CN107986330A - A kind of Bi5O7I nano lamellar materials and its preparation method and application - Google Patents
A kind of Bi5O7I nano lamellar materials and its preparation method and application Download PDFInfo
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- CN107986330A CN107986330A CN201711281044.6A CN201711281044A CN107986330A CN 107986330 A CN107986330 A CN 107986330A CN 201711281044 A CN201711281044 A CN 201711281044A CN 107986330 A CN107986330 A CN 107986330A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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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
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- 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
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The present invention provides a kind of Bi5O7I nano lamellar materials and its preparation method and application, are related to conductor photocatalysis material technical field.A kind of Bi5O7The preparation method of I nano lamellar materials, including：Bismuth-containing compound and salt compounded of iodine are dissolved in ethylene glycol, the pH value of solution is adjusted to 8~10, carries out hydro-thermal reaction.This method preparation process is simple, of low cost, and controllability is strong, is adapted to large-scale production.A kind of Bi5O7I nano lamellar materials, by above-mentioned Bi5O7The preparation method of I nano lamellar materials is prepared.It is with preferable visible ray sensing capability and degrading phenol pollutant ability.
Description
Technical field
The present invention relates to conductor photocatalysis material technical field, and more particularly to a kind of Bi5O7I nano lamellar materials and
Its preparation method and application.
Background technology
The seriousness of environmental pollution at present, it has also become one directly threatens human survival, is badly in need of solving, very important asks
Topic.Phenolic compound refers to that the hydrogen atom in aromatic hydrocarbon on phenyl ring is optionally substituted by a hydroxyl group generated compound.Phenolic compound
Water solubility increases with the increase of hydroxy number, and due to that can form intermolecular hydrogen bonding, most phenolic compounds have higher
Boiling point, it is difficult to volatilize, can exist for a long time in the environment such as soil, water.In the synthesis of phenolic compound, extraction and use process
In, part phenolic compound is released in environment, causes environmental pollution.If phenol wastewater is that big, dirt is endangered in the world today
One of wide industrial wastewater of scope is contaminated, is the important sources of water pollution in environment.If these waste water are directly arranged without processing
Put, air, rivers, ocean, underground water, soil and food can be polluted, strong influence is caused to existence biological on the earth.Mesh
Before, phenolic compound is classified as the blacklist of 129 kinds of priority pollutants, the improvement of the pollutant containing phenol by American National Environmental Protection Agency
It is one of Environmental Chemistry primary study task.
TiO is found from Fujishima in 1972 etc.2It can rise hydrogen production by water decomposition under ultraviolet light, numerous researchers
Sight start invest photocatalysis research field.In early stage, the research hotspot of photocatalysis field is concentrated mainly on solar energy conversion
Aspect.But since the quantum efficiency of used light-catalyzed reaction system is relatively low, catalytic activity is poor, therefore even to this day, directly
Connect using sunlight as light source to carry out the progress that photocatalysis does not obtain real practicality also.It is most widely used at present
It is TiO2Photochemical catalyst, people have carried out substantial amounts of research work for such catalyst.But from the point of view of the utilization rate of sunlight,
Using titanium dioxide as the wide bandgap semiconductor catalysis material of representative, also there are following defect：First, the light absorption wavelength of semiconductor
It is narrow, it is low using the efficiency of sunlight mainly in ultra-violet (UV) band；Second, the recombination rate of photo-generated carrier is very high, cause quantum efficiency
Relatively low, these factors constrain the practical application in industry of Photocatalitic Technique of Semiconductor to a certain extent.Therefore, new height is found
Imitate photochemical catalyst has become the development trend of current photocatalysis field.
The content of the invention
It is an object of the invention to provide a kind of Bi5O7The preparation method of I nano lamellar materials, this method preparation process letter
Single, of low cost, controllability is strong, is adapted to large-scale production.
Another object of the present invention is to provide a kind of Bi5O7I nano lamellar materials, have preferable visible ray induction energy
Power and degrading phenol pollutant ability.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of Bi5O7The preparation method of I nano lamellar materials, including：Bismuth-containing compound and salt compounded of iodine are dissolved
In ethylene glycol, the pH value of solution is adjusted to 8~10, carries out hydro-thermal reaction.
The present invention proposes a kind of Bi5O7I nano lamellar materials, by above-mentioned Bi5O7The preparation method system of I nano lamellar materials
It is standby to form.
