CN107029752B - A kind of preparation method of platinum/graphen-perovskite-foamed nickel catalyst agent - Google Patents
A kind of preparation method of platinum/graphen-perovskite-foamed nickel catalyst agent Download PDFInfo
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- CN107029752B CN107029752B CN201710435187.1A CN201710435187A CN107029752B CN 107029752 B CN107029752 B CN 107029752B CN 201710435187 A CN201710435187 A CN 201710435187A CN 107029752 B CN107029752 B CN 107029752B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 45
- 239000010439 graphite Substances 0.000 claims abstract description 45
- 229910002321 LaFeO3 Inorganic materials 0.000 claims abstract description 44
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- 239000006260 foam Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 22
- 229910021389 graphene Inorganic materials 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000005260 corrosion Methods 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 8
- 239000003792 electrolyte Substances 0.000 claims description 8
- 235000007164 Oryza sativa Nutrition 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- 239000002585 base Substances 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- WACRXVBKMRXTCA-UHFFFAOYSA-N platinum sodium Chemical compound [Na].[Pt] WACRXVBKMRXTCA-UHFFFAOYSA-N 0.000 claims description 7
- 235000009566 rice Nutrition 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 229910003594 H2PtCl6.6H2O Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910020851 La(NO3)3.6H2O Inorganic materials 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000007767 bonding agent Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 21
- 239000007789 gas Substances 0.000 abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 238000004070 electrodeposition Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000001666 catalytic steam reforming of ethanol Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 1
- 229910001868 water Inorganic materials 0.000 description 8
- 241000209094 Oryza Species 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001802 infusion Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910017771 LaFeO Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- -1 No. 2 catalyst Chemical compound 0.000 description 1
- 229910002845 Pt–Ni Inorganic materials 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000009767 auto-combustion synthesis reaction Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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Abstract
The invention discloses a kind of preparation methods of platinum/graphen-perovskite-foamed nickel catalyst agent, prepare graphite oxide aqueous solution using hummer method first, then prepare brownish red suspension, and successively carry out hydrothermal synthesis-washing-filtering and prepare graphene-LaFeO3Foam nickel electrode, last electrodeposition Pt obtain Pt/ graphene-LaFeO3Foamed nickel catalyst agent.The catalyst can be used for carbon monoxide preferential oxidation in hydrogen-rich gas, Oxidation of Carbon Monoxide, hydrogen production by ethanol steam reforming reaction, synthesis gas prepare low-carbon alcohol catalysis reaction in, before the use process of catalyst using reducibility gas be lower than 150 ~ 200oReduction treatment under conditions of C.
Description
Technical field
The present invention relates to the preparation sides that a kind of Pt metal is carried on the catalyst in graphene-perovskite-foam nickel carrier
Method belongs to catalyst field.
Background technique
LaFeO3 is a kind of typically with perovskite (ABO3) structure rare earth metal composite oxide, the Ca-Ti ore type
Compound has and can have more Lacking oxygen and good thermal stability, and B ions are with mixed while keeping structure
The advantages that closing valence state and abnormal valence state, and being concerned in catalytic field, preparation method mainly have auto-combustion method, hydro-thermal method,
Sol-gel method, solid phase method, coprecipitation, chemical vapour deposition technique, drop leaching-pyrolysismethod, microemulsion method and wet chemistry method
Deng, preparating mechanism and process conditions, there were significant differences, and the catalysis material surface property and structure for causing distinct methods to prepare are poor
Different very big, but all perovskites have an obvious shortcoming, i.e., extremely low (usual specific surface area is in 3-5m for specific surface area2/ g) and
Limit use of the perovskite in catalytic field.
Graphene as it is presently found it is most thin, maximum intensity is conductive, heating conduction, the strongest one kind of optical property are novel
(such as pure grapheme material, surface area can reach 2000 ~ 4000m to nano material2/ g) it is very promising catalyst carrier, but
Current technology is difficult on a large scale, high-quality, and inexpensive prepares grapheme material, and seriously constrains graphene in the industry
Application.There are many methods to be developed at present and prepares the dilute compound of graphite.Especially by the dilute side of reduction-oxidation graphite
Method may be implemented high-volume, low cost to prepare graphite dilute, and the dilute surface of graphite oxide can also be made full use of abundant oxygen-containing
Functional group, thus further to its functionalization to adjust the performance that graphite oxide is dilute or reduction-oxidation graphite is dilute.So far, stone
Ink refining is successfully compound with inorganic nanoparticles, organic crystal, polymer, metal organic complex, biomaterial etc., this
A little dilute composite materials of graphite are widely used in lithium ion battery, supercapacitor, fuel cell, photocatalysis, biosensor
Etc..In addition, being rarely reported for the preparation of graphene-perovskite compound, mainly since perovskite is in preparation process
In be usually required to 300-700 DEG C of roasting, can be formed under high temperature, but graphene is as carbon material, usually less than
