CN106552628A - A kind of porous Fe xCo3-xO4The preparation method and nanocages of nanocages and application - Google Patents
A kind of porous Fe xCo3-xO4The preparation method and nanocages of nanocages and application Download PDFInfo
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Abstract
The invention provides a kind of porous FexCo3-xO4The preparation method and nanocages of nanocages and application.In PVP solution, by the Fe ions that adulterate in the precursor solution for prepare six cyano cobalts acid cobalt (Co-Co PBAs), can effective modulation Co-Co PBAs pattern.By the doping type Fe for preparingyCo1-y- Co PBAs calcinings can prepare porous FexCo3-xO4Nanocages, wherein x=0-1, nanocages size are 50-300nm.The FexCo3-xO4Nanocages area with the difference of such material of former report in document is：The method prepare doping type transition metal oxide nano cage ferrum cobalt content it is adjustable, nanocages pattern sizes are adjustable.The nanocages can be as Fenton, class Fenton's reaction catalyst, by activating PMS, PS or H2O2Produce the organic pollution in living radical species degraded sewage.
Description
Technical field
The present invention relates to the use of a kind of porous FexCo3-xO4The preparation method of nanocages, and its application in Fenton's reaction in catalytic degradation organic pollution.
Background technology
Doping type transition metal oxide has a wide range of applications in fields such as battery electrode reaction, photocatalysis, Fenton's reaction, magnetic materials in recent years.The method for preparing doping type transition metal oxide also has a lot, including sol-gal process, coprecipitation and hydro-thermal method etc..But the specific surface area of the nano material for preparing is generally relatively low.And most of catalytic reactions occur on the surface of catalyst, therefore, the preparation of the transition metal nano-catalyst of bigger serface still has challenge.With the intensification that people are recognized to nanocatalyst, the impact that the pattern of catalyst undoubtedly can be important to its active dopant.The short grained nanocatalyst being prepared by a conventional method to obtain, is easy to the aggregation of generation catalyst in catalytic reaction process and causes catalyst to inactivate.Therefore, if the catalyst similar to nanocages of the nanometer little particle accumulation of porous type can be prepared, its application prospect must be very wide.
Six cyano cobalts acid cobalt (Co-Co PBAs) are that the Nomenclature Composition and Structure of Complexes changes very abundant metal organic framework compound (MOFs), and such compound is widely studied because itself having the various excellent physicochemical properties such as absorption, catalysis, photic magnetic.Corresponding transition metal oxide can be transformed into by calcining such MOFs.And the doping for passing through ion then contributes to the pattern of modulation Co-Co PBAs.Therefore, by adding iron ion in the mother solution in the material preparation process, we are successfully realized FeyCo1-yThe controlledly synthesis of-Co PBAs nanospheres patterns and size.By calcining above-mentioned nanosphere, its successful conversion is corresponding doping type Fe by wexCo3-xO4Nano transition metal oxides.The nano material has the property of porous, and similar to nanocages, with larger specific surface area, therefore can play higher activity in various catalytic fields.
The content of the invention
It is contemplated that a kind of new porous Fe of exploitationxCo3-xO4Nanocages, and develop its purposes in Fenton catalytic field.
Its preparation process is as follows：
By K4 [Co (CN) 6] wiring solution-forming A, wherein K4 [Co (CN) 6] concentration is C, 0mmol/L<C<20mmol/L；
By iron containing compoundses FeCl2Or Fe (NO3)2With cobalt compound CoCl2Or Co (NO3)2Mixing wiring solution-forming B；Wherein Fe ions and Co ion molar concentrations sum are 1-2 times of K4 [Co (CN) 6] concentration in above-mentioned solution A.
PVP surfactants are added in solution B, the concentration of its PVP is 10-50g/L.
By step 1) resulting solution A is slowly added to above-mentioned steps 3) in resulting solution B, continues stirring 10-60min under room temperature.Aged at room temperature 1-25h.Centrifuge washing is dried afterwards.
By above-mentioned steps 4) gains calcining, you can obtain porous Fe xCo3-xO4 nanocages, wherein x=0-1；Its calcining heat is 300-1000 degree, and calcination time is 0.5-4h.