The present invention proposes a kind of Bi5O7The application in catalyzing and degrading pollutant under visible light of I nano lamellar materials.
A kind of Bi of the embodiment of the present invention5O7The beneficial effect of I nano lamellar materials and its preparation method and application is：
A kind of Bi provided by the invention5O7I nano lamellar materials and preparation method thereof, using bismuth-containing compound and salt compounded of iodine as
Reactant, in the system of ethylene glycol, under conditions of pH value is 8~10, Bi is prepared using one step of hydro-thermal method5O7I nano-sheets
Material.Water is not contained in the reaction system of the present invention, avoids the hydrolysis of bismuth-containing compound, contributes to the progress of reaction.Solution
Within the range, the product structure of generation is homogeneous, regular appearance for pH value.Hydro-thermal reaction is high-temperature high-voltage reaction, under this condition,
Bismuth-containing compound and the product of salt compounded of iodine reaction generation have preferable crystalline form and regular pattern, can obtain the small sheet of size
Material.Obtained Bi5O7I nano lamellar materials have preferable visible ray sensing capability and degrading phenol pollutant ability.The party
Method preparation simple process and low cost is honest and clean, and controllability is strong, is adapted to large-scale production.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described.It should be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore it is not construed as pair
The restriction of scope.For those of ordinary skill in the art, without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the Bi that the embodiment of the present invention 1 provides5O7The XRD spectra of I nano lamellar materials；
Fig. 2 is the Bi that the embodiment of the present invention 1 provides5O7The SEM spectrograms of I nano lamellar materials；
Fig. 3 is the Bi that the embodiment of the present invention 1 provides5O7Degradation rate of the I nano lamellar materials to phenolic comp ' ds pollution.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
Below to a kind of Bi of the embodiment of the present invention5O7I nano lamellar materials and its preparation method and application carry out specifically
It is bright.
A kind of Bi provided in an embodiment of the present invention5O7The preparation method of I nano lamellar materials, including：
Bismuth-containing compound is dissolved in ethylene glycol, adds salt compounded of iodine, is sufficiently stirred dissolving.In the present invention, using containing
Bismuth compound is with salt compounded of iodine as raw material, and ethylene glycol is as reaction dissolvent.Bismuth-containing compound is not susceptible to hydrolyze in ethylene glycol, has
Help the progress of reaction.Particularly, water cannot be contained in solvent of the invention, water can influence the progress of reaction and the life of product
Into.
In order to enable reaction progress is complete, the Bi of regular appearance is obtained5O7I materials, in the present invention preferably embodiment
In, the amount ratio of the material of the iodine in bismuth element and salt compounded of iodine in bismuth-containing compound is 1:1~2.Preferably, bismuth-containing compound
In bismuth element and salt compounded of iodine in iodine material amount ratio can be 2:3、3:5、4:5、4:7.
Further, in the present invention preferably embodiment, bismuth-containing compound includes bismuth nitrate, five nitric hydrate bismuths, chlorine
Change at least one of bismuth, salt compounded of iodine includes any one or at least two in potassium iodide, tetrabutylammonium iodide, sodium iodide.
The pH value of solution is adjusted to 8~10 with pH adjusting agent.The pH value of solution has the function that important in the present invention, molten
Within the range, the product of generation is target product to the pH value of liquid, if changing pH value, the product generated can also change.It is preferred that
Ground, the pH value of solution is 9~10, it is highly preferred that the pH value of solution is 9.2,9.5,9.8.PH adjusting agent include sodium hydroxide,
At least one of potassium hydroxide, ammonium hydroxide.
After having adjusted pH value, mixed solution is transferred in hydrothermal reaction kettle, hydro-thermal is anti-under conditions of 120~180 DEG C
Answer 6~16h.The hydro-thermal reaction of the present invention is high-temperature high-voltage reaction, under this condition, bismuth-containing compound and salt compounded of iodine reaction generation
Product has preferable crystalline form and regular pattern, can obtain the small flaky material of size.Due to product crystalline form and pattern
Difference, the performance of product are also different.
After reaction, treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to precipitation
Washing purification is carried out, obtains yellow solid powder.Preferably, wash number is 2~4 times.
After purification, solid powder is placed in baking oven, when drying 11~13 is small under conditions of 50~70 DEG C.To solid powder
End is fully ground, up to Bi5O7I nano lamellar materials.