150 DEG C will burn totally (pure graphene, aerial ignition temperature are relatively higher).
Furthermore, it is however generally that common noble metal has palladium, platinum, ruthenium, silver, rhodium, wherein especially most with platinum, rhodium noble metal application surface
Extensively.For transition elements noble metal catalyst, d electron orbit is all unfilled, the easy adsorption reaction object gas molecule in surface, and strong
It spends moderate, advantageously forms " reactive compound " intermediate state, show higher catalytic activity, while also there is high temperature resistant, anti-
The comprehensive good characteristic such as oxidation, corrosion-resistant, and become important catalyst activity component, but noble metal is due to earth reserves
Less, expensive to hinder its method application, and for noble metal/perovskite catalyst, due to the specific surface of perovskite
Product is lower, and noble metal usually can all reunite and reduce catalytic activity.In addition, for gas-solid catalysis, a such as oxidation
For carbon preferential oxidation, Oxidation of Carbon Monoxide, hydrogen production by ethanol steam reforming reaction, synthesis gas prepare the reaction of low-carbon alcohol catalysis,
Although the unique mesopore orbit structure of catalyst has great advantage in terms of Selective Separation, it will limit molecule and quickly expand
It dissipates, is unfavorable for the generation of intended catalyzed reaction, but macropore is conducive to quickly spread, be in progress in terms of mass-and heat-transfer significant, therefore
It is proposed the mesoporous and compound composite material of macropore multi-stage porous.
Summary of the invention
The invention proposes a kind of preparation method of platinum/graphen-perovskite-foamed nickel catalyst agent, deposited in the catalyst
Micropore-mesopore between graphene-graphene, the slit pore between graphene and perovskite, the macropore between perovskite and perovskite,
The macropore of nickel foam, the i.e. catalyst possess micropore-mesopore-macropore hierarchical porous structure simultaneously, and by strike, so that
The surface of the uniform load carriers of Pt nano particle, catalytic activity are much higher than similar catalyst, pass through the limited solution of hydro-thermal method
It has determined the low problem of surface area of the Complex Problem of graphene and perovskite, perovskite, has prepared that introduce macropore effective by electrode
Solve carbon monoxide preferential oxidation in hydrogen-rich gas, Oxidation of Carbon Monoxide, hydrogen production by ethanol steam reforming reaction, synthesis gas
A series of mass transfer problem of vapor solids such as low-carbon alcohol catalysis reaction is prepared, and your gold of electrodeposition process effective solution used
Belong to the problem easy to reunite in catalyst surface.
Platinum/graphen-perovskite-foamed nickel catalyst the agent the preparation method comprises the following steps:
(1) graphite oxide aqueous solution is prepared using hummer method, the brown color graphite oxide for obtaining 0.5-2mg/mL is water-soluble
Liquid；
(2) using above-mentioned graphene oxide water solution as solvent, La (NO is sequentially added thereto3)3.6H2O, NaOH and
Na2CO3, magnetic agitation 1h at 10-15 DEG C obtains brownish red suspension；
(3) special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing is added in above-mentioned brown liquid；Then to
It is passed through inert gas in reaction kettle, for emptying the air in reaction kettle, opens the matched agitating device of reaction kettle, is stirred at room temperature
30 minute, it is then shut off the valve of inert gas, hydrothermal reaction kettle is fully sealed, sets heating mantle in hydrothermal reaction kettle surrounding,
Setting program heating；
(4) when temperature reaches 260 DEG C ~ 320 DEG C 12 ~ 48h of constant temperature, removal heating mantle is slowly cooled to room temperature, opens hydro-thermal
Reaction kettle obtains grey black solution；
(5) grey black solution is filtered, is successively filtered by vacuum, supersound washing obtains grey black sediment, and 40 DEG C of drying obtain
Clean grey black graphene-LaFeO3Powder；
(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in nickel foam
On, 40 DEG C of drying obtain flake graphite alkene-LaFeO3Foam nickel electrode；
(7) using the electrode prepared as working electrode, it is to electrode with platinum-base material, is 5% with mass fraction
H2PtCl6.6H2O or Pt (NH3)2(NO2)2For electrolyte, current density 1-2A/dm3, time 1-2h, 25 ~ 30 DEG C of temperature exists
Flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle on foam nickel electrode obtains Pt/ graphene-LaFeO3Nickel foam is urged
Agent.
