CN106365206A - Preparation method of FeCO3 rhombohedron - Google Patents
Preparation method of FeCO3 rhombohedron Download PDFInfo
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- CN106365206A CN106365206A CN201610822051.1A CN201610822051A CN106365206A CN 106365206 A CN106365206 A CN 106365206A CN 201610822051 A CN201610822051 A CN 201610822051A CN 106365206 A CN106365206 A CN 106365206A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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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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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
Abstract
The invention discloses a preparation method of an FeCO3 rhombohedron. The method comprises the following steps: adding a ferric iron salt and NaHCO3 into an ethanol-glycerol mixed solvent, and stirring to obtain a transparent solution; heating the solution, and carrying out solvothermal reaction; and after the reaction finishes, centrifugating the product, and washing to obtain the FeCO3 rhombohedron. All the raw materials are cheap common reagents and agents in the market. The preparation technique is simple to operate and easy to control. The product has regular shape and favorable repetitiveness. The method can obtain FeCO3 rhombohedron micro/nano particles with different sizes, is suitable for mass production, and has great application value in the fields of microwave absorption, lithium ion batteries and the like.
Description
Technical field
The present invention relates to a kind of feco3Rhombohedral preparation method is and in particular to a kind of feco of size adjustable3Rhombohedron
The preparation method of micro-nano granules, belongs to functional material preparing technical field.
Background technology
feco3Belong to trigonal system, be the broad-spectrum transition metal carbonate of a class, be to prepare fe2o3And fe3o4Micro-nano
The important precursor of rice material, have that microscopic appearance is adjustable, physical and chemical performance is excellent, good environmental adaptability the features such as.As one kind
Typical magnetic absorbing material, feco3Show preferably at aspects such as ferrofluid, magnetic recording medium, electromagnetism stealth, data storages
Magnetic absorbing performance；On the other hand, feco3Chemical property project, play in cathode material for lithium ion battery field
Important using value.
In recent years, feco3The structure regulating of micro Nano material causes the extensive concern of people, and relevant report shows, leads to
Cross reasonable selection reaction system, control reaction process, such as medicine ball, hollow ball, lamellar, wire, Hemicentrotus seu Strongylocentrotuss shape can be obtained, stand
The different feco of the different morphologies such as square3Micro nano structure.For example, " congcong zhang, weijian liu,
dongyang chen, jiayi huang, xiaoyuan yu, xueyan huang, and yueping fang,
Electrochimica acta, 2015,182,559-564 " report with iron sulfate, carbamide as raw material, deionized water is
Solvent, prepares, 100 DEG C of reaction certain times, the feco that the length of side is 300 nm by hydro-thermal method3Cubic block, research finds
It has good chemical property as lithium ion battery negative material, and initial capacity reaches 1796 mahg-1；“bin yao,
zhaojun ding, xiaoyu feng, longwei yin, qiang shen, yuanchang shi, and
Jianxin zhang, electrochimica acta, 2014,148,283-290 " reports with ferric chloride hexahydrate
(fecl3∙6h2O), carbamide, ascorbic acid are raw material, and deionized water is solvent, reacts certain time by hydro-thermal method at 160 DEG C
Prepare a diameter of 15-30 μm of feco3Flower-like microsphere, related electrochemical property test shows feco3Flower-like microsphere is one
Plant very promising lithium ion battery negative material.
Design and synthesis size adjustable, the feco of novel in shape3Micro Nano material, explores different exposure crystal faces, has crystallized
The influencing mechanism to electrochemistry, microwave absorbing property such as whole property, multipolarity structure, it has also become the study hotspot problem in this field.
feco3Rhombohedron has special microscopic appearance, it is possible to produce excellent physicochemical characteristic.At present, both at home and abroad with regard to feco3Pedicellus et Pericarpium Trapae
Face body synthesis technique is few with the report of performance study, and is commonly present reaction process complexity, poor controllability, product in preparation process
The shortcomings of thing low yield, topography uniformity difference, is it is difficult to realize mass production.