The centrifuge washing is dried, and concrete operations are:Centrifuge speed 6000-12000r/min, centrifugation time 1-10min, are washed with the mixed liquor of the one kind in water or ethanol or two kinds, are dried at 25 DEG C -100 DEG C.
The FexCo3-xO4 nanocages for preparing according to the method described above, wherein x=0-1, nanocages size are 50-300nm.
The above-mentioned FexCo3-xO4 nanocages stated can be applied in Fenton or class Fenton's reaction degradable organic pollutant and cell electrode catalyst reaction as catalyst.
With FexCo3-xO4 nanocages H2O2, PS or PMS presence under conditions of under dirty organic pollutants are degraded, preferable degradation effect can be obtained.
The invention has the advantages that：
1) porous Fe for preparingxCo3-xO4Nanocages have higher specific surface area, therefore higher activity can be shown in catalytic applications.
2) nanocages have ferromagnetism simultaneously, after aqueous solution catalytic reaction, in that context it may be convenient to using magnet adsorption recycling.
2) the preparation scheme is simple.
Description of the drawings
Fig. 1 is the Fe prepared in embodiment 10.8Co2.2O4TEM (transmission electron microscope) photo of nanocages.
Fig. 2 is the Fe prepared in embodiment 10.8Co2.2O4SEM (scanning electron microscope) photo of nanocages.
Fig. 3 is the Fe prepared in embodiment 10.8Co2.2O4The XRD spectra of nanocages.
During Fig. 4 is embodiment 5, using Fe0.8Co2.2O4Activity figure of the nanocages as Fenton's reaction catalyst degradation bisphenol-A.
Specific embodiment
Embodiment 1
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.0262g cobalt nitrates and the mixing of 0.0179g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6gPVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues stirring 30min, aged at room temperature 20h.5min (8000r/min) is centrifuged afterwards, and water-ethanol mixed liquor (v/v=50/50) is washed three times, and 60 degree are dried 20h and obtain Fe0.5Co0.5- Co PBAs nanosphere presomas.The calcining 1 hour of 500 degree of above-mentioned presoma can be obtained into Fe0.8Co2.2O4Nanocages.To gained Fe0.8Co2.2O4Nanocages are characterized：Fig. 1 is Fe0.8Co2.2O4TEM (transmission electron microscope) photo of nanocages, it can be seen that the nanometer for preparing is done to be uniformly dispersed, pattern rule and the property with porous, with higher specific surface area；Fig. 2 is real Fe0.8Co2.2O4SEM (scanning electron microscope) photo of nanocages, it can be seen that the nanometer for preparing is done to be uniformly dispersed, pattern rule and the property with porous；Fig. 3 is Fe0.8Co2.2O4The XRD spectra of nanocages, it can be seen that the nanocages for obtaining are the transition metal mixed oxides of pure phase, has no the appearance of impurity peaks.
Embodiment 2
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.0315g cobalt nitrates and the mixing of 0.0144g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6gPVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues stirring 30min, aged at room temperature 20h.From 5min (8000r/min), water-ethanol mixed liquor (v/v=50/50) is washed three times, and 60 degree are dried 20h and obtain Fe0.4Co0.6- Co PBAs nanosphere presomas.The calcining 1 hour of 500 degree of above-mentioned presoma can be obtained into Fe0.7Co2.3O4Nanocages.
Embodiment 3
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.0367g cobalt nitrates and the mixing of 0.0108g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6g PVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues stirring 30min, aged at room temperature 20h.Centrifugation 5min (8000r/min), water-ethanol mixed liquor (v/v=50/50) are washed three times, and 60 degree are dried 20h and obtain Fe0.3Co0.7- Co PBAs nanosphere presomas.The calcining 1 hour of 500 degree of above-mentioned presoma can be obtained into Fe0.5Co2.5O4Nanocages.
