CN106669664A - Preparation method of water/ethylene glycol co-heating-based reduced graphene oxide loaded nano platinum composite material - Google Patents
Preparation method of water/ethylene glycol co-heating-based reduced graphene oxide loaded nano platinum composite material Download PDFInfo
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- CN106669664A CN106669664A CN201611197807.4A CN201611197807A CN106669664A CN 106669664 A CN106669664 A CN 106669664A CN 201611197807 A CN201611197807 A CN 201611197807A CN 106669664 A CN106669664 A CN 106669664A
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- graphene oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/44—Palladium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of a water/ethylene glycol co-heating-based reduced graphene oxide loaded nano platinum composite material. The preparation method comprises the following steps: preparing an aqueous solution of chloroplatinic acid and an ethylene glycol solution of graphene oxide GO, putting a reaction kettle in a tubular furnace, and heating the tubular furnace at a temperature-raising rate of 10 DEG C/min to a reaction temperature, wherein the reaction temperature is 180-220 DEG C and the reaction lasts for 2 hours; and after reaction, obtaining a block, washing the block with pure water and ethanol successively, and then performing vacuum drying to obtain the reduced graphene oxide loaded nano platinum composite material rGO/Pt. The preparation method disclosed by the invention has the advantages that the preparation method is simple in process, economical and environment-friendly and high in utilization ratio of graphene oxide, and the structure and property of the integral composite material are stable and reliable.
Description
Technical field
The invention belongs to the preparation field of load type metal catalyst, specifically refer to a kind of redox graphene load and receive
Miboplatin composite（rGO/Pt）Preparation method.
Background technology
Nano-catalytic is increasingly subject to the attention of people as an important branch of nanometer technology.Nanometer alloy platinum material is used as one
Important Industrial Catalysis material is planted, is had in fields such as petroleum cracking, sulfuric acid preparation, fuel cell, vehicle maintenance services
Extensive purposes.Alloy platinum material (Pt) price is high, in order to reduce the consumption of platinum and keep catalytic performance high, leads in practical application
Pt nano particle is often carried on different base（Support carrier）.
Graphene is another new carbon after fullerene and CNT, is current world field of new
The focus of research.Grapheme material has many excellent performances, such as good conductive and heat conductivility, the machinery of superelevation are by force
The electrical properties of degree and uniqueness, are that Pt catalyst preferably supports carrier.The grapheme material of broad sense includes Graphene and its spreads out
It is biological（Graphene oxide GO and redox graphene rGO）.RGO refers to not exclusively to be removed by the method such as chemically or thermally
A kind of two-dimentional carbon material obtained after oxygen-containing functional group in graphene oxide, can show during as catalytic carrier and compare stone
Black alkene and the bigger specific surface areas of graphene oxide GO and electro-chemical activity（Referring to Wang Zegao, graphene film and reduction-oxidation
The controllable preparation of graphene powder and Study of effects of doping [Ph.D. Dissertation], University of Electronic Science and Technology, 2014）.
Currently, redox graphene load Platinum Nanoparticles composite（rGO/Pt）Preparation mainly use ethylene glycol solvent
Hot method, with graphene oxide GO and chloroplatinic acid as raw material, ethylene glycol plays dual parts of solvent and reducing agent, makes graphite oxide
Alkene GO and chloroplatinic acid are separately converted to redox graphene rGO and Pt nano particle.For example, Gao Haili etc. is using ethylene glycol solvent warm
One-step method is prepared for rGO/Pt, and is applied to the electro-catalysis of methyl alcohol oxidation（Referring to Gao Haili etc., one-step method prepares reduction-state oxygen
Graphite alkene carries nano platinum particle and its electrocatalysis characteristic to methyl alcohol oxidation,Acta PhySico-Chimica Sinica, 2015, 31(11):
2117-2123）；Wang etc. develops a kind of hot method of the ethylene glycol solvent of microwave radiation technology and is prepared for rGO/Pt, and is applied to fiber
Element is converted into the catalytic reaction of sorbierite（Referring to Ding Wang et.al, Pt Nanocatalysts Supported on
Reduced Graphene Oxide for Selective Conversion of Cellulose or Cellobiose to
Sorbitol, ChemSusChem2014, 7: 1398-1406）.The hot method of ethylene glycol solvent prepares rGO/Pt has operation letter
Advantage that is single, being easy to grasp, but there is an obvious defect：The reduction efficiency of graphene oxide GO is not high, often only has
Part（It is local）RGO is converted into, the structure and unstable properties of composite materials is caused, regrettably, be yet there are no up to now
The document report of the problem is solved, the popularization and application of rGO/Pt is seriously limited.It is therefore desirable to be improved to this.
The content of the invention
The invention aims to the shortcoming and defect for overcoming prior art to exist, and provide a kind of process is simple, warp
Ji is environmentally friendly and graphene oxide utilization rate is high, and the structure of integral composite is common based on water/ethylene glycol with stable and reliable for performance
The redox graphene load Platinum Nanoparticles composite material and preparation method thereof of heat.
