CN108212187A - Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst - Google Patents
Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst Download PDFInfo
- Publication number
- CN108212187A CN108212187A CN201810077487.1A CN201810077487A CN108212187A CN 108212187 A CN108212187 A CN 108212187A CN 201810077487 A CN201810077487 A CN 201810077487A CN 108212187 A CN108212187 A CN 108212187A
- Authority
- CN
- China
- Prior art keywords
- preparation
- photochemical catalyst
- dopant
- ammonium hydroxide
- organic solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title description 3
- 238000002360 preparation method Methods 0.000 claims abstract description 34
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 20
- 239000002019 doping agent Substances 0.000 claims abstract description 20
- 239000001509 sodium citrate Substances 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 13
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- OQUFOZNPBIIJTN-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium Chemical compound [Na].OC(=O)CC(O)(C(O)=O)CC(O)=O OQUFOZNPBIIJTN-UHFFFAOYSA-N 0.000 claims 1
- 229910017053 inorganic salt Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 15
- 238000007146 photocatalysis Methods 0.000 abstract description 13
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 48
- 230000000052 comparative effect Effects 0.000 description 20
- 239000000047 product Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 235000011083 sodium citrates Nutrition 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000011541 reaction mixture Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 5
- 229940012189 methyl orange Drugs 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N bismuth(III) nitrate Inorganic materials [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000004941 influx Effects 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000005945 translocation Effects 0.000 description 1
Classifications
-
- 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- B01J35/39—
-
- B01J35/61—
Abstract
Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst belongs to photocatalysis technology field.Preparation method includes：Fe will be contained3+Dopant dissolved with Bi (NO3)3And mixing in the alkali organic solvent solution of sodium citrate, hydro-thermal reaction is carried out under conditions of containing ammonium hydroxide.Photochemical catalyst is made according to above-mentioned preparation method.Fe can be incorporated into Bi2O2CO3Lattice in, Bi can be improved2O2CO3Absorption to visible ray, so as to improve Bi2O2CO3Visible light photocatalysis active.
Description
Technical field
The present invention relates to photocatalysis technology fields, and Bi is adulterated in particular to a kind of Fe2O2CO3The system of photochemical catalyst
Preparation Method and Fe doping Bi2O2CO3Photochemical catalyst.
Background technology
With the rapid development of industry, environmental pollution is increasingly severe.Using solar energy, degraded by photocatalysis technology dirty
Dye object is a kind of pollution treatment technology of energy-saving and environmental protection, it is considered to be solves that environmental problem is most effective, most promising side
Method.Bi2O2CO3A kind of novel photochemical catalyst, can degradable organic pollutant under ultraviolet light, have than commercial P25 higher
Activity.However, Bi2O2CO3Energy gap be about 3.4eV, it is impossible to absorb visible ray.In addition, the ultraviolet light in sunlight only accounts for
About 4.5%, and visible ray accounts for about 45%.Thus, make Bi2O2CO3It is limited by very large in practical application.
Bi is improved therefore, it is necessary to take effective measures2O2CO3To the sensibility of visible ray, enhance it in visible ray
Absorption region.
In view of this, it is special to propose the present invention.
Invention content
The purpose of the present invention is to provide a kind of Fe to adulterate Bi2O2CO3The preparation method of photochemical catalyst can improve
Bi2O2CO3Absorption to visible ray, so as to improve Bi2O2CO3Visible light photocatalysis active.
Another object of the present invention is to provide a kind of Fe doping Bi2O2CO3Photochemical catalyst increases the absorption of visible ray
By force, it is seen that light photocatalytic activity enhances.
What the embodiment of the present invention was realized in：
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：Fe will be contained3+Dopant dissolved with Bi
(NO3)3And mixing in the alkali organic solvent solution of sodium citrate, hydro-thermal reaction is carried out under conditions of containing ammonium hydroxide.
A kind of Fe adulterates Bi2O2CO3Photochemical catalyst is made according to above-mentioned preparation method.
