CN105489906B - A kind of carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano and preparation method thereof - Google Patents
A kind of carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano and preparation method thereof Download PDFInfo
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- H01M4/90—Selection of catalytic material
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Abstract
The present invention relates to a kind of carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano as proton membrane fuel battery cathod redox reactions and preparation method thereof, it is black powder, the nano particle diameter for being carried on carbon nano tube surface is 10 15 nanometers, for core shell structure, core is palladium metal, and shell is vanadium phosphorus oxygen compound.It is prepared by oleyl amine revulsion.Method controllability provided by the present invention is strong, need not be passed through protective gas in thermal annealing process, safe operation, the anti methanol toxication of products therefrom catalyst and the stability of catalytic oxygen reduction reaction be improved significantly.
Description
Technical field
The invention belongs to elctro-catalyst field, and in particular to one kind is used as proton membrane fuel battery cathod redox reactions
Carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano and preparation method thereof.
Background technology
Methanol fuel cell is due to high-energy-density, low operating temperature, cleanliness without any pollution, it is portable the features such as, turn into
The study hotspot of current high-efficiency cleaning energy conversion apparatus.The anode reaction of methanol fuel cell is reacted for methanol electro-oxidizing, cloudy
Extremely redox reactions, because the redox reactions overpotential of its negative electrode is high, dynamics is slow, and reaction is difficult to, because
This is often using high surface area carbon loading platinum particle as elctro-catalyst.Because the cost of platinum is higher, in acidity
Under the conditions of long-play less stable so that the commercialization of methanol fuel cell is by high cost, the problems such as the low life-span
Greatly limitation.In addition, methanol crossover also has very big influence for the actual conversion performance of electrode and transformation efficiency.By
Separated in yin, yang the two poles of the earth of fuel cell by one layer of proton membrane, methanol is easier to penetrate into negative electrode, and is used as cathode catalysis
The platinum of material also has higher catalytic activity to methanol electro-oxidizing, therefore easily causes the mixed potential of negative electrode, makes anti-
Efficiency is answered significantly to decline.With platinum class seemingly, but price is relatively low for the atomic structure of palladium metal, therefore is reduced as novel oxygen
Catalysts cause extensive concern.Recent studies have found that palladium metal in the system containing methanol to redox reactions
With certain selectivity, but still tend to methanol oxidation and oxygen reduction while there is catalytic activity.In order to further change
The catalytic performance of kind palladium catalyst, shell can be introduced and form core shell structure, form physics resistance to reactive material from molecular level
Every making oxygen, the diffusion velocity of methanol molecules obtains selective control.So as to improve choosing of the catalyst to two kinds of electrocatalytic reactions
Selecting property.
The content of the invention
It is an object of the invention to solve palladium on carbon nano-particle for methanol oxidation and the catalysis of redox reactions choosing
The problem of selecting property is relatively low, causes negative electrode mixed potential, and transformation efficiency reduces, there is provided one kind is used as proton membrane fuel battery cathod oxygen
Carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano of gas reduction reaction and preparation method thereof, by a kind of easy
Easy-operating method introduces vanadium, phosphorus, oxygen compound as shell, forms core shell structure, the methanol tolerance oxidation for improving catalyst is steady
It is qualitative.
The present invention adopts the following technical scheme that：A kind of carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano, its
For black powder, the nano particle diameter for being carried on carbon nano tube surface is 10-15 nanometers, is core shell structure, core is porpezite
Category, shell is vanadium phosphorus oxygen compound.
The present invention also provides the preparation method of above-mentioned carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano, leads to
Oleyl amine revulsion is crossed, with palladium acetylacetonate, vanadium acetylacetonate is prepared as presoma, tri octyl phosphine as surfactant
Carbon nanotube loaded palladium-vanadium composite nanoparticle, then thermal anneal process through the air, obtain carbon nanotube loaded palladium@
Vanadium phosphorus oxygen compound core-shell nano, core are Pd nano particle, and shell is vanadium-phosphorus-oxygen compound.
In the preferred embodiment of the present invention, above-mentioned preparation method comprises the following steps that：
（1）Tri octyl phosphine is taken, leads to nitrogen 30 minutes, palladium acetylacetonate, the three of vanadium acetylacetonate addition nitrogen saturation are pungent
In base phosphine, ultrasound is allowed to fully dissolve；
（2）By step 1）Obtained mixed solution is injected into oleyl amine, is heated to 200-300 °C, is reacted 1 hour；
（3）By step 2）Solution after reaction terminates is added in n-hexane and alcohol mixed solution, makes a large amount of nano-particles
Separate out, by centrifuging the nano-particle separated out；
（4）By 10-100 mg CNTs ultrasonic disperses in 100-500 mL toluene solution, oleyl amine, stirring are added
Reaction, products therefrom pass through centrifugation；
（5）By step 3）And step 4）In obtained solid be scattered in again in 100-1000 mL n-hexanes, in 70-100
Solvent evaporated under the conditions of °C；
（6）By step 5）In obtained solid 80-300 °C is heated in Muffle furnace, be incubated 1-5 hours, obtain final
Product.
