CN105776249A - Manganese hexacyanoferrate nano cube and preparation method thereof - Google Patents
Manganese hexacyanoferrate nano cube and preparation method thereof Download PDFInfo
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- CN105776249A CN105776249A CN201610300070.8A CN201610300070A CN105776249A CN 105776249 A CN105776249 A CN 105776249A CN 201610300070 A CN201610300070 A CN 201610300070A CN 105776249 A CN105776249 A CN 105776249A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
- C01C3/12—Simple or complex iron cyanides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/38—Particle morphology extending in three dimensions cube-like
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a manganese hexacyanoferrate nano cube and a preparation method thereof. The preparation method of the manganese hexacyanoferrate nano cube comprises the following steps: dissolving an appropriate amount of potassium ferricyanide and manganese salt in deionized water respectively, and carrying out ultrasonic dissolution to prepare a manganese hexacyanoferrate solution and a manganese salt solution; then adding an appropriate amount of polyvinylpyrrolidone to the manganese salt solution, carrying out ultrasonic dissolution, dropwise adding the manganese hexacyanoferrate solution slowly, and continuously performing magnetic stirring for a period of time after dropwise adding is ended; then centrifugally washing the prepared product, and drying to prepare the manganese hexacyanoferrate nano cube. By testing the manganese hexacyanoferrate powder prepared by the preparation method disclosed by the invention with an X-ray diffractometer and an scanning electron microscope, the manganese hexacyanoferrate is a nano cube which is uniform in particle size distribution and relatively small in size, and can be made into a material for manufacturing an electrochromic device, a secondary battery electrode material, a biosensor and the like.
Description
Technical field
The present invention relates to field of material technology, be specifically related to a kind of Manganese hexacyanoferrate nano cubic block and preparation method thereof.
Background technology
Manganese hexacyanoferrate, its molecular formula is Mn3[Fe(CN)6]2·xH2O, is a kind of common Prussian blue derivant.Its oxygen
Change state and reduction-state and present yellow and colourless respectively, and there is excellent electrochemical reversibility and stability and easily prepare
Etc. advantage.Therefore can be as electrochromic material, secondary battery material, hydrogen storage material, electrochemical catalysis material etc..
Preparation method about Manganese hexacyanoferrate mainly has hydrothermal synthesis method, template synthesis method, microemulsion method and liquid at present
The phase sedimentation method etc..Wherein hydrothermal synthesis method can obtain the product of different-shape by the control of experiment condition, however it is necessary that
High-temperature and high-pressure conditions and generated time are longer；Although electrochemical deposition method operating process is simple, but cannot be by reasonably adjusting
The pattern of product is controlled by joint experiment condition；Template synthesis method can control the shape of product by selecting suitable template
Looks and size, but after utilizing templated synthesis nano material, how to remove template and ensure that removing technique does not receives to synthesized
It is the most unsolved current a great problem that the pattern of rice material and character produce harmful effect；The experimental provision letter of microemulsion method
Single, the nano-powder grain diameter prepared is little and is difficult to reunite, but the surfactant that consumed of the method and the amount of solvent
A lot, it is difficult to remove these Organic substances from the final particle surface obtained, and relatively costly.With other preparation method from compared with,
The operating process of liquid-phase precipitation method nano materials is simple, and the response time is short, and reaction end end processing sequences is simple.But
Currently used liquid-phase precipitation method is required for when preparing Manganese hexacyanoferrate standing a period of time, and required time is from 2 h to 24 h, quiet
Time of putting, the too short acquisition size that is just difficult to was less, the nano-powder that pattern is homogeneous.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of Manganese hexacyanoferrate nano cubic block and
Preparation method.Preparation method technique of the present invention is simple, and required time is short, and available size is less, the Manganese hexacyanoferrate that pattern is homogeneous
Nano cubic block.
Technical solution of the present invention is specifically described as follows.
