CN104556245B - A kind of hamburger nano oxidized iron material of shape and its production and use - Google Patents
A kind of hamburger nano oxidized iron material of shape and its production and use Download PDFInfo
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- CN104556245B CN104556245B CN201410851224.3A CN201410851224A CN104556245B CN 104556245 B CN104556245 B CN 104556245B CN 201410851224 A CN201410851224 A CN 201410851224A CN 104556245 B CN104556245 B CN 104556245B
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Abstract
The invention provides a kind of hamburger nano oxidized iron material of shape, described material is powder, its microscopic pattern is hamburger shape of stacking, and the described nano oxidized iron material of hamburger shape uses following methods to prepare: add source of iron in the aqueous solution containing dispersant and end-capping reagent；When stirring, adding the alkaline matter containing amido in above-mentioned solution, the pH making solution is 10；Then above-mentioned mixed solution is transferred to carry out in autoclave hydro-thermal reaction, is cooled to room temperature after reaction, generates brick-red precipitation；Finally the brick-red precipitate obtained is washed, dries, the nano oxidized iron material of hamburger shape can be obtained.Nano-sized iron oxide novel in shape prepared by the present invention, its structure is hamburger shape, and prepared nano-sized iron oxide granule is homogeneous, productivity is high, is suitable for industrialization large-scale 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 iron oxides, except having the fundamental characteristics of nano material, the light resistance also having had, weatherability, magnetic, catalysis active, 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 include FeO, Fe3O4And the α-Fe of iron sesquioxide series2O3、β-Fe2O3、γ-Fe2O3.In addition, also α, β, γ-FeOOH hydrated ferric oxide.α-Fe2O3、γ-Fe2O3、Fe3O4It is that more several ferrum oxides are applied in research at present, it is believed that along with people are to its structure and the further investigation of performance, they can show broader development prospect.
It is known that the pattern of nano material and size determine its performance and application, therefore, the research emphasis of nano material is always prepared in the regulation and control of pattern and size.At present, researcher synthesizes many different nano-sized iron oxides by methods such as traditional sedimentation method, template, thermal decompositions, such as the most spherical, rod, dish type, linear, tubular, Semen arachidis hypogaeae shape, pinaster shape, cube, spindle etc., also have the most complicated Hemicentrotus seu Strongylocentrotus shape, polyhedron shape, biconial etc..But, the nano-sized iron oxide only having these appearance structure is the industrial requirement that can not meet quickly growth, and meanwhile, these methods generally exist the defects such as operation complexity, cost height, cycle length, poor controllability, and synthesized product is the most homogeneous, purity is low, it is impossible to realize industrial volume production.
Summary of the invention
The present 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 granule is homogeneous, productivity is high, is suitable for industrialization large-scale production.
Realizing the technical scheme that above-mentioned purpose of the present invention used is:
A kind of hamburger nano oxidized iron material of shape, described material is powder, and its microscopic pattern is hamburger shape of stacking, and the described nano oxidized iron material of hamburger shape uses following methods to prepare: add source of iron in the aqueous solution containing dispersant and end-capping reagent；When stirring, adding the alkaline matter containing amido in above-mentioned solution, the pH making solution is 10；Then above-mentioned mixed solution is transferred to carry out in autoclave hydro-thermal reaction, is cooled to room temperature after reaction, generates brick-red precipitation；Finally the brick-red precipitate obtained is washed, dries, the nano oxidized iron material of hamburger shape can be obtained.
Present invention also offers the preparation method of the nano oxidized iron material of hamburger shape that preparation is 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 the material of the iron ion added is 0.015～0.05mmol/mL；
(2) when stirring, adding the alkaline matter containing amido in above-mentioned solution, the initial pH making obtained mixed solution is 9～11；
(3) transferring in autoclave by above-mentioned mixed solution, under conditions of 160～220 DEG C after hydro-thermal reaction 16～48h, generate brick-red precipitation, reaction naturally cools to room temperature after terminating；
(4) the brick-red precipitate obtained in upper step is washed, dries, 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 carboxymethyl cellulose, and described source of iron is potassium ferrocyanide or the potassium ferricyanide.
Described in step (2), the alkaline matter containing amido is carbamide, ammonia, hydrazine hydrate or Methanamide.
Using centrifuge washing or filtering and washing, described drying temperature 60 C in step (4), drying time is 24h.
Compared with prior art, the invention have the advantages that 1) the method obtained hamburger shape nano-sized iron oxide novel in shape, granule is uniform, purity is high, and has good dispersibility.2) this nano-sized iron oxide has good absorption property, can remove contaminated ion in water body as adsorbent.3) method that the present invention uses is easy and simple to handle, low cost, controllability strong, is suitable for industrialization large-scale production.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the nano oxidized iron material of hamburger shape prepared by the present embodiment；
Fig. 2 is the SEM figure of the nano oxidized iron material of hamburger shape prepared by the present embodiment.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention done detailed specific description, but protection scope of the present invention is not limited to following example.
