CN108855069A - A kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst and the application in CO catalysis reaction - Google Patents
A kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst and the application in CO catalysis reaction Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 89
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 19
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 188
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 106
- 239000000243 solution Substances 0.000 claims description 75
- 235000019441 ethanol Nutrition 0.000 claims description 66
- 239000007787 solid Substances 0.000 claims description 56
- 238000003756 stirring Methods 0.000 claims description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 22
- UJMDYLWCYJJYMO-UHFFFAOYSA-N benzenetricarboxylic Acid Natural products OC(=O)C1=CC=CC(C(O)=O)=C1C(O)=O UJMDYLWCYJJYMO-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 16
- 238000006722 reduction reaction Methods 0.000 claims description 15
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 14
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 2
- 210000000988 bone and bone Anatomy 0.000 claims 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims 1
- 239000012621 metal-organic framework Substances 0.000 abstract description 29
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 230000003647 oxidation Effects 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000002082 metal nanoparticle Substances 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 63
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 47
- 229910002091 carbon monoxide Inorganic materials 0.000 description 47
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 47
- 239000000047 product Substances 0.000 description 31
- 229910002651 NO3 Inorganic materials 0.000 description 18
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 10
- 229960000935 dehydrated alcohol Drugs 0.000 description 10
- 238000004817 gas chromatography Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 150000004687 hexahydrates Chemical class 0.000 description 10
- 239000012046 mixed solvent Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 239000012495 reaction gas Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 7
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- 150000000703 Cerium Chemical class 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 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
- 239000010959 steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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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
- 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
- B01J23/63—Platinum group metals with rare earths or actinides
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- 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
- B01D53/864—Removing carbon monoxide or hydrocarbons
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The present invention discloses a kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst, using the metal organic framework containing Ce as template/presoma, utilize the porosity and bigger serface of metal organic framework, Pt metal nano particle is loaded into its surface, it is then dried and is handled with high-temperature roasting, to obtain the nano bar-shape Pt/CeO for being used for CO low-temperature catalytic oxidation2Loaded catalyst.The preparation method is simple, it is reproducible, preparation-obtained catalyst has the advantages that low Pt metal load capacity, good dispersion, the microscopic appearance of catalyst are controllable, the catalyst is also equipped with excellent CO low-temperature catalytic oxidation performance, it is applied in CO catalysis reaction, under suitable reaction temperature, the conversion ratio of CO can reach 100%, have extensive prospects for commercial application.
Description
Technical field
The present invention relates to catalyst preparation technical fields, and in particular to be a kind of nano bar-shape Pt/CeO2Support type is urged
The preparation method of agent and nano bar-shape Pt/CeO2Loaded catalyst is in the reaction of carbon monoxide (CO) low-temperature catalytic oxidation
Application.
Background technique
Carbon monoxide (CO) is typical flammable, toxic compounds, is difficult to react with other substances in air,
But easily in conjunction with the hemoprotein in human body.When the carbonomonoxide concentration in air reaches 400ppm, CO will occur
Poisoning, the serious death for causing people.Currently, a large amount of CO discharges mainly from carbonaceous materials such as petroleum, coals not
The industry behavior such as completely burned, including thermal power plant, Industrial Boiler, Metallurgical Factory, oil plant, chemical plant, steel plant all generates
A large amount of CO, in addition vehicle exhaust also generates a large amount of CO, so that CO annual emissions occupy the first place of world's hazardous atmosphere pollutant.Cause
This, a large amount of CO discharge is not only harmful to human body, while can cause serious environmental problem.Studies have shown that the low-temperature catalyzed oxygen of CO
Change is the method for most effective, most viable elimination CO.As it can be seen that developing the industrial catalyst of low temperature elimination CO has environmental protection
Significance researches and develops attention and concern of the CO low-temperature oxidation catalyst by researcher of high efficiency and low cost.