In the preferred embodiment of the present invention, step 1）Described tri octyl phosphine dosage is 0.5-5 mL, levulinic
Ketone palladium addition is 30-100 mg, and vanadium acetylacetonate addition is 10-100 mg.
In the preferred embodiment of the present invention, step 2）Described oleyl amine dosage is 1-10 mL.
In the preferred embodiment of the present invention, step 3）Described n-hexane addition is 5-20 mL, and ethanol adds
Measure as 10-50 mL.
In the preferred embodiment of the present invention, step 4）Described oleyl amine addition is 0.1-0.5 mL, and stirring is anti-
It it is 1-4 hours between seasonable.
The present invention obtains carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano grain by a kind of simple method
Son, products therefrom structure is unified, is evenly distributed, controllability is strong；The Muffle furnace of use makes annealing treatment, need not in thermal annealing process
It is passed through protective gas, safe operation, atomic rearrangement and oxide complex shell is realized while surfactant is removed
Formed, the anti methanol toxication of products therefrom catalyst and the stability of catalytic oxygen reduction reaction be improved significantly.
Brief description of the drawings
Fig. 1 is the transmission electricity that the carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano of gained is prepared in embodiment 1
Mirror figure；
Fig. 2 is the X ray that the carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano of gained is prepared in embodiment 1
Diffraction pattern；
Fig. 3 is that the carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano of gained is prepared in embodiment 1, business platinum/
The cyclic voltammetric and steady-state polarization of charcoal and carbon nanotube loaded Pd nano particle.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, without structure
Into limitation of the present invention.
Embodiment 1
（1）2 mL tri octyl phosphines are taken, lead to nitrogen 30 minutes, the mg of palladium acetylacetonate 58, the mg of vanadium acetylacetonate 22 are added
In the tri octyl phosphine of nitrogen saturation, ultrasound is allowed to fully dissolve；
（2）By step 1）Obtained mixed solution is injected into 5 mL oleyl amines, is heated to 300 °C, is reacted 1 hour；
（3）By step 2）Solution after reaction terminates is added in 5 mL n-hexanes and 30 mL alcohol mixed solutions, is made a large amount of
Nano-particle separates out, by centrifuging the nano-particle separated out；
（4）By 50 mg CNTs ultrasonic disperses in 200 mL toluene solution, 0.3 mL oleyl amines are added, stirring is anti-
Answer 4 hours, products therefrom passes through centrifugation；
（5）By step 3）And step 4）In obtained solid be scattered in again in 100 mL n-hexanes, under the conditions of 70 °C
Solvent evaporated；
（6）By step 5）In obtained solid 200 °C are heated in Muffle furnace, be incubated 3 hours, obtain final product；
Thus it is black powder that carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano, which is made, is carried on carbon and receives
The average grain diameter of the nano-particle of nanotube surface is 12 nanometers, is core shell structure, and core is palladium metal, and shell is not exclusively cladding
Vanadium phosphorus oxygen compound.
As seen from Figure 1, gained nano-particle is core shell structure, and the coarse endless site preparation of shell coats core.
As seen from Figure 2, the composition of shown nano-particle is palladium and vanadium, phosphorus, oxygen compound.
By preparing the carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano of gained and business in embodiment in Fig. 31
The cyclic voltammetric and steady-state polarization of platinum/charcoal and carbon nanotube loaded Pd nano particle are compared as can be seen that carbon nanometer
The methanol tolerance catalytic oxygen reduction reaction stability of pipe supported palladium@vanadium phosphorus oxygen compound core-shell nanos is higher.
Embodiment 2
（1）3 mL tri octyl phosphines are taken, lead to nitrogen 30 minutes, the mg of palladium acetylacetonate 73, the mg of vanadium acetylacetonate 38 are added
In the tri octyl phosphine of nitrogen saturation, ultrasound is allowed to fully dissolve；
（2）By step 1）Obtained mixed solution is injected into 5 mL oleyl amines, is heated to 300 °C, is reacted 1 hour；
（3）By step 2）Solution after reaction terminates is added in 20 mL n-hexanes and 50 mL alcohol mixed solutions, is made big
Measure nano-particle to separate out, by centrifuging the nano-particle separated out；
（4）By 100 mg CNTs ultrasonic disperses in 200 mL toluene solution, 0.5 mL oleyl amines are added, stirring is anti-
Answer 4 hours, products therefrom passes through centrifugation；
（5）By step 3）And step 4）In obtained solid be scattered in again in 500 mL n-hexanes, under the conditions of 70 °C
Solvent evaporated；
（6）By step 5）In obtained solid 300 °C are heated in Muffle furnace, be incubated 3 hours, obtain final product.
