CN109499565A - A kind of method that one-step method prepares carbon supported platinum nano particle - Google Patents
A kind of method that one-step method prepares carbon supported platinum nano particle Download PDFInfo
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- CN109499565A CN109499565A CN201910001774.9A CN201910001774A CN109499565A CN 109499565 A CN109499565 A CN 109499565A CN 201910001774 A CN201910001774 A CN 201910001774A CN 109499565 A CN109499565 A CN 109499565A
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- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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Abstract
The invention belongs to function nano technical field of material, provide a kind of method that one-step method prepares carbon supported platinum nano particle.This method is added deionized water and configures reaction solution, act on the solution using normal pressure microplasma under argon atmosphere and reacted, can directly generate carbon supported platinum nano particle using ethyl alcohol and platinum presoma as raw material.Compared with prior art, this method is simple and quick, environmentally protective, controllability is good, is without the use of reducing agent, there is great directive significance and application prospect in terms of preparing function nano material.
Description
Technical field
The invention belongs to function nano technical field of material, and in particular to a kind of one-step method prepares carbon supported platinum nano
The method of particle.
Technical background
Carbon supported platinum nano particle is good catalyst, in environmental improvement, petrochemical industry, fuel cell, fragrance, dyestuff
Equal fields are widely used.Traditional preparation method be using impregnation-reduction method, by carbon carrier be immersed in containing platinum from
Son solution in, make a certain amount of platinum ion of its adsorption, then by drying, roasting, reduction and etc. obtain target production
Product.But this method technique is cumbersome, the reaction time is long, energy consumption is high, very sensitive to the acid-base property of solution, and is difficult control load
The size and content of Pt nanoparticle on carbon.
Patent CN200510049593.1 disclose it is a kind of using ethylene glycol be solvent and reducing agent, carbon carrier is dispersed in
The method of carbon supported platinum nano particle is prepared in ethylene glycol containing platinum salt and acetate.This method not only needs to add volume
Outer carbon carrier, and need to be heated to 160-180 DEG C, react 2-3h；The present invention is directly generated by ethyl alcohol during the reaction
Carbon carrier, and be not required to heat, reacting 5-10min at normal temperature can be obtained target product.
Patent CN201610069833.2 disclose it is a kind of using ultrasound and stirring alternate treatment carboxylic carbon nano-tube, second
Two pure and mild platinum base precursor mixtures, the method for preparing carbon nanotube loaded platinum base nanocatalyst.This method complex steps, no
Only carbon nanotube, which will pass through free radical functionalization, the pretreatment process such as carboxylated, and reaction process, needs ultrasound and stir process
20-40h, simultaneous reactions temperature is controlled at 160 to 197 DEG C, less economical；The present invention is not required to any pretreatment process, under room temperature
Reaction 5-10min can be obtained target product.
Plasmaassisted preparation nano material is a kind of novel green synthesis method, since its activity is high, reaction speed
The advantages such as fast, pollution-free are spent, are paid attention to by numerous scientific workers at present.
Patent CN201710481112.7, which is disclosed, a kind of prepares mesoporous carbon-loaded palladium nano-particles using electric glow discharge method
Method.This method also will additionally add mesoporous carbon carrier, and reaction solution need to be by the pretreatment work such as stirring, centrifugation and drying
Sequence.In addition, this method carries out under vacuum, it need to be vacuumized pressure control with vacuum pump in 60Pa-120Pa, and the function that discharges
Rate is 330W-660W, and production cost has been significantly greatly increased；The present invention is not required to any pretreatment process, directly raw during the reaction
It is carried out at carbon carrier, and under normal pressure, does not have to additional configuration vacuum equipment.In addition, discharge power of the invention only needs 2W-5W,
With very high economy.
Patent CN201810637595.X, which is disclosed, a kind of utilizes radio frequency plasma irradiation load and complex catalyst precursor
The method that body prepares loaded catalyst.This method not only will additionally add load, while alcohols being needed to mention as oxygen source solvent
Oxygen supply.In addition reaction process plasma reaction chamber needs vacuum equipment to vacuumize pressure control in 0.1Pa-1Pa, and discharges
Power is up to 50~500W.The present invention is not required to additionally add load, directly generates during the reaction.Furthermore this method is normal
Pressure carries out, and power only needs 2W-5W, without any oxygen source solvent.Process flow is greatly simplified, production cost is reduced.