Catalyst type currently used for CO low-temperature catalytic oxidation is abundant, mainly there is noble metal catalyst (Pt, Pd, Au
Deng), non-precious metal catalyst (Mn, Cu, Co etc.) and molecular sieve catalyst (types such as ZSM-5, modenite)；Wherein support type
The advantages that noble metal catalyst is high, stability is good, the service life is long with its low temperature active and widely studied, however the expensive gold of support type
The high cost of metal catalyst is the problem of such Catalyst application has to face, and noble metal is negative in reduction catalyst
Carrying capacity guarantees that the good catalytic performance of catalyst is the main direction of studying of loaded noble metal catalyst simultaneously.Such as it opens
(Z.Zhang et al, Nature Communications 2017,8,16100) reports support type Pt/Al2O3It is monatomic to urge
The preparation (load capacity 0.2wt%) of agent still remains good work after the catalyst recycles 60 times under long-time high-temperature
Property, but reaction temperature need to be up to 200 DEG C, can be only achieved 100% CO conversion ratio.
Numerous researchs find CeO2With excellent oxidation susceptibility and special ionic valence condition controllability, it can be improved and urge
The oxygen storage capacity and thermal stability of agent are a kind of good Industrial Catalysis agent carriers.For example, Chinese patent CN102744063A
Directlying adopt cerium salt (cerium nitrate hexahydrate) is (600 DEG C, 3h) preparation CeO of presoma high-temperature roasting2Carrier；Chinese patent CN
Using cerium salt (cerium nitrate hexahydrate), (sodium hydroxide or potassium hydroxide) precipitating obtains CeO to 104162424A under alkaline condition2It carries
Body.Both methods prepares CeO2Pd nano particle is loaded after carrier again, although preparation method process flow is simple, your gold
Belong to the dispersibility of Pd nano particle and its cannot still obtain accuracy controlling with the interaction of carrier.
Furthermore existing research shows that loaded noble metal catalyst catalysis CO oxidation activity is also influenced by catalyst morphology, leads to
The performance for crossing the pattern of certain means regulation catalyst to enhance catalyst is one of the hot spot direction in catalyst research field.Example
Such as Wang (X.Wang et al, Journal of Materials Chemistry A 2014,2,5616) passes through fuse salt
Synthetic method and hydro-thermal method have synthesized monocrystalline SnO2Nanometer rods, SnO2Microballoon and SnO2The nano-catalytic of the different-shapes such as nanoparticle
Agent, research find monocrystalline SnO2Although nanometer rods are because its close structure causes its specific surface area smaller, SnO2Nanometer rods
(110) crystal face preferentially exposes, and substantially increases its catalytic activity, best instead to the performance of CO catalysis oxidation.
In conclusion synthesizing has certain pattern, high dispersive, low-load amount by the synthetic method for changing catalyst
Loaded noble metal catalyst is to realize the industrialized key precondition of CO low-temperature catalytic oxidation.
Summary of the invention
The purpose of the present invention is to provide a kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst, using containing
Ce metal organic framework prepares nano bar-shape Pt/CeO as template2Loaded catalyst, and by nano bar-shape Pt/CeO2It is negative
Supported catalyst is reacted applied to CO low-temperature catalytic oxidation, guarantees CO low temperature on the basis of reducing catalyst noble metal load capacity
High activity needed for catalysis oxidation.
In order to achieve the above objectives, solution of the invention is：
A kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst, includes the following steps：
1,3,5- benzenetricarboxylic acid solid is added in solvent by step 1, is stirred to being completely dissolved, is obtained molar concentration and exist
The 1,3,5- benzenetricarboxylic acid solution of 40~100mM；
Step 2, the polyvinylpyrrolidine that 0.001~0.3g is added into the 1,3,5- benzenetricarboxylic acid solution that step 1 obtains
Ketone (PVP) continues stirring and dissolving, obtains mixed solution；
Molar concentration is added into the mixed solution that step 2 obtains in the Ce (NO of 90~400mM for step 33)3·6H2O's
Ethanol solution continues after being stirred to react, and by obtained solid product by centrifuge separation, washing, drying, obtaining the metal containing cerium has
Machine skeleton, is denoted as Ce-MOF；
Step 4, the Ce-MOF for obtaining step 3 are re-dispersed into the H that molar concentration is 0.01~3.5mM2PtCl6First
In alcoholic solution, after stirring, the tetrabutyl ammonium borohydride that 0.5~2g is added at room temperature carries out reduction reaction, reaction to be restored
After, obtained solid is separated, washed, dried with high-temperature roasting to get nano bar-shape Pt/CeO2Loaded catalyst,
Wherein the load capacity of Pt is 0.005~0.5wt%.
