CN104556237A - Ferrous carbonate hexahedron and preparation method thereof - Google Patents
Ferrous carbonate hexahedron and preparation method thereof Download PDFInfo
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- CN104556237A CN104556237A CN201410746946.2A CN201410746946A CN104556237A CN 104556237 A CN104556237 A CN 104556237A CN 201410746946 A CN201410746946 A CN 201410746946A CN 104556237 A CN104556237 A CN 104556237A
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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, particularly relate to a kind of iron protocarbonate hexahedron and preparation method thereof.
Background technology
Iron protocarbonate, molecular formula is FeCO
3, belong to trigonal system, crystalline structure belongs to diamond structure, due to the crystalline structure of its uniqueness, is preparation Fe always
3o
4and Fe
2o
3the study hotspot of presoma.Have the synthetic method of bibliographical information different-shape iron protocarbonate in recent years, such as by by reductive agent as xitix, urea and iron trichloride mix, then obtain iron protocarbonate elliposoidal structure by hydrothermal method; If introduce tensio-active agent polyvinylpyrrolidone further in above-mentioned system, then can obtain the iron protocarbonate ball of ganoid micro-meter scale.To polyhedral iron protocarbonate and how to obtain polyhedral iron protocarbonate and but seldom report in prior art.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of iron protocarbonate hexahedron and preparation method thereof, adopt hydrothermal method to make iron protocarbonate hexahedron, its preparation method is simple, and crystallinity is high.
The present invention proposes a kind of iron protocarbonate hexahedron, iron protocarbonate hexahedron is FeCO
3phase hexahedron crystalline structure, the hexahedral length of side of iron protocarbonate is between 500-5000nm.
Preferably, the hexahedral length of side of iron protocarbonate is between 800-4000nm.
Preferably, the hexahedral length of side of iron protocarbonate is between 1500-2500nm.
The invention allows for the hexahedral preparation method of a kind of iron protocarbonate, comprise the steps:
S1, by Iron dichloride tetrahydrate, urea and deionized water in molar ratio for the ratio of 1-5:3-15:2000-3000 stirs;
S2, the solution stirred in S1 to be joined in autoclave, then autoclave is put into baking oven, be heated to 120-180 DEG C, insulation 3-18 hour;
S3, autoclave take out reaction product after naturally cooling to room temperature, by reaction product deionized water and dehydrated alcohol repetitive scrubbing to the aqueous solution in neutral, be then centrifugally precipitated thing and throw out dried in an oven, obtaining iron protocarbonate hexahedron powder.
Preferably, in S1, Iron dichloride tetrahydrate, urea and deionized water are 2-4:6-12:2000-3000 in molar ratio; Preferably, Iron dichloride tetrahydrate, urea and deionized water are 2.5-3.5:8-12:2000-3000 in molar ratio; More preferably, Iron dichloride tetrahydrate, urea and deionized water are 3:10:2000-3000 in molar ratio.
Preferably, in S2, be heated to 140-170 DEG C, insulation 5-15 hour; Preferably, be heated to 150-170 DEG C, insulation 7-12 hour; More preferably, be heated to 160 DEG C, be incubated 10 hours.
Preferably, in S2, carry out heat temperature raising with the temperature rise rate of 2-3 DEG C/min.
Preferably, in S2, the compactedness of solution in autoclave is 60%-85%; Preferably, compactedness is 65%-80%; More preferably, compactedness is 70%-75%.
In the present invention, iron protocarbonate hexahedron utilizes Iron dichloride tetrahydrate and urea as raw material, by the ferrous hexahedron powder of water heat transfer carbonic acid, in reaction process, do not need to add dispersion agent and tensio-active agent, the hexahedral crystallinity of obtained iron protocarbonate is high; Without the need to adding the materials such as template in preparation process, convenient post-treatment, temperature of reaction is low, the reaction times is short, reaction process is simple, inexpensive; In preparation process environmental protection, do not use any poisonous and hazardous organic reagent.
Accompanying drawing explanation
Fig. 1 adopts scanning electronic microscope SEM observation to take the Photomicrograph obtained afterwards to iron protocarbonate hexahedron powder.
Fig. 2 is the XRD spectra recorded Fig. 1 Phlips X ' Pert type X-ray diffraction instrument.
Embodiment
Embodiment 1
The embodiment of the present invention 1 proposes the hexahedral preparation method of a kind of iron protocarbonate, comprises the steps:
S1, the Iron dichloride tetrahydrate of 3mmol, the urea of 10mmol are dissolved in the deionized water of 50mL, under magnetic stirrer, obtain uniform solution;
S2, the solution stirred in S1 is joined volume is in the tetrafluoroethylene autoclave inner bag of 70mL, then autoclave is put into baking oven, is heated to 160 DEG C, is incubated 10 hours;
S3, autoclave take out reaction product after naturally cooling to room temperature, by reaction product deionized water and dehydrated alcohol repetitive scrubbing to the aqueous solution in neutral, be then centrifugally precipitated thing and throw out dried in an oven, obtaining iron protocarbonate hexahedron powder.
