CN108101119B - Preparation method of iron oxide nanosheet material - Google Patents

Preparation method of iron oxide nanosheet material Download PDF

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CN108101119B
CN108101119B CN201711472977.3A CN201711472977A CN108101119B CN 108101119 B CN108101119 B CN 108101119B CN 201711472977 A CN201711472977 A CN 201711472977A CN 108101119 B CN108101119 B CN 108101119B
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iron oxide
ferric chloride
oxide nanosheet
nanosheet material
temperature
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CN108101119A (en
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张建
刘国栋
崔超
张磊
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Guilin Baolongda New Material Co ltd
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Jining University
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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
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide (Fe2O3)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM

Abstract

The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of an iron oxide nanosheet material. The method prepares the iron oxide nanosheet material by using a single raw material and simple one-step calcination, the thickness of the nanosheet is controllable, the preparation process is simple, the economy is high, the prepared nanosheet material is excellent in catalytic performance and stability, and the method is suitable for industrial production and has a wide market application prospect.

Description

Preparation method of iron oxide nanosheet material
Technical Field
The invention belongs to the technical field of inorganic material preparation, and particularly relates to a preparation method of an iron oxide nanosheet material.
Background
In recent years, the situation of environmental pollution and energy crisis has become more severe. Changes the energy consumption structure mainly based on the traditional fossil fuel, and is beneficial to solving the energy crisis and the environmental pollution. The nano iron oxide has excellent weather resistance, huge specific surface area and abundant surface active groups, is an excellent catalyst and is widely applied to the aspect of catalyzing and degrading organic pollutants. Meanwhile, the iron oxide material can also be used as a lithium ion battery cathode material and has higher theoretical capacity. The nano-sheet structure material has a special two-dimensional structure, so that the specific surface area and the number of active sites can be greatly increased. So far, only few methods for preparing iron oxide nanosheets have been described. The invention patent (201610136119.0) discloses a method for preparing iron oxide nanosheets by irradiating iron-nickel alloy with laser light. The invention patent (201610408147.3) discloses a method for preparing iron oxide nanosheets by hydrothermal reaction of a high-pressure reaction kettle and continuous reaction of sodium lactate. The invention patent (201710120611.3) discloses a method for preparing iron oxide nanosheets by hydrothermal reaction of P123 and an ethylene glycol organic solvent high-pressure reaction kettle. The invention patent (201710631273.X) reports a method for preparing iron oxide nanosheets by mixing surface-modified copper oxide nanowire dispersion liquid and a soluble iron source and then carrying out hydrothermal reaction. The invention patent (201710463430.0) reports a method for preparing iron oxide nanosheets by using ethylene glycol as a solvent, and performing solvothermal calcination. Iron oxide nanosheets have attracted extensive attention and research enthusiasm of researchers at home and abroad due to excellent performance, but the currently reported method needs harsh experimental conditions, has complex process and high cost, and is difficult to realize industrialization.
Disclosure of Invention
The invention aims to provide a preparation method of an iron oxide nanosheet material, wherein the iron oxide nanosheet material is prepared by a single raw material and a one-step simple calcination method, the thickness of the nanosheet is controllable, and the catalytic performance and the structural stability are improved. The method has the advantages of simple process flow, low cost and suitability for large-scale production.
The preparation method of the iron oxide nanosheet material provided by the invention is prepared by taking ferric chloride as a raw material and utilizing a calcining method, and comprises the following steps of:
(1) grinding ferric chloride salt into powder and spreading on a carrier;
(2) calcining the carrier which is paved with ferric chloride powder in an atmosphere, wherein the calcining process comprises two steps: the first step is to heat up to 180 ℃ and 270 ℃ at the heating rate of 5-20 ℃/min and keep the temperature for 30-120 min; the second step is to continue heating up to 300-500 ℃ at the heating rate of 1-10 ℃/min, keeping the temperature for 30-180 min, and cooling to room temperature to obtain a calcined product;
(3) and (3) washing the calcined product obtained in the step (2) with a detergent for 1-3 times, and drying to obtain the iron oxide nanosheet material.
Wherein:
the ferric chloride salt is one or two of hydrated ferric chloride or hydrated ferrous chloride.
Spreading ferric chloride powder on the carrier at a spreading amount of 0.01-0.5g/cm2。
