CN108101119A - The preparation method of oxidation nanometer sheet material - Google Patents
The preparation method of oxidation nanometer sheet material Download PDFInfo
- Publication number
- CN108101119A CN108101119A CN201711472977.3A CN201711472977A CN108101119A CN 108101119 A CN108101119 A CN 108101119A CN 201711472977 A CN201711472977 A CN 201711472977A CN 108101119 A CN108101119 A CN 108101119A
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- China
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- sheet material
- preparation
- nanometer sheet
- iron
- oxidation nanometer
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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)
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- 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
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- 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
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- 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 technical field of preparation for inorganic material, and in particular to using the chlorate of iron as raw material, nanometer sheet material is prepared for using the method for dinectly bruning for a kind of preparation method of ferric oxide nano sheet material.This method is prepared for ferric oxide nano sheet material using single raw material and simple one-step calcination, and nanometer sheet thickness is controllable, and preparation process is simple, economy is strong, prepared nanometer sheet material catalytic performance and excellent in stability, suitable for industrialized production, market application foreground is extensive.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, and in particular to a kind of preparation side of ferric oxide nano sheet material
Method.
Background technology
In recent years, the situation of environmental pollution and energy crisis was increasingly severe.Change based on conventional fossil fuel
Energy consumption structure, it is all of great advantage for solving energy crisis and environmental pollution.Nano-sized iron oxide have excellent weatherability,
Huge specific surface area and abundant surface active groups, are a kind of excellent catalyst, in catalytic degradation organic contamination object space
Face is widely used.Meanwhile iron oxide material can also be used for lithium ion battery negative material, have higher theoretical capacity.Nanometer
Quantity of the chip architecture material since specific surface area and active sites with special two-dimensional structure, can be greatly increased.So far, only
There is the preparation method seldom on ferric oxide nano piece.Patent of invention (201610136119.0) discloses a kind of utilization laser and shines
Penetrate the method that iron-nickel alloy prepares ferric oxide nano piece.Patent of invention (201610408147.3) discloses a kind of anti-using high pressure
Continue the method for preparing ferric oxide nano piece with sodium lactate reaction after answering kettle hydro-thermal.Patent of invention (201710120611.3) is announced
A kind of method for preparing ferric oxide nano piece using P123 and ethylene glycol organic solvent autoclave hydro-thermal reaction.Invention is special
Sharp (201710631273.X) reports a kind of cupric oxide nano line dispersion liquid using surface modification and soluble source of iron mixes
The method that then hydro-thermal reaction prepares ferric oxide nano piece.Patent of invention (201710463430.0) reports a kind of utilization second two
The method that alcohol prepares ferric oxide nano piece for the method that solvent elder generation solvent heat is calcined again.Ferric oxide nano piece is due to its excellent property
The extensive concern of domestic and international scientific research person and research enthusiasm can be caused, but the method reported at present needs harsh experiment item
Part, complex process are of high cost, it is difficult to realize industrialization.
The content of the invention
It is simple using single raw material and a step present invention aims at a kind of preparation method of oxidation nanometer sheet material of offer
The method of calcining is prepared for ferric oxide nano sheet material, and nanometer sheet thickness is controllable, improves the stability of catalytic performance and structure.
Simple, at low cost, the suitable large-scale production of present invention process flow.
The preparation method of oxidation nanometer sheet material of the present invention is using the chlorate of iron as raw material, utilizes calcining
Prepared by method, comprise the following steps：
(1) chlorate of iron in grind into powder and is laid on carrier；
(2) carrier for the chlorination salt powder for having iron that tiles is calcined in atmosphere, calcine technology is in two steps：The first step is with 5-
20 DEG C/min of heating rate is warming up to 180-270 DEG C, is kept for 30-120 minutes；Second step continues to heat up, with 1-10 DEG C/minute
The heating rate of clock rises to 300-500 DEG C, is kept for 30-180 minutes, and calcined product is obtained after being cooled to room temperature；
(3) gained calcined product in step (2) is washed 1-3 times with detergent, dry oxidation nanometer sheet material.
Wherein：
The chlorate of iron is one or both of iron chloride or frerrous chloride compounding.
The chlorination salt powder of iron is 0.01-0.5g/cm in carrier tiling amount2。
Atmosphere is one kind in air, nitrogen or argon gas in step (2).
Detergent is one kind in water, acetone or alcohol in step (3).
Drying temperature is 80-150 DEG C in step (3), when drying time is 1-24 small.
Carrier is one kind in crucible, evaporating dish or masking foil in step (1).