Embodiment 2
The embodiment of the present invention 2 proposes the hexahedral preparation method of a kind of iron protocarbonate, comprises the steps:
S1, the Iron dichloride tetrahydrate of 2.5mmol, the urea of 8mmol are dissolved in the deionized water of 48mL, under magnetic stirrer, obtain uniform solution;
S2, the solution stirred in S1 is joined volume is in the tetrafluoroethylene autoclave inner bag of 70mL, then autoclave is put into baking oven, is heated to 170 DEG C, is incubated 8 hours;
S3, autoclave take out reaction product after naturally cooling to room temperature, by reaction product deionized water and dehydrated alcohol repetitive scrubbing to the aqueous solution in neutral, be then centrifugally precipitated thing and throw out dried in an oven, obtaining iron protocarbonate hexahedron powder.
Embodiment 3
The embodiment of the present invention 3 proposes the hexahedral preparation method of a kind of iron protocarbonate, comprises the steps:
S1, the Iron dichloride tetrahydrate of 4mmol, the urea of 14mmol are dissolved in the deionized water of 54mL, under magnetic stirrer, obtain uniform solution;
S2, the solution stirred in S1 is joined volume is in the tetrafluoroethylene autoclave inner bag of 70mL, then autoclave is put into baking oven, is heated to 150 DEG C, is incubated 15 hours;
S3, autoclave take out reaction product after naturally cooling to room temperature, by reaction product deionized water and dehydrated alcohol repetitive scrubbing to the aqueous solution in neutral, be then centrifugally precipitated thing and throw out dried in an oven, obtaining iron protocarbonate hexahedron powder.
SEM observation and XRD analysis is carried out according to the iron protocarbonate hexahedron that above-described embodiment prepares.
With reference to Fig. 1, from SEM photo, the output of products therefrom is very large, and crystallinity is high, and particle is hexahedral shape, and hexahedral size dimension is distributed in about 500 ~ 5000nm, particularly between 800-4000nm, more specifically between 1500-2500nm.
With reference to Fig. 2, from XRD spectra, products therefrom is iron protocarbonate FeCO3 phase crystalline structure (JCPDS card no.01-083-1764)
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (8)
1. an iron protocarbonate hexahedron, iron protocarbonate hexahedron is FeCO
3phase hexahedron crystalline structure, the hexahedral length of side of iron protocarbonate is between 500-5000nm.
2. iron protocarbonate hexahedron according to claim 1, the hexahedral length of side of iron protocarbonate is between 800-4000nm.
3. iron protocarbonate hexahedron according to claim 2, the hexahedral length of side of iron protocarbonate is between 1500-2500nm.
4. the hexahedral preparation method of iron protocarbonate, is characterized in that, comprise the steps:
S1, by Iron dichloride tetrahydrate, urea and deionized water in molar ratio for the ratio of 1-5:3-15:2000-3000 stirs;
S2, the solution stirred in S1 to be joined in autoclave, then autoclave is put into baking oven, be heated to 120-180 DEG C, insulation 3-18 hour;
S3, autoclave take out reaction product after naturally cooling to room temperature, by reaction product deionized water and dehydrated alcohol repetitive scrubbing to the aqueous solution in neutral, be then centrifugally precipitated thing and throw out dried in an oven, obtaining iron protocarbonate hexahedron powder.
5. the hexahedral preparation method of iron protocarbonate according to claim 4, is characterized in that, in S1, Iron dichloride tetrahydrate, urea and deionized water are 2-4:6-12:2000-3000 in molar ratio; Preferably, Iron dichloride tetrahydrate, urea and deionized water are 2.5-3.5:8-12:2000-3000 in molar ratio; More preferably, Iron dichloride tetrahydrate, urea and deionized water are 3:10:2000-3000 in molar ratio.
6. the hexahedral preparation method of the iron protocarbonate according to claim 4 or 5, is characterized in that, in S2, is heated to 140-170 DEG C, insulation 5-15 hour; Preferably, be heated to 150-170 DEG C, insulation 7-12 hour; More preferably, be heated to 160 DEG C, be incubated 10 hours.
7. the hexahedral preparation method of the iron protocarbonate according to any one of claim 4-6, is characterized in that, in S2, carries out heat temperature raising with the temperature rise rate of 2-3 DEG C/min.
8. the hexahedral preparation method of the iron protocarbonate according to any one of claim 4-7, is characterized in that, in S2, the compactedness of solution in autoclave is 60%-85%; Preferably, compactedness is 65%-80%; More preferably, compactedness is 70%-75%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365206A (en) * | 2016-09-13 | 2017-02-01 | 济南大学 | Preparation method of FeCO3 rhombohedron |
| CN112675810A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Amorphous high-efficiency phosphorus removal adsorption material, preparation method and water treatment application thereof |
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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 |
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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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365206A (en) * | 2016-09-13 | 2017-02-01 | 济南大学 | Preparation method of FeCO3 rhombohedron |
| CN106365206B (en) * | 2016-09-13 | 2018-03-27 | 济南大学 | A kind of FeCO3The preparation method of rhombohedron |
| CN112675810A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Amorphous high-efficiency phosphorus removal adsorption material, preparation method and water treatment application thereof |
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