Embodiment 4
By 0.0332g K4[Fe(CN)6] be dissolved in 10ml deionized waters and be uniformly mixing to obtain solution A, 0.0419g cobalt nitrates and the mixing of 0.0072g iron chloride are dissolved in into 10ml deionized water obtained solution B, 0.6g PVP are added in solution B and is stirred.Solution A is slowly dropped in B and continues stirring 30min, aged at room temperature 20h.Centrifugation 5min (8000r/min), water-ethanol mixed liquor (v/v=50/50) are washed three times, and 60 degree are dried 20h and obtain Fe0.2Co0.8- Co PBAs nanosphere presomas.The calcining 1 hour of 500 degree of above-mentioned presoma can be obtained into Fe0.3Co2.7O4Nanocages.
Embodiment 5
Take the Fe that 0.01g embodiments 1 are obtained0.8Co2.2O4During nanocages add the bisphenol-A organic pollution of 50ml, 0.01g PMS are added afterwards.Investigate Fe0.8Co2.2O4Activity of the nanocages as Fenton's reaction activation of catalyst PMS degradable organic pollutants.Reaction condition is：Catalyst concn 0.1g/L, bisphenol A concentration 20mg/L, the aqueous solution of PMS concentration 0.2g/L, pH=6.0, T=298K.Fig. 4 is that the present embodiment utilizes Fe0.8Co2.2O4Activity figure of the nanocages as Fenton's reaction catalyst degradation bisphenol-A, it can be seen that, its degradation rate to bisphenol-A can reach 96% in 60 minutes, illustrate higher activity is shown in the catalytic applications, react its application prospect in organic pollutant degradation catalysis.
The above; one of specific embodiment only of the invention, but protection scope of the present invention do not limit to and this, any those of ordinary skill in the art disclosed herein technical scope in; without the variation and replacement of inventive concept, all should be encompassed within protection domain.Therefore, the protection domain that protection scope of the present invention should be limited by claims is defined.
Claims (5)
1. a kind of porous FexCo3-xO4The preparation method of nanocages, it is characterised in that：
Its preparation process is as follows：
1) by K4[Co(CN)6] wiring solution-forming A, wherein K4[Co(CN)6] concentration be C, 0mmol/L<C<20mmol/L；
2) by iron containing compoundses FeCl2Or Fe (NO3)2With cobalt compound CoCl2Or Co (NO3)2Mixing wiring solution-forming
B；Wherein Fe ions and Co ion molar concentrations sum are K in above-mentioned solution A4[Co(CN)6] 1-2 times of concentration；
3) PVP surfactants are added in solution B, the concentration of its PVP is 10-50g/L；
4) by step 1) resulting solution A is slowly added to above-mentioned steps 3) in resulting solution B, continues stirring under room temperature
10-60min；Aged at room temperature 1-25h；Centrifuge washing is dried afterwards；
5) by above-mentioned steps 4) gains calcining, you can obtain porous FexCo3-xO4Nanocages, wherein x=0-1；
Its calcining heat is 300-1000 degree, and calcination time is 0.5-4h.
2. according to the Fe described in right 1xCo3-xO4The preparation method of nanocages, it is characterised in that：
The centrifuge washing is dried, and concrete operations are:Centrifuge speed 6000-12000r/min, centrifugation time is
1-10min, is washed with the mixed liquor of the one kind in water or ethanol or two kinds, is dried at 25 DEG C -100 DEG C.
3. a kind of Fe prepared according to right 1 or 2 methods describedsxCo3-xO4Nanocages, it is characterised in that：
Wherein x=0-1, nanocages size are 50-300nm.
4. the FexCo3-xO4 nanocages described in a kind of claim 3 have in Fenton or the degraded of class Fenton's reaction as catalyst
Application in organic pollutants and cell electrode catalyst reaction.