Wherein La (NO3)3.6H2O:NaOH:Na2CO3Molar ratio be 1:10 ~ 15:3 ~ 6.
Wherein temperature-programmed mode are as follows: be warming up to 100 DEG C first with the heating rate of 1 ~ 2 DEG C/min, kept for 1 hour, so
1 ~ 2 DEG C/min is warming up to 260 ~ 320 DEG C afterwards, is kept for 12 ~ 48 hours, terminates.
The mode being wherein filtered by vacuum is to be filtered using water-ring vacuum pump, and the mode of supersound washing is successively to use quality
The dilute hydrochloric acid that score is 5 ~ 7%, anhydrous propanone, dehydrated alcohol, deionized water are repeatedly washed.
Electrically conductive graphite, binder, graphene-LaFeO3The mass ratio of powder is 1:1:8 mixing, is ground in the agate mortar
Mill, and it is uniform that appropriate dehydrated alcohol mixing paste is added, and it was evenly coated in nickel foam.
Wherein electrolyte may be H2PtCl6.6H2O and NiSO4Mixture, mass ratio be 1:3 be used to form Pt-
Ni/ graphene-LaFeO3Foamed nickel catalyst agent.
In addition, the catalyst can be used for carbon monoxide preferential oxidation in hydrogen-rich gas, Oxidation of Carbon Monoxide, ethanol steam
Reformation hydrogen production reaction, synthesis gas are prepared in the reaction of low-carbon alcohol catalysis, are existed before the use process of catalyst using reducibility gas
Reduction treatment under conditions of lower than 150 ~ 200 DEG C, only using hydrogen-rich gas CO preferential oxidation as example in embodiment.
Figure of description
Table 1 is the specific surface area and Particle size data of catalyst and comparative example；
Fig. 1 is catalyst and comparative example activity data figure.
Specific embodiment
The catalyst performance condition that CO-PROX reacts in hydrogen-rich atmosphere are as follows: in H before reaction2/N2300 in gaseous mixtureoC
Reduction pretreatment 1 hour.Corresponding volume space velocity is 24000ml/gcat.H, unstrpped gas group become 1 vol.% CO, and 1
vol.% O2, 50 vol.% H2, 0-12.5 vol.% CO2, 0-15 vol.% H2O and N2Balance Air.
Comparative example 1
No. 1-roasting method prepares LaFeO3- infusion process supporting Pt:
By the lanthanum nitrate of special ratios, ferric nitrate is dissolved in deionized water, and a certain proportion of lemon is added into mixed solution
Lemon acid and ethylene glycol, 85oStirring is to whole dissolutions under C, and 120oC oven drying for 24 hours, 600o2h is roasted under C, obtains LaFeO3, connect
Using six hydration chloroplatinic acids of solution dipping method dipping, it is dry to obtain Pt/LaFeO3, i.e. No. 1 catalyst.
Comparative example 2
No. 2-Hummer prepare graphene-infusion process supporting Pt:
Hummer is conventional method, is filtered, washed, dries, six hydration chloroplatinic acid of dipping, dry to obtain Pt/ graphene, i.e.,
No. 2 catalyst, theoretically activity should be very high, but during actually preparation, due to repeatedly washing drying, so that original point
Scattered graphene sheet layer is reunited again, causes surface area very low, and graphene itself, without macropore, mass transfer is seriously obstructed, and finally makes
It is very low to obtain catalytic activity.
Comparative example 3
No. 3-hydro-thermal method prepares compound-infusion process supporting Pt:
Graphene-LaFeO is prepared using the consistent hydro-thermal method of the application3Carrier, six hydration chloroplatinic acid of dipping are dry to obtain
Pt/ graphene-LaFeO3, i.e. No. 3 catalyst, active effect is relatively low, be primarily due to carrier itself be not present it is more
Macropore, cause gas transfer to be obstructed, and the dispersibility of infusion process supporting Pt is poor, reunites, particle radius is larger.
