CN114873648B - Preparation method of two-dimensional iron oxyhydroxide nano-sheet - Google Patents
Preparation method of two-dimensional iron oxyhydroxide nano-sheet Download PDFInfo
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Abstract
The invention provides a preparation method of a two-dimensional ferric hydroxide nano-sheet, which comprises the following steps: (1) Dissolving a strong reducing agent and alkali in water to obtain a reaction solution; (2) Dissolving iron naphthenate in an organic solvent to obtain a metal precursor reaction solution; (3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), stirring at normal temperature, and then performing airtight reaction; and then centrifugally cleaning and drying the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet. The invention uses the iron naphthenate as a precursor to directly react with the strong reducing agent/alkali solution, and prepares the two-dimensional iron oxyhydroxide nano-sheet by a two-phase method, the preparation process does not involve high temperature and high pressure, the surfactant is not needed, the two-dimensional iron oxyhydroxide is synthesized in one step, the process is simple, the safety is good, and the large-scale production is easy.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a two-dimensional iron oxyhydroxide nano sheet.
Background
Iron oxyhydroxide (FeOOH) widely exists in natural environments, has visible light photoresponse and abundant surface hydroxyl groups, and is widely applied to the fields of photocatalysis, environmental management, desulfurization, energy storage and the like. Because of the extremely thin thickness of the two-dimensional material, the two-dimensional iron oxyhydroxide may have more excellent physicochemical properties than other morphologies of iron oxyhydroxide. For example, as a photochemical conversion system, two-dimensional iron oxyhydroxide facilitates carrier transport to the surface of a material, thereby improving photochemical properties. At present, a wet chemical method is mainly adopted for preparing the two-dimensional ferric oxide hydroxide, ferric salt is generally dissolved in a solvent, a precipitator is added, and then hydrothermal treatment is carried out to obtain the ferric oxide hydroxide nano-sheet.
Patent application number CN 201610383389.1 discloses a method for preparing iron oxyhydroxide nano-sheet, in which 100-120 ℃ high-temperature hydrothermal is required. This preparation method involves a high temperature hydrothermal process, and thus the equipment requirements are relatively high. In addition, sodium borohydride with strong reducibility and organic auxiliary agents or hydrogen peroxide with strong oxidability are needed to be added in many synthesis processes. The synthesis methods are relatively complex, the process is complex, and certain potential safety hazards exist. Therefore, for producing the two-dimensional ferric oxide hydroxide, the preparation method with simpler process is beneficial to the large-scale production, and is quite significant.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects and the shortcomings in the background art and providing a preparation method of a two-dimensional ferric hydroxide nano-sheet.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving a strong reducing agent and alkali in water to obtain a reaction solution;
(2) Dissolving iron naphthenate in an organic solvent to obtain a metal precursor reaction solution;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), stirring at normal temperature, and then performing airtight reaction (without stirring); and then centrifugally cleaning and drying the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
According to the preparation method of the two-dimensional ferric oxide hydroxide nano-sheet, hydrazine hydrate is matched with alkali, organic iron ions in an organic phase react with liquid-phase hydroxyl ions at an oil-water interface, and the two-dimensional ferric oxide hydroxide nano-sheet can be obtained. In the process, the reaction is controlled by an interface, the reaction rate is relatively slow, nucleation growth is slow, the material grows faster in the dominant direction, the dominant crystal faces grow preferentially, and other directions are restrained, so that a two-dimensional structure is formed, and a sheet-shaped structure is formed.
In the above preparation method, preferably, in step (1), the strong reducing agent is hydrazine hydrate, and the base is alkali metal hydroxide. In the invention, the hydrazine hydrate may have complexation in addition to strong reduction, which is beneficial to the reaction at the interface.
Preferably, the alkali metal hydroxide is at least one of sodium hydroxide and potassium hydroxide.
Preferably, in the step (2), the organic solvent is at least one of xylene and cyclohexane. The solvent is relatively safe and low in toxicity, and the iron naphthenate can be well dissolved in the solvent. Further preferably, the organic solvent is xylene.
Preferably, in the step (1), the mass ratio of the alkali metal hydroxide to the hydrazine hydrate is 1 (0.01-2), and the mass ratio of the alkali to the water is 1 (1-100); the reaction of the invention requires obvious alkaline conditions, but too much hydrazine hydrate is too alkaline, which easily leads to dissolution of the product.