In step 1, the solvent be one of methanol, ethyl alcohol, deionized water and n,N-Dimethylformamide (DMF) or
It is a variety of.
In step 3, the Ce (NO3)3·6H2Ce in the ethanol solution of O3+With 1,3,5- benzene front three in the mixed solution
The mole dosage ratio of acid is 1：1, the temperature of the reaction is 30~100 DEG C, and the time of the reaction is 2h~for 24 hours.
In step 4, the Ce-MOF and the H2PtCl6Methanol solution usage ratio be (0.1~0.5) g：(30~
100) mL, wherein Ce-MOF is calculated by mass, H2PtCl6Methanol solution in terms of volume.
In step 4, the time of the reduction reaction is 10~60min.
In step 4, the temperature of the drying is 60 DEG C, and the process of the high-temperature roasting is that obtained solid is put into Muffle furnace
In, it is that 1~5 DEG C/min roasts 1~10h under conditions of maturing temperature is 200~500 DEG C in heating rate.
Using above-mentioned nano bar-shape Pt/CeO2The nano bar-shape Pt/CeO of the preparation method preparation of loaded catalyst2Load
Application of the type catalyst in CO catalysis reaction.
After adopting the above technical scheme, a kind of nano bar-shape Pt/CeO of the present invention2The preparation method of loaded catalyst, is adopted
Use the metal organic framework containing Ce will be golden using the porosity and bigger serface of metal organic framework as template/presoma
Belong to Pt nano particle and load to its surface, be then dried and handled with high-temperature roasting, is used for the low-temperature catalyzed oxygen of CO to obtain
The nano bar-shape Pt/CeO of change2Loaded catalyst.The preparation method is simple, reproducible, preparation-obtained catalyst tool
Have the advantages that low Pt metal load capacity, good dispersion, the microscopic appearance of catalyst are controllable, it is low which is also equipped with excellent CO
Warm catalytic oxidation performance has extensive prospects for commercial application.
Detailed description of the invention
Fig. 1 is Pt/CeO prepared by embodiment 12The transmission electron microscope picture (TEM) of nano bar-shape catalyst, scale 100nm；
Fig. 2 is Pt/CeO prepared by embodiment 12Energy dispersion X-ray spectrometer (EDX) element of nano bar-shape catalyst
Distribution map, scale is 50nm in Fig. 2 a.
Specific embodiment
In order to further explain the technical solution of the present invention, being explained in detail below by specific embodiment the present invention
It states.
Embodiment 1
Catalyst preparation：
The 1 of 2.1g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 100mM, 0.1g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 200mM3)3·6H2The ethanol solution of O continues to stir at 80 DEG C
Reaction 16 hours is mixed, to which after reaction, products therefrom obtains white powder Ce- by centrifuge separation, ethanol washing, drying
MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 1mM2PtCl6Methanol solution in,
After stirring, the tetrabutyl ammonium borohydride that 1.0g is added carries out reduction reaction, reacts 30 minutes at room temperature.To the end of reacting
Afterwards, product is centrifuged, ethanol washing, after 60 DEG C of dryings, products therefrom is put into Muffle furnace, with the heating of 5 DEG C/min
Rate roasts 4h to 300 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal be
0.3wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 4.34g
(NO3)3·6H2O) solid is added in 50mL dehydrated alcohol, and ultrasonic 5min obtains the Ce (NO of 200mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
The Pt/CeO that embodiment 1 is prepared2Nano bar-shape catalyst carries out structural characterization：
TEM characterization test instrument is Jeol Ltd. JEM-2010 type transmission electron microscope, acceleration voltage：
200kV, as a result as shown in Figure 1, the results showed that prepared Pt/CeO2The pattern of catalyst is nano bar-shape.
EDX characterization test instrument is the INCA-7426 type energy dispersion X-ray spectrometer of England Oxford instrument company, knot
Fruit is as shown in Figure 2, the results showed that prepared Pt/CeO2In the structure of loaded catalyst, cerium (Ce) element and platinum (Pt) member
Element is uniformly distributed.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 60 DEG C, CO conversion ratio is 76%；When reaction temperature is 80 DEG C, CO conversion
Rate is 100%, and it is still 100% that catalyst runs rear CO conversion ratio for 24 hours at 80 DEG C, it was demonstrated that nano bar-shape Pt/CeO2It is negative
Supported catalyst has excellent stability.
