CN104556237B - Ferrous carbonate hexahedron and preparation method thereof - Google Patents
Ferrous carbonate hexahedron and preparation method thereof Download PDFInfo
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- CN104556237B CN104556237B CN201410746946.2A CN201410746946A CN104556237B CN 104556237 B CN104556237 B CN 104556237B CN 201410746946 A CN201410746946 A CN 201410746946A CN 104556237 B CN104556237 B CN 104556237B
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- hexahedron
- ferrous carbonate
- ferrous
- carbonate
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Abstract
The invention discloses a ferrous carbonate hexahedron and a preparation method thereof. The ferrous carbonate hexahedron is a FeCO3-phase hexahedron crystal structure, wherein the side length of the ferrous carbonate hexahedron is 500-5000nm. The preparation method comprises the following steps: uniformly stirring ferrous chloride tetrahydrate, urea and deionized water in a mole ratio of (1-5):(3-15):(2000-3000); adding the uniform solution into a high-pressure autoclave, putting the high-pressure autoclave into a drying oven, heating to 120-180 DEG C, and keeping the temperature for 3-18 hours; and naturally cooling the high-pressure autoclave to room temperature, taking out the reaction product, repeatedly washing the reaction product with deionized water and anhydrous ethanol until the water solution is neutral, centrifugating to obtain a precipitate, and drying the precipitate in a drying oven to obtain the ferrous carbonate hexahedron powder. The method does not need to add any dispersing agent or surfactant; the prepared ferrous carbonate hexahedron has high crystallinity; and the preparation process has the advantages of convenient after-treatment, low reaction temperature, short reaction time, simple reaction technique and low cost.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of ferrous carbonate hexahedron and preparation method thereof.
Background technology
Ferrous carbonate, molecular formula is FeCO3, belonging to trigonal system, crystal structure belongs to diamond structure, due to its uniqueness
Crystal structure, always prepares Fe3O4And Fe2O3The study hotspot of presoma.There is document report different-shape carbonic acid in recent years
Ferrous synthetic method, such as by the way that reducing agent such as ascorbic acid, urea and ferric trichloride are well mixed, then by hydro-thermal method
Obtain ferrous carbonate elliposoidal structure；If being further introduced into surfactant polyvinylpyrrolidone in above-mentioned system, can
To obtain the ferrous carbonate ball of the smooth micro-meter scale in surface.To polyhedral ferrous carbonate and how to obtain in prior art
Polyhedral ferrous carbonate is but seldom reported.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes a kind of ferrous carbonate hexahedron and its preparation side
Method, using hydro-thermal method ferrous carbonate hexahedron is made, and its preparation method is simple, and crystallinity is high.
The present invention proposes a kind of ferrous carbonate hexahedron, and ferrous carbonate hexahedron is FeCO3Phase hexahedron crystal structure,
The hexahedral length of side of ferrous carbonate is between 500-5000nm.
Preferably, the hexahedral length of side of ferrous carbonate is between 800-4000nm.
Preferably, the hexahedral length of side of ferrous carbonate is between 1500-2500nm.
The invention allows for a kind of hexahedral preparation method of ferrous carbonate, comprises the steps：
S1, by Iron dichloride tetrahydrate, urea and deionized water in molar ratio be 1-5：3-15：The ratio of 2000-3000
Stir；
S2, the solution stirred in S1 is added in autoclave, then autoclave is put in baking oven, be heated to
120-180 DEG C, it is incubated 3-18 hours；
S3, autoclave are naturally cooled to and take out after room temperature product, by product deionized water and absolute ethyl alcohol
Cyclic washing, in neutrality, is then centrifuged for being precipitated thing and in an oven dries sediment to the aqueous solution, obtains ferrous carbonate
Hexahedron powder.
Preferably, in S1, Iron dichloride tetrahydrate, urea and deionized water are in molar ratio 2-4：6-12：2000-
3000；Preferably, Iron dichloride tetrahydrate, urea and deionized water are in molar ratio 2.5-3.5：8-12：2000-3000；More
Preferably, Iron dichloride tetrahydrate, urea and deionized water are in molar ratio 3：10：2000-3000.