Content of the invention
It is an object of the invention to provide a kind of feco3Rhombohedral preparation method, the method is raw materials used cheap, instead
Answer system simple, reaction process is easily-controllable, combined coefficient is high, product morphology homogeneity with reproducible, particle size is adjustable, suitable
Industrialization, has larger practical application meaning.
Concrete technical scheme of the present invention is as follows:
A kind of feco3Rhombohedral preparation method, the method comprises the following steps:
(1) by trivalent iron salt, nahco3It is added in ethanol and the mixed solvent of glycerol, stir to obtain clear solution；
(2) solution of step (1) is heated, carry out solvent thermal reaction；
(3), after reacting, product is centrifuged, washs, obtain feco3Rhombohedron.
In above-mentioned preparation method, described trivalent iron salt is halogenide or the nitrate of ferrum.
In above-mentioned preparation method, trivalent iron salt and nahco3Mol ratio be 1:8-14.
In above-mentioned preparation method, in mixed solvent, ethanol is 0.5-8:1 with the volume ratio of glycerol.
In above-mentioned preparation method, concentration in the clear solution of step (1) for the trivalent iron salt is 0.06-0.12 mol/l.
In above-mentioned preparation method, the temperature of solvent thermal reaction is 170-220 DEG C, and the response time is 3-30 h.
In above-mentioned preparation method, solvent thermal reaction is carried out in confined conditions.
In above-mentioned preparation method, gained feco3Rhombohedron belongs to trigonal system, and each face is parallel four sides of rule
Shape, the length of side of parallelogram is 0.25-6.0 μm, a size of 0.5-12.0 μm of rhombohedral particle.
The present invention by the selection of iron salt, alkali and solvent species and consumption, by simple solvent thermal reaction
Feco to regular appearance, size adjustable3Rhombohedron.The present invention is raw materials used be cheap common agents in market with
Medicine, preparation technology simple to operate it is easy to control, product morphology is regular and reproducible, various sizes of feco can be obtained3
Rhombohedron micro-nano granules, it is adaptable to mass production, have larger application valency in fields such as microwave absorption, lithium ion batteries
Value.
Cost of material selected by the present invention is low, source is wide, and synthesis technique is simple, and response parameter is easy to set up, and product morphology is advised
Whole, reproducible, particle size distribution range is narrow, and yield is high, is conducive to mass production, to exploration feco3Rhombohedral structure
With the internal relation of performance, there is important scientific meaning and practice significance.
Brief description
Fig. 1 is the feco of the embodiment of the present invention 1 synthesis3Rhombohedral x-ray diffraction (xrd) collection of illustrative plates.
Fig. 2 is the feco of the embodiment of the present invention 1 synthesis3Rhombohedral scanning electron microscope (sem) picture.
Fig. 3 is the feco of the embodiment of the present invention 1 synthesis3Rhombohedral sem picture.
Fig. 4 is the α-fe of comparative example 1 synthesis of the present invention2o3The xrd collection of illustrative plates of bowl structure.
Fig. 5 is the α-fe of comparative example 1 synthesis of the present invention2o3The sem picture of bowl structure.
Specific embodiment
Below by embodiment, the present invention will be further elaborated, the description below only for explain the present invention, not
Its content is defined.
Embodiment 1
1.1 by the fecl of 0.676 g3∙6h2O, the nahco of 1.800 g3It is added to 12.5 ml ethanol and 12.5 ml glycerol
In mixed solvent, stirring obtains clear solution；
1.2 transfer to above-mentioned solution in reactor, confined reaction 16 h at 200 DEG C；
1.3 products, after centrifugation and washing, obtain feco3Rhombohedron.The phase structure of product and microscopic appearance are respectively
As Figure 1-3.Fig. 1 is feco3Rhombohedral xrd collection of illustrative plates, it can be found that x-ray diffraction peak value and jcpds card (83-1764)
It is consistent it was demonstrated that products therefrom is trigonal system feco3Siderite phase；Fig. 2 and Fig. 3 is feco3Rhombohedral sem picture, can
To find feco3Each face of rhombohedron is the parallelogram of rule, and the length of side is 1.6-2.6 μm, and rhombohedral particle is a size of
2.4-4.0 μm, particle dispersion is good, and size distribution ranges are narrow.
