CN104556245A - Hamburger-shaped nanometer ferric oxide material, and preparation method and usage thereof - Google Patents
Hamburger-shaped nanometer ferric oxide material, and preparation method and usage thereof Download PDFInfo
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- CN104556245A CN104556245A CN201410851224.3A CN201410851224A CN104556245A CN 104556245 A CN104556245 A CN 104556245A CN 201410851224 A CN201410851224 A CN 201410851224A CN 104556245 A CN104556245 A CN 104556245A
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Abstract
The invention provides a hamburger-shaped nanometer ferric oxide material which is powdery, and the microcosmic morphology of the material is laminated hamburger-shaped. The hamburger-shaped nanometer ferric oxide material is prepared through the following steps: adding an iron source into a water solution containing a dispersing agent and an end-capping reagent; under a stirring state, adding an alkali material containing an amido group into the solution, so as to enable the pH value of the solution to be 10; then transferring the mixed solution into a high pressure reaction vessel for hydrothermal reaction, after the reaction, cooling to the room temperature, and generating brick-red deposit; finally, washing and drying the obtained brick-red deposit, namely obtaining the hamburger-shaped nanometer ferric oxide material. The nanometer ferric oxide material provided by the invention is novel in appearance and has a hamburger-shaped structure, and the prepared nanometer ferric oxide is uniform in particles, high in productivity and is suitable for industrialized mass production.
Description
Technical field
The present invention relates to the preparation field of nano material, particularly relate to the preparation method of a kind of hamburger shape nano-sized iron oxide.
Background technology
Nano-sized iron oxide is the nano-grade matter of ferriferous oxide, except the fundamental characteristics with nano material, the light resistance also had, weatherability, magnetic, catalytic activity, and uniqueness to UV absorption and shielding properties.These characteristics make it have a wide range of applications in fields such as magnetic material, ceramic material, pigment, catalyst, gas sensor, optics, medical science, and it is at present after titanium dioxide, the nanometer materials of second largest industrialization in world wide.Mainly comprise FeO, Fe
3o
4and the α-Fe of di-iron trioxide series
2o
3, β-Fe
2o
3, γ-Fe
2o
3.In addition, α, β, γ-FeOOH hydrated ferric oxide is also had.α-Fe
2o
3, γ-Fe
2o
3, Fe
3o
4be that more several iron oxide are applied in research at present, believe that they can show more vast potential for future development along with people are to the further investigation of its stuctures and properties.
As everyone knows, the pattern of nano material and size determine its performance and application, and therefore, the regulation and control of pattern and size are the research emphasis of preparation nano material always.At present, researcher synthesizes many different nano-sized iron oxides by methods such as traditional precipitation method, template, thermal decompositions, as simply spherical, clavate, dish type, linear, tubular, peanut shape, pine tree shape, cube, spindle etc., also have more complicated sea urchin shape, polyhedron shape, biconial etc.But, the nano-sized iron oxide of these appearance structure is only had to be to meet the quick industrial requirement increased, simultaneously, these defects such as method ubiquity complicated operation, cost is high, the cycle is long, poor controllability, and synthesized product is homogeneous not, purity is low, can not realize industrial volume production.
Summary of the invention
The invention provides a kind of hamburger shape nano-sized iron oxide and preparation method thereof, prepared nano-sized iron oxide novel in shape, this hamburger shape is not yet seen in other Patents documents, and prepared nano-sized iron oxide particle is homogeneous, productive rate is high, is applicable to industrialization large-scale production.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
The nano oxidized iron material of a kind of hamburger shape, described material is Powdered, and its microscopic pattern is stacked hamburger shape, and the nano oxidized iron material of described hamburger shape adopts following methods preparation: in the aqueous solution containing dispersant and end-capping reagent, add source of iron; Under the state stirred, in above-mentioned solution, add the alkaline matter containing amido, make the pH of solution be 10; Then above-mentioned mixed solution is transferred in autoclave and carry out hydro-thermal reaction, be cooled to room temperature after reaction, generate brick-red precipitation; Finally obtained brick-red sediment is washed, dried, the nano oxidized iron material of hamburger shape can be obtained.
