CN112320852A - Preparation method of spindle-shaped nano iron oxyhydroxide - Google Patents
Preparation method of spindle-shaped nano iron oxyhydroxide Download PDFInfo
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- CN112320852A CN112320852A CN202011317773.4A CN202011317773A CN112320852A CN 112320852 A CN112320852 A CN 112320852A CN 202011317773 A CN202011317773 A CN 202011317773A CN 112320852 A CN112320852 A CN 112320852A
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- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
The invention discloses a preparation method of spindle-shaped nano iron oxyhydroxide, which comprises the following steps: taking a proper amount of FeCl3·6H2Aqueous O solution, diluted HCl solution and NH4HCO3Adjusting the pH value of the solution to about 2, and placing the solution in a round-bottom flask; stirring at 30 ℃ in a constant-temperature water bath kettle, raising the temperature by 5 ℃ every 0.5h, raising the temperature to 80 ℃, and reacting for 2h at constant temperature; naturally cooling to room temperature, standing overnight, washing with water, centrifuging, and dialyzing for 48h to obtain the nano beta-FeOOH. The prepared nano iron oxyhydroxide is spindle-shaped, uniform in size, good in dispersity and small in particle size, has a high specific surface area and good surface activity, can be applied to treating pollutants containing cations, anions, organic acids or gases, and has the potential of being applied to more fields such as biology, medical treatment and the like due to good physicochemical property and biocompatibility. In addition, the method has the advantages of simple process, low energy consumption, small equipment quantity and convenient popularization.
Description
Technical Field
The invention relates to the technical field of nano composite materials, in particular to a preparation method of spindle-shaped nano iron oxyhydroxide.
Background
Iron oxides include two major types of iron hydroxides and iron oxides, which are various in types, have different phase structures and physical and chemical properties, and are widely applied to various fields such as batteries, coatings, catalysts, gas sensors, magnet raw materials and the like at present. Among them, iron oxyhydroxide (FeOOH) has a high specific surface area and good surface activity, and has been applied to the treatment of pollutants containing cations, anions, organic acids or gases in previous studies, and its good physicochemical properties and biocompatibility also make it have potential for application in more fields such as biology, medical treatment, and the like.
The iron oxyhydroxide has various crystal forms, wherein the crystal form of beta-FeOOH is relatively stable, but the beta-FeOOH synthesized by the prior art has larger general size and limits the application range to a certain extent, so that the technology is considered to be developed to synthesize the nano-scale beta-FeOOH with smaller size, so that the nano-scale beta-FeOOH can be applied to more fields.
The existing technology for synthesizing the nano iron oxide hydroxide has the following defects: 1. the synthesized beta-FeOOH has larger size, and the application range of the beta-FeOOH is limited to a certain extent; 2. many technologies adopt a high-temperature calcination method, and the requirements on reaction equipment and the like are high when the reaction conditions are high; 3. many techniques add additional surfactants such as CTAB, which correspondingly increases the cost of the experiment.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of spindle-shaped nano iron oxyhydroxide, and aims to provide a method for preparing iron oxyhydroxide nanoparticles with smaller particle size, which has the advantages of simple preparation process, low energy consumption, less equipment quantity and short process flow.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of spindle-shaped nano iron oxyhydroxide comprises the following steps:
I. taking 20 mL0.05mol/L-0.2 mol/L FeCl3·6H2Aqueous O solution, diluted HCl solution and NH4HCO3Adjusting the pH value of the solution to 1.5-2.5 to obtain a solution A, and placing the solution A in a round-bottom flask;
II, placing the round-bottom flask filled with the solution A in a constant-temperature water bath kettle with the water surface not higher than the bottle mouth, heating the water bath kettle, raising the temperature of the solution A to 30 ℃, starting stirring, continuously heating the water bath kettle, controlling the temperature of the solution A to rise by 5 ℃ every 0.5 hour, and after the temperature of the solution A rises to 80 ℃, carrying out constant-temperature reaction for 2 hours to obtain a solution B;
and III, naturally cooling the solution B to room temperature, standing overnight, washing with water, centrifuging, and dialyzing for 48 hours to obtain the nano beta-FeOOH.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the technology has the advantages that: 1. the nano-scale beta-FeOOH with smaller size is synthesized, and the application range of the nano-scale beta-FeOOH can be widened; 2. the synthesis process is mild, and the conditions such as high temperature and high pressure are not needed; 3. the experimental cost is low, only ferric chloride hexahydrate is used as a reaction raw material, ammonium bicarbonate is used as a precipitator, no surfactant and the like are needed, and the synthetic steps are simple.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a TEM photograph of β -FeOOH. As can be seen from the images, the beta-FeOOH synthesized by the technology has a spindle shape and an average diameter of about 80 nm;
FIG. 2 is a graph of the hydrated particle size of β -FeOOH. The image was measured at room temperature 21.9 ℃ and humidity 53%. As shown in the figure, the hydrated particle size of the beta-FeOOH is 78 +/-5 nm through detection of DLS.