As a development branch of plasma technique, microplasma preparation nano material is increasingly becoming one in recent years
A new research hotspot, it has, and at low cost, small in size, structure is simple, security risk is small, can run, have very under atmospheric pressure
The advantages that high active particle density and good stability.Have at present and prepares nano silver using microplasma technology, receives
The report (Yan T.et al, Chem.Commun.2014,50 (24), 3144-3147) of rice electrum, but there is no to utilize and be somebody's turn to do
Technology one-step method prepares the report of carbon supported platinum nano particle.The present invention utilizes the advantage of microplasma technology, while by platinum
Presoma and carbon source (ethyl alcohol) mixing are made into reaction solution, open one in normal pressure not by any chemical reducing agent one-step method
Synthesize the approach of carbon supported platinum nano particle.
Summary of the invention
In view of the deficiencies of the prior art, the present invention utilizes many advantages of the microplasma in terms of preparing nano material,
It is proposed a kind of method that carbon supported platinum nano particle is prepared based on microplasma technology one-step method.This method has normal temperature and pressure
It operates, be simple and efficient, is environmentally protective, is low in cost, controllability is good, excellent without using any surfactant and chemical reducing agent etc.
Gesture.
Technical solution of the present invention:
A kind of method that one-step method prepares carbon supported platinum nano particle, steps are as follows:
(1) using deionized water as solvent, ethyl alcohol and platinum presoma are rapidly joined in deionized water and is stirred evenly, obtained anti-
Answer solution.
(2) it takes 10mL reaction solution to be added in microplasma reactor, microplasma reactor is placed in magnetic force and is stirred
It mixes on device, even good reaction unit.It opens mass flowmenter and leads to 5min argon gas, argon flow 20sccm, it is ensured that inert atmosphere.
(3) magnetic agitation meter, revolving speed 200rpm, it is ensured that Pt nanoparticle energy uniform load is on carbon are opened；Increase simultaneously
Big argon flow opens DC power supply, generates microplasma discharge and act on reaction solution, then adjust electricity to 50sccm
Pressure guarantees plasma power in 2-5W, and reaction produces carbon supported platinum nano particle.
Further, in the reaction solution volume fraction of ethanol be 15%-25%, Pt ion concentration be 0.15~
1.5mM。
Further, the platinum presoma is chloroplatinic acid.
Further, the microplasma processing reaction solution time is 5-10min.
Further, in the carbon supported platinum nano particle, the Pt nanoparticle average-size being supported on carbon is 2-
6nm.By volume fraction of ethanol and Pt ion concentration in control reaction solution, the load of Pt nanoparticle in product is adjusted
Amount.
The principle of the present invention: the present invention utilize microplasma nonequilibrium behavior, allow part high-energy electron deexcitation,
It cracks ethyl alcohol and generates nano-sized carbon, while part electronics can also restore platinum ion generation Platinum Nanoparticles and be directly loaded on carbon.In addition, anti-
Solution is continuously agitated during answering, and can ensure that Pt nanoparticle is uniformly supported on carbon.
The method of the present invention the utility model has the advantages that
(1) it carries out at normal temperatures and pressures, is not required to be equipped with additional vacuum system；
(2) reaction power is extremely low, substantially reduces production cost；
(3) easy to operate, reaction speed is fast, and one-step method obtains carbon supported platinum nano particle；
(4) it is not required to any surfactant, stabilizer and chemical reducing agent, it is environmentally protective；
(5) controllability is good, can flexibly control the load capacity of platinum.
Detailed description of the invention
Fig. 1 is the TEM pattern of carbon supported platinum nano particle made from the embodiment of the present invention 1.
Fig. 2 is the TEM diffraction pattern of carbon supported platinum nano particle made from the embodiment of the present invention 1.