To achieve the above object, the technical scheme is that
（1）The ethylene glycol solution of graphene oxide GO is prepared, ethylene glycol volume is 15-25 milliliters；The aqueous solution of chloroplatinic acid is prepared,
The volume of water is 5-15 milliliters；Above-mentioned chloroplatinic acid is every milligram of graphene oxide GO corresponding 1/9-5/9 with the usage ratio of GO
Micromole's chloroplatinic acid；Above-mentioned two solution is mixed, is uniformly dispersed, be transferred in reactor；This step（1）Middle preparation chloroplatinic acid
The aqueous solution and prepare the ethylene glycol solution of graphene oxide GO order in no particular order；
（2）Reactor is placed in tube furnace, reaction temperature, range of reaction temperature are heated to 5-200 DEG C/min of heating rate
It it is 180-220 DEG C, reaction continues 2-4 hours；Reaction obtains block after terminating, and it is washed using pure water and ethanol successively
Wash, be then vacuum dried, obtain redox graphene load Platinum Nanoparticles composite rGO/Pt.
The present invention is improved to traditional hot method of ethylene glycol solvent, using water and the common hot method of ethylene glycol, realizes rGO/Pt
Efficient preparation, improve the stability of product structure and performance.
Using the such scheme of the inventive method, the reduction effect of graphene oxide GO can be significantly improved, significantly carried
The purity of rGO/Pt high, makes its structure and performance more stablize.In addition, present invention water instead of part ethylene glycol, reduce
The consumption of organic solvent, has not only reduced financial cost and more environmentally-friendly.
The present invention is described further with reference to specification drawings and specific embodiments.
Brief description of the drawings
Fig. 1 is penetrated for the X that the preferred embodiment of the present invention gives the rGO/Pt that the inventive method and traditional preparation methods are obtained
Line diffraction（XRD）Comparing result figure；
The X-ray diffraction of the rGO/Pt of Fig. 2 embodiment of the present invention 1（XRD）Figure；
The X-ray diffraction of the rGO/Pt of Fig. 3 embodiment of the present invention 2（XRD）Figure；
The X-ray diffraction of the rGO/Pt of Fig. 4 embodiment of the present invention 3（XRD）Figure；
The X-ray diffraction of the rGO/Pt of Fig. 5 embodiment of the present invention 4（XRD）Figure；
The X-ray diffraction of the rGO/Pt of Fig. 6 embodiment of the present invention 5（XRD）Figure；
The X-ray diffraction of the rGO/Pt of Fig. 7 embodiment of the present invention 6（XRD）Figure；
RGO/Pt transmission electron microscopes (TEM) figure prepared by Fig. 8 preferred embodiment of the present invention.
Specific embodiment
The present invention is specifically described below by embodiment, is served only for being further described the present invention, no
It is understood that to be limiting the scope of the present invention, the technician in the field can be according to the content of foregoing invention to the present invention
Make some nonessential modifications and adaptations.
Embodiment 1
The aqueous solution of chloroplatinic acid is prepared, the wherein consumption of chloroplatinic acid is 25 micromoles, and the volume of ultra-pure water is 5 milliliters；Prepare GO
Ethylene glycol solution, wherein the consumption of GO be 90 milligrams, ethylene glycol volume be 25 milliliters；Above-mentioned two solution is mixed, ultrasound point
Dissipate uniform, be transferred in reactor.Reactor is placed in tube furnace, reaction temperature as 200 DEG C is set, after reacting 2 hours, first
Product is washed with ultra-pure water and ethanol afterwards, is then vacuum dried, obtain black powder（rGO/Pt）.
XRD analysis are carried out to preparing product, as a result as shown in Figure 2.XRD results are analyzed and are understood, the product has
The characteristic peak of the characteristic peak of significant rGO and Pt, the acid of reaction raw materials chloroplatinic acid and GO has disappeared, and illustrates that GO all effectively turns
RGO, and success supporting Pt are turned to, illustrates that the preparation of rGO/Pt works well.
Embodiment 2
Key step and condition are with embodiment 1 in the present embodiment, but the volume of ultra-pure water is 15 milliliters, and the volume of ethylene glycol is
15 milliliters.XRD analysis are carried out to preparing product, as a result as shown in Figure 3.XRD interpretations of result equally illustrate the preparation effect of rGO/Pt
Fruit is good.
Embodiment 3
Key step and condition are with embodiment 1 in the present embodiment, but the consumption of chloroplatinic acid is 10 micromoles.Enter to preparing product
Row XRD analysis, as a result as shown in Figure 4.XRD interpretations of result equally illustrate that the preparation of rGO/Pt works well.
Embodiment 4
Key step and condition are with embodiment 1 in the present embodiment, but the consumption of chloroplatinic acid is 50 micromoles.Enter to preparing product
Row XRD analysis, as a result as shown in Figure 5.XRD interpretations of result equally illustrate that the preparation of rGO/Pt works well.