Compared with prior art, the present invention it has the advantages that.
(1) present invention is prepared for ferric oxide nano piece using single raw material and one-step calcination, simple for process, is forged in the first step
The controllable FeOCl of thickness is cracked to form in burning by the chlorate to heating rate and the control regulation and control iron of soaking time to receive
Rice piece, and the control of the heating of second step and heat preservation can regulate and control FeOCl transformation generation iron oxide, and then regulate and control nanometer sheet
Thickness, it is controllable to realize thickness, does not introduce organic matter, easy to operate, of low cost, solves ferric oxide nano sheet material system
The technical issues of standby complex process, with high costs etc.；
(2) preparation method and technology of the present invention is easy, and environmental sound is at low cost, should suitable for large-scale industrial production
It is extensive with prospect；
(3) the ferric oxide nano sheet material prepared by the present invention is had excellent performance, as catalyst, can in pH neutral, often
Excellent catalytic performance is shown under mild sunlight, catalytic activity and stable structure sex expression are excellent.
Description of the drawings
The XRD diagram of obtained ferric oxide nano sheet material in Fig. 1, embodiment 1；
The TEM figures of obtained ferric oxide nano sheet material in Fig. 2, embodiment 1；
The dyestuff degradation figure of obtained ferric oxide nano sheet material in Fig. 3, embodiment 1.
Specific embodiment
With reference to embodiment and Figure of description, the present invention will be further described.
Embodiment 1
By iron chloride hexahydrate, grind into powder is laid in alumina crucible in mortar, and trichloride hydrate iron powder exists
The amount to tile on alumina crucible is 0.25g/cm2, will in air be calcined after alumina crucible lid lid, calcine technology is divided to two
Step：The first step is warming up to 220 DEG C with 15 DEG C/min, is kept for 60 minutes；Second step continues to heat up, and 350 are warming up to 5 DEG C/min
DEG C, it is kept for 60 minutes, is cooled to room temperature to obtain calcined product, calcined product is washed 3 times with ethyl alcohol, dry 12 is small at 100 DEG C
When, obtain oxidation nanometer sheet material.
As shown in Figure 1, calcined product is iron oxide, and as shown in Figure 2, ferric oxide nano structure is nanometer sheet.
0.05g ferric oxide nano sheet materials obtained by the present embodiment are added in 100mL rhodamine B solution to (concentration is
5mg/L), after stirring 40min in dark, add in 0.5mL hydrogen peroxide (concentration 30wt%) and carry out degradation experiment, from the figure 3, it may be seen that
Ferric oxide nano sheet material can degradable organic pollution in 40min.
Embodiment 2
As described in Example 1, except that adding in chloride hydrate ferrous iron.Gained ferric oxide nano piece can be complete in 40min
Degradable organic pollution.
Embodiment 3
As described in Example 1, except that the amount of iron chloride hexahydrate is 0.03g/cm2.Gained ferric oxide nano piece
It can degradable organic pollution in 40min.
Embodiment 4
As described in Example 1, except that the amount of iron chloride hexahydrate is 0.5g/cm2.Gained ferric oxide nano piece exists
40min degradable organic pollutants are up to 92%.
Embodiment 5
As described in Example 1, except that being calcined in nitrogen atmosphere.Gained ferric oxide nano piece can be complete in 40min
Degradable organic pollution.
Embodiment 6
As described in Example 1, except that the calcining first step is to be warming up to 270 DEG C of calcinings with 20 DEG C/min, 30 are kept
Minute.Gained ferric oxide nano piece is in 40min degradable organic pollutants up to 98%.
Embodiment 7
As described in Example 1, except that the first step is warming up to 180 DEG C of calcinings with 5 DEG C/min, kept for 120 minutes.
Gained ferric oxide nano piece is in 40min degradable organic pollutants up to 95%.
Embodiment 8
As described in Example 1, except that it is to be warming up to 500 DEG C of calcinings with 2 DEG C/min that second step, which continues heating, protect
It holds 30 minutes.Gained ferric oxide nano piece is in 40min degradable organic pollutants up to 93%.
Embodiment 9
As described in Example 1, except that it is to be warming up to 300 DEG C of calcinings with 5 DEG C/min that second step, which continues heating, protect
It holds 180 minutes.Gained ferric oxide nano piece is in 40min degradable organic pollutants up to 100%.
Embodiment 10
As described in Example 1, except that product is washed with water 3 times, in 80 DEG C of dry gained ferric oxide nanos for 24 hours
Piece is in 40min degradable organic pollutants up to 100%.