Thus it is black powder that carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano, which is made, is carried on carbon and receives
The average grain diameter of the nano-particle of nanotube surface is 15 nanometers, is core shell structure, and core is palladium metal, and shell is not exclusively cladding
Vanadium phosphorus oxygen compound.
Above embodiment describes the general principle and principal character of the present invention.The technical staff of the industry should
Understand, protection scope of the present invention is not restricted to the described embodiments, any change expected without creative work or
Replace, should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with claims institute
The protection domain of restriction is defined.
Claims (6)
1. a kind of preparation method of carbon nanotube loaded palladium@vanadium phosphorus oxygen compound core-shell nano, it is characterised in that step is such as
Under：
（1）Tri octyl phosphine is taken, leads to nitrogen 30 minutes, by palladium acetylacetonate, vanadium acetylacetonate adds the tri octyl phosphine of nitrogen saturation
In, ultrasound is allowed to fully dissolve；
（2）By step 1）Obtained mixed solution is injected into oleyl amine, is heated to 200-300 °C, is reacted 1 hour；
（3）By step 2）Solution after reaction terminates is added in n-hexane and alcohol mixed solution, separates out a large amount of nano-particles,
By centrifuging the nano-particle separated out；
（4）By 10-100 mg CNTs ultrasonic disperses in 100-500 mL toluene solution, addition oleyl amine, stirring reaction,
Products therefrom passes through centrifugation；
（5）By step 3）And step 4）In obtained solid be scattered in again in 100-1000 mL n-hexanes, at 70-100 °C
Under the conditions of solvent evaporated；
（6）By step 5）In obtained solid 80-300 °C is heated in Muffle furnace, be incubated 1-5 hours, finally produced
Thing.
2. preparation method according to claim 1, it is characterised in that step 1）Described tri octyl phosphine dosage is 0.5-5
ML, palladium acetylacetonate addition are 30-100 mg, and vanadium acetylacetonate addition is 10-100 mg.
3. preparation method according to claim 1, it is characterised in that step 2）Described oleyl amine dosage is 1-10 mL.
4. preparation method according to claim 1, it is characterised in that step 3）Described n-hexane addition is 5-20
ML, amount of alcohol added are 10-50 mL.
5. preparation method according to claim 1, it is characterised in that step 4）Described oleyl amine addition is 0.1-0.5
ML, stirring reaction time are 1-4 hours.
6. the carbon nanotube loaded palladium@vanadium phosphorus oxygen compound that the preparation method any one of claim 1-5 is prepared
Core-shell nano, it is characterised in that it is black powder, and the nano particle diameter for being carried on carbon nano tube surface is 10-15
Nanometer, is core shell structure, core is palladium metal, and shell is vanadium phosphorus oxygen compound.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5045297A (en) * | 1989-03-31 | 1991-09-03 | E. I. Du Pont De Nemours And Company | Selective oxidation of carbon monoxide in a mixture |
| CN1872417A (en) * | 2006-06-08 | 2006-12-06 | 武汉理工大学 | Nucleocapsid catalyst in use for fuel cell and preparation method |
| CN101664685A (en) * | 2009-09-27 | 2010-03-10 | 西北师范大学 | Low-platinum high active core-shell structure catalyst and preparation method thereof |
| CN102664275A (en) * | 2012-04-23 | 2012-09-12 | 北京化工大学 | Carbon-loaded kernel-shell copper-palladium-platinum catalyst for fuel battery and preparation method thereof |
| CN103191746A (en) * | 2013-03-20 | 2013-07-10 | 北京化工大学 | Carbon supported core-shell structure nano metal catalyst as well as preparation method and application thereof |
| CN104226312A (en) * | 2013-06-20 | 2014-12-24 | 北京化工大学 | Core-shell structure catalyst, and preparation method and application thereof |
-
2015
- 2015-11-30 CN CN201510854572.0A patent/CN105489906B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5045297A (en) * | 1989-03-31 | 1991-09-03 | E. I. Du Pont De Nemours And Company | Selective oxidation of carbon monoxide in a mixture |
| CN1872417A (en) * | 2006-06-08 | 2006-12-06 | 武汉理工大学 | Nucleocapsid catalyst in use for fuel cell and preparation method |
| CN101664685A (en) * | 2009-09-27 | 2010-03-10 | 西北师范大学 | Low-platinum high active core-shell structure catalyst and preparation method thereof |
| CN102664275A (en) * | 2012-04-23 | 2012-09-12 | 北京化工大学 | Carbon-loaded kernel-shell copper-palladium-platinum catalyst for fuel battery and preparation method thereof |
| CN103191746A (en) * | 2013-03-20 | 2013-07-10 | 北京化工大学 | Carbon supported core-shell structure nano metal catalyst as well as preparation method and application thereof |
| CN104226312A (en) * | 2013-06-20 | 2014-12-24 | 北京化工大学 | Core-shell structure catalyst, and preparation method and application thereof |
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