Embodiment 4
No. 4-hydro-thermal method prepares compound-nickel foam-electro-deposition preparation supporting Pt:
(1) graphite oxide aqueous solution is prepared using hummer method first, obtains the brown color graphite oxide water of 1.5mg/mL
Solution；(2) using above-mentioned graphene oxide water solution as solvent, the La (NO that molar ratio is 1:15:6 is sequentially added thereto3)3 .6H2O, NaOH and Na2CO3, 15oMagnetic agitation 1h under C obtains brownish red suspension；(3) above-mentioned brown liquid is added
Special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing；Then inert gas is passed through into reaction kettle, it is anti-for emptying
The air in kettle is answered, the matched agitating device of reaction kettle is opened, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas,
Hydrothermal reaction kettle is fully sealed, sets heating mantle, setting program heating: 1 in hydrothermal reaction kettle surroundingoThe heating rate of C/min
It is warming up to 100oC, is kept for 1 hour, and then 1oC/min is warming up to 260oC, keeps reaching 260 when temperature in 12 hours (4)oC constant temperature
12 ~ 48h removes heating mantle, is slowly cooled to room temperature, and opens hydrothermal reaction kettle, obtains grey black solution；(5) grey black is filtered
Solution is successively filtered by vacuum, supersound washing acquisition grey black sediment, and 40oC drying obtains clean grey black graphene-
LaFeO3Powder；(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in foam
On nickel, 40oC drying, obtains flake graphite alkene-LaFeO3Foam nickel electrode；(7) using the electrode prepared as working electrode,
It is the H for being 1% with mass fraction to electrode with platinum-base material2PtCl6.6H2Or Pt (NH3)2(NO2) 2 be electrolyte, current density
For 2A/dm3, time 1h, temperature 30oC is in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle, is obtained on foam nickel electrode
Obtain Pt/ graphene-LaFeO3Foamed nickel catalyst agent.
Embodiment 5
No. 4-hydro-thermal method prepares compound-nickel foam-electro-deposition preparation supporting Pt:
(1) graphite oxide aqueous solution is prepared using hummer method first, the brown color graphite oxide for obtaining 2mg/mL is water-soluble
Liquid；(2) using above-mentioned graphene oxide water solution as solvent, the La (NO that molar ratio is 1:15:6 is sequentially added thereto3)3 .6H2O, NaOH and Na2CO3, 15oMagnetic agitation 1h under C obtains brownish red suspension；(3) above-mentioned brown liquid is added
Special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing；Then inert gas is passed through into reaction kettle, it is anti-for emptying
The air in kettle is answered, the matched agitating device of reaction kettle is opened, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas,
Hydrothermal reaction kettle is fully sealed, sets heating mantle, setting program heating: 1 in hydrothermal reaction kettle surroundingoThe heating rate of C/min
It is warming up to 100oC, is kept for 1 hour, and then 1oC/min is warming up to 280oC, keeps reaching 260 when temperature in 12 hours (4)oC constant temperature
12 ~ 48h removes heating mantle, is slowly cooled to room temperature, and opens hydrothermal reaction kettle, obtains grey black solution；(5) grey black is filtered
Solution is successively filtered by vacuum, supersound washing acquisition grey black sediment, and 40oC drying obtains clean grey black graphene-
LaFeO3Powder；(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in foam
On nickel, 40oC drying, obtains flake graphite alkene-LaFeO3Foam nickel electrode；(7) using the electrode prepared as working electrode,
It is the H for being 3% with mass fraction to electrode with platinum-base material2PtCl6.6H2Or Pt (NH3)2(NO2) 2 be electrolyte, current density
For 2A/dm3, time 1h, temperature 30oC is in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle, is obtained on foam nickel electrode
Obtain Pt/ graphene-LaFeO3Foamed nickel catalyst agent.
