CN107175116A - The preparation method of FeOCl/iron hydroxide nanosheet composite material - Google Patents
The preparation method of FeOCl/iron hydroxide nanosheet composite material Download PDFInfo
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- CN107175116A CN107175116A CN201710552571.XA CN201710552571A CN107175116A CN 107175116 A CN107175116 A CN 107175116A CN 201710552571 A CN201710552571 A CN 201710552571A CN 107175116 A CN107175116 A CN 107175116A
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- feocl
- preparation
- iron
- iron hydroxide
- composite material
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The preparation method of FeOCl of the present invention/iron hydroxide nanosheet composite material, belongs to technical field of preparation for inorganic material, using the chlorate of iron as raw material, and the method cracked using high-temperature quick is prepared for the composite with nanometer chip architecture.The present invention utilizes single raw material, and a step is prepared for FeOCl/iron hydroxide nanosheet composite material, and the thickness of nanometer sheet is controllable, and the ratio of FeOCl and iron hydroxide is also controllable, solve solid phase reaction preparation FeOCl thickness it is big the problem of；Preparation method is easy, and cost is low, environmental sound, and suitable for large-scale industrial production, application prospect is extensive；FeOCl/iron hydroxide nanosheet composite material excellent performance obtained by preparation, as Fenton reaction reagents, can be used under pH neutral, normal temperature and sunshine or visible ray, increase catalytic activity and structural stability.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, and in particular to a kind of FeOCl/iron hydroxide nanometer sheet is answered
The preparation method of condensation material.
Background technology
Today's society, the environmental problem caused by water pollution has seriously threatened the living environment and body of the mankind
Body health.Therefore, Organic substance in water is quickly and completely degraded and has become current scientific research and the urgent of actual production is essential
Ask.As advanced oxidation technology, Fenton reactions can be by the degradable dioxy into environmental sound of organic contamination in water
Change carbon, water and inorganic salts etc., and with cheap, easy to use, it is easy to the advantages of industrialized production, cause people's
Extensive concern and great interest.But because homogeneous Fenton reagent easily produces the shortcoming of iron sludge, people started in recent years
The degraded of water pollutant is carried out using heterophase Fenton reagent.But current heterophase Fenton reagent usually requires strict
Condition (such as acid, ultraviolet or high temperature), significantly limit its practical application.Therefore develop a kind of environmental sound and
The heterophase Fenton reagent that can be used in a mild condition has become current scientific research and the research of practical application area heat
Point and difficult point.
At present, homogeneous and heterogeneous Fenton reagent the most commonly used during the compound of iron.To solve heterophase Fenton
The compound of iron and other materials are combined to improve the stabilization of catalytic activity and structure by shortcoming present in reaction, people
Property.For example, patent of invention (201410483396.X) reports a kind of heterogeneous light Fenton catalyst and application thereof；Patent of invention
(201410785253.4) Manganese Ferrite or the economic benefits and social benefits light Fenton denitrogenation method of its carbon composite are reported；Patent of invention
(201410572458.4) a kind of heterogeneous ultraviolet-Fenton oxidation catalyst and its preparation and application are reported.
Although composite can effectively improve the activity of catalyst and the stability of structure, preparation technology is more multiple
It is miscellaneous.The recombination process of two or more materials usually requires synthesis steps more than two steps, and technological process is long, and cost is higher.Chlorine
Iron oxide is also excellent heterophase Fenton reagent, and gas chromatography in water can be degraded, such as patent of invention
(201210152982.7) a kind of processing method of waste water from dyestuff is reported.FeOCl as a kind of stratified material, interlayer by
Van der Waals force is constituted, and weaker interlaminar action power can be other molecules and carry out intercalation, such as patent of invention
(201210008230.3) a kind of preparation method of the intercalation compound of ethylenediamine intercalation FeOCl is reported.FeOCl
Synthetic method have vapour deposition and two kinds of solid phase reaction.Costly, the FeOCl prepared by solid phase reaction of vapour deposition
The thickness of piece is up to hundreds of nanometers.Using simple and cheap raw material, easy one-step method prepares oxychloride iron-based nanometer sheet
Composite, the difficult point as current scientific research and production application.
The content of the invention
The invention provides a kind of preparation method of FeOCl/iron hydroxide nanosheet composite material, it is intended that
FeOCl/iron hydroxide nanosheet composite material is prepared for using high-temperature quick cracking process, nanometer sheet thickness is controllable, improved
The stability of catalytic performance and structure volume, the preparation method technological process is simple, cost is low and suitable large-scale production.
The preparation method of FeOCl of the present invention/iron hydroxide nanosheet composite material, using the chlorate of iron as raw material, profit
The method cracked with high-temperature quick is prepared for the composite with nanometer chip architecture.
