CN108686677A - Nano catalytic material Preparation method and use with palladium oxide shell-nickel oxide nuclear structure - Google Patents
Nano catalytic material Preparation method and use with palladium oxide shell-nickel oxide nuclear structure Download PDFInfo
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- CN108686677A CN108686677A CN201810440142.8A CN201810440142A CN108686677A CN 108686677 A CN108686677 A CN 108686677A CN 201810440142 A CN201810440142 A CN 201810440142A CN 108686677 A CN108686677 A CN 108686677A
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- 229910003445 palladium oxide Inorganic materials 0.000 title claims abstract description 40
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 33
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 title description 27
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000002245 particle Substances 0.000 claims abstract description 70
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 35
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 235000011187 glycerol Nutrition 0.000 claims abstract description 15
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 claims abstract 13
- 239000000243 solution Substances 0.000 claims description 25
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine hydrate Chemical class O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 9
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 5
- 229910001453 nickel ion Inorganic materials 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 229910017920 NH3OH Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- PYRZPBDTPRQYKG-UHFFFAOYSA-N cyclopentene-1-carboxylic acid Chemical compound OC(=O)C1=CCCC1 PYRZPBDTPRQYKG-UHFFFAOYSA-N 0.000 claims 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006073 displacement reaction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- -1 metal oxide compound Chemical class 0.000 abstract 1
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 13
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 150000002940 palladium Chemical class 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002816 nickel compounds Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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
- B01J23/70—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
- B01J23/892—Nickel and noble metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
- B01J35/398—Egg yolk like
-
- 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
- B01J37/12—Oxidising
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Biomedical Technology (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of nano catalytic material preparation methods with palladium oxide shell-nickel oxide nuclear structure, the method comprises the steps of firstly, preparing nano metal nickel particles, Metal Palladium electrode potential is then utilized to be higher than the property of metallic nickel, being reacted with the displacement of palladium ion by nickel particles surface in palladium ion solution makes palladium ion restore and be deposited on the Metal Palladium clad that nickel particles surface formation thickness is nanometer scale by metallic nickel, obtains the nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle.In glycerine, the nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle is oxidized to ozone and can be used as vehicle exhaust gas systems material, the nano-oxide compound particle with palladium oxide shell-nickel oxide nuclear structure.The present invention prepares the nano-noble metal oxide compound particle with palladium oxide shell-nickel oxide nuclear structure, to substitute the palladium oxide particle used in current catalytic purifier for motor vehicle exhaust.
Description
Technical field
The present invention provides a kind of nano catalytic material preparation methods with palladium oxide shell-nickel oxide nuclear structure, belong to
Sparking machine testing commissioning device field.
Technical background
Palladium oxide is a kind of catalytic purification of motor vehicle tail gas material of function admirable.Currently, in catalytic cleaning of car tail gas
It is that a certain amount of palladium salt is made an addition into slurry (the also known as water prepared by powder-type coating material and water mixing and ball milling in material preparation
Pulp washing material, English washcoat) in and it is close coated on catalyst carrier (generally honeycomb ceramic carrier or metal beehive carrier)
The surface for collecting passage aisle is then coated with the carrier heating roasting molding of catalyst.In sintering process, the palladium salt in slurry
Fired and oxidation transformation is attached in the coating material of catalyst support surface and sub-micron or micron with catalytic action
Grade palladium oxide particle.Since the palladium oxide particle used as motor vehicle vent gas purification catalysis material is mainly in catalytic process
The palladium atom of particle surface participates in catalysis reaction, and the palladium atom of particle center portion is not joined generally because that can not contact tail gas molecule
It is reacted with catalysis, therefore reduces effective rate of utilization of palladium during exhaust purification catalytic in tail gas cleaner for motor-driven vehicle.Therefore,
Present inventor (ZL 201310272768.X) in patent of invention before proposes a kind of method making nano palladium oxide,
So that catalyst washing slurry, which is added, and roasts the variation of chemical form will not occur again during molding, while oxidation is improved
The available specific surface area of palladium.Simultaneously a kind of method making nano-hollow palladium oxide is invented to further increase using oxidation
The specific surface area of palladium reduces required palladium oxide amount under the premise of ensureing same specific surface area.But in use
It was found that high temperature (1000 DEG C) behind efficiency reduces, it is possible to heat occur and cave in because of the insufficient strength of hollow-core construction.Purport of the present invention
The shortcomings that overcoming two technologies in front, kernel of the nickel core as nano palladium oxide is made, enhances the intensity of nano-particle, significantly
Promote the available specific surface area of nano palladium oxide.Purpose be meet country about automotive emission standard under the premise of,
The effective rate of utilization for further increasing palladium in tail gas cleaner for motor-driven vehicle reduces motor vehicle to reduce the dosage of precious metal palladium
The production cost of vent gas catalytic cleaner.