The atmosphere in the step (2) is one of air, nitrogen or argon.
And (4) in the step (3), the detergent is one of water, acetone or ethanol.
In the step (3), the drying temperature is 80-150 ℃, and the drying time is 1-24 hours.
The carrier in the step (1) is one of a crucible, an evaporating dish or tin foil paper.
Compared with the prior art, the invention has the following beneficial effects.
(1) The iron oxide nanosheets are prepared by using a single raw material and one-step calcination, the process is simple, the ferric chloride cracking of iron is regulated and controlled by controlling the heating rate and the heat preservation time in the first-step calcination to generate the iron oxychloride nanosheets with controllable thickness, the iron oxychloride conversion is regulated and controlled by controlling the heating and heat preservation in the second step to generate the iron oxide, the thickness of the nanosheets is further regulated and controlled, the thickness is controllable, organic matters are not introduced, the operation is simple and convenient, the cost is low, and the technical problems of complex preparation process, high cost and the like of the iron oxide nanosheets are solved;
(2) the preparation method and the process are simple and convenient, have no harm to the environment, have low cost, are suitable for large-scale industrial production and have wide application prospect;
(3) the iron oxide nanosheet material prepared by the method is excellent in performance, can be used as a catalyst, can show excellent catalytic performance at a neutral pH value, normal temperature and sunlight, and is excellent in catalytic activity and structural stability.
Drawings
FIG. 1 is an XRD pattern of the iron oxide nanosheet material prepared in example 1;
FIG. 2 is a TEM image of the iron oxide nanosheet material prepared in example 1;
FIG. 3 is a dye degradation diagram of the iron oxide nanosheet material prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples and figures of the specification.
Example 1
Grinding ferric trichloride hydrate into powder in a mortar, and spreading the powder in an alumina crucible, wherein the spreading amount of the ferric trichloride hydrate powder on the alumina crucible is 0.25g/cm2The aluminum oxide crucible is covered and then calcined in the air, and the calcination process comprises two steps: in the first step, the temperature is increased to 220 ℃ at the speed of 15 ℃/min, and the temperature is kept for 60 min; the second step is to continue heating, the temperature is raised to 350 ℃ at the rate of 5 ℃/min, the temperature is kept for 60 min, the temperature is cooled to room temperature to obtain a calcined product, and the calcined product is calcinedAnd washing the product with ethanol for 3 times, and drying at 100 ℃ for 12 hours to obtain the oxidized nanosheet material.
As can be seen from fig. 1, the calcined product is iron oxide, and as can be seen from fig. 2, the iron oxide nanostructure is a nanosheet.
0.05g of the iron oxide nanosheet material obtained in the example is added into 100mL of rhodamine B solution (the concentration is 5mg/L), and after stirring in the dark for 40min, 0.5mL of hydrogen peroxide (the concentration is 30 wt%) is added for a degradation experiment, and as can be seen from FIG. 3, the iron oxide nanosheet material can completely degrade organic pollutants within 40 min.
Example 2
As described in example 1, except that ferrous chloride hydrate was added. The obtained iron oxide nanosheet can completely degrade organic pollutants within 40 min.
Example 3
As described in example 1, except that the amount of hydrated ferric chloride was 0.03g/cm2. The obtained iron oxide nanosheet can completely degrade organic pollutants within 40 min.
Example 4
As described in example 1, except that the amount of hydrated ferric chloride was 0.5g/cm2. The obtained iron oxide nano-sheet degrades organic pollutants by 92% in 40 min.
Example 5
As described in example 1, except that the calcination was carried out in a nitrogen atmosphere. The obtained iron oxide nanosheet can completely degrade organic pollutants within 40 min.
Example 6
As described in example 1, except that the first calcination step was calcination at 20 ℃/min ramp to 270 ℃ for 30 min. The obtained iron oxide nano-sheet degrades organic pollutants by 98% in 40 min.
Example 7
The procedure is as in example 1 except that the first step is calcined at 5 ℃/min up to 180 ℃ for 120 minutes. The obtained iron oxide nano-sheet degrades organic pollutants by 95% in 40 min.
Example 8
The procedure is as described in example 1, except that the second step is continued by calcining at 2 ℃/min up to 500 ℃ for 30 minutes. The obtained iron oxide nano-sheet degrades organic pollutants by 93% in 40 min.
Example 9
The procedure is as described in example 1, except that the second step is continued by calcining at 5 ℃/min up to 300 ℃ for 180 minutes. The obtained iron oxide nanosheet can degrade organic pollutants by 100% in 40 min.
Example 10
As described in example 1, except that the product was washed 3 times with water and dried at 80 ℃ for 24h, the obtained iron oxide nanoplates degraded organic contaminants by 100% in 40 min.
Example 11
As described in example 1, except that the product was washed 1 time with acetone and dried at 150 ℃ for 1h, the obtained iron oxide nanoplates degraded organic contaminants by 100% in 40 min.