The preparation method of FeOCl of the present invention/iron hydroxide nanosheet composite material, comprises the following steps：
(1) by the chlorate of iron in mortar grind into powder, and be laid on carrier；
(2) by the carrier for the powder that tiles as fast pyrolysis 2s-60s at a temperature of 300-600 DEG C；
(3) product of the thermal cracking of step (2) is washed 1-3 times with detergent, finally dried at a temperature of 60-100 DEG C
3-15h。
It is ferrous that the chlorate of iron described in step (1) includes iron chloride, frerrous chloride, Ferric Chloride Hydrated, chloride hydrate
In one or more of combinations.
Described carrier is one kind in aluminium foil, masking foil or alumina crucible.
The detergent is acetone or water.
The quality of tiling powder is 0.001g-0.03g/cm on described carrier2。
Compared with prior art, beneficial effects of the present invention are：
(1) present invention utilizes single raw material, and a step is prepared for FeOCl/iron hydroxide nanosheet composite material, nanometer
The thickness of piece is controllable, and the ratio of FeOCl and iron hydroxide is also controllable, solves the FeOCl thickness of solid phase reaction preparation
Big the problem of.
(2) preparation method is easy, and cost is low, environmental sound, and suitable for large-scale industrial production, application prospect is extensive.
(3) FeOCl/iron hydroxide nanosheet composite material excellent performance obtained by preparing, reacts as Fenton and tries
Agent, can be used under pH neutral, normal temperature and sunshine or visible ray, increase catalytic activity and structural stability.
Brief description of the drawings
Fig. 1 is the SEM figures of FeOCl/iron hydroxide in embodiment 1；
Fig. 2 is the EDS figures of FeOCl/iron hydroxide in embodiment 1；
Fig. 3 is dye molecule degraded figure in embodiment 1.
Embodiment
The present invention is further described with reference to specific embodiment, so that those skilled in the art do further
Understand, but and be not so limited the present invention.
Embodiment 1
Iron chloride hexahydrate is ground, gained powder is coated on masking foil, quality is 0.005g/cm2.By it 400
Fast pyrolysis 5s at a temperature of DEG C, is then washed twice with acetone, is placed in 80 DEG C of dry 8h.
As shown in Figure 1, the pattern of FeOCl/iron hydroxide is nanometer sheet, and thickness is less than 20nm.As shown in Figure 2, nanometer
Piece is the compound of FeOCl and iron hydroxide, and FeOCl content is 54%.
0.01g FeOCls/iron hydroxide nanosheet composite material is added to 20mL, concentration is 5mg/L rhodamine B
In solution, in dark after stirring 30min, add 0.1mL hydrogen peroxide (concentration is 30wt%) and carry out degradation experiment.By Fig. 3 to sieve
Red bright B degraded understands that FeOCl/iron hydroxide nanosheet composite material can degradable rhodamine B in 10min.
Embodiment 2
As described in Example 1, except that at a temperature of 400 DEG C fast pyrolysis 10s.FeOCl/iron hydroxide
The average thickness of nanometer sheet is 50nm, and the content of FeOCl is for 32%, 10min to the degraded of rhodamine B up to 95%.
Embodiment 3
As described in Example 1, except that iron chloride hexahydrate is coated on alumina crucible, in 550 DEG C of temperature
Lower fast pyrolysis 5s.The average thickness of FeOCl/iron hydroxide nanometer sheet is 20nm, and the content of FeOCl is 42%,
10min is to the degraded of rhodamine B up to 90%.
Embodiment 4
As described in Example 1, except that being coated on iron chloride grind into powder on aluminium foil.FeOCl/hydrogen-oxygen
The average thickness for changing iron nanometer sheet is 15nm, and the content of FeOCl is for 65%, 10min to the degraded of rhodamine B up to 100%.
Embodiment 5
As described in Example 1, except that being coated on frerrous chloride grind into powder on aluminium foil, quality is
0.02g/cm2.The average thickness of FeOCl/iron hydroxide nanometer sheet is 15nm, and the content of FeOCl is 80%, 10min
To the degraded of rhodamine B up to 100%.
Embodiment 6
As described in Example 1, except that it is 0.02g/cm to add quality2.FeOCl/iron hydroxide nanometer sheet
Average thickness is 30nm, and the content of FeOCl is for 38%, 10min to the degraded of rhodamine B up to 95%.