The advantageous effect of the embodiment of the present invention is：
Fe provided by the invention adulterates Bi2O2CO3The preparation method of photochemical catalyst, through inventor the study found that by Fe3+It mixes
It is miscellaneous to enter Bi2O2CO3Lattice in, Bi can be effectively improved2O2CO3Absorption to visible ray, so as to effectively increase Bi2O2CO3's
Visible light photocatalysis active.Inventor also found simultaneously, will contain Fe3+Dopant mixed in alkali organic solvent solution
It is miscellaneous, Fe3+In Bi2O2CO3Doping effect in lattice is good, and the grain size of the substance of synthesis is small, large specific surface area, so that being made
Bi2O2CO3Visible light photocatalysis active be further enhanced.
Fe provided by the invention adulterates Bi2O2CO3Photochemical catalyst is made according to above-mentioned preparation method, thus it is similarly
Has the advantages of influx and translocation to visible ray, visible light photocatalysis active enhancing.
Description of the drawings
It 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 understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range, 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 scanning electron microscope (SEM) photograph of comparative example of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of test example of the present invention；
Fig. 3 is the XRD spectrum of test example of the present invention and comparative example；
Fig. 4 is test example in Fig. 3 and comparative example in 2 θ=30.2oThe amplification collection of illustrative plates at place；
Fig. 5 is the XPS High Resolution Spectrums of test example of the present invention；
Fig. 6 is the UV-Vis DRS spectrogram of test example of the present invention and comparative example；
Fig. 7 is the expression activitiy curve of test example of the present invention and comparative example to methyl orange degradation.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below will be in the embodiment of the present invention
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.
Bi is adulterated to the Fe of the embodiment of the present invention below2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Light
Catalyst is specifically described.
The present invention provides a kind of Fe doping Bi2O2CO3The preparation method of photochemical catalyst, including：Fe will be contained3+Dopant
Dissolved with Bi (NO3)3And mixing in the alkali organic solvent solution of sodium citrate, hydro-thermal reaction is carried out under conditions of containing ammonium hydroxide.
Bi2O2CO3It is a kind of typical bismuth-system compound oxide, by Bi2O2 2+And CO3 2–Composition, the space structure of bending
Unique photocatalysis performance is shown under ultraviolet-visible light irradiation.Through inventor the study found that by Fe3+Doping enters
Bi2O2CO3Lattice in, Bi can be effectively improved2O2CO3Absorption to visible ray, so as to effectively increase Bi2O2CO3Visible ray
Photocatalytic activity.
Containing Fe3+Dopant as source of iron, Fe is provided3+Into Bi2O2CO3Lattice in.Some in the present invention are specific
Embodiment in, containing Fe3+Dopant use containing Fe3+Inorganic salts provide Fe3+.Further, preferably implement at some
In mode, this contains Fe3+Dopant be Fe (NO3)3.In addition, in some other embodiment of the present invention, this contains Fe3+'s
Dopant can also be FeCl3、Fe2(SO4)3Wait strong acid weak base salts.
It is used as using above-mentioned source of iron containing Fe3+Dopant, in Bi2O2CO3Lattice in doping effect it is good；Energy simultaneously
The generation of by-product is effectively avoided, so as to improve the quality of product.
In the specific embodiment of the present invention, Fe3+Be entrained in Bi (NO3)3And in the solution system of sodium citrate into
Row, addition ammonium hydroxide carries out hydro-thermal reaction completion after source of iron is added in solution system.
Bi(NO3)3And the solution system of sodium citrate is basic organic solution system.Through inventor the study found that containing Fe3+
Dopant be doped in alkaline reagent, Fe3+In Bi2O2CO3Doping effect in lattice is good；Meanwhile Fe3+Dopant
It carries out that the generation smaller catalyst of grain size, increasing specific surface area, so as to improve the light of catalyst can be controlled in organic solvent
Catalytic activity.In some preferred embodiments of the invention, which is n,N-Dimethylformamide.
The addition of ammonium hydroxide can be controlled to Fe3+Doping.In preferred embodiments of the present invention, the mass concentration of ammonium hydroxide is
25~35%.Preferably, it is 25~30%.It is highly preferred that it is 28%, naturally it is also possible to for such as：25%th, 26%, 27%,
29%th, 30%, 31%, 32%, 33%, 34%, 35% etc..