Embodiment 6
No. 4-hydro-thermal method prepares compound-nickel foam-electro-deposition preparation supporting Pt:
(1) graphite oxide aqueous solution is prepared using hummer method first, the brown color graphite oxide for obtaining 2mg/mL is water-soluble
Liquid；(2) using above-mentioned graphene oxide water solution as solvent, the La (NO that molar ratio is 1:15:6 is sequentially added thereto3)3 .6H2O, NaOH and Na2CO3, 15oMagnetic agitation 1h under C obtains brownish red suspension；(3) above-mentioned brown liquid is added
Special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing；Then inert gas is passed through into reaction kettle, it is anti-for emptying
The air in kettle is answered, the matched agitating device of reaction kettle is opened, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas,
Hydrothermal reaction kettle is fully sealed, sets heating mantle, setting program heating: 1 in hydrothermal reaction kettle surroundingoThe heating rate of C/min
It is warming up to 100oC, is kept for 1 hour, and then 1oC/min is warming up to 300oC, keeps reaching 260 when temperature in 12 hours (4)oC constant temperature
12 ~ 48h removes heating mantle, is slowly cooled to room temperature, and opens hydrothermal reaction kettle, obtains grey black solution；(5) grey black is filtered
Solution is successively filtered by vacuum, supersound washing acquisition grey black sediment, and 40oC drying obtains clean grey black graphene-
LaFeO3Powder；(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in foam
On nickel, 40oC drying, obtains flake graphite alkene-LaFeO3Foam nickel electrode；(7) using the electrode prepared as working electrode,
It is the H for being 5% with mass fraction to electrode with platinum-base material2PtCl6.6H2Or Pt (NH3)2(NO2) 2 be electrolyte, current density
For 2A/dm3, time 1h, temperature 30oC is in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle, is obtained on foam nickel electrode
Obtain Pt/ graphene-LaFeO3Foamed nickel catalyst agent.
Embodiment 7
No. 4-hydro-thermal method prepares compound-nickel foam-electro-deposition preparation supporting Pt:
(1) graphite oxide aqueous solution is prepared using hummer method first, the brown color graphite oxide for obtaining 2mg/mL is water-soluble
Liquid；(2) using above-mentioned graphene oxide water solution as solvent, the La (NO that molar ratio is 1:15:6 is sequentially added thereto3)3 .6H2O, NaOH and Na2CO3, 15oMagnetic agitation 1h under C obtains brownish red suspension；(3) above-mentioned brown liquid is added
Special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing；Then inert gas is passed through into reaction kettle, it is anti-for emptying
The air in kettle is answered, the matched agitating device of reaction kettle is opened, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas,
Hydrothermal reaction kettle is fully sealed, sets heating mantle, setting program heating: 1 in hydrothermal reaction kettle surroundingoThe heating rate of C/min
It is warming up to 100oC, is kept for 1 hour, and then 1oC/min is warming up to 320oC, keeps reaching 260 when temperature in 12 hours (4)oC constant temperature
12 ~ 48h removes heating mantle, is slowly cooled to room temperature, and opens hydrothermal reaction kettle, obtains grey black solution；(5) grey black is filtered
Solution is successively filtered by vacuum, supersound washing acquisition grey black sediment, and 40oC drying obtains clean grey black graphene-
LaFeO3Powder；(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in foam
On nickel, 40oC drying, obtains flake graphite alkene-LaFeO3Foam nickel electrode；(7) using the electrode prepared as working electrode,
It is the H for being 7% with mass fraction to electrode with platinum-base material2PtCl6.6H2Or Pt (NH3)2(NO2) 2 be electrolyte, current density
For 2A/dm3, time 1h, temperature 30oC is in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle, is obtained on foam nickel electrode
Obtain Pt/ graphene-LaFeO3Foamed nickel catalyst agent.
Embodiment 8
No. 4-hydro-thermal method prepares compound-nickel foam-electro-deposition preparation supporting Pt:
(1) graphite oxide aqueous solution is prepared using hummer method first, the brown color graphite oxide for obtaining 2mg/mL is water-soluble
Liquid；(2) using above-mentioned graphene oxide water solution as solvent, the La (NO that molar ratio is 1:15:6 is sequentially added thereto3)3 .6H2O, NaOH and Na2CO3, 15oMagnetic agitation 1h under C obtains brownish red suspension；(3) above-mentioned brown liquid is added
Special high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle, sealing；Then inert gas is passed through into reaction kettle, it is anti-for emptying
The air in kettle is answered, the matched agitating device of reaction kettle is opened, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas,
Hydrothermal reaction kettle is fully sealed, sets heating mantle, setting program heating: 1 in hydrothermal reaction kettle surroundingoThe heating rate of C/min
It is warming up to 100oC, is kept for 1 hour, and then 1oC/min is warming up to 320oC, keeps reaching 260 when temperature in 12 hours (4)oC constant temperature
12 ~ 48h removes heating mantle, is slowly cooled to room temperature, and opens hydrothermal reaction kettle, obtains grey black solution；(5) grey black is filtered
Solution is successively filtered by vacuum, supersound washing acquisition grey black sediment, and 40oC drying obtains clean grey black graphene-
LaFeO3Powder；(6) by electrically conductive graphite, binder, graphene-LaFeO3Powder mixing is suppressed under 3Mpa pressure in foam
On nickel, 40oC drying, obtains flake graphite alkene-LaFeO3Foam nickel electrode；(7) using the electrode prepared as working electrode,
It is to electrode with platinum-base material, is the H of 1:3 with mass ratio2PtCl6.6H2And NiSO4For electrolyte (total quality is 7%), electricity
Current density is 2A/dm3, time 1h, temperature 30oC is in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice on foam nickel electrode
Particle obtains Pt-Ni/ graphene-LaFeO3Foamed nickel catalyst agent.