Invention content
It is an object of the invention to prepare a kind of coat with palladium oxide to aoxidize nickel particles (i.e. with palladium oxide shell-nickel oxide
Nuclear structure), can be used as the nano-oxide compound particle of catalytic purification of motor vehicle tail gas.Due to palladium oxide shell-nickel oxide
The nano-oxide compound particle center portion of nuclear structure is nickel oxide, when as catalytic purification of motor vehicle tail gas materials'use, with
Solid palladium particle used in current motor vehicle vent gas purification catalysis coating is compared, in motor vehicle tail-gas purifying effect phase
With in the case of, the dosage of precious metal palladium can be reduced, the effective rate of utilization of palladium is improved, reduces catalytic purifier for motor vehicle exhaust
Production cost.
In order to achieve the above objectives, the present invention uses following technical scheme to realize.
Nano-oxide compound particle preparation of the present invention with palladium oxide shell-nickel oxide nuclear structure is by following
What technological approaches was realized.
A kind of nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure, includes the following steps:
The first step:Prepare metallic Ni particles;
Second step:In metallic Ni particles expoeridium palladium metal, nanometer metal palladium-nickel with palladium shell-nickel nuclear structure is made
Compound particle;
Third walks:Using glycerine as nanometer metal palladium-nickel compound particle carrier fluid, and heat glycerine to 250 DEG C or more,
And the nano-oxide compound particle of palladium oxide shell-nickel oxide nuclear structure is prepared using ozone as oxidant.
Further to improve, the method that metallic Ni particles are prepared in the first step is:Configuration concentration is 0.5mol/l's
Nickel sulfate solution 1000ml, and complexing agent sodium citrate is added by the ﹕ 2 of nickel sulfate/sodium citrate molar ratio=1;500ml is taken to be hydrated
NH is added in hydrazine3It is 11 that OH, which adjusts hydrazine hydrate solution pH value,;Under the conditions of room temperature and mechanical agitation and ultrasonic vibration, by hydrazine hydrate
With NH3OH mixed solutions pour into nickel sulfate solution and react 5 minutes, make hydrazine hydrate reduction nickel ion nano metal nickel particles.
Further to improve, the average diameter grain of the nickel particles is 200nm.
Further to improve, the second step includes the following steps:Configuration concentration is the palladium nitrate solution of 0.2mol/l
1000ml, it is 3 that nitric acid, which is added, and adjusts palladium nitrate solution pH value;Under room temperature and mechanical agitation, by nickel particles deionization
It makes an addition in palladium nitrate solution and reacts 20 minutes after water cleaning, obtain having nanometer metal palladium-nickel of palladium shell-nickel nuclear structure compound
Particle.
Further to improve, in the third step, the heating temperature of glycerine is 275~285 DEG C.
Further to improve, the speed that is passed through of the ozone is 1 liter per minute.
Palladium oxide shell-oxygen made from the above-mentioned nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure
The nano-oxide compound particle for changing nickel nuclear structure is used for motor vehicle tail-gas purifying.
Specifically, the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure is as follows:
The first step:Simultaneously a certain amount of complexing agent is added in configuration nickel ion solution.A certain amount of alkali is added in reducing agent hydrazine hydrate
Property solution adjust its pH value be strong basicity.Mixed Ni solion and hydrazine hydrate solution prepare nano level metal nickel particles.
Second step:It prepares palladium ion solution and a certain amount of complexing agent is added.The nickel particles of preparation are placed in acidity, are utilized
Metal Palladium electrode potential is higher than the property of metallic nickel electrode potential, by between palladium ion in nickel particles surface nickel atoms and solution
Displacement reaction, so that palladium ion in solution restore and be deposited on the gold that nickel particles surface forms thickness as nanometer scale by metallic nickel
Belong to palladium clad, nanometer metal palladium-nickel compound particle with palladium shell-nickel nuclear structure is made.
Third walks:With oxidizing above-mentioned nanometer metal palladium shell-nickel core compound particle, it is made to be changed into nano palladium oxide
Shell-nickel oxide core compound particle.In this regard, the nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle is placed in by the present invention
In glycerine, heating glycerine is to 260~285 DEG C, then the ozone generated by ozone generator is imported and contains nanometer metal palladium-
In the glycerine of nickel compound particle, oxidation nanometer Metal Palladium-nickel compound particle becomes nano palladium oxide shell-compound grain of nickel oxide core
Son, it is multiple to obtain can be used as vehicle exhaust gas systems material, the nano-oxide with palladium oxide shell-nickel oxide nuclear structure
Close particle.
Third step is a crucial step of the invention in above-mentioned technological approaches, i.e., must make the metal state nickel of compound particle center portion
Atom is substantially oxidized as nickel oxide, to prevent the metal state nickel of the compound particle center portion remaining under high-temperature catalytic working condition former
Son due to there is higher migration to compound particle diffusion into the surface, to reduce the superficial catalytic activation of compound particle.To prevent
Reunion when nanometer metal palladium-nickel compound particle aoxidizes in air, present invention employs the palladium of oxidized metal in the liquid phase-nickel is multiple
The method for closing particle.For this purpose, nanometer metal palladium-nickel compound particle is placed in glycerine (290 DEG C of boiling point), heating glycerine is extremely
260~285 DEG C, then the ozone generated by ozone generator importing ozone is contained the third the three of nanometer metal palladium-nickel compound particle
Nanometer metal palladium-nickel compound particle is oxidized to palladium oxide by the oxidant in alcohol as nanometer metal palladium-nickel compound particle
The nano-oxide compound particle of shell-nickel oxide nuclear structure.In oxidation process, it for the purpose of oxidant is using smelly to use ozone
The importing of carrier of oxygen plays the role of unordered stirring and prevents particle aggregation.The purpose for heating glycerine to 260~285 DEG C is logical
It crosses and improves oxidizing temperature and promote oxygen atom to the diffusion of nanometer metal palladium-nickel compound particle center portion, to realize to Metal Palladium-
Nickel compound particle it is fully oxidized.