Through inventor the study found that control Bi (NO3)3, sodium citrate, alkali organic solvent, containing Fe3+Dopant and
The amount ratio of ammonium hydroxide is 0.8~1.2g：0.15~0.45g：8~12ml：0.02g~0.15g：During 3~8ml, Fe3+
Bi2O2CO3Lattice in doped with preferable effect；The grain size of obtained substance is small, large specific surface area, visible light photocatalysis
Performance is strong.
Preferably, Bi (the NO3)3, sodium citrate, alkali organic solvent, containing Fe3+Dopant and ammonium hydroxide amount ratio
For 0.9~1.1g：0.25~0.35g：9~11ml：0.05g~0.15g：4~6ml.
Further, the Bi (NO3)3, sodium citrate, alkali organic solvent, containing Fe3+Dopant and ammonium hydroxide dosage
Than preferably controlling as 0.97g：0.3g：10ml：0.1g： 5ml.
Hydro-thermal reaction is transferred in water heating kettle after ammonium hydroxide has been added and carries out.For the present invention preferably in embodiment, hydro-thermal is anti-
It is seasonable to keep reaction temperature for 170~190 DEG C and keep the temperature 1~12h at such a temperature, ensure that reactant is abundant in hydro-thermal reaction
It reacts and by-product is avoided to generate as far as possible.Preferably, reaction temperature is 175~185 DEG C, the reaction time is 9~11h.Into one
Step preferably, reaction temperature be 170 DEG C, reaction time 10h.
After the completion of hydro-thermal reaction, after water heating kettle cooling, product is washed and is dried, you can is prepared
Bi2O2CO3Photochemical catalyst.
Alternately sediment obtained by the reaction is cleaned using distilled water and ethyl alcohol in washing operation, until product is clear
Wash clean.
Preferably controlled at 55~65 DEG C when dry, and keep completing for 7~9 hours at such a temperature.In the present invention
In some specific embodiments, drying temperature is preferably 60 DEG C, which is preferably 8h, makes to do
Dry effect is good, while avoids having an impact the performance of product.
The present invention provides a kind of Fe doping Bi2O2CO3Photochemical catalyst is made according to above-mentioned preparation method, thus it has
The advantages that good absorption effect, grain size to visible ray are small, large specific surface area, it is seen that light photocatalytic activity is strong.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：
S1, by 0.97gBi (NO3)310mlN is dissolved in 0.3g sodium citrates, in dinethylformamide, obtains reacting molten
Liquid.
S2,0.1gFe (NO are added in into reaction solution3)3, it stirs evenly, adds in the ammonium hydroxide that 5ml mass concentrations are 28%,
Obtain reaction mixture.
S3, reaction mixture is transferred in water heating kettle, 12h is kept the temperature at a temperature of 170 DEG C, separation of solid and liquid after cooling obtains
To head product.
S4, head product distilled water and ethyl alcohol are alternately cleaned up, dry 8h, obtains Bi at a temperature of 60 DEG C2O2CO3
Photochemical catalyst.
A kind of Fe according to made from above-mentioned preparation method adulterates Bi2O2CO3Photochemical catalyst.
Embodiment 2
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：
S1, by 0.8gBi (NO3)38mlN is dissolved in 0.15g sodium citrates, in dinethylformamide, obtains reacting molten
Liquid.
S2,0.02gFe (NO are added in into reaction solution3)3, it stirs evenly, adds in the ammonium hydroxide that 3ml mass concentrations are 35%,
Obtain reaction mixture.
S3, reaction mixture is transferred in water heating kettle, 11h is kept the temperature at a temperature of 175 DEG C, separation of solid and liquid after cooling obtains
To head product.
S4, head product distilled water and ethyl alcohol are alternately cleaned up, dry 8h, obtains Bi at a temperature of 60 DEG C2O2CO3
Photochemical catalyst.
A kind of Fe according to made from above-mentioned preparation method adulterates Bi2O2CO3Photochemical catalyst.
Embodiment 3
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：
S1, by 0.9gBi (NO3)39mlN is dissolved in 0.25g sodium citrates, in dinethylformamide, obtains reacting molten
Liquid.