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (5)
1. a kind of preparation method of platinum/graphen-perovskite-foamed nickel catalyst agent, it is characterised in that: (1) use first
Hummer method prepares graphite oxide aqueous solution, obtains the brown color graphite oxide aqueous solution of 0.5 ~ 2mg/mL；(2) with above-mentioned oxidation
Graphene aqueous solution is solvent, sequentially adds La (NO thereto3)3 .6H2O, NaOH and Na2CO3, 10 ~ 15oMagnetic agitation under C
1h obtains brownish red suspension；(3) high temperature resistant, high pressure, alkali corrosion hydrothermal reaction kettle is added in above-mentioned brown liquid, it is close
Envelope；Then it is passed through inert gas into reaction kettle, for emptying the air in reaction kettle, opens the matched stirring dress of reaction kettle
It sets, is stirred at room temperature 30 minutes, is then shut off the valve of inert gas, hydrothermal reaction kettle is fully sealed, in hydrothermal reaction kettle surrounding
Set heating mantle, setting program heating；(4) when temperature reaches 260oC~320o12 ~ 48h of constant temperature when C removes heating mantle, slowly cold
But to room temperature, hydrothermal reaction kettle is opened, obtains grey black solution；(5) grey black solution is filtered, is successively filtered by vacuum, ultrasound is washed
It washs and obtains grey black sediment, 40oC drying obtains clean grey black graphene-LaFeO3Powder；(6) by electrically conductive graphite, bonding
Agent, graphene-LaFeO3Powder mixing, under 3Mpa pressure, compacting is in nickel foam, and 40oC drying, obtains flake graphite alkene-
LaFeO3Foam nickel electrode；It (7) is to electrode, with mass fraction with platinum-base material using the electrode prepared as working electrode
For 1 ~ 7% H2PtCl6.6H2O or Pt (NH3)2(NO2)2For electrolyte, current density 1-2A/dm3, time 1-2h, temperature
25~30oC, in flake graphite alkene-LaFeO3Uniform deposition platinum sodium rice particle on foam nickel electrode obtains Pt/ graphene-
LaFeO3Foamed nickel catalyst agent.
2. preparation method as described in claim 1, wherein La (NO3)3 .6H2O:NaOH:Na2CO3Molar ratio be 1:10 ~ 15:
3~6。
3. such as the described in any item preparation methods of claims 1 or 2, wherein temperature-programmed mode are as follows: first with 1 ~ 2oC/min's
Heating rate is warming up to 100oC, is kept for 1 hour, and then 1 ~ 2oC/min is warming up to 260 ~ 320oC is kept for 12 ~ 48 hours, is terminated.
4. preparation method as described in claim 1, wherein the mode being filtered by vacuum is to be filtered using water-ring vacuum pump, ultrasound
The mode of washing is the dilute hydrochloric acid for the use of mass fraction being successively 5 ~ 7%, and anhydrous propanone, dehydrated alcohol, deionized water repeatedly washes
It washs.
5. preparation method as described in claim 1, wherein electrically conductive graphite, binder, graphene-LaFeO3The mass ratio of powder
It for 1:1:9 mixing, grinds in the agate mortar, and appropriate dehydrated alcohol is added and mixes, and will be in its even spread nickel foam.
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| CN103050572A (en) * | 2012-12-06 | 2013-04-17 | 燕山大学 | Perovskite/graphene composite membrane electrode manufacturing method |
| CN103736491A (en) * | 2014-01-17 | 2014-04-23 | 河北工业大学 | Graphene compounded methane catalyst and preparation method thereof |
| CN105186011A (en) * | 2015-06-17 | 2015-12-23 | 深圳大学 | Perovskite type/graphene composite material, preparation method and applications thereof |
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