FIG. 3 is an infrared spectrum of β -FeOOH. The image was taken at room temperature 23 ℃ and humidity 33% and the sample was in powder form. As can be seen from the images, absorption bands at 622cm-1 and 790cm-1 correspond to the Fe-O-Fe and Fe-O vibration peaks in beta-FeOOH, and absorption bands near 1618cm-1 and 3415cm-1 are related to H-O-H deformation vibration and O-H stretching vibration; therefore, the successful synthesis of beta-FeOOH can be judged.
FIG. 4 is an XPS plot of β -FeOOH. The image is taken at room temperature 22 ℃ and humidity 39% and the sample is in powder form. The images show the basic constituent elements Fe, O, H and Cl in β -FeOOH.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of spindle-shaped nano iron oxyhydroxide comprises the following steps:
I. taking 20mL0.05mol/L FeCl3·6H2Aqueous O solution, diluted HCl solution and NH4HCO3Adjusting the pH value of the solution to 1.5 to obtain a solution A, and placing the solution A in a round-bottom flask;
II, placing the round-bottom flask filled with the solution A in a constant-temperature water bath kettle with the water surface not higher than the bottle mouth, heating the water bath kettle, raising the temperature of the solution A to 30 ℃, starting stirring, continuously heating the water bath kettle, controlling the temperature of the solution A to rise by 5 ℃ every 0.5 hour, and after the temperature of the solution A rises to 80 ℃, carrying out constant-temperature reaction for 2 hours to obtain a solution B;
and III, naturally cooling the solution B to room temperature, standing overnight, washing with water, centrifuging, and dialyzing for 48 hours to obtain the nano beta-FeOOH.
Example 2:
a preparation method of spindle-shaped nano iron oxyhydroxide comprises the following steps:
I. taking 20mL0.2mol/L FeCl3·6H2Aqueous O solution, diluted HCl solution and NH4HCO3Adjusting the pH value of the solution to 2.5 to obtain a solution A, and placing the solution A in a round-bottom flask;
II, placing the round-bottom flask filled with the solution A in a constant-temperature water bath kettle with the water surface not higher than the bottle mouth, heating the water bath kettle, raising the temperature of the solution A to 30 ℃, starting stirring, continuously heating the water bath kettle, controlling the temperature of the solution A to rise by 5 ℃ every 0.5 hour, and after the temperature of the solution A rises to 80 ℃, carrying out constant-temperature reaction for 2 hours to obtain a solution B;
and III, naturally cooling the solution B to room temperature, standing overnight, washing with water, centrifuging, and dialyzing for 48 hours to obtain the nano beta-FeOOH.
Example 3:
the prepared beta-FeOOH particles are observed under a transmission electron microscope, and the obtained TEM picture is shown in figure 1, and the image shows that the beta-FeOOH synthesized by the technology is spindle-shaped, has the average diameter of about 80nm, uniform size, good dispersibility, small particle size, higher specific surface area and good surface activity.
Example 4:
the prepared beta-FeOOH nano particles are subjected to dynamic light scattering detection (the indoor temperature is 21.9 ℃, and the humidity is 53%), the obtained hydrated particle size is shown in figure 2, and the hydrated particle size of the beta-FeOOH is 78 +/-5 nm through DLS detection.
Example 5:
the prepared beta-FeOOH nano particles are subjected to infrared spectrum detection, and an obtained infrared spectrogram is shown in figure 3 (the image is detected at the indoor temperature of 23 ℃ and the humidity of 33 percent, and a sample is powdery). As can be seen from the images, absorption bands at 622cm-1 and 790cm-1 correspond to the Fe-O-Fe and Fe-O vibration peaks in beta-FeOOH, and absorption bands near 1618cm-1 and 3415cm-1 are related to H-O-H deformation vibration and O-H stretching vibration; therefore, the successful synthesis of beta-FeOOH can be judged.