Description of the drawings
Fig. 1 is nano palladium oxide-nickel oxide compound particle figure;
Fig. 2 is the X-ray diffraction spectrogram of nano palladium oxide-nickel oxide compound particle.
Specific implementation mode
Embodiment 1
Configuration concentration is the nickel sulfate solution 1000ml of 0.5mol/l, and by the ﹕ 2 of nickel sulfate/sodium citrate molar ratio=1 plus
Enter complexing agent sodium citrate.500ml hydrazine hydrates are taken, a certain amount of NH is added3It is 11 that OH, which adjusts hydrazine hydrate solution pH value,.In room temperature and
Under the conditions of mechanical agitation and ultrasonic vibration, by hydrazine hydrate and NH3OH mixed solutions pour into nickel sulfate solution and react 5 minutes, make water
It closes hydrazine and restores nickel ion, the metallic Ni particles that obtained average grain diameter is about 200nm.
Configuration concentration is the palladium nitrate solution 1000ml of 0.2mol/l, and a certain amount of nitric acid is added and adjusts palladium nitrate solution pH value
It is 3.Under room temperature and mechanical agitation, palladium nitrate is made an addition to after nanometer nickel particles obtained above are spent ionized water cleaning
It is reacted 20 minutes in solution, obtains the nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle.
500ml is made an addition to after nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle is cleaned with deionized water
Glycerine in, glycerine of the heating containing nanometer metal palladium-nickel compound particle is to 275~285 DEG C, and with 1 liter per minute
Flow is passed through ozone oxidation Metal Palladium-nickel compound particle 20 minutes thereto, is made with palladium oxide shell-nickel oxide nuclear structure
Nano palladium oxide-nickel oxide compound particle, pattern is as shown in Fig. 1, and attached drawing 2 is prepared with palladium oxide shell-nickel oxide
X-ray diffraction spectra of the nano palladium oxide of nuclear structure-nickel oxide compound particle.
According to experiment, above-mentioned a condition can carry out a certain amount of adjusting, such as the diameter grain of metallic Ni particles, in 150-
250nm, that is reacted in palladium nitrate solution can also can be adjusted as needed often.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made by within principle etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure, which is characterized in that including as follows
Step:
The first step:Prepare metallic Ni particles;
Second step:In metallic Ni particles expoeridium palladium metal, it is compound that nanometer metal palladium-nickel with palladium shell-nickel nuclear structure is made
Particle;
Third walks:Using glycerine as nanometer metal palladium-nickel compound particle carrier fluid, and glycerine is heated to 250 DEG C or more, and with
The nano-oxide compound particle of palladium oxide shell-nickel oxide nuclear structure is prepared as oxidant for ozone.
2. the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure as described in claim 1, feature
It is, the method that metallic Ni particles are prepared in the first step is:Configuration concentration is the nickel sulfate solution 1000ml of 0.5mol/l,
And complexing agent sodium citrate is added by the ﹕ 2 of nickel sulfate/sodium citrate molar ratio=1;500ml hydrazine hydrates are taken, NH is added3OH is adjusted
Hydrazine hydrate solution pH value is 11;Under the conditions of room temperature and mechanical agitation and ultrasonic vibration, by hydrazine hydrate and NH3OH mixed solutions fall
Enter nickel sulfate solution to react 5 minutes, makes hydrazine hydrate reduction nickel ion, obtain nano metal nickel particles.
3. the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure as claimed in claim 2, feature
It is, the average diameter grain of the nickel particles is 200nm.
4. the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure as described in claim 1, feature
It is, the second step includes the following steps:Configuration concentration is the palladium nitrate solution 1000ml of 0.2mol/l, and nitric acid is added and adjusts
Palladium nitrate solution pH value is 3;Under room temperature and mechanical agitation, palladium nitrate is made an addition to after nickel particles are cleaned with deionized water
It is reacted 20 minutes in solution, obtains the nanometer metal palladium with palladium shell-nickel nuclear structure-nickel compound particle.
5. the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure as described in claim 1, feature
It is, in the third step, the heating temperature of glycerine is 275~285 DEG C.
6. the nano catalytic material preparation method with palladium oxide shell-nickel oxide nuclear structure as described in claim 1, feature
It is, the speed that is passed through of the ozone is 1 liter per minute.
7. any nano catalytic material preparation method systems with palladium oxide shell-nickel oxide nuclear structure of claim 1-6
The nano-oxide compound particle of the palladium oxide shell-nickel oxide nuclear structure obtained is used for motor vehicle tail-gas purifying.
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