Embodiment 2
2.1 by the Fe(NO3)39H2O (fe (no of 1.010 g3)3∙9h2O), the nahco of 1.701 g3It is added to 13.0 ml ethanol
In the mixed solvent of 22.0 ml glycerol, stirring obtains clear solution；
2.2 transfer to above-mentioned solution in reactor, confined reaction 3 h at 170 DEG C；
2.3 products, after centrifugation and washing, obtain the feco that the length of side is 0.4-0.7 μm3Rhombohedron, rhombohedral particle
A size of 0.7-1.3 μm.
Embodiment 3
3.1 by the fe (no of 1.010 g3)3∙9h2O, the nahco of 2.290 g3It is added to 22.5 ml ethanol and 5.5 ml glycerol
Mixed solvent in, stirring obtain clear solution；
3.2 transfer to above-mentioned solution in reactor, confined reaction 25 h at 190 DEG C；
3.3 products, after centrifugation and washing, obtain the feco that the length of side is 1.4-2.4 μm3Rhombohedron, rhombohedral particle
A size of 2.1-3.6 μm.
Embodiment 4
4.1 by the fecl of 0.676 g3∙6h2O, the nahco of 2.110 g3It is added to 23.0 ml ethanol and 3.0 ml glycerol
In mixed solvent, stirring obtains clear solution；
4.2 transfer to above-mentioned solution in reactor, confined reaction 8 h at 180 DEG C；
4.3 products, after centrifugation and washing, obtain the feco that the length of side is 1.0-1.6 μm3Rhombohedron, rhombohedral particle
A size of 1.7-2.8 μm.
Embodiment 5
5.1 by the fe (no of 1.010 g3)3∙9h2O, the nahco of 2.800 g3It is added to 20.0 ml ethanol and 3.0 ml glycerol
Mixed solvent in, stirring obtain clear solution；
5.2 transfer to above-mentioned solution in reactor, confined reaction 11 h at 210 DEG C；
5.3 products, after centrifugation and washing, obtain the feco that the length of side is 2.7-3.4 μm3Rhombohedron, rhombohedral particle
A size of 3.2-4.8 μm.
Embodiment 6
6.1 by the fecl of 0.676 g3∙6h2O, the nahco of 2.750 g3It is added to 19.0 ml ethanol and 10.0 ml glycerol
In mixed solvent, stirring obtains clear solution；
6.2 transfer to above-mentioned solution in reactor, confined reaction 23 h at 220 DEG C；
6.3 products, after centrifugation and washing, obtain the feco that the length of side is 4.3-5.1 μm3Rhombohedron, rhombohedral particle
A size of 7.0-9.8 μm.
Embodiment 7
7.1 by the fecl of 0.676 g3∙6h2O, the nahco of 1.800 g3It is added to 19.0 ml ethanol and 6.0 ml glycerol
In mixed solvent, stirring obtains clear solution；
7.2 transfer to above-mentioned solution in reactor, confined reaction 16 h at 200 DEG C；
7.3 products, after centrifugation and washing, obtain the feco that the length of side is 1.4-2.0 μm3Rhombohedron, rhombohedral particle
A size of 2.0-3.5 μm.
Embodiment 8
8.1 by the fe (no of 1.010 g3)3∙9h2O, the nahco of 1.850 g3It is added to 26.0 ml ethanol and 8.0 ml glycerol
Mixed solvent in, stirring obtain clear solution；
8.2 transfer to above-mentioned solution in reactor, confined reaction 27 h at 170 DEG C；
8.3 products, after centrifugation and washing, obtain the feco that the length of side is 0.7-1.1 μm3Rhombohedron, rhombohedral particle
A size of 1.2-2.1 μm.