The present invention provides a kind of Bi5O7I nano lamellar materials, by above-mentioned Bi5O7The preparation method of I nano lamellar materials
It is made.Pass through Bi made from above-mentioned preparation method5O7I nano lamellar material structures are homogeneous, band gap is narrow, can should be able to by light sensation
Power is strong, has extremely strong photocatalytic degradation capability to phenols organic pollution, and environmental improvement and green energy resource, which are utilized, has weight
Want meaning.
Due to above-mentioned Bi5O7I nano lamellar materials have pollutant extremely strong photocatalytic degradation capability, and the present invention also carries
Above-mentioned Bi is supplied5O7The I nano lamellar materials application in catalyzing and degrading pollutant under visible light, it is preferable that pollutant includes phenol
Class organic pollution.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 1.56g are dissolved in 66mL ethylene glycol, 0.996g potassium iodide is added, is sufficiently stirred molten
Solution.With the pH value of sodium hydrate regulator solution to 10.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 6h under conditions of 150 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Embodiment 2
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 0.73g are dissolved in 33mL ethylene glycol, 0.498g potassium iodide is added, is sufficiently stirred molten
Solution.With the pH value of sodium hydrate regulator solution to 10.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 6h under conditions of 150 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Embodiment 3
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 0.73g are dissolved in 33mL ethylene glycol, 0.498g potassium iodide is added, is sufficiently stirred molten
Solution.With the pH value of sodium hydrate regulator solution to 10.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 12h under conditions of 150 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Embodiment 4
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 1.56g are dissolved in 66mL ethylene glycol, 0.996g potassium iodide is added, is sufficiently stirred molten
Solution.With the pH value of sodium hydrate regulator solution to 10.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 12h under conditions of 120 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Embodiment 5
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 1.56g are dissolved in 66mL ethylene glycol, 0.5g potassium iodide is added, is sufficiently stirred dissolving.
With the pH value of sodium hydrate regulator solution to 9.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 12h under conditions of 120 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Embodiment 6
Present embodiments provide a kind of Bi5O7I nano lamellar materials, are mainly prepared by the following method：
Five nitric hydrate bismuths of 1.56g are dissolved in 66mL ethylene glycol, 0.5g potassium iodide is added, is sufficiently stirred dissolving.
With the pH value of sodium hydrate regulator solution to 9.
Mixed solution is transferred in hydrothermal reaction kettle, the hydro-thermal reaction 16h under conditions of 140 DEG C.
Treat that product is cooled to room temperature, centrifugation is carried out to product, with deionized water and ethanol to washing of precipitate 3 times, is obtained
To yellow solid powder.
Solid powder is placed in baking oven, when drying 12 is small under conditions of 60 DEG C.Solid powder is fully ground,
Up to Bi5O7I nano lamellar materials.
Test example
Bi prepared by 50mg embodiments 1~6 is chosen respectively5O7I nano lamellar materials, it is the double of 20ppm to be placed in 50mL concentration
In phenol solution A, lucifuge secretly adsorbs 60min first, then irradiates lower carry out in visible ray (800W xenon lamps, with 420nm optical filters)
React 1 it is small when, during which take sample once at interval of certain time, filtrate surveyed with ultra-violet and visible spectrophotometer
Acquired results are carried out data processing by amount.As a result it is as follows：
1 measurement result of table
As shown in Table 1, the Bi that embodiment 1~6 provides5O7I nano lamellar materials are respectively provided with preferable drop to bisphenol-A solution
Solution rate.Wherein, the Bi that embodiment 1 provides5O7The degradation rate highest of I nano lamellar materials, carries out it XRD and microscopic appearance inspection
Survey.
The Bi provided from Fig. 1 and Fig. 2, embodiment 15O7The crystalline form shape of I nano lamellar materials is unified, homogeneous, pattern
Regular, size is small, is that component is single, the uniform flake nano material of micro-optic structure.From the figure 3, it may be seen that what embodiment 1 provided
Bi5O7The visible light reaction 1 of I nano lamellar materials it is small when can degradable target contaminant bisphenol-A, it is while total organic in system
Carbon removal rate (mineralization rate) reaches more than 90%, illustrates that pollutant and its degradation intermediate are thoroughly removed, will not produce two
Secondary pollution.