Fig. 3 is the TEM pattern of carbon nano-particle made from the embodiment of the present invention 2.
Fig. 4 is the TEM diffraction pattern of carbon nano-particle made from the embodiment of the present invention 2.
Fig. 5 is the TEM pattern of carbon supported platinum nano particle made from the embodiment of the present invention 3.
Fig. 6 is the TEM pattern of carbon supported platinum nano particle made from the embodiment of the present invention 4.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated.
Embodiment 1
After microplasma reactor is washed with deionized water completely, it is dried for standby.Using deionized water as solvent, by ethyl alcohol and
Chloroplatinic acid, which rapidly joins, stirs evenly configuration reaction solution in deionized water.Wherein volume fraction of ethanol is 20%, deionized water
Volume fraction is 80%, and chloroplatinic acid concentration is 0.9mM.It takes the above-mentioned solution of 10mL to be added in microplasma reactor, will react
Device is placed on magnetic stirring apparatus, even good reaction unit.The logical 5min argon gas of opening mass flowmenter, argon flow 20sccm, really
Protect inert atmosphere.Magnetic agitation meter, revolving speed 200rpm are opened later, and increase argon flow to 50sccm.Open direct current
Source generates microplasma discharge and acts on reaction solution, and control plasma power reacts 10min in 3W or so
Obtain the solution of carbon containing supported platinum nano particle.
The above-mentioned reacted solution of a drop is taken to carry out transmission electron microscope detection, as a result as shown in Figure 1.It can be seen that there is platinum nanometer
Particles generation, and being uniformly supported on carbon, the size of platinum grain in 2-6nm, illustrate this method can a step prepare carbon Supported Pt Nanoparticles
Nano particle.Fig. 2 shows the TEM diffraction pattern of carbon supported platinum nano particle made from this method, diffraction ring just with the difference of platinum
Crystal face is corresponding, it was demonstrated that Pt nanoparticle generated is crystalline structure, and carbon is amorphous structure.
Embodiment 2
With embodiment 1, difference is for treatment process and operating condition: solution does not have chlorination platinic acid.
The above-mentioned reacted solution of a drop is taken to carry out transmission electron microscope detection, as a result as shown in Figure 3, it can be seen that have carbon nanometer
Particles generation.Fig. 4 shows the TEM diffraction pattern of carbon nano-particle made from this method, does not see diffraction ring, further proves
The carbon nano-particle arrived is amorphous structure.
Embodiment 3
With embodiment 1, difference is for treatment process and operating condition: the concentration of Chlorine in Solution platinic acid is 0.15mM.
The above-mentioned reacted solution of a drop is taken to carry out transmission electron microscope detection, as a result as shown in Figure 5, it can be seen that have a small amount of
Pt nanoparticle is generated and is supported on carbon, illustrates that this method can adjust Pt nanoparticle by controlling the concentration of chloroplatinic acid
Load capacity.
Embodiment 4
With embodiment 1, difference is for treatment process and operating condition: the concentration of Chlorine in Solution platinic acid is 1.5mM.
The above-mentioned reacted solution of a drop is taken to carry out transmission electron microscope detection, as a result as shown in Figure 6, it can be seen that have a large amount of
Pt nanoparticle is generated and is supported on carbon, further proves that this method can be received by controlling the concentration of chloroplatinic acid to adjust platinum
The load capacity of rice grain.
The figures above and specific embodiment explain the present invention in detail.It is to be appreciated that the present invention is unlimited
In above-mentioned specific real mode.Those skilled in the art can do various deformations or amendments within the scope of the claims, this is not
Influence substantive content of the invention.