Example 6:
the prepared beta-FeOOH nanoparticles were subjected to X-ray photoelectron spectroscopy, and the XPS graph obtained is shown in FIG. 4 (the image was measured at an indoor temperature of 22 ℃ and a humidity of 39%, and the sample was in the form of powder). The images show the basic constituent elements Fe, O, H and Cl in β -FeOOH. The composition of the synthesized β -FeOOH particles can be further determined.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (1)
1. A preparation method of spindle-shaped nanometer iron oxyhydroxide is characterized by comprising the following steps:
I. taking 20 mL0.05mol/L-0.2 mol/L FeCl3·6H2Aqueous O solution, diluted HCl solution and NH4HCO3Adjusting the pH value of the solution to 1.5-2.5 to obtain a solution A, and placing the solution A in a round-bottom flask;
II, placing the round-bottom flask filled with the solution A in a constant-temperature water bath kettle with the water surface not higher than the bottle mouth, heating the water bath kettle, raising the temperature of the solution A to 30 ℃, starting stirring, continuously heating the water bath kettle, controlling the temperature of the solution A to rise by 5 ℃ every 0.5 hour, and after the temperature of the solution A rises to 80 ℃, carrying out constant-temperature reaction for 2 hours to obtain a solution B;
and III, naturally cooling the solution B to room temperature, standing overnight, washing with water, centrifuging, and dialyzing for 48 hours to obtain the nano beta-FeOOH.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023201974A1 (en) * | 2022-04-22 | 2023-10-26 | 浙江华源颜料股份有限公司 | Iron oxyhydroxide and use thereof in synergistic degradation of antibiotic with persulfate |
Citations (5)
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| CN105129862A (en) * | 2015-08-09 | 2015-12-09 | 中国科学院合肥物质科学研究院 | Preparation method and applications of rice-grain-like nanometer magnetic iron oxide |
| CN108439477A (en) * | 2018-06-07 | 2018-08-24 | 安徽工业大学 | A kind of preparation method of order mesoporous FeOOH nanometer rods |
| CN108910960A (en) * | 2018-08-24 | 2018-11-30 | 合肥学院 | A kind of preparation method of β-FeOOH Nano capsule |
| CN109264789A (en) * | 2018-09-30 | 2019-01-25 | 江苏大学 | FeOOH nano spindle and preparation method thereof |
| CN111620381A (en) * | 2020-06-04 | 2020-09-04 | 陕西科技大学 | beta-FeOOH nano rod and preparation method thereof |
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2020
- 2020-11-23 CN CN202011317773.4A patent/CN112320852A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105129862A (en) * | 2015-08-09 | 2015-12-09 | 中国科学院合肥物质科学研究院 | Preparation method and applications of rice-grain-like nanometer magnetic iron oxide |
| CN108439477A (en) * | 2018-06-07 | 2018-08-24 | 安徽工业大学 | A kind of preparation method of order mesoporous FeOOH nanometer rods |
| CN108910960A (en) * | 2018-08-24 | 2018-11-30 | 合肥学院 | A kind of preparation method of β-FeOOH Nano capsule |
| CN109264789A (en) * | 2018-09-30 | 2019-01-25 | 江苏大学 | FeOOH nano spindle and preparation method thereof |
| CN111620381A (en) * | 2020-06-04 | 2020-09-04 | 陕西科技大学 | beta-FeOOH nano rod and preparation method thereof |
Non-Patent Citations (3)
| Title |
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| 张修华等: "均匀纺锤形β-FeOOH超微粒的制备与表征", 《湖北大学学报(自然科学版)》 * |
| 张霞等: "纺锤形β-FeOOH的形成过程研究", 《化学物理学报》 * |
| 程丹丹等: "纳米β-FeOOH对水中Cr(Ⅵ)吸附性能的研究", 《山东大学学报(理学版)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023201974A1 (en) * | 2022-04-22 | 2023-10-26 | 浙江华源颜料股份有限公司 | Iron oxyhydroxide and use thereof in synergistic degradation of antibiotic with persulfate |
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Application publication date: 20210205 |