The present invention provides the preparation method of a kind of Manganese hexacyanoferrate nano cubic block, specifically comprises the following steps that
1. the equimolar potassium ferricyanide and manganese salt are dissolved in isopyknic deionized water respectively, obtain potassium ferricyanide solution and manganese
Saline solution；
2. polyvinylpyrrolidone is joined in manganese salt solution, obtain mixed solution；
3. being slowly added dropwise the potassium ferricyanide solution that 1. step is prepared in mixed solution, rate of addition controls to drip at 1-2 per second, adds
Complete
Rear continuation stirs to not precipitating generation；Finally centrifugal collection product, is dried after repeatedly washing with deionized water and ethanol,
I.e. prepare Manganese hexacyanoferrate nano cubic block.
Above-mentioned steps 1. in, manganese salt is one or both in manganese chloride, manganese acetate or manganese sulfate.
Above-mentioned steps 1. in, the molar concentration of potassium ferricyanide solution and manganese salt is all between 5 ~ 20mmol/L.
Above-mentioned steps 1. in, the mean molecule quantity of polyvinylpyrrolidone is about 200000.
Above-mentioned steps 1. in, the mol ratio of polyvinylpyrrolidone and manganese salt is 20:1 ~ 100:1.
Above-mentioned steps 1. in, described deionized water is at least to remove Cl-、[Fe(CN)6]3+、Mn2+And Fe3+Water.
Above-mentioned steps 3. in, baking temperature is 45 DEG C～80 DEG C.
The present invention also provides for the Manganese hexacyanoferrate nano cubic block that a kind of above-mentioned preparation method obtains, and described Manganese hexacyanoferrate is for receiving
Meter level, microstructure is bar-shaped, even size distribution.The nano cubic block length of side is 500-700 nm.
Compared with prior art, beneficial effects of the present invention is as follows:
1, the length of side and the dispersibility of nano cubic block is controlled by changing the consumption of polyvinylpyrrolidone.Increasing along with amount
Adding, size diminishes, and dispersibility improves.
2, preparation technology is simple, and the requirement to equipment is low, and the prices of raw materials are cheap, is readily obtained, and cost is relatively low.
3, experimental situation is required low, escaping gas will not be produced, harmless.
Accompanying drawing explanation
Fig. 1 uses the SEM photograph of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 1.
Fig. 2 uses the SEM picture of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 2.
Fig. 3 uses the XRD spectra of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 1.
Detailed description of the invention
Describe the present invention below in conjunction with embodiment, but the following example is not limited to the present invention, under
Polyvinylpyrrolidone in row embodiment is PVP K60, it is possible to selecting the product of commercially available similar performance, every do not have other
The change made under any spirit without departing from the present invention and principle, modify, substitute, combine, simplify, be accordingly to be regarded as equivalence
Substitute mode, is included in protection scope of the present invention.
Embodiment 1
1) 0.0126 g manganese chloride and the 0.0329 g potassium ferricyanide are distinguished ultrasonic disperse in 20 mL deionized waters.
2) to 1) in manganese chloride solution in add 0.555 g PVP K60 ultrasonic dissolution, then by 1) in the potassium ferricyanide
Solution slowly drips in manganese chloride solution, simultaneously magnetic agitation.Drip complete follow-up continuous magnetic agitation to the most more precipitating
Stop after generation.
3) by 2) turbid solution for preparing is centrifugal obtains powder product, by obtained product deionized water and dehydrated alcohol
Centrifuge washing, is dried 12 h at 45 DEG C and i.e. prepares the Manganese hexacyanoferrate nano cubic block that the length of side is 600 nm.
Fig. 1 uses the SEM photograph of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 1.
Embodiment 2
1) 0.0346 g manganese acetate and the 0.0658 g potassium ferricyanide are distinguished ultrasonic disperse in 20 mL deionized waters.