In the step (2), the mass ratio of the iron naphthenate to the organic solvent is 1 (1-100); in the step (3), the volume ratio of the reaction solution to the metal precursor reaction solution is 1 (0.01-10).
Preferably, in the step (1), the mass ratio of the alkali metal hydroxide to the hydrazine hydrate is 1 (0.01-1); in the step (2), the mass ratio of the iron naphthenate to the organic solvent is 1 (2-10); in the step (3), the volume ratio of the reaction solution to the metal precursor reaction solution is 1 (0.08-0.15).
Preferably, in the step (3), the stirring time at normal temperature is 1-300 min, and the stirring at normal temperature is performed under normal pressure; the temperature of the airtight reaction is 40-95 ℃, and the time of the airtight reaction is 0.1-24 h. The temperature of the closed reaction is too low, and the reaction is difficult to carry out; the temperature of the airtight reaction is too high, so that agglomerates are easy to form, and the flaky two-dimensional iron oxyhydroxide nano-sheets with good dispersibility are not formed.
Further preferably, the stirring time at normal temperature is 10-30 min; the temperature of the airtight reaction is 50-80 ℃, and the time of the airtight reaction is 0.5-5 h.
Preferably, no surfactant is added in the preparation process of the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention uses the iron naphthenate as a precursor to directly react with the strong reducing agent/alkali solution, and prepares the two-dimensional iron oxyhydroxide nano-sheet by a two-phase method, the preparation process does not involve high temperature and high pressure, the surfactant is not needed, the two-dimensional iron oxyhydroxide is synthesized in one step, the process is simple, the safety is good, and the large-scale production is easy.
2. The invention can directly react with industrial grade ferric naphthenate and alkali solution to prepare the high-purity ferric hydroxide nano-sheet, and has the advantages of easily available raw materials and low cost.
3. The two-dimensional ferric oxide hydroxide nano-sheet prepared by the invention has a polycrystalline structure, the size range is 200-800 nanometers, and the thickness is 2-10 nanometers.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a transmission electron microscope image of a two-dimensional iron oxyhydroxide nanoplatelet prepared in example 1.
FIG. 2 is an electron diffraction pattern of a two-dimensional iron oxyhydroxide nanoplatelet prepared in example 1.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and sodium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the sodium hydroxide to the hydrazine hydrate to the water is 1:1:10;
(2) Dissolving iron naphthenate in dimethylbenzene to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the dimethylbenzene is 1:5;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; stirring for 30min at normal temperature and normal pressure, and hermetically reacting at 60 ℃ for 0.5h; and then carrying out centrifugal cleaning and vacuum drying on the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
The two-dimensional ferric hydroxide prepared in example 1 is shown in a transmission electron microscope chart in FIG. 1, and the electron diffraction chart in FIG. 2. The prepared two-dimensional ferric oxide hydroxide nano-sheet is of a polycrystalline structure, the size range is 200-800 nanometers, and the thickness is 2-10 nanometers.
Example 2:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and sodium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the sodium hydroxide to the hydrazine hydrate to the water is 1:0.01:1;
(2) Dissolving iron naphthenate in dimethylbenzene to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the dimethylbenzene is 1:5;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; performing airtight reaction for 0.5h at the normal temperature and the normal pressure for 30min and at the temperature of 80 ℃; and then carrying out centrifugal cleaning and vacuum drying on the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
Example 3:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and potassium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the potassium hydroxide to the hydrazine hydrate to the water is 1:0.1:10;
(2) Dissolving iron naphthenate in cyclohexane to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the cyclohexane is 1:10;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; performing airtight reaction for 0.5h at the normal temperature and the normal pressure for 30min and at the temperature of 50 ℃; and then carrying out centrifugal cleaning and vacuum drying on the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
Example 4:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and potassium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the potassium hydroxide to the hydrazine hydrate to the water is 1:0.1:10;
(2) Dissolving iron naphthenate in dimethylbenzene to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the dimethylbenzene is 1:2.5;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; performing airtight reaction for 2 hours at the normal temperature and the normal pressure for 30min and at the temperature of 60 ℃; and then carrying out centrifugal cleaning and vacuum drying on the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
Example 5:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and sodium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the sodium hydroxide to the hydrazine hydrate to the water is 1:0.01:1;
(2) Dissolving iron naphthenate in dimethylbenzene to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the dimethylbenzene is 1:5;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; performing airtight reaction for 4 hours at 50 ℃ under normal temperature and normal pressure for 10 min; and then carrying out centrifugal cleaning and vacuum drying on the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
Comparative example 1:
the preparation method of the two-dimensional iron oxyhydroxide nano sheet comprises the following steps:
(1) Dissolving hydrazine hydrate and sodium hydroxide in water to obtain a reaction solution; wherein the mass ratio of the sodium hydroxide to the hydrazine hydrate to the water is 1:5:50;
(2) Dissolving iron naphthenate in dimethylbenzene to obtain a metal precursor reaction solution; the mass ratio of the iron naphthenate to the xylene is 1:5;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), wherein the volume ratio of the reaction solution to the metal precursor reaction solution is 1:0.1; stirring for 30min, and hermetically reacting at 70 ℃ for 0.5h; no obvious solid product was obtained after the reaction.