Embodiment 7
As described in Example 1, except that at a temperature of 400 DEG C fast pyrolysis 50s.FeOCl/iron hydroxide
The average thickness of nanometer sheet is 60nm, and the content of FeOCl is for 10%, 10min to the degraded of rhodamine B up to 85%
Embodiment 8
As described in Example 1, except that in alumina crucible at a temperature of 600 DEG C fast pyrolysis 2s.Oxychloride
The average thickness of iron/iron hydroxide nanometer sheet is 20nm, and the content of FeOCl is degradeds of 30%, the 10min to rhodamine B
Up to 95%
Embodiment 9
As described in Example 1, except that anhydrous frerrous chloride is coated on aluminium foil, quality is 0.01g/cm2.Chlorine
The average thickness of iron oxide/iron hydroxide nanometer sheet is 20nm, and the content of FeOCl is drops of 60%, the 10min to rhodamine B
Solution is up to 100%.
Embodiment 10
As described in Example 1, except that by product in 90 DEG C of dry 12h.FeOCl/iron hydroxide nanometer sheet
Average thickness is 20nm, and the content of FeOCl is for 54%, 10min to the degraded of rhodamine B up to 100%.
Rhodamine B is carried out using FeOCl/iron hydroxide nanosheet composite material obtained by embodiment 1-10 preparations
Degradation experiment, the data of gained refer to table 1.
| Degradation time | Degradation rate | |
| Embodiment 1 | 10min | 100% |
| Embodiment 2 | 10min | 95% |
| Embodiment 3 | 10min | 90% |
| Embodiment 4 | 10min | 100% |
| Embodiment 5 | 10min | 100% |
| Embodiment 6 | 10min | 95% |
| Embodiment 7 | 10min | 85% |
| Embodiment 8 | 10min | 95% |
| Embodiment 9 | 10min | 100% |
| Embodiment 10 | 10min | 100% |
Table 1.
Claims (6)
1. a kind of preparation method of FeOCl/iron hydroxide nanosheet composite material, it is characterised in that using the chlorate of iron as
Raw material, the method cracked using high-temperature quick is prepared for the composite with nanometer chip architecture.
2. the preparation method of FeOCl according to claim 1/iron hydroxide nanosheet composite material, its feature exists
In comprising the following steps：
(1) by the chlorate of iron in mortar grind into powder, and be laid on carrier；
(2) by the carrier for the powder that tiles as fast pyrolysis 2s-60s at a temperature of 300-600 DEG C；
(3) product of the thermal cracking of step (2) is washed 1-3 times with detergent, 3- is finally dried at a temperature of 60-100 DEG C
15h。
3. the preparation method of FeOCl according to claim 1 or 2/iron hydroxide nanosheet composite material, its feature
It is, the chlorate of the iron described in step (1) is included in iron chloride, frerrous chloride, Ferric Chloride Hydrated, chloride hydrate ferrous iron
One or more of combinations.
4. the preparation method of FeOCl according to claim 2/iron hydroxide nanosheet composite material, its feature exists
In described carrier is one kind in aluminium foil, masking foil or alumina crucible.
5. the preparation method of FeOCl according to claim 2/iron hydroxide nanosheet composite material, its feature exists
In the detergent is acetone or water.
6. the preparation method of FeOCl according to claim 2/iron hydroxide nanosheet composite material, its feature exists
In the quality for the powder that tiled on described carrier is 0.001g-0.03g/cm2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726577A (en) * | 2018-06-22 | 2018-11-02 | 济宁学院 | A kind of preparation method of ferrous sulfide nanometer sheet material |
| CN114618592A (en) * | 2022-03-18 | 2022-06-14 | 浙江稽山印染有限公司 | Preparation method of efficient heterogeneous Fenton catalyst and application of efficient heterogeneous Fenton catalyst in printing and dyeing wastewater treatment |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517484A (en) * | 2016-12-27 | 2017-03-22 | 武汉纺织大学 | Method for treating organic wastewater by use of ferric oxychloride to catalyze and activate mono-persulfate |
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2017
- 2017-07-07 CN CN201710552571.XA patent/CN107175116A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517484A (en) * | 2016-12-27 | 2017-03-22 | 武汉纺织大学 | Method for treating organic wastewater by use of ferric oxychloride to catalyze and activate mono-persulfate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726577A (en) * | 2018-06-22 | 2018-11-02 | 济宁学院 | A kind of preparation method of ferrous sulfide nanometer sheet material |
| CN108726577B (en) * | 2018-06-22 | 2020-07-24 | 济宁学院 | Preparation method of ferrous sulfide nanosheet material |
| CN114618592A (en) * | 2022-03-18 | 2022-06-14 | 浙江稽山印染有限公司 | Preparation method of efficient heterogeneous Fenton catalyst and application of efficient heterogeneous Fenton catalyst in printing and dyeing wastewater treatment |
| CN114618592B (en) * | 2022-03-18 | 2023-10-31 | 浙江稽山印染有限公司 | Preparation method of efficient heterogeneous Fenton catalyst and application of catalyst in treatment of printing and dyeing wastewater |
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