2) to 1) in manganese chloride solution in add 0.222g PVP K60 ultrasonic dissolution, then by 1) in the potassium ferricyanide molten
Liquid slowly drips in manganese chloride solution, simultaneously magnetic agitation.Drip complete follow-up continuous magnetic agitation to the most more precipitating product
Stop after life.
3) by 2) turbid solution for preparing is centrifugal obtains powder product, by obtained product deionized water and dehydrated alcohol
Centrifuge washing, is dried 12 h at 60 DEG C and i.e. prepares the Manganese hexacyanoferrate nano cubic block that the length of side is 700 nm.
Fig. 2 uses the SEM picture of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 2.
Embodiment 3
1) 0.0151 g manganese sulfate and the 0.0329 g potassium ferricyanide are distinguished ultrasonic disperse in 20 mL deionized waters.
2) to 1) in manganese chloride solution in add 1.111g PVP K60 ultrasonic dissolution, then by 1) in the potassium ferricyanide molten
Liquid slowly drips in manganese chloride solution, simultaneously magnetic agitation.Drip complete follow-up continuous magnetic agitation to the most more precipitating product
Stop after life.
3) by 2) turbid solution for preparing is centrifugal obtains powder product, by obtained product deionized water and dehydrated alcohol
Centrifuge washing, is dried 12 h at 80 DEG C and i.e. prepares the Manganese hexacyanoferrate nano cubic block that the length of side is 500 nm.
Fig. 3 uses the XRD spectra of Manganese hexacyanoferrate nano cubic block prepared by the embodiment of the present invention 1, and it is equal in 2 θ values
16.4o、23.5o、33.9o、41.8o、49.6o、52.4oWith 55.1oCharacteristic peak occurs, contrasts with standard diffraction spectrogram, it was demonstrated that produce
Thing is Manganese hexacyanoferrate.
Claims (8)
1. the preparation method of a Manganese hexacyanoferrate nano cubic block, it is characterised in that specifically comprise the following steps that
1. the equimolar potassium ferricyanide and manganese salt are dissolved in isopyknic deionized water respectively, obtain potassium ferricyanide solution and manganese
Saline solution；
2. polyvinylpyrrolidone is joined in manganese salt solution, obtain mixed solution；
3. in mixed solution, it is slowly added dropwise the potassium ferricyanide solution that 1. step is prepared, continues stirring after adding to not precipitating product
Raw；
Finally centrifugal collection product, is dried after repeatedly washing with deionized water and ethanol, i.e. prepares Manganese hexacyanoferrate nano cubic
Block.
Preparation method the most according to claim 1, it is characterised in that: step 1. in, manganese salt is manganese chloride, manganese acetate or sulfur
Acid cadmium in one or both.
Preparation method the most according to claim 1, it is characterised in that: step 1. in, rubbing of potassium ferricyanide solution and manganese salt
That concentration is all between 5 ~ 20mmol/L.
Preparation method the most according to claim 1, it is characterised in that: step 1. in, the average mark of polyvinylpyrrolidone
Son amount is about 200000.
Preparation method the most according to claim 1, it is characterised in that: step 1. in, polyvinylpyrrolidone and manganese salt
Mol ratio is 20:1 ~ 100:1.
Preparation method the most according to claim 1, it is characterised in that: step 1. in, described deionized water is at least to go
Except Cl-、[Fe(CN)6]3+、Mn2+And Fe3+Water.
Preparation method the most according to claim 1, it is characterised in that: step 3. in, baking temperature is 45 DEG C～80 DEG C.