Embodiment 9
9.1 by the fe (no of 1.010 g3)3∙9h2O, the nahco of 2.470 g3It is added to 27.0 ml ethanol and 4.0 ml glycerol
Mixed solvent in, stirring obtain clear solution；
9.2 transfer to above-mentioned solution in reactor, confined reaction 29 h at 210 DEG C；
9.3 products, after centrifugation and washing, obtain the feco that the length of side is 3.7-4.6 μm3Rhombohedron, rhombohedral particle
A size of 5.2-7.4 μm.
Embodiment 10
10.1 by the fecl of 0.676 g3∙6h2O, the nahco of 2.680 g3It is added to 24.0 ml ethanol and 4.0 ml glycerol
In mixed solvent, stirring obtains clear solution；
10.2 transfer to above-mentioned solution in reactor, confined reaction 4 h at 220 DEG C；
10.3 products, after centrifugation and washing, obtain the feco that the length of side is 4.1-4.9 μm3Rhombohedron, rhombohedral particle
A size of 6.3-7.5 μm.
Comparative example 1
1.1 by the fecl of 0.676 g3∙6h2O, the nahco of 1.800 g3, be added in 25 ml alcohol solvents, stirring obtain
Bright solution；
1.2 with embodiment 1；
1.3 with embodiment 1.
The phase structure of product and microscopic appearance are respectively as shown in Figures 4 and 5.Fig. 4 is the product of synthesis in comparative example 1
Xrd collection of illustrative plates, it can be seen that products therefrom is α-fe2o3, not feco3；Fig. 5 is the α-fe of synthesis in comparative example 12o3
The sem picture of product, it can be found that product grain mid-portion concave, forms bowl structure, and particle diameter is 110-145 nm,
Female a diameter of 53-67 nm.
From comparative example 1, when reaction system is added without glycerol it is impossible to synthesize feco3Rhombohedron, can only obtain
Grain dispersibility preferable α-fe2o3Bowl structure, illustrates the species of solvent for the synthesis of product structure and pattern and controllable growth
There is important function.
Comparative example 2
2.1 by the fecl of 0.676 g3∙6h2O, the nahco of 1.000 g3It is added to 2 ml ethanol and the mixing of 12 ml glycerol
In solvent, stirring obtains clear solution；
2.2 transfer to above-mentioned solution in reactor, confined reaction 12 h at 200 DEG C；
2.3 products, after centrifugation and washing, obtain bad dispersibility, reunite the obvious, big (0.7-3.5 of size distribution ranges
μm) feco3Random granule, the consumption that raw material is described is to feco3The formation of rhombohedron pattern has considerable influence.
Comparative example 3
3.1 by the fecl of 0.676 g3∙6h2O, the carbamide of 1.5 g are added to the mixed solvent of 22 ml ethanol and 4ml ethylene glycol
In, stirring obtains clear solution；
3.2 transfer to above-mentioned solution in reactor, confined reaction 18 h at 190 DEG C；
3.3 products, after centrifugation and washing, obtain bad dispersibility, reunite the obvious, big (0.4-2.7 of size distribution ranges
μm) α-fe2o3Random granule, the species that raw material is described is to feco3The formation of rhombohedron pattern has considerable influence.
Comparative example 4
4.1 by the fe (no of 1.010 g3)3∙9h2O, the na of 2.050 g2co3It is added to 12.5 ml deionized waters and 12.5 ml
In the mixed solvent of glycerol, stirring obtains clear solution；
4.2 transfer to above-mentioned solution in reactor, confined reaction 14 h at 200 DEG C；
4.3 products, after centrifugation and washing, obtain bad dispersibility, reunite obvious, a size of 0.2-0.4 μm of fe3o4
Random granule, the species that raw material is described is to feco3The formation of rhombohedron pattern has considerable influence.