Embodiment 2
Catalyst preparation：
The 1 of 1.0g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL deionized water, is filled
Divide stirring to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 47.6mM, 0.1g PVP solid is then added, after
Continue after being uniformly mixed, 50mL is added, the Ce (NO that molar concentration is 95.2mM3)3·6H2The ethanol solution of O, at 60 DEG C
Continue to be stirred to react 20 hours, to which after reaction, products therefrom obtains white powder by centrifuge separation, ethanol washing, drying
Last Ce-MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 1mM2PtCl6Methanol it is molten
In liquid, after stirring, the tetrabutyl ammonium borohydride that 1.3g is added carries out reduction reaction, reacts 30 minutes at room temperature.Wait react
After, product is centrifuged, ethanol washing, after 60 DEG C of dryings, products therefrom is put into Muffle furnace, with 3 DEG C/min's
Heating rate roasts 4h to 300 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal be
0.3wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 2.07g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 95.2mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 80 DEG C, after CO conversion ratio is 100%, and catalyst is run for 24 hours at 80 DEG C
CO conversion ratio is still 100%, it was demonstrated that nano bar-shape Pt/CeO2Loaded catalyst has excellent stability.
Embodiment 3
Catalyst preparation：
The 1 of 2.1g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 100mM, 0.001g PVP solid is then added, continue
After being uniformly mixed, 50mL is added, the Ce (NO that molar concentration is 200mM3)3·6H2The ethanol solution of O continues at 60 DEG C
It is stirred to react 24 hours, to which after reaction, products therefrom obtains white powder by centrifuge separation, ethanol washing, drying
Ce-MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 1mM2PtCl6Methanol solution
In, after stirring, the tetrabutyl ammonium borohydride that 1.3g is added carries out reduction reaction, reacts 30 minutes at room temperature.Wait react knot
Shu Hou, product are centrifuged, ethanol washing, and after dry, products therefrom is put into Muffle furnace, with the heating speed of 5 DEG C/min
Rate roasts 2h to 400 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal is 0.3wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 4.34g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 200mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 130 DEG C, CO conversion ratio is 100%.
Embodiment 4
Catalyst preparation：
The 1 of 4.2g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 200mM, 0.2g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 400mM3)3·6H2The ethanol solution of O continues to stir at 80 DEG C
Reaction 20 hours is mixed, to which after reaction, products therefrom obtains white powder Ce- by centrifuge separation, ethanol washing, drying
MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 1mM2PtCl6Methanol solution in,
After stirring, the tetrabutyl ammonium borohydride that 1.0g is added carries out reduction reaction, reacts 30 minutes at room temperature.To the end of reacting
Afterwards, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating rate of 1 DEG C/min
To 500 DEG C, 1h is roasted to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal is 0.3wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 8.68g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 400mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 110 DEG C, CO conversion ratio is 100%.
Embodiment 5
Catalyst preparation：
The 1 of 2.1g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 100mM, 0.2g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 200mM3)3·6H2The ethanol solution of O continues to stir at 60 DEG C
Reaction 24 hours is mixed, to which after reaction, products therefrom obtains white powder Ce- by centrifuge separation, ethanol washing, drying
MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 1mM2PtCl6Methanol solution in,
After stirring, the tetrabutyl ammonium borohydride that 1.0g is added carries out reduction reaction, reacts 30 minutes at room temperature.To the end of reacting
Afterwards, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating rate of 3 DEG C/min
To 400 DEG C, 2h is roasted to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal is 0.3wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 4.34g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 200mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 110 DEG C, CO conversion ratio is 100%.
Embodiment 6
Catalyst preparation：
The 1 of 2.1g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 100mM, 0.1g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 200mM3)3·6H2The ethanol solution of O continues to stir at 90 DEG C
Reaction 12 hours is mixed, to which after reaction, products therefrom obtains white powder Ce- by centrifuge separation, ethanol washing, drying
MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 500mg for the H of 2mM2PtCl6Methanol solution in,
After stirring, the tetrabutyl ammonium borohydride that 1.5g is added carries out reduction reaction, reacts 40 minutes at room temperature.To the end of reacting
Afterwards, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating rate of 5 DEG C/min
To 300 DEG C, 6h is roasted to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal is 0.35wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 4.34g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 200mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 51.8mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 2mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 80 DEG C, CO conversion ratio is 100%.