Preferably, in S2,140-170 DEG C is heated to, is incubated 5-15 hours；Preferably, 150-170 DEG C is heated to, is protected
Warm 7-12 hours；It is highly preferred that being heated to 160 DEG C, 10 hours are incubated.
Preferably, in S2, heat temperature raising is carried out with the heating rate of 2-3 DEG C/min.
Preferably, in S2, compactedness of the solution in autoclave is 60%-85%；Preferably, compactedness is 65%-
80%；It is highly preferred that compactedness is 70%-75%.
In the present invention, ferrous carbonate hexahedron is by the use of Iron dichloride tetrahydrate and urea as raw material, by hydro-thermal method
Carbonate synthesis ferrous iron hexahedron powder, during the course of the reaction, it is not necessary to add dispersant and surfactant, obtained carbonic acid is sub-
The hexahedral crystallinity of iron is high；Need not add the materials such as template in preparation process, convenient post-treatment, reaction temperature is low, reaction
Time is short, reaction process is simple, inexpensive；In preparation process environmental protection, any poisonous and hazardous organic examination is not used
Agent.
Description of the drawings
Fig. 1 be to ferrous carbonate hexahedron powder using SEM SEM observation after shoot the micro- photograph for obtaining
Piece.
Fig. 2 is the XRD spectra for using Fig. 1 Phlips X ' Pert type X-ray diffraction instrument to measure.
Specific embodiment
Embodiment 1
The embodiment of the present invention 1 proposes a kind of hexahedral preparation method of ferrous carbonate, comprises the steps：
S1, the urea of the Iron dichloride tetrahydrate of 3mmol, 10mmol is dissolved in the deionized water of 50mL, in magnetic force
Uniform solution is obtained under agitator stirring；
S2, the solution stirred in S1 is added to volume be 70mL polytetrafluoroethylene (PTFE) autoclave inner bag in, then will
Autoclave is put in baking oven, is heated to 160 DEG C, is incubated 10 hours；
S3, autoclave are naturally cooled to and take out after room temperature product, by product deionized water and absolute ethyl alcohol
Cyclic washing, in neutrality, is then centrifuged for being precipitated thing and in an oven dries sediment to the aqueous solution, obtains ferrous carbonate
Hexahedron powder.
Embodiment 2
The embodiment of the present invention 2 proposes a kind of hexahedral preparation method of ferrous carbonate, comprises the steps：
S1, the urea of the Iron dichloride tetrahydrate of 2.5mmol, 8mmol is dissolved in the deionized water of 48mL, in magnetic force
Uniform solution is obtained under agitator stirring；
S2, the solution stirred in S1 is added to volume be 70mL polytetrafluoroethylene (PTFE) autoclave inner bag in, then will
Autoclave is put in baking oven, is heated to 170 DEG C, is incubated 8 hours；
S3, autoclave are naturally cooled to and take out after room temperature product, by product deionized water and absolute ethyl alcohol
Cyclic washing, in neutrality, is then centrifuged for being precipitated thing and in an oven dries sediment to the aqueous solution, obtains ferrous carbonate
Hexahedron powder.
Embodiment 3
The embodiment of the present invention 3 proposes a kind of hexahedral preparation method of ferrous carbonate, comprises the steps：
S1, the urea of the Iron dichloride tetrahydrate of 4mmol, 14mmol is dissolved in the deionized water of 54mL, in magnetic force
Uniform solution is obtained under agitator stirring；
S2, the solution stirred in S1 is added to volume be 70mL polytetrafluoroethylene (PTFE) autoclave inner bag in, then will
Autoclave is put in baking oven, is heated to 150 DEG C, is incubated 15 hours；
S3, autoclave are naturally cooled to and take out after room temperature product, by product deionized water and absolute ethyl alcohol
Cyclic washing, in neutrality, is then centrifuged for being precipitated thing and in an oven dries sediment to the aqueous solution, obtains ferrous carbonate
Hexahedron powder.