Claims (10)
1. a kind of method that one-step method prepares carbon supported platinum nano particle, which comprises the following steps:
(1) using deionized water as solvent, ethyl alcohol and platinum presoma are rapidly joined in deionized water and is stirred evenly, it is molten to obtain reaction
Liquid；
(2) it takes 10mL reaction solution to be added in microplasma reactor, microplasma reactor is placed in magnetic stirring apparatus
On, connect good reaction unit；It opens mass flowmenter and leads to 5min argon gas, argon flow 20sccm, it is ensured that inert atmosphere；
(3) magnetic agitation meter, revolving speed 200rpm, it is ensured that Pt nanoparticle energy uniform load is on carbon are opened；Increase argon simultaneously
Throughput opens DC power supply, generates microplasma discharge and act on reaction solution, then adjust voltage and protect to 50sccm
Plasma power is demonstrate,proved in 2-5W, reaction produces carbon supported platinum nano particle.
2. the method that a kind of one-step method according to claim 1 prepares carbon supported platinum nano particle, which is characterized in that described
Volume fraction of ethanol is 15%-25% in reaction solution, and Pt ion concentration is 0.15~1.5mM.
3. the method that a kind of one-step method according to claim 1 or 2 prepares carbon supported platinum nano particle, which is characterized in that
The platinum presoma is chloroplatinic acid.
4. the method that a kind of one-step method according to claim 1 or 2 prepares carbon supported platinum nano particle, which is characterized in that
The microplasma processing reaction solution time is 5-10min.
5. the method that a kind of one-step method according to claim 3 prepares carbon supported platinum nano particle, which is characterized in that described
Microplasma handles the reaction solution time as 5-10min.
6. according to claim 1, a kind of method that one-step method prepares carbon supported platinum nano particle, feature described in 2 or 5 exist
In in the carbon supported platinum nano particle, the Pt nanoparticle average-size being supported on carbon is 2-6nm.
7. the method that a kind of one-step method according to claim 3 prepares carbon supported platinum nano particle, which is characterized in that in institute
It states in carbon supported platinum nano particle, the Pt nanoparticle average-size being supported on carbon is 2-6nm.
8. the method that a kind of one-step method according to claim 4 prepares carbon supported platinum nano particle, which is characterized in that in institute
It states in carbon supported platinum nano particle, the Pt nanoparticle average-size being supported on carbon is 2-6nm.
9. according to claim 1, a kind of method that one-step method prepares carbon supported platinum nano particle, feature described in 2,5,7 or 8
It is, by volume fraction of ethanol and Pt ion concentration in control reaction solution, adjusts the load capacity of platinum in product.
10. the method that a kind of one-step method according to claim 6 prepares carbon supported platinum nano particle, which is characterized in that logical
Volume fraction of ethanol and Pt ion concentration in control reaction solution are crossed, the load capacity of platinum in product is adjusted.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113828303A (en) * | 2021-09-15 | 2021-12-24 | 江南大学 | High-value utilization method of precious metal waste catalyst |
| CN113828303B (en) * | 2021-09-15 | 2024-05-28 | 江南大学 | High-value utilization method of noble metal waste catalyst |
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| CN102600835A (en) * | 2012-03-16 | 2012-07-25 | 南京大学 | Preparation method of hollow carbon nanocage loaded platinum-based composite catalysts |
| CN104190412A (en) * | 2014-08-29 | 2014-12-10 | 北京大学 | Platinum/carbon-based nano composite material, and preparation method and application thereof |
| CN108855166A (en) * | 2018-06-20 | 2018-11-23 | 郑州轻工业学院 | A kind of loaded catalyst and preparation method thereof, application |
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- 2019-01-02 CN CN201910001774.9A patent/CN109499565B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102600835A (en) * | 2012-03-16 | 2012-07-25 | 南京大学 | Preparation method of hollow carbon nanocage loaded platinum-based composite catalysts |
| CN104190412A (en) * | 2014-08-29 | 2014-12-10 | 北京大学 | Platinum/carbon-based nano composite material, and preparation method and application thereof |
| CN108855166A (en) * | 2018-06-20 | 2018-11-23 | 郑州轻工业学院 | A kind of loaded catalyst and preparation method thereof, application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113828303A (en) * | 2021-09-15 | 2021-12-24 | 江南大学 | High-value utilization method of precious metal waste catalyst |
| CN113828303B (en) * | 2021-09-15 | 2024-05-28 | 江南大学 | High-value utilization method of noble metal waste catalyst |
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