Embodiment 11
As described in Example 1, except that product is washed 1 time with acetone, received in 150 DEG C of dry iron oxide obtained by 1h
Rice piece is in 40min degradable organic pollutants up to 100%.
Claims (8)
1. a kind of preparation method of oxidation nanometer sheet material, it is characterised in that：Using the chlorate of iron as raw material, the side of calcining is utilized
It is prepared by method.
2. the preparation method of oxidation nanometer sheet material according to claim 1, it is characterised in that：Comprise the following steps：
(1) chlorate of iron in grind into powder and is laid on carrier；
(2) carrier for the chlorination salt powder for having iron that tiles is calcined in atmosphere, calcine technology is in two steps：The first step is with 5-20
DEG C/min heating rate be warming up to 180-270 DEG C, kept for 30-120 minutes；Second step continues to heat up, with 1-10 DEG C/min
Heating rate rise to 300-500 DEG C, kept for 30-180 minute, calcined product obtained after being cooled to room temperature；
(3) gained calcined product in step (2) is washed 1-3 times with detergent, dry oxidation nanometer sheet material.
3. the preparation method of oxidation nanometer sheet material according to claim 1 or 2, it is characterised in that：The chlorate of iron is
One or both of iron chloride or frerrous chloride compounding.
4. the preparation method of oxidation nanometer sheet material according to claim 3, it is characterised in that：The chlorination salt powder of iron exists
Carrier tiling amount is 0.01-0.5g/cm2。
5. the preparation method of oxidation nanometer sheet material according to claim 2, it is characterised in that：Atmosphere is in step (2)
One kind in air, nitrogen or argon gas.
6. the preparation method of oxidation nanometer sheet material according to claim 2, it is characterised in that：Detergent in step (3)
For one kind in water, acetone or alcohol.
7. the preparation method of oxidation nanometer sheet material according to claim 2, it is characterised in that：Dry temperature in step (3)
It spends for 80-150 DEG C, when drying time is 1-24 small.
8. the preparation method of oxidation nanometer sheet material according to claim 2, it is characterised in that：Carrier is in step (1)
One kind in crucible, evaporating dish or masking foil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711472977.3A CN108101119B (en) | 2017-12-29 | 2017-12-29 | Preparation method of iron oxide nanosheet material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711472977.3A CN108101119B (en) | 2017-12-29 | 2017-12-29 | Preparation method of iron oxide nanosheet material |
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| CN108101119A true CN108101119A (en) | 2018-06-01 |
| CN108101119B CN108101119B (en) | 2020-01-03 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816231A (en) * | 2018-06-22 | 2018-11-16 | 济宁学院 | Carbon coating ferric oxide nano sheet material and preparation method thereof |
| CN108899494A (en) * | 2018-06-22 | 2018-11-27 | 济宁学院 | Porous nitrogen-doped carbon intercalation coated iron oxide nano-plates 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491429A (en) * | 2011-11-16 | 2012-06-13 | 华东师范大学 | Preparation method of FeOCl |
| JP2013166659A (en) * | 2012-02-14 | 2013-08-29 | Kawamura Institute Of Chemical Research | Method for producing metal oxide nano-sheet and metal oxide nano-sheet |
-
2017
- 2017-12-29 CN CN201711472977.3A patent/CN108101119B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491429A (en) * | 2011-11-16 | 2012-06-13 | 华东师范大学 | Preparation method of FeOCl |
| JP2013166659A (en) * | 2012-02-14 | 2013-08-29 | Kawamura Institute Of Chemical Research | Method for producing metal oxide nano-sheet and metal oxide nano-sheet |
Non-Patent Citations (1)
| Title |
|---|
| 中南矿冶学院冶金研究室: "《氯化冶金》", 31 March 1978, 冶金工业出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108816231A (en) * | 2018-06-22 | 2018-11-16 | 济宁学院 | Carbon coating ferric oxide nano sheet material and preparation method thereof |
| CN108899494A (en) * | 2018-06-22 | 2018-11-27 | 济宁学院 | Porous nitrogen-doped carbon intercalation coated iron oxide nano-plates material and preparation method thereof |
| 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 |
| 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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| CN108101119B (en) | 2020-01-03 |
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Effective date of registration: 20230227 Address after: 541299 No. 18, North Welfare Road, Dingjiang Town, Lingchuan County, Guilin City, Guangxi Zhuang Autonomous Region Patentee after: Guilin Baolongda New Material Co.,Ltd. Address before: No.16 Haichuan Road, Jining high tech Zone, Shandong Province, 272001 Patentee before: JINING University |