Claims (5)

1. A preparation method of an iron oxide nanosheet material is characterized by comprising the following steps: the method is characterized in that ferric chloride is used as a raw material and prepared by a calcination method;
when the ferric chloride salt is ferric chloride hydrate, the preparation method comprises the following steps:
(1) grinding ferric chloride salt into powder and spreading on a carrier;
(2) calcining the carrier which is paved with ferric chloride powder in an atmosphere, wherein the atmosphere is one of air, nitrogen or argon, and the calcining process comprises two steps: the first step is to heat up to 180 ℃ and 270 ℃ at the heating rate of 5-20 ℃/min and keep the temperature for 30-120 min; the second step is to continue heating up to 300-500 ℃ at the heating rate of 1-10 ℃/min, keeping the temperature for 30-180 min, and cooling to room temperature to obtain a calcined product;
(3) washing the calcined product obtained in the step (2) with a detergent for 1-3 times, and drying to obtain an iron oxide nanosheet material;
when the chloride salt of iron is ferrous chloride hydrate, the preparation method comprises the following steps:
(1) grinding ferric chloride salt into powder and spreading on a carrier;
(2) calcining the carrier which is paved with ferric chloride powder in air, wherein the calcining process comprises two steps: the first step is to heat up to 180 ℃ and 270 ℃ at the heating rate of 5-20 ℃/min and keep the temperature for 30-120 min; the second step is to continue heating up to 300-500 ℃ at the heating rate of 1-10 ℃/min, keeping the temperature for 30-180 min, and cooling to room temperature to obtain a calcined product;
(3) washing the calcined product obtained in the step (2) with a detergent for 1-3 times, and drying to obtain an iron oxide nanosheet material;
when the chloride salt of the iron is a compound of hydrated ferrous chloride and hydrated ferric chloride, the preparation method comprises the following steps;
(1) grinding ferric chloride salt into powder and spreading on a carrier;
(2) calcining the carrier which is paved with ferric chloride powder in an atmosphere, wherein the atmosphere is air, and the calcining process comprises two steps: the first step is to heat up to 180 ℃ and 270 ℃ at the heating rate of 5-20 ℃/min and keep the temperature for 30-120 min; the second step is to continue heating up to 300-500 ℃ at the heating rate of 1-10 ℃/min, keeping the temperature for 30-180 min, and cooling to room temperature to obtain a calcined product;
(3) and (3) washing the calcined product obtained in the step (2) with a detergent for 1-3 times, and drying to obtain the iron oxide nanosheet material.
2. The method for preparing an iron oxide nanosheet material according to claim 1, wherein: spreading ferric chloride powder on the carrier at a spreading amount of 0.01-0.5g/cm2。
3. The method for preparing an iron oxide nanosheet material according to claim 1, wherein: and (4) in the step (3), the detergent is one of water, acetone or ethanol.
4. The method for preparing an iron oxide nanosheet material according to claim 1, wherein: in the step (3), the drying temperature is 80-150 ℃, and the drying time is 1-24 hours.
5. The method for preparing an iron oxide nanosheet material according to claim 1, wherein: the carrier in the step (1) is one of a crucible, an evaporating dish or tin foil paper.
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CN108899494B (en) * 2018-06-22 2021-11-02 济宁学院 Porous nitrogen-doped carbon intercalation coated iron oxide nano-plate material and preparation method thereof
CN108816231B (en) * 2018-06-22 2020-01-03 济宁学院 Carbon-coated iron oxide nanosheet material and preparation method thereof
CN109095506A (en) * 2018-08-13 2018-12-28 南京滕峰科技有限公司 A kind of preparation method and purposes of nano-sheet iron oxide

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