Embodiment 7
Catalyst preparation：
The 1 of 1.5g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 40mL ethyl alcohol and 60mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 71.4mM, 0.3g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 142.8mM3)3·6H2The ethanol solution of O continues at 80 DEG C
It is stirred to react 20 hours, to which after reaction, products therefrom obtains white powder by centrifuge separation, ethanol washing, drying
Ce-MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 500mg for the H of 3.5mM2PtCl6Methanol it is molten
In liquid, after stirring, the tetrabutyl ammonium borohydride that 1.5g is added carries out reduction reaction, reacts 40 minutes at room temperature.Wait react
After, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating of 5 DEG C/min
Rate roasts 6h to 300 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal be
0.5wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce (NO of 3.1g3)3·
6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 142.8mM3)3·6H2The ethanol solution of O.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 90.7mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 3.5mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 80 DEG C, CO conversion ratio is 100%.
Embodiment 8
Catalyst preparation：
The 1 of 1.5g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 71.4mM, 0.3g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 142.8mM3)3·6H2The ethanol solution of O continues at 80 DEG C
It is stirred to react 15 hours, to which after reaction, products therefrom obtains white powder by centrifuge separation, ethanol washing, drying
Ce-MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 300mg for the H of 0.5mM2PtCl6Methanol it is molten
In liquid, after stirring, the tetrabutyl ammonium borohydride that 0.8g is added carries out reduction reaction, reacts 20 minutes at room temperature.Wait react
After, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating of 5 DEG C/min
Rate roasts 3h to 300 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal be
0.1wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce (NO of 3.1g3)3·
6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 142.8mM3)3·6H2The ethanol solution of O.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 13mg2PtCl6·6H2O) solid is added
In the methanol of 50mL, ultrasonic 5min obtains the H of 0.5mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 90 DEG C, CO conversion ratio is 100%.
Embodiment 9
Catalyst preparation：
The 1 of 1.5g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 50mL ethyl alcohol and 50mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 71.4mM, 0.3g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 142.8mM3)3·6H2The ethanol solution of O continues at 80 DEG C
It is stirred to react 15 hours, to which after reaction, products therefrom obtains white powder by centrifuge separation, ethanol washing, drying
Ce-MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 250mg for the H of 0.01mM2PtCl6Methanol
In solution, after stirring, the tetrabutyl ammonium borohydride that 0.5g is added carries out reduction reaction, reacts 20 minutes at room temperature.To anti-
After answering, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the liter of 5 DEG C/min
Warm rate roasts 5h to 300 DEG C to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal be
0.005wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce (NO of 3.1g3)3·
6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 142.8mM3)3·6H2The ethanol solution of O.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 0.26mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 0.01mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 220 DEG C, CO conversion ratio is 100%.
Embodiment 10
Catalyst preparation：
The 1 of 2.1g, 3,5- benzenetricarboxylic acid solid is first added to the in the mixed solvent of 30mL ethyl alcohol and 70mL DMF, is sufficiently stirred
It mixes to being completely dissolved, obtains 1,3, the 5- benzenetricarboxylic acid solution that concentration is 100mM, 0.1g PVP solid is then added, continues to stir
It mixes and 50mL is added after mixing, the Ce (NO that molar concentration is 200mM3)3·6H2The ethanol solution of O continues to stir at 70 DEG C
Reaction 24 hours is mixed, to which after reaction, products therefrom obtains white powder Ce- by centrifuge separation, ethanol washing, drying
MOF.Then, 50mL, molar concentration are dispersed again by the Ce-MOF solid of 300mg for the H of 1mM2PtCl6Methanol solution in,
After stirring, the tetrabutyl ammonium borohydride that 1.5g is added carries out reduction reaction, reacts 30 minutes at room temperature.To the end of reacting
Afterwards, product is centrifuged, ethanol washing, after dry, products therefrom is put into Muffle furnace, with the heating rate of 3 DEG C/min
To 300 DEG C, 3h is roasted to get nano bar-shape Pt/CeO2Loaded catalyst, wherein the load capacity of Pt metal is 0.26wt%.
