-gamma carrier in the step (1) is 6: 1000.
Comparative example 6
The present comparative example provides a noble metal catalyst and a method for preparing the same, the noble metal catalyst including Pt, Na, and a nAl- γ support, the Pt content being 0.01 wt%, the Na content being 2 wt%; the preparation is as described in example 1, with the only difference that: the mass ratio of the platinum tetraammine nitrate in the step (2) to the nAl-gamma carrier in the step (1) is 0.2: 1000.
The removal rate of formaldehyde by the noble metal catalyst obtained in the above examples and comparative examples was tested by the following method:
and (3) placing 30mg of noble metal catalyst in a testing instrument, controlling the temperature to be 25 ℃ and the relative humidity to be 35%, testing at the space velocity of 200000 mL/(g.h), wherein the initial concentration of formaldehyde is 120ppm, and calculating the concentration of formaldehyde in the gas after 9h of catalysis, thereby obtaining the formaldehyde removal rate.
The results of the formaldehyde removal test of the noble metal catalysts obtained in the above examples and comparative examples are shown in Table 1.
TABLE 1
It should be noted that the noble metal catalyst in table 1 is named as w-x-yAl-z, where w is the mass ratio of platinum element, x is the mass ratio of sodium element, y is the code number of the alumina carrier, and z is the crystal phase of the alumina carrier.
The following points can be derived from table 1:
(1) as can be seen from examples 1 to 6, the use of gamma-phase nano Al2O3The noble metal catalyst prepared by the carriers (nAl-gamma and aAl-gamma) has excellent catalytic effect, can still realize high-efficiency catalytic decomposition of formaldehyde when the content of Pt is reduced to 0.05 wt%, greatly reduces the consumption of noble metal and saves the production cost on the premise of ensuring the catalytic performance of the formaldehyde; from the aspect of formaldehyde removal rate, different carriers catalyze noble metalsThe catalytic effect of the catalyst has obvious influence, and the good and bad order is gamma-phase nano Al2O3Carrier & gtdelta phase nano Al2O3Carrier & gttheta phase nano Al2O3Carrier & gtalpha phase nano Al2O3A carrier;
(2) comparing example 1 with examples 7 and 8, it can be seen that since the Na content of the noble metal catalyst in example 7 is 0.5 wt%, which is lower than the preferable 1-2 wt% of the present invention, the activity of the catalyst is lowered and the formaldehyde removal rate is lowered; since the Na content of the noble metal catalyst in example 8 is 3 wt% which is more than the preferable 1-2 wt% of the present invention, the catalyst activity is also decreased and the formaldehyde removal rate is decreased;
(3) comparing example 1 with comparative examples 1 to 3, it can be seen that the carrier species in comparative example 1 is alpha-phase nano Al2O3The carrier (nAl-alpha) in comparative example 2 is theta phase nano Al2O3The carrier (nAl-theta) in comparative example 3 is gamma-phase micron Al2O3A carrier (mAl-gamma); due to different carrier types and crystal phases, the active noble metal loading sites on the surface of the carrier are few, so that the formaldehyde adsorption sites on the surface of the noble metal catalyst are few, the catalytic activity is reduced, and the formaldehyde removal rate is low;
(4) comparing example 1 with comparative example 4, it can be seen that the activity of the prepared noble metal catalyst is low and the formaldehyde removal rate is low because sodium hydroxide is not added in step (2) in comparative example 4;
(5) comparing example 1 with comparative examples 5 and 6, it can be seen that, since the Pt content of the noble metal catalyst in comparative example 5 is 0.3 wt% which is 0.05-0.2 wt% better than the preferred Pt content of the present invention, although the catalytic effect is not changed much, most of the noble metal does not play a catalytic role, which results in the waste of noble metal resources and increases the production cost; since the Pt content of the noble metal catalyst in comparative example 6 is 0.01 wt% which is lower than the preferable 0.05 to 0.2 wt% of the present invention, the amount of the noble metal active sites is insufficient, the activity and stability of the catalyst are poor, long-term efficient oxidative decomposition of formaldehyde is difficult to be achieved, and the formaldehyde catalytic rate is low.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A low-loading amount of a noble metal catalyst, characterized in that the noble metal catalyst comprises a noble metal, an adjunct component, and a support; the content of the noble metal is 0.05-0.2 wt%; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3And (3) a carrier.
2. The noble metal catalyst of claim 1 wherein the promoter component is present in an amount of 1 to 2 wt.%;
preferably, the noble metal comprises Pt;
preferably, the adjuvant component comprises an alkali metal element, further preferably Na.
3. A method for preparing the noble metal catalyst of claim 1 or 2, comprising the steps of:
(1) mixing a carrier and a solvent at one time to obtain a suspension; the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier;
(2) and (2) adding a noble metal salt and an auxiliary agent into the suspension obtained in the step (1) for secondary mixing, and sequentially drying, roasting and reducing to obtain the noble metal catalyst.
4. The method of claim 3, wherein the solvent of step (1) comprises deionized water;
preferably, in the suspension liquid in the step (1), the content of the carrier is 1-20 wt%.
5. The production method according to claim 3 or 4, wherein the noble metal salt of step (2) comprises platinum tetraammine nitrate;
preferably, the auxiliary agent in step (2) comprises sodium hydroxide.
6. The production method according to any one of claims 3 to 5, wherein the mass ratio of the noble metal salt of step (2) to the carrier of step (1) is (1-4): 1000;
preferably, the mass ratio of the auxiliary agent in the step (2) to the carrier in the step (1) is (2-5): 100.
7. The method according to any one of claims 3 to 6, wherein the time for the secondary mixing in step (2) is 1 to 6 hours;
preferably, the drying in the step (2) comprises rotary steaming and drying which are carried out in sequence;
preferably, the temperature of the rotary evaporation is 40-80 ℃;
preferably, the drying temperature is 60-100 ℃;
preferably, the drying time is 1-12 h.
8. The method according to any one of claims 3 to 7, wherein the temperature for the calcination in step (2) is 200-800 ℃;
preferably, the roasting time of the step (2) is 1-8 h;
preferably, the reduction of step (2) is carried out in a hydrogen atmosphere;
preferably, the temperature of the reduction in the step (2) is 100-700 ℃;
preferably, the reduction time in step (2) is 0.5-6 h.
9. The method according to any one of claims 3 to 8, characterized by comprising the steps of:
(1) mixing a carrier and deionized water at one time to obtain suspension with the carrier content of 1-20 wt%;
wherein the carrier comprises gamma-phase nano Al2O3Support and/or delta phase nano Al2O3A carrier;
(2) adding noble metal salt and an auxiliary agent into the suspension obtained in the step (1) for secondary mixing for 1-6h, sequentially carrying out rotary evaporation at 40-80 ℃, drying for 1-12h at 60-100 ℃, roasting for 1-8h at 200-800 ℃, and reducing for 0.5-6h at 100-700 ℃ in a hydrogen atmosphere to obtain a noble metal catalyst;
wherein the mass ratio of the noble metal salt to the carrier in the step (1) is controlled to be (1-4):1000, and the mass ratio of the auxiliary agent to the carrier in the step (1) is controlled to be (2-5): 100.
10. Use of a noble metal catalyst according to claim 1 or 2 for the removal of formaldehyde.
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