SEM observations and XRD analysis are carried out according to the ferrous carbonate hexahedron that above-described embodiment is prepared.
With reference to Fig. 1, from SEM photograph knowableing to, the yield of products therefrom is very big, and crystallinity is high, particle in hexahedral shape, six
The size dimension of face body is distributed in 500～5000nm or so, specifically between 800-4000nm, specifically in 1500-
Between 2500nm.
With reference to Fig. 2, knowable to XRD spectra, products therefrom is ferrous carbonate FeCO3 phase crystal structure (JCPDS card
no.01-083-1764)
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (10)
1. a kind of ferrous carbonate hexahedron, ferrous carbonate hexahedron is FeCO3Phase hexahedron crystal structure, ferrous carbonate hexahedron
The length of side between 1500-5000nm；The hexahedral phase crystal structure of the ferrous carbonate is JCPDS card no.01-083-
1764；
Prepare the ferrous carbonate hexahedron to comprise the steps：
S1, by Iron dichloride tetrahydrate, urea and deionized water in molar ratio be 2.5-3.5：8-12：The ratio of 2000-3000
Stir；
S2, the solution stirred in S1 is added in autoclave, then autoclave is put in baking oven, be heated to 120-180
DEG C, it is incubated 3-18 hours；
S3, autoclave are naturally cooled to and take out after room temperature product, by product deionized water and absolute ethyl alcohol repeatedly
Wash to the aqueous solution in neutrality, be then centrifuged for being precipitated thing and in an oven dry sediment, obtain the face of ferrous carbonate six
Body powder.
2. ferrous carbonate hexahedron according to claim 1, the hexahedral length of side of ferrous carbonate 1500-2500nm it
Between.
3. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S1, Iron dichloride tetrahydrate, urea
It is in molar ratio 3 with deionized water：10：2000-3000.
4. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, is heated to 140-170 DEG C, protects
Warm 5-15 hours.
5. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, is heated to 150-170 DEG C, protects
Warm 7-12 hours.
6. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, is heated to 160 DEG C, insulation 10
Hour.
7. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, with the intensification speed of 2-3 DEG C/min
Rate carries out heat temperature raising.
8. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, solution filling out in autoclave
Degree of filling is 60%-85%.
9. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, compactedness is 65%-80%.
10. ferrous carbonate hexahedron according to claim 1, it is characterised in that in S2, compactedness is 70%-75%.
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| CN106365206B (en) * | 2016-09-13 | 2018-03-27 | 济南大学 | A kind of FeCO3The preparation method of rhombohedron |
| CN112675810B (en) * | 2020-12-02 | 2022-10-11 | 哈尔滨工业大学 | Amorphous high-efficiency phosphorus removal adsorption material, preparation method and water treatment application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153151A (en) * | 2011-04-29 | 2011-08-17 | 中国科学院合肥物质科学研究院 | Ferroferric oxide porous ball having micro-nano structure, and preparation method of ferroferric oxide porous ball |
| CN102280640A (en) * | 2011-07-12 | 2011-12-14 | 南开大学 | Novel anode material for lithium-ion secondary battery |
| CN103413941A (en) * | 2013-07-23 | 2013-11-27 | 华南农业大学 | Lithium ion battery cathode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102153151A (en) * | 2011-04-29 | 2011-08-17 | 中国科学院合肥物质科学研究院 | Ferroferric oxide porous ball having micro-nano structure, and preparation method of ferroferric oxide porous ball |
| CN102280640A (en) * | 2011-07-12 | 2011-12-14 | 南开大学 | Novel anode material for lithium-ion secondary battery |
| CN103413941A (en) * | 2013-07-23 | 2013-11-27 | 华南农业大学 | Lithium ion battery cathode material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| "碳酸亚铁的制备及电化学性能";刘伟健等;《电池》;20141031;第44卷(第5期);第280页右栏第1段、第281页左栏倒数第1段以及图2 * |
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