Present invention also offers the preparation method preparing the nano oxidized iron material of hamburger shape stated, comprise the following steps: (1) at normal temperatures and pressures, source of iron is added in the aqueous solution containing dispersant and end-capping reagent, wherein the concentration of dispersant is 5 ~ 20mg/mL, the concentration of end-capping reagent is 0.8 ~ 2.5mg/mL, and the amount of substance of the iron ion added is 0.015 ~ 0.05mmol/mL;
(2) under the state stirred, in above-mentioned solution, add the alkaline matter containing amido, make the initial pH of obtained mixed solution be 9 ~ 11;
(3) above-mentioned mixed solution is transferred in autoclave, after the Water Under thermal response 16 ~ 48h of 160 ~ 220 DEG C, generate brick-red precipitation, after reaction terminates, naturally cool to room temperature;
(4) the brick-red sediment obtained in upper step is washed, dried, the nano-sized iron oxide of hamburger shape can be obtained.
Dispersant described in step (1) is PVP K-30, and described end-capping reagent is sodium carboxymethylcellulose, and described source of iron is potassium ferrocyanide or the potassium ferricyanide.
Alkaline matter containing amido described in step (2) is urea, ammoniacal liquor, hydrazine hydrate or formamide.
Adopt centrifuge washing or filtering and washing in step (4), described bake out temperature 60 DEG C, drying time is 24h.
Compared with prior art, the present invention has the following advantages: 1) hamburger shape nano-sized iron oxide novel in shape, uniform particles, the purity that obtain of the method is high, and has good dispersiveness.2) this nano-sized iron oxide has good absorption property, can remove contaminated ion in water body as adsorbent.3) method of the present invention's use is easy and simple to handle, cost is low, controllability is strong, is applicable to industrialization large-scale production.
Accompanying drawing explanation
The XRD collection of illustrative plates of hamburger shape nano oxidized iron material of Fig. 1 prepared by the present embodiment;
The SEM figure of hamburger shape nano oxidized iron material of Fig. 2 prepared by the present embodiment.
Detailed description of the invention
Below in conjunction with specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The preparation method of the nano oxidized iron material of hamburger shape provided in the present embodiment is as follows: at normal temperatures and pressures, potassium ferrocyanide is added in the aqueous solution containing dispersant and end-capping reagent, wherein the concentration of dispersant is 20mg/mL, the concentration of end-capping reagent is 2.5mg/mL, the amount of substance of the iron ion added is 0.03mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethylcellulose.
Under the state stirred, in above-mentioned solution, add ammoniacal liquor, make the initial pH of obtained mixed solution be 9;
Above-mentioned mixed solution is transferred in autoclave, after the Water Under thermal response 16h of 220 DEG C, generates brick-red precipitation, after reaction terminates, naturally cool to room temperature;
Centrifuge washing is carried out to the brick-red sediment obtained in upper step, dries 24h, the nano-sized iron oxide of hamburger shape can be obtained for 60 DEG C.
As shown in Figure 1, its SEM schemes as shown in Figure 2 the XRD collection of illustrative plates of the nano-sized iron oxide of hamburger shape prepared in the present embodiment, and can find out clearly by Fig. 2, its microstructure of nano oxidized iron material prepared by the present invention is stacked hamburger shape.
Embodiment 2
The preparation method of the nano oxidized iron material of hamburger shape provided in the present embodiment is as follows: at normal temperatures and pressures, the potassium ferricyanide is added in the aqueous solution containing dispersant and end-capping reagent, wherein the concentration of dispersant is 5mg/mL, the concentration of end-capping reagent is 0.8mg/mL, the amount of substance of the iron ion added is 0.05mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethylcellulose.
Under the state stirred, in above-mentioned solution, add formamide, make the initial pH of obtained mixed solution be 10;
Above-mentioned mixed solution is transferred in autoclave, after the Water Under thermal response 36h of 200 DEG C, generates brick-red precipitation, after reaction terminates, naturally cool to room temperature;
Centrifuge washing is carried out to the brick-red sediment obtained in upper step, dries 24h, the nano-sized iron oxide of hamburger shape can be obtained for 60 DEG C.
Embodiment 3
The preparation method of the nano oxidized iron material of hamburger shape provided in the present embodiment is as follows: at normal temperatures and pressures, potassium ferrocyanide is added in the aqueous solution containing dispersant and end-capping reagent, wherein the concentration of dispersant is 10mg/mL, the concentration of end-capping reagent is 1.4mg/mL, the amount of substance of the iron ion added is 0.015mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethylcellulose.
Under the state stirred, in above-mentioned solution, add hydrazine hydrate, make the initial pH of obtained mixed solution be 11;
Above-mentioned mixed solution is transferred in autoclave, after the Water Under thermal response 48h of 180 DEG C, generates brick-red precipitation, after reaction terminates, naturally cool to room temperature;
Filtering and washing is carried out to the brick-red sediment obtained in upper step, dries 24h, the nano-sized iron oxide of hamburger shape can be obtained for 60 DEG C.