A kind of in conclusion Bi provided by the invention5O7I nano lamellar materials and preparation method thereof, with bismuth-containing compound and
In the system of ethylene glycol, under conditions of pH value is 8~10, Bi is prepared using one step of hydro-thermal method as reactant for salt compounded of iodine5O7I
Nano lamellar material.The present invention reaction system in do not contain water, avoid the hydrolysis of bismuth-containing compound, contribute to reaction into
OK.Within the range, the product structure of generation is homogeneous, regular appearance for the pH value of solution.Hydro-thermal reaction is high-temperature high-voltage reaction,
Under the conditions of being somebody's turn to do, bismuth-containing compound and the product of salt compounded of iodine reaction generation have preferable crystalline form and regular pattern, can obtain ruler
Very little small flaky material.Obtained Bi5O7There is I nano lamellar materials preferable visible ray sensing capability and degrading phenol to pollute
Thing ability.This method preparation process is simple, of low cost, and controllability is strong, is adapted to large-scale production.
Embodiments described above is part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
- A kind of 1. Bi5O7The preparation method of I nano lamellar materials, it is characterised in that including：Bismuth-containing compound and salt compounded of iodine are dissolved In ethylene glycol, the pH value of solution is adjusted to 8~10, carries out hydro-thermal reaction.
- 2. Bi according to claim 15O7The preparation method of I nano lamellar materials, it is characterised in that further include：Hydro-thermal is anti- After the completion of answering, purify and dry product, then be ground.
- 3. Bi according to claim 25O7The preparation method of I nano lamellar materials, it is characterised in that the product after grinding For flake nano material.
- 4. Bi according to claim 15O7The preparation method of I nano lamellar materials, it is characterised in that hydro-thermal reaction includes： The solution reacts 6~16h under conditions of 120~180 DEG C.
- 5. Bi according to claim 15O7The preparation method of I nano lamellar materials, it is characterised in that the bismuth-containing chemical combination The amount ratio of bismuth element and the material of the iodine in the salt compounded of iodine in thing is 1:1~2.
- 6. Bi according to claim 1 or 55O7The preparation method of I nano lamellar materials, it is characterised in that the bismuth-containing Compound includes at least one of bismuth nitrate, five nitric hydrate bismuths, bismuth chloride.
- 7. Bi according to claim 65O7The preparation method of I nano lamellar materials, it is characterised in that the salt compounded of iodine includes Any one in potassium iodide, tetrabutylammonium iodide, sodium iodide or at least two.
- 8. Bi according to claim 75O7The preparation method of I nano lamellar materials, it is characterised in that pH adjusting agent bag Include at least one of sodium hydroxide, potassium hydroxide, ammonium hydroxide.
- A kind of 9. Bi5O7I nano lamellar materials, it is characterised in that by such as claim 1~8 any one of them Bi5O7I nanometers The preparation method of flaky material is prepared.
- 10. Bi as claimed in claim 95O7The application in catalyzing and degrading pollutant under visible light of I nano lamellar materials, it is excellent Selection of land, the pollutant include phenols organic pollution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113998734A (en) * | 2021-11-09 | 2022-02-01 | 淮阴师范学院 | Bi5O7Preparation method of Br nanosheet |
| CN115364873A (en) * | 2022-08-22 | 2022-11-22 | 电子科技大学长三角研究院(湖州) | Hollow tubular ultrathin photocatalyst and preparation method thereof |
-
2017
- 2017-12-06 CN CN201711281044.6A patent/CN107986330A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| JUANLI HAN ET AL.: ""Temperature effect on phase transition and morphological transformation of BiOI microspheres toBi5O7I microstructures"", 《MATERIALS LETTERS》 * |
| YANG BAI ET AL.: ""Facet-Dependent Photocatalytic N2 Fixation of Bismuth-Rich Bi5O7I Nanosheets"", 《ACS APPLIED MATERIALS & INTERFACES》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113998734A (en) * | 2021-11-09 | 2022-02-01 | 淮阴师范学院 | Bi5O7Preparation method of Br nanosheet |
| CN113998734B (en) * | 2021-11-09 | 2024-01-26 | 淮阴师范学院 | Bi 5 O 7 Preparation method of Br nanosheets |
| CN115364873A (en) * | 2022-08-22 | 2022-11-22 | 电子科技大学长三角研究院(湖州) | Hollow tubular ultrathin photocatalyst and preparation method thereof |
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