Comparative example 5
5.1 by the fecl of 0.676 g3∙6h2O, the nahco of 2.400 g3It is added to 14.0 ml ethanol and 8.0 ml isopropanols
In mixed solvent, stirring obtains clear solution；
5.2 transfer to above-mentioned solution in reactor, confined reaction 20 h at 190 DEG C；
5.3 products after centrifugation and washing, obtain bad dispersibility, reunite substantially, a size of 0.3-0.6 μm of α-
fe2o3Ellipsoid granule, the species that solvent is described is to feco3The formation of rhombohedron pattern has considerable influence.
Claims (8)
1. a kind of feco3Rhombohedral preparation method, is characterized in that comprising the following steps:
(1) by trivalent iron salt, nahco3It is added in ethanol and the mixed solvent of glycerol, stir to obtain clear solution；
(2) solution of step (1) is heated, carry out solvent thermal reaction；
(3), after reacting, product is centrifuged, washs, obtain feco3Rhombohedron.
2. preparation method according to claim 1, is characterized in that: described trivalent iron salt is halogenide or the nitrate of ferrum.
3. preparation method according to claim 1, is characterized in that: ethanol is 0.5-8:1 with the volume ratio of glycerol.
4. preparation method according to claim 1, is characterized in that: trivalent iron salt and nahco3Mol ratio be 1:8-14.
5. the preparation method according to any one of claim 1-4, is characterized in that: trivalent iron salt is dense in clear solution
Spend for 0.06-0.12 mol/l.
6. the preparation method according to any one of claim 1-5, is characterized in that: the temperature of solvent thermal reaction is 170-
220 DEG C, the response time is 5-30 h.
7. the preparation method according to any one of claim 1-5, is characterized in that: solvent thermal reaction enters in confined conditions
OK.
8. the preparation method according to any one of claim 1-7, is characterized in that: gained feco3Rhombohedron belongs to three prismatic crystals
System, each face is the parallelogram of rule, and the length of side of each parallelogram is 0.25-6.0 μm, rhombohedral particle chi
Very little for 0.5-12.0 μm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3058810A (en) * | 1960-06-01 | 1962-10-16 | Phillips Petroleum Co | Process for producing ferrous carbonate and removing oil from ammonia therewith |
| US4657752A (en) * | 1985-04-16 | 1987-04-14 | Phillips Petroleum Company | Process for preparing ferrous carbonate |
| CN104556237A (en) * | 2014-12-08 | 2015-04-29 | 中国科学院合肥物质科学研究院 | Ferrous carbonate hexahedron and preparation method thereof |
| CN104761001A (en) * | 2014-10-25 | 2015-07-08 | 青岛科技大学 | Preparation method of cubic ferrous carbonate |
| CN105552329A (en) * | 2015-12-23 | 2016-05-04 | 芜湖天弋能源科技有限公司 | Preparation method for precursor FeCO3 of lithium ion battery positive electrode material LiPeO4 |
-
2016
- 2016-09-13 CN CN201610822051.1A patent/CN106365206B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3058810A (en) * | 1960-06-01 | 1962-10-16 | Phillips Petroleum Co | Process for producing ferrous carbonate and removing oil from ammonia therewith |
| US4657752A (en) * | 1985-04-16 | 1987-04-14 | Phillips Petroleum Company | Process for preparing ferrous carbonate |
| CN104761001A (en) * | 2014-10-25 | 2015-07-08 | 青岛科技大学 | Preparation method of cubic ferrous carbonate |
| CN104556237A (en) * | 2014-12-08 | 2015-04-29 | 中国科学院合肥物质科学研究院 | Ferrous carbonate hexahedron and preparation method thereof |
| CN105552329A (en) * | 2015-12-23 | 2016-05-04 | 芜湖天弋能源科技有限公司 | Preparation method for precursor FeCO3 of lithium ion battery positive electrode material LiPeO4 |
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