Claims (5)
1. the nano oxidized iron material of hamburger shape, it is characterized in that: described material is Powdered, its microscopic pattern is stacked hamburger shape, and the nano oxidized iron material of described hamburger shape adopts following methods preparation: in the aqueous solution containing dispersant and end-capping reagent, add source of iron; Under the state stirred, in above-mentioned solution, add the alkaline matter containing amido, make the pH of solution be 10; Then above-mentioned mixed solution is transferred in autoclave and carry out hydro-thermal reaction, be cooled to room temperature after reaction, generate brick-red precipitation; Finally obtained brick-red sediment is washed, dried, the nano oxidized iron material of hamburger shape can be obtained.
2. the preparation method of the nano oxidized iron material of hamburger according to claim 1 shape, it is characterized in that comprising the following steps: (1) at normal temperatures and pressures, source of iron is added in the aqueous solution containing dispersant and end-capping reagent, wherein the concentration of dispersant is 5 ~ 20mg/mL, the concentration of end-capping reagent is 0.8 ~ 2.5mg/mL, and the amount of substance of the iron ion added is 0.015 ~ 0.05mmol/mL;
(2) under the state stirred, in above-mentioned solution, add the alkaline matter containing amido, make the initial pH of obtained mixed solution be 9 ~ 11;
(3) above-mentioned mixed solution is transferred in autoclave, after the Water Under thermal response 16 ~ 48h of 160 ~ 220 DEG C, generate brick-red precipitation, after reaction terminates, naturally cool to room temperature;
(4) the brick-red sediment obtained in upper step is washed, dried, the nano-sized iron oxide of hamburger shape can be obtained.
3. the preparation method of the nano oxidized iron material of hamburger according to claim 2 shape, it is characterized in that: the dispersant described in step (1) is PVP K-30, described end-capping reagent is sodium carboxymethylcellulose, and described source of iron is potassium ferrocyanide or the potassium ferricyanide.
4. the preparation method of the nano oxidized iron material of hamburger according to claim 2 shape, is characterized in that: the alkaline matter containing amido described in step (2) is urea, ammoniacal liquor, hydrazine hydrate or formamide.
5. the preparation method of the nano oxidized iron material of hamburger according to claim 2 shape, is characterized in that: adopt centrifuge washing or filtering and washing in step (4), described bake out temperature 60 DEG C, drying time is 24h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107162062A (en) * | 2017-06-19 | 2017-09-15 | 华南理工大学 | A kind of rod-like nano iron oxide and preparation method thereof |
| CN107935055A (en) * | 2018-01-10 | 2018-04-20 | 合肥学院 | The stratiform α Fe that a kind of visible ray enhancing absorbs2O3The preparation method of nanometer cake |
| CN108285175A (en) * | 2018-02-13 | 2018-07-17 | 黑龙江大学 | The preparation method and applications of pseudo-cubic di-iron trioxide nanocages with multilevel hierarchy |
| CN108483897A (en) * | 2018-04-09 | 2018-09-04 | 徐冬 | A kind of preparation method of ceramic pigment nano-powder |
| CN111766274A (en) * | 2020-07-07 | 2020-10-13 | 华准科技(绍兴)有限公司 | Pd-modified α -Fe2O3Nano material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162062A (en) * | 2017-06-19 | 2017-09-15 | 华南理工大学 | A kind of rod-like nano iron oxide and preparation method thereof |
| CN107935055A (en) * | 2018-01-10 | 2018-04-20 | 合肥学院 | The stratiform α Fe that a kind of visible ray enhancing absorbs2O3The preparation method of nanometer cake |
| CN108285175A (en) * | 2018-02-13 | 2018-07-17 | 黑龙江大学 | The preparation method and applications of pseudo-cubic di-iron trioxide nanocages with multilevel hierarchy |
| CN108483897A (en) * | 2018-04-09 | 2018-09-04 | 徐冬 | A kind of preparation method of ceramic pigment nano-powder |
| CN108483897B (en) * | 2018-04-09 | 2020-08-25 | 佛山意达加精密陶瓷科技有限公司 | Preparation method of ceramic pigment nano powder |
| CN111766274A (en) * | 2020-07-07 | 2020-10-13 | 华准科技(绍兴)有限公司 | Pd-modified α -Fe2O3Nano material and preparation method and application thereof |
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