Embodiment 5
Key step and condition are with embodiment 1 in the present embodiment, but reaction temperature is set to 180 DEG C.Carried out to preparing product
XRD analysis, as a result as shown in Figure 6.XRD interpretations of result equally illustrate that the preparation of rGO/Pt works well.
Embodiment 6
Key step and condition are with embodiment 1 in the present embodiment, but reaction temperature is set to 220 DEG C.Carried out to preparing product
XRD analysis, as a result as shown in Figure 7.XRD interpretations of result equally illustrate that the preparation of rGO/Pt works well.
Preferred embodiment
The present embodiment prepares rGO/Pt（a）Condition：Solvent is 25 milliliters of ethylene glycol and 5 milliliters of water, 90 milligrams of GO, 25
Micromole's chloroplatinic acid, 180 DEG C of reaction temperature；RGO/Pt is prepared using conventional method（b）Condition：Solvent is 30 milliliters of ethylene glycol
（Plus a small amount of NaOH）, remaining condition and rGO/Pt（a）Unanimously.
Referring in Fig. 1, XRD results show that the inventive method prepares rGO/Pt（a）In have highly significant rGO
Characteristic peak with the characteristic peak of Pt, and GO disappears substantially, illustrates that GO is all efficiently converted into rGO, and successfully load
Pt is gone up；The rGO/Pt that conventional method is prepared（b）In there is obvious GO characteristic peaks, and Pt characteristic peaks are also more micro-
It is weak, illustrate also to have remained the substantial amounts of GO not reduced effectively in material, while also undesirable to the load effect of Pt.
Claims (1)
1. a kind of redox graphene hot altogether based on water/ethylene glycol loads Platinum Nanoparticles composite material and preparation method thereof, its feature
It is to comprise the following steps：
（1）The ethylene glycol solution of graphene oxide GO is prepared, wherein ethylene glycol volume is 15-25 milliliters；Prepare the water of chloroplatinic acid
Solution, the volume of water is 5-15 milliliters；Above-mentioned chloroplatinic acid is every milligram of graphene oxide with the usage ratio of graphene oxide GO
GO 1/9-5/9 micromole's chloroplatinic acids of correspondence；Above-mentioned two solution is mixed, is uniformly dispersed, be transferred in reactor；This step
（1）The middle aqueous solution for preparing chloroplatinic acid and prepare the ethylene glycol solution of graphene oxide GO order in no particular order；
（2）Reactor is placed in tube furnace, reaction temperature is heated to 5-20 DEG C/min of heating rate, range of reaction temperature is
180-220 DEG C, reaction continues 2-4 hours；Reaction obtains block after terminating, and it is washed using pure water and ethanol successively,
Then it is vacuum dried, obtains redox graphene load Platinum Nanoparticles composite rGO/Pt.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110120516A (en) * | 2019-06-20 | 2019-08-13 | 西北师范大学 | A kind of preparation method of antimony/redox graphene composite material |
| CN111530455A (en) * | 2020-05-18 | 2020-08-14 | 中国工程物理研究院材料研究所 | Method for thermally synthesizing Pt/C catalyst by reducing chloroplatinic acid solvent with ethylene glycol |
| CN112366329A (en) * | 2020-11-20 | 2021-02-12 | 新疆大学 | Preparation method of three-dimensional coal-based graphene supported platinum catalyst |
Citations (2)
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| CN101745384A (en) * | 2009-12-14 | 2010-06-23 | 浙江大学 | Platinum/graphene nano electro-catalyst and preparation method thereof |
| CN102068983A (en) * | 2010-12-20 | 2011-05-25 | 宁波工程学院 | Preparation method of proton exchange membrane fuel cell catalyst |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101745384A (en) * | 2009-12-14 | 2010-06-23 | 浙江大学 | Platinum/graphene nano electro-catalyst and preparation method thereof |
| CN102068983A (en) * | 2010-12-20 | 2011-05-25 | 宁波工程学院 | Preparation method of proton exchange membrane fuel cell catalyst |
Non-Patent Citations (1)
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| MING-YU YEN等: ""Platinum nanoparticles/graphene composite catalyst as a novel composite counter electrode for high performance dye-sensitized solar cells"", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110120516A (en) * | 2019-06-20 | 2019-08-13 | 西北师范大学 | A kind of preparation method of antimony/redox graphene composite material |
| CN111530455A (en) * | 2020-05-18 | 2020-08-14 | 中国工程物理研究院材料研究所 | Method for thermally synthesizing Pt/C catalyst by reducing chloroplatinic acid solvent with ethylene glycol |
| CN111530455B (en) * | 2020-05-18 | 2023-09-12 | 中国工程物理研究院材料研究所 | Method for thermally synthesizing Pt/C catalyst by adopting ethylene glycol to reduce chloroplatinic acid solvent |
| CN112366329A (en) * | 2020-11-20 | 2021-02-12 | 新疆大学 | Preparation method of three-dimensional coal-based graphene supported platinum catalyst |
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