Wherein, Ce (NO3)3·6H2The ethanol solution of O is prepared as：By the cerous nitrate hexahydrate (Ce of 4.34g
(NO3)3·6H2O) dehydrated alcohol of 50mL is added in solid, and ultrasonic 5min obtains the Ce (NO of 200mM3)3·6H2The ethyl alcohol of O is molten
Liquid.
H2PtCl6Methanol solution be prepared as：By the chloroplatinic acid hexahydrate (H of 25.9mg2PtCl6·6H2O) solid adds
Enter in the methanol of 50mL, ultrasonic 5min obtains the H of 1mM2PtCl6Methanol solution.
Catalyst test：
Catalysis reaction carries out in atmospheric fixed bed reactor, and reaction gas group becomes CO/O2/N2=1/4/95, reaction produces
Object is analyzed by gas-chromatography (TCD detector) on-line checking.
Experimental result：When reaction temperature is 80 DEG C, CO conversion ratio is 100%.
Above-described embodiment and schema and non-limiting product form and style of the invention, any technical field it is common
The appropriate changes or modifications that technical staff does it all should be regarded as not departing from patent category of the invention.
Claims (7)
1. a kind of nano bar-shape Pt/CeO2The preparation method of loaded catalyst, it is characterised in that：Include the following steps：
1,3,5- benzenetricarboxylic acid solid is added in solvent by step 1, is stirred to being completely dissolved, obtain molar concentration 40~
The 1,3,5- benzenetricarboxylic acid solution of 100mM；
The polyvinylpyrrolidone of 0.001~0.3g is added in step 2,1,3, the 5- benzenetricarboxylic acid solution obtained toward step 1, after
Continuous stirring and dissolving, obtains mixed solution；
Molar concentration is added into the mixed solution that step 2 obtains in the Ce (NO of 90~400mM for step 33)3·6H2The ethyl alcohol of O
Solution continues after being stirred to react, and by obtained solid product by centrifuge separation, washing, drying, obtains the organic bone of metal containing cerium
Frame is denoted as Ce-MOF；
Step 4, the Ce-MOF for obtaining step 3 are re-dispersed into the H that molar concentration is 0.01~3.5mM2PtCl6Methanol it is molten
In liquid, after stirring, the tetrabutyl ammonium borohydride that 0.5~2g is added at room temperature carries out reduction reaction, and reaction to be restored terminates
Afterwards, obtained solid is separated, washed, dried with high-temperature roasting to get nano bar-shape Pt/CeO2Loaded catalyst, wherein
The load capacity of Pt is 0.005~0.5wt%.
2. a kind of nano bar-shape Pt/CeO according to claim 12The preparation method of loaded catalyst, it is characterised in that：
In step 1, the solvent is one of methanol, ethyl alcohol, deionized water and n,N-Dimethylformamide or a variety of.
3. a kind of nano bar-shape Pt/CeO according to claim 12The preparation method of loaded catalyst, it is characterised in that：
In step 3, the Ce (NO3)3·6H2Ce in the ethanol solution of O3+With mole of 1,3,5- benzenetricarboxylic acid in the mixed solution
Amount ratio is 1：1, the temperature of the reaction is 30~100 DEG C, and the time of the reaction is 2h~for 24 hours.
4. a kind of nano bar-shape Pt/CeO according to claim 12The preparation method of loaded catalyst, it is characterised in that：
In step 4, the Ce-MOF and the H2PtCl6Methanol solution usage ratio be (0.1~0.5) g：(30~100) mL,
Wherein Ce-MOF is calculated by mass, H2PtCl6Methanol solution in terms of volume.
5. a kind of nano bar-shape Pt/CeO according to claim 12The preparation method of loaded catalyst, it is characterised in that：
In step 4, the time of the reduction reaction is 10~60min.
6. a kind of nano bar-shape Pt/CeO according to claim 12The preparation method of loaded catalyst, it is characterised in that：
In step 4, the temperature of the drying is 60 DEG C, and the process of the high-temperature roasting is that obtained solid is put into Muffle furnace, is being risen
Warm rate is that 1~5 DEG C/min roasts 1~10h under conditions of maturing temperature is 200~500 DEG C.
7. using a kind of nano bar-shape Pt/CeO as described in claim 12The nanometer of the preparation method preparation of loaded catalyst
Rodlike Pt/CeO2Application of the loaded catalyst in CO catalysis reaction.
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