5. according to the application described in right 4, it is characterised in that：
Use FexCo3-xO4Nanocages are in H2O2, PS or PMS exist under conditions of under dirty organic pollutants are carried out
Degraded.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107293761A (en) * | 2017-08-02 | 2017-10-24 | 中南大学 | A kind of Co@N C composite positive poles, preparation method and the application in lithium-air battery |
| CN109174105A (en) * | 2018-10-11 | 2019-01-11 | 天津工业大学 | A kind of preparation method of magnetic catalyst derived from double MOFs |
| CN109275329A (en) * | 2018-09-18 | 2019-01-25 | 北京科技大学 | A kind of preparation method of nano core-shell absorbing material |
| CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
| CN109592721A (en) * | 2019-01-21 | 2019-04-09 | 北京航空航天大学 | A kind of porous Ni (OH)2Nanocages and preparation method thereof |
| CN113198473A (en) * | 2021-04-29 | 2021-08-03 | 清创人和生态工程技术有限公司 | Transition metal oxide Fenton catalyst and preparation method and application thereof |
| CN115703077A (en) * | 2021-08-10 | 2023-02-17 | 中国科学院大连化学物理研究所 | PB @ MoS 2 Application of catalyst in heterogeneous Fenton-like reaction |
| CN115779909A (en) * | 2022-11-28 | 2023-03-14 | 淮阴师范学院 | Cobalt-doped cerium-iron oxide catalyst rich in oxygen vacancies and capable of being magnetically separated and preparation method thereof |
| CN115869956A (en) * | 2022-12-15 | 2023-03-31 | 西安交通大学 | FeCo with a domain-restricted structure 2 O 4 Photoelectrocatalysis thin film material, preparation method and application thereof |
| CN116139863A (en) * | 2023-01-04 | 2023-05-23 | 中南大学 | Red mud-based PBAs derived metal oxide Fenton catalyst and preparation method and application thereof |
| CN117558564A (en) * | 2023-12-06 | 2024-02-13 | 贵州大学 | Mn doped ZnO@cobalt oxide nano film and preparation method and application thereof |
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Cited By (16)
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| CN107293761A (en) * | 2017-08-02 | 2017-10-24 | 中南大学 | A kind of Co@N C composite positive poles, preparation method and the application in lithium-air battery |
| CN107293761B (en) * | 2017-08-02 | 2019-06-28 | 中南大学 | A kind of Co@N-C composite positive pole, preparation method and the application in lithium-air battery |
| CN109275329A (en) * | 2018-09-18 | 2019-01-25 | 北京科技大学 | A kind of preparation method of nano core-shell absorbing material |
| CN109174105A (en) * | 2018-10-11 | 2019-01-11 | 天津工业大学 | A kind of preparation method of magnetic catalyst derived from double MOFs |
| CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
| CN109289852B (en) * | 2018-10-26 | 2021-07-13 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
| CN109592721A (en) * | 2019-01-21 | 2019-04-09 | 北京航空航天大学 | A kind of porous Ni (OH)2Nanocages and preparation method thereof |
| CN109592721B (en) * | 2019-01-21 | 2021-05-25 | 北京航空航天大学 | Porous Ni (OH)2Nano cage and preparation method thereof |
| CN113198473A (en) * | 2021-04-29 | 2021-08-03 | 清创人和生态工程技术有限公司 | Transition metal oxide Fenton catalyst and preparation method and application thereof |
| CN115703077A (en) * | 2021-08-10 | 2023-02-17 | 中国科学院大连化学物理研究所 | PB @ MoS 2 Application of catalyst in heterogeneous Fenton-like reaction |
| CN115703077B (en) * | 2021-08-10 | 2024-05-14 | 中国科学院大连化学物理研究所 | PB@MoS2Application of catalyst in heterogeneous Fenton-like reaction |
| CN115779909A (en) * | 2022-11-28 | 2023-03-14 | 淮阴师范学院 | Cobalt-doped cerium-iron oxide catalyst rich in oxygen vacancies and capable of being magnetically separated and preparation method thereof |
| CN115779909B (en) * | 2022-11-28 | 2024-05-14 | 淮阴师范学院 | Cobalt-doped cerium-iron oxide catalyst rich in oxygen vacancies and capable of being magnetically separated and preparation method thereof |
| CN115869956A (en) * | 2022-12-15 | 2023-03-31 | 西安交通大学 | FeCo with a domain-restricted structure 2 O 4 Photoelectrocatalysis thin film material, preparation method and application thereof |
| CN116139863A (en) * | 2023-01-04 | 2023-05-23 | 中南大学 | Red mud-based PBAs derived metal oxide Fenton catalyst and preparation method and application thereof |
| CN117558564A (en) * | 2023-12-06 | 2024-02-13 | 贵州大学 | Mn doped ZnO@cobalt oxide nano film and preparation method and application thereof |
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Application publication date: 20170405 |