CN106939429A - A kind of preparation method of new oxygen reduction electro-catalyst - Google Patents
A kind of preparation method of new oxygen reduction electro-catalyst Download PDFInfo
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- CN106939429A CN106939429A CN201710154918.5A CN201710154918A CN106939429A CN 106939429 A CN106939429 A CN 106939429A CN 201710154918 A CN201710154918 A CN 201710154918A CN 106939429 A CN106939429 A CN 106939429A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
Abstract
The present invention relates to materials synthesis field, more particularly to a kind of preparation method of new oxygen reduction electro-catalyst.A kind of preparation method of new oxygen reduction electro-catalyst, containing having the following steps：Stratiform manganese oxide solid powder is dispersed among acid solution, is transferred to after stirring in the autoclave of polytetrafluoroethyllining lining, reaction 24h is stood at a temperature of 100 DEG C, products therefrom obtains described electrode catalyst after being filtered, washed and dried and drying.The invention provides a kind of method that two-step method prepares oxygen reduction electro-catalyst, the preparation method has the advantages that flow is simple, easy to control, yield is big, be easy to industrialization.The oxygen reduction electro-catalyst of preparation shows good catalytic performance as electrode active material in hydrogen reduction performance test.
Description
Technical field
The present invention relates to materials synthesis field, more particularly to a kind of preparation method of new oxygen reduction electro-catalyst.
Background technology
The regenerative resource of cleaning is to tackle one of effective way of the energy and environmental crisis, in many regenerative resources
In, chemical energy source energy transformation ratio is high, is easy to carry, is always the focus of research.Wherein, metal-air battery is due to pole
High theoretical energy density, therefore received much concern as electrokinetic cell system of new generation.
Traditional cathodic oxygen reduction catalyst such as precious metals pt/C is not suitable for because price is high, scarcity of resources
Industrial application.At present, exploitation novel non-noble metal catalyst turns into a current big study hotspot.MnO2Due to money
Source is abundant, cheap and advantages of environment protection, and causing researcher as cathodic oxygen reduction catalyst widely notes.
The MnO of different crystal forms structure2Oxygen reduction catalytic activity order be：α-MnO2>γ-MnO2>β-MnO2.At present, there are many researchs
α-MnO have been synthesized using different methods2, and it is applied to hydrogen reduction catalytic reaction.For example, Cheng etc.
(Chem.Mater., 2010,22,898-905), by hydro-thermal method, using potassium permanganate as oxidant, manganese sulfate is closed as reducing agent
Into α-MnO2Oxygen reduction catalyst；Xiao etc. (J.Phys.Chem.C, 2010,114,1694-1700) utilizes potassium permanganate
α-MnO have been synthesized with hydrochloric acid reaction2The oxygen reduction catalyst of nanotube；Cheng etc. (J.Mater.Chem.A, 2016,4,
16462-16468) using potassium chlorate as oxidant, manganese acetate has synthesized α-MnO as reducing agent2Oxygen reduction catalyst.At present,
Using layered manganese oxide (δ-MnO2) synthesize α-MnO as reactant2The research of oxygen reduction catalyst is rarely reported.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of new oxygen reduction electro-catalyst.
A kind of preparation method of new oxygen reduction electro-catalyst, containing having the following steps：Stratiform manganese oxide solid powder is disperseed
To acid solution, it is transferred in the autoclave of polytetrafluoroethyllining lining, is stood at a temperature of 100 DEG C anti-after stirring
24h is answered, products therefrom obtains described electrode catalyst through filtering, washing, dry.
Further, described acid is sulfuric acid.
Further, the sour molar concentration is 0.3~0.4mol./L.
Further, layered manganese oxide is synthesized suddenly by containing as follows：Glucose and potassium permanganate are added to distilled water
Among solution, gel is obtained after being stirred vigorously, the gel is positioned at 110 DEG C after then remaining water is fallen and dries 12h
Obtain xerogel；Finally xerogel is calcined after 2h, and products therefrom is obtained into described stratiform through filtering, washing, dry
Manganese oxide.
Further, the mol ratio of the glucose and potassium permanganate is 3:2.
Further, the calcining heat is 450 DEG C.
The present invention has the advantages that：
Oxygen reduction electro-catalyst is prepared the invention provides a kind of 2 footwork, the preparation method has that flow is simple, controlling party
Just, yield is big, the advantages of be easy to industrialization.The oxygen reduction electro-catalyst of preparation is as electrode active material, in hydrogen reduction performance
Good catalytic performance is shown in test.
Brief description of the drawings
Fig. 1 is catalyst X-ray diffractogram prepared by embodiments of the invention 1.
Fig. 2 is catalyst scanning electron microscope (SEM) photograph prepared by embodiments of the invention 1.
The performance map that Fig. 3 reduces for the electrocatalytic oxidation of the prepared catalyst of embodiments of the invention 1.
Embodiment
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Unless otherwise instructed, stratiform manganese oxide of the invention is synthesized as follows：By 0.03mol glucose with
0.02mol potassium permanganate is added to 100mL distilled water solutions, and gel is obtained after being stirred vigorously, and then falls remaining water
After going, the gel is positioned at 110 DEG C dry 12h and obtains xerogel；Finally xerogel is calcined after 2h at 450 DEG C, and
By products therefrom through filtering, washing, dry, that is, obtain described stratiform manganese oxide.