8. the Manganese hexacyanoferrate nano cubic block that the preparation method as described in one of claim 1-7 prepares, its feature
It is: the length of side of nano cubic block is 500-700 nm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021510A (en) * | 2017-05-05 | 2017-08-08 | 同济大学 | In block ferro-cobalt Prussian blue analogue nano material of fringing cube and preparation method thereof |
| CN108133832A (en) * | 2017-12-05 | 2018-06-08 | 西北工业大学 | A kind of nano hollow structure is Prussian blue and its preparation method of homologue |
| CN108493423A (en) * | 2018-04-11 | 2018-09-04 | 南京林业大学 | A kind of nanometer Prussian Blue sodium-ion battery positive material and preparation method thereof |
| CN108579656A (en) * | 2018-03-23 | 2018-09-28 | 天津师范大学 | Prussian blue has the nano particle and its preparation method and application of face-centred cubic structure |
| CN111943226A (en) * | 2020-08-30 | 2020-11-17 | 温州大学 | Method for regulating morphology of manganese cobalt Prussian blue crystals by using surfactant |
| CN114804152A (en) * | 2021-06-09 | 2022-07-29 | 吴学文 | KMn 3+ [Fe 2+ （CN） 6 ]Preparation method of (1) |
| CN114917880A (en) * | 2022-05-17 | 2022-08-19 | 山东大学 | Reusable nitrogen oxide adsorbent, preparation method and application |
| CN115920122A (en) * | 2022-12-19 | 2023-04-07 | 常州大学 | Phototherapy antibacterial hydrogel carbomer @ HPB-Cypate and preparation method thereof |
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| CN103251962A (en) * | 2012-02-17 | 2013-08-21 | 苏州迈格锐意医药科技有限公司 | Magnetic resonance contrast material and preparation method thereof, and contrast agent |
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| HUAN PANG ET AL.: "Uniform manganese hexacyanoferrate hydrate nanocubes featuring superior performance for low-cost supercapacitors and nonenzymatic electrochemical sensors", 《NANOSCALE》 * |
| S. JANCY SOPHIA ET AL.: "Amperometry Detection of Hydrazine Using Hexacyanoferrate Nanoparticles Modified Glassy Carbon Electrode", 《ADVANCED ELECTROCHEMISTRY》 * |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021510A (en) * | 2017-05-05 | 2017-08-08 | 同济大学 | In block ferro-cobalt Prussian blue analogue nano material of fringing cube and preparation method thereof |
| CN107021510B (en) * | 2017-05-05 | 2019-03-01 | 同济大学 | In blocky cobalt-iron Prussian blue analogue nano material of fringing cube and preparation method thereof |
| CN108133832A (en) * | 2017-12-05 | 2018-06-08 | 西北工业大学 | A kind of nano hollow structure is Prussian blue and its preparation method of homologue |
| CN108579656A (en) * | 2018-03-23 | 2018-09-28 | 天津师范大学 | Prussian blue has the nano particle and its preparation method and application of face-centred cubic structure |
| CN108579656B (en) * | 2018-03-23 | 2021-03-16 | 天津师范大学 | Prussian blue nano-particles with face-centered cubic structure and preparation method and application thereof |
| CN108493423A (en) * | 2018-04-11 | 2018-09-04 | 南京林业大学 | A kind of nanometer Prussian Blue sodium-ion battery positive material and preparation method thereof |
| CN111943226A (en) * | 2020-08-30 | 2020-11-17 | 温州大学 | Method for regulating morphology of manganese cobalt Prussian blue crystals by using surfactant |
| CN111943226B (en) * | 2020-08-30 | 2023-08-11 | 温州大学 | Method for regulating and controlling morphology of manganese-cobalt Prussian blue crystal by using surfactant |
| CN114804152A (en) * | 2021-06-09 | 2022-07-29 | 吴学文 | KMn 3+ [Fe 2+ （CN） 6 ]Preparation method of (1) |
| CN114917880A (en) * | 2022-05-17 | 2022-08-19 | 山东大学 | Reusable nitrogen oxide adsorbent, preparation method and application |
| CN115920122A (en) * | 2022-12-19 | 2023-04-07 | 常州大学 | Phototherapy antibacterial hydrogel carbomer @ HPB-Cypate and preparation method thereof |
| CN115920122B (en) * | 2022-12-19 | 2024-03-15 | 常州大学 | Phototherapy antibacterial hydrogel carbomer@HPB-cypad and preparation method thereof |
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