Claims (9)
1. The preparation method of the two-dimensional iron oxyhydroxide nano sheet is characterized by comprising the following steps of:
(1) Dissolving a strong reducing agent and alkali in water to obtain a reaction solution; the strong reducing agent is hydrazine hydrate;
(2) Dissolving iron naphthenate in an organic solvent to obtain a metal precursor reaction solution;
(3) Adding the metal precursor reaction solution in the step (2) into the reaction solution in the step (1), stirring at normal temperature, and then performing a closed reaction, wherein the stirring at normal temperature is performed at normal pressure, and the temperature of the closed reaction is 40-95 ℃; and then centrifugally cleaning and drying the obtained material to obtain the two-dimensional ferric hydroxide nano-sheet.
2. The process according to claim 1, wherein in step (1), the base is an alkali metal hydroxide.
3. The method according to claim 2, wherein the alkali metal hydroxide is at least one of sodium hydroxide and potassium hydroxide.
4. The method according to claim 1, wherein in the step (2), the organic solvent is at least one of xylene and cyclohexane.
5. The preparation method according to any one of claims 1 to 4, wherein in the step (1), the mass ratio of the alkali metal hydroxide to the hydrazine hydrate is 1 (0.01 to 2); in the step (2), the mass ratio of the iron naphthenate to the organic solvent is 1 (1-100); in the step (3), the volume ratio of the reaction solution to the metal precursor reaction solution is 1 (0.01-10).
6. The preparation method according to claim 5, wherein in the step (1), the mass ratio of the alkali metal hydroxide to the hydrazine hydrate is 1 (0.01-1); in the step (2), the mass ratio of the iron naphthenate to the organic solvent is 1 (2-10); in the step (3), the volume ratio of the reaction solution to the metal precursor reaction solution is 1 (0.08-0.15).
7. The method according to any one of claims 1 to 4, wherein in the step (3), the stirring time at normal temperature is 1 to 300min, and the airtight reaction time is 0.1 to 24h.
8. The preparation method according to claim 7, wherein the stirring time at normal temperature is 10-30 min; the temperature of the airtight reaction is 50-80 ℃, and the time of the airtight reaction is 0.5-5 h.
9. The preparation method according to any one of claims 1 to 4, wherein no surfactant is added in the preparation process of the preparation method.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101468816A (en) * | 2007-12-28 | 2009-07-01 | Tdk株式会社 | Process for production of iron oxyhydroxide particles |
| CN108927101A (en) * | 2018-07-06 | 2018-12-04 | 济南大学 | A kind of acicular nanometer FeOOH adsorbent and preparation method thereof |
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| US20110201702A1 (en) * | 2009-08-14 | 2011-08-18 | Sumit Bali | Ultra small synthetic doped ferrihydrite with nanoflake morphology for synthesis of alternative fuels |
| CN104445427B (en) * | 2014-12-04 | 2016-03-02 | 浙江大学 | A kind of alpha-feooh nanometer sheet and preparation method thereof |
| CN108314087B (en) * | 2018-03-12 | 2019-11-08 | 清华大学 | A kind of preparation method and applications of the super particle of unformed FeOOH |
| CN109046226B (en) * | 2018-08-24 | 2021-03-26 | 南昌大学 | Preparation method and application of iron oxyhydroxide nanosheet for treating anionic dye sewage |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468816A (en) * | 2007-12-28 | 2009-07-01 | Tdk株式会社 | Process for production of iron oxyhydroxide particles |
| CN108927101A (en) * | 2018-07-06 | 2018-12-04 | 济南大学 | A kind of acicular nanometer FeOOH adsorbent and preparation method thereof |
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