Embodiment 1
Stratiform manganese oxide solid powder obtained by the 0.4g above methods is dispersed among 30mL sulfuric acid solutions, wherein, sulfuric acid
Concentration be 0.3mol/L, be transferred to after stirring in the autoclave of polytetrafluoroethyllining lining, at a temperature of 100 DEG C stand
24h is reacted, products therefrom is through the electrode catalyst described in filtering, washing then drying to obtain.
Then above-mentioned electrode catalyst is characterized, its X-ray diffractogram such as Fig. 1, it will be seen from figure 1 that its with
α-the MnO of JCPDF standard card PDF#44-0141 models2Correspondence；Fig. 2 prepares the scanning electron microscope (SEM) photograph of catalyst for the present embodiment, from
It can be seen that it is a kind of monodimension nano stick structure in figure.In raw material selected by this preparation method, anion comprises only sulfuric acid
Root, is conducive to inductive formation α-MnO2。
Embodiment 2
Electrode catalyst prepared by embodiment 1 is made into electrode, surveyed in alkaline solution, 1600 revs/min of rotating speed
Try the hydrogen reduction performance of electro-catalysis (prepared by its electrode and experimentation is prior art, is not described in detail herein).Its electricity is urged
Change the performance map of hydrogen reduction as shown in figure 3, its initial reduction current potential is 0.87V, limiting current density is 5.56mA cm-2, 3mA
cm-2Current potential be located at 0.75V, show excellent hydrogen reduction performance.
Embodiment described above only expresses embodiments of the present invention, and it describes more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent or equivalent transformation
Art scheme, all should fall within the scope and spirit of the invention.
Claims (6)
1. a kind of preparation method of new oxygen reduction electro-catalyst, it is characterised in that containing having the following steps：Stratiform manganese oxide is consolidated
Body powder is dispersed among acid solution, is transferred to after stirring in the autoclave of polytetrafluoroethyllining lining, in 100 DEG C of temperature
Lower to stand reaction 24h, products therefrom obtains described electrode catalyst after filtering, washing, drying.
2. a kind of preparation method of new oxygen reduction electro-catalyst according to claim 1, it is characterised in that：Described acid
For sulfuric acid.
3. a kind of preparation method of new oxygen reduction electro-catalyst according to claim 1, it is characterised in that：It is described sour
Molar concentration is 0.3~0.4mol/L.
4. a kind of preparation method of new oxygen reduction electro-catalyst according to claim 1, it is characterised in that：It is layered
Manganese oxide is synthesized by following steps：Glucose and potassium permanganate are added to distilled water solution, coagulated after being stirred vigorously
Glue, is positioned at 110 DEG C dry 12h by the gel after then remaining water is fallen and obtains xerogel；Finally xerogel is forged
2h is burnt, and products therefrom is obtained into described stratiform manganese oxide through filtering, washing, dry.
5. a kind of preparation method of new oxygen reduction electro-catalyst according to claim 4, it is characterised in that：The grape
Sugar is 3 with the mol ratio of potassium permanganate:2.
6. a kind of preparation method of new oxygen reduction electro-catalyst according to claim 4, it is characterised in that：The calcining
Temperature is 450 DEG C.
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| CN201710154918.5A CN106939429A (en) | 2017-03-15 | 2017-03-15 | A kind of preparation method of new oxygen reduction electro-catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855159A (en) * | 2018-06-27 | 2018-11-23 | 广东工业大学 | A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative |
| CN115092966A (en) * | 2022-07-04 | 2022-09-23 | 嘉应学院 | Mixed-phase MnO of three-dimensional lamellar structure for toluene catalytic combustion 2 Preparation method of (1) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289591A (en) * | 1980-05-02 | 1981-09-15 | General Electric Company | Oxygen evolution with improved Mn stabilized catalyst |
| CN103193273A (en) * | 2013-05-03 | 2013-07-10 | 广东工业大学 | Preparation method of extra-long manganese dioxide nanowires |
| CN105895929A (en) * | 2016-04-25 | 2016-08-24 | 广东工业大学 | Electrode catalyst of metal-air battery and preparation method and application of electrode catalyst |
-
2017
- 2017-03-15 CN CN201710154918.5A patent/CN106939429A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4289591A (en) * | 1980-05-02 | 1981-09-15 | General Electric Company | Oxygen evolution with improved Mn stabilized catalyst |
| CN103193273A (en) * | 2013-05-03 | 2013-07-10 | 广东工业大学 | Preparation method of extra-long manganese dioxide nanowires |
| CN105895929A (en) * | 2016-04-25 | 2016-08-24 | 广东工业大学 | Electrode catalyst of metal-air battery and preparation method and application of electrode catalyst |
Non-Patent Citations (2)
| Title |
|---|
| DAVID M. ROBINSON ET AL.: ""Photochemical Water Oxidation by Crystalline Polymorphs of Manganese Oxides: Structural Requirements for Catalysis"", 《J.AM.CHEM.SOC.》 * |
| 黄夏青: ""α、δ-MnO2的制备及对邻二甲苯深度催化氧化的研究"，", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855159A (en) * | 2018-06-27 | 2018-11-23 | 广东工业大学 | A kind of phosphatization cobalt and its preparation method and application with the synthesis of Prussian blue derivative |
| CN115092966A (en) * | 2022-07-04 | 2022-09-23 | 嘉应学院 | Mixed-phase MnO of three-dimensional lamellar structure for toluene catalytic combustion 2 Preparation method of (1) |
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