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 the material of the iron ion added is 0.03mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethyl cellulose.
When stirring, adding ammonia in above-mentioned solution, the initial pH making obtained mixed solution is 9；
Above-mentioned mixed solution is transferred in autoclave, under conditions of 220 DEG C after hydro-thermal reaction 16h, generates brick
Red precipitate, reaction naturally cools to room temperature after terminating；
Brick-red precipitate obtained in upper step is centrifuged washing, dries 24h, the nano-sized iron oxide of hamburger shape can be obtained for 60 DEG C.
The XRD figure spectrum of the nano-sized iron oxide of hamburger shape prepared in the present embodiment is as it is shown in figure 1, its SEM schemes as in figure 2 it is shown, can be found out clearly by Fig. 2, and its microstructure of nano oxidized iron material prepared by the present invention is hamburger shape of stacking.
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 the material of the iron ion added is 0.05mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethyl cellulose.
When stirring, adding Methanamide in above-mentioned solution, the initial pH making obtained mixed solution is 10；
Transferring in autoclave by above-mentioned mixed solution, under conditions of 200 DEG C after hydro-thermal reaction 36h, generate brick-red precipitation, reaction naturally cools to room temperature after terminating；
Brick-red precipitate obtained in upper step is centrifuged washing, 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 the material of the iron ion added is 0.015mmol/mL, described dispersant is PVP K-30, and described end-capping reagent is sodium carboxymethyl cellulose.
When stirring, adding hydrazine hydrate in above-mentioned solution, the initial pH making obtained mixed solution is 11；
Transferring in autoclave by above-mentioned mixed solution, under conditions of 180 DEG C after hydro-thermal reaction 48h, generate brick-red precipitation, reaction naturally cools to room temperature after terminating；
Brick-red precipitate obtained in upper step is carried out filtering and washing, dries 24h, the nano-sized iron oxide of hamburger shape can be obtained for 60 DEG C.
Claims (4)
1. the nano oxidized iron material of hamburger shape, it is characterised in that: described material is powder, its microscopic pattern in
Hamburger shape of stacking, the described nano oxidized iron material of hamburger shape uses following methods to prepare: to containing dispersant and end-blocking
The aqueous solution of agent adds source of iron；When stirring, in above-mentioned solution, add the alkaline matter containing amido, make
The pH of solution is 10；Then above-mentioned mixed solution is transferred to carry out in autoclave hydro-thermal reaction, cools down after reaction
To room temperature, generate brick-red precipitation；Finally the brick-red precipitate obtained is washed, dries, the Chinese can be obtained
The nano oxidized iron material of castellatus；
Concrete preparation method comprises the following steps: (1) at normal temperatures and pressures, water-soluble to containing dispersant and end-capping reagent
Adding source of iron in liquid, wherein the concentration of dispersant is 5～20mg/mL, and the concentration of end-capping reagent is 0.8～2.5mg/mL, institute
The amount of the material of the iron ion added is 0.015～0.05mmol/mL；
(2) when stirring, in above-mentioned solution, add the alkaline matter containing amido, make obtained mixing
The initial pH of solution is 10；
(3) above-mentioned mixed solution is transferred in autoclave, under conditions of 160～220 DEG C hydro-thermal reaction 16～
After 48h, generating brick-red precipitation, reaction naturally cools to room temperature after terminating；
(4) the brick-red precipitate obtained in upper step is washed, dries, the nanometer of hamburger shape can be obtained
Ferrum oxide.
Hamburger the most according to claim 1 nano oxidized iron material of shape, it is characterised in that: described in step (1)
Dispersant be PVP K-30, described end-capping reagent is sodium carboxymethyl cellulose, and described source of iron is ferrous
Potassium cyanide or the potassium ferricyanide.
Hamburger the most according to claim 1 nano oxidized iron material of shape, it is characterised in that: described in step (2)
Alkaline matter containing amido is carbamide, ammonia, hydrazine hydrate or Methanamide.
Hamburger the most according to claim 1 nano oxidized iron material of shape, it is characterised in that: step (4) uses
Centrifuge washing or filtering and washing, described drying temperature 60 C, drying time is 24h.
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| CN107935055B (en) * | 2018-01-10 | 2020-01-31 | 合肥学院 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
| CN108285175B (en) * | 2018-02-13 | 2020-06-23 | 黑龙江大学 | Application of quasi-cubic iron sesquioxide nano cage with multi-stage structure |
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