S2,0.05gFe (NO are added in into reaction solution3)3, it stirs evenly, adds in the ammonium hydroxide that 4ml mass concentrations are 30%,
Obtain reaction mixture.
S3, reaction mixture is transferred in water heating kettle, 9h is kept the temperature at a temperature of 185 DEG C, separation of solid and liquid after cooling obtains
Head product.
S4, head product distilled water and ethyl alcohol are alternately cleaned up, dry 9h, obtains Bi at a temperature of 55 DEG C2O2CO3
Photochemical catalyst.
A kind of Fe according to made from above-mentioned preparation method adulterates Bi2O2CO3Photochemical catalyst.
Embodiment 4
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：
S1, by 1.1gBi (NO3)311mlN is dissolved in 0.35g sodium citrates, in dinethylformamide, obtains reacting molten
Liquid.
S2,0.05gFe (NO are added in into reaction solution3)3, it stirs evenly, adds in the ammonium hydroxide that 6ml mass concentrations are 30%,
Obtain reaction mixture.
S3, reaction mixture is transferred in water heating kettle, 8h is kept the temperature at a temperature of 190 DEG C, separation of solid and liquid after cooling obtains
Head product.
S4, head product distilled water and ethyl alcohol are alternately cleaned up, dry 8h, obtains Bi at a temperature of 60 DEG C2O2CO3
Photochemical catalyst.
A kind of Fe according to made from above-mentioned preparation method adulterates Bi2O2CO3Photochemical catalyst.
Embodiment 5
A kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, including：
S1, by 1.2gBi (NO3)312mlN is dissolved in 0.45g sodium citrates, in dinethylformamide, obtains reacting molten
Liquid.
S2,0.15gFe (NO are added in into reaction solution3)3, it stirs evenly, adds in the ammonium hydroxide that 8ml mass concentrations are 25%,
Obtain reaction mixture.
S3, reaction mixture is transferred in water heating kettle, 10h is kept the temperature at a temperature of 180 DEG C, separation of solid and liquid after cooling obtains
To head product.
S4, head product distilled water and ethyl alcohol are alternately cleaned up, dry 7h, obtains Bi at a temperature of 65 DEG C2O2CO3
Photochemical catalyst.
A kind of Fe according to made from above-mentioned preparation method adulterates Bi2O2CO3Photochemical catalyst.
Bi is adulterated with Fe made from embodiment 12O2CO3Photochemical catalyst is as test example, with conventional Bi2O2CO3Photocatalysis
Agent is as a comparison case.
Electron-microscope scanning analysis is carried out to test example and comparative example.Fig. 1 is the scanning electron microscope (SEM) photograph of comparative example, conventional
Bi2O2CO3The structure of photochemical catalyst is flower-like microsphere.Fig. 2 is the scanning electron microscope (SEM) photograph of test example, doped with Fe in the test example3+'s
Bi2O2CO3The structure of photochemical catalyst is the cyclic annular microballoon similar to comparative example.Illustrate in test example doped with Fe3+Bi2O2CO3
Conventional Bi in photochemical catalyst and comparative example2O2CO3Photochemical catalyst has similar microstructure.
Meanwhile it can be seen that in test example doped with Fe according to Fig. 1 and Fig. 23+Bi2O2CO3The bouquet of photochemical catalyst half
Diameter is significantly less than Bi conventional in comparative example2O2CO3The bouquet radius of photochemical catalyst, illustrates preparation method system provided by the invention
The Fe doping Bi obtained2O2CO3Photochemical catalyst has smaller grain size, larger specific surface area, is conducive to improve the photocatalysis of product
Performance.
X-ray diffraction analysis is carried out to test example and comparative example, obtained Fig. 3 is the XRD spectrum of test example and comparative example,
Fig. 4 is test example in Fig. 3 and comparative example in 2 θ=30.2oThe amplification collection of illustrative plates at place.
From the figure 3, it may be seen that doped with Fe in test example3+Bi2O2CO3Conventional Bi in photochemical catalyst and comparative example2O2CO3Light
All diffraction maximums of catalyst all correspond to tetragonal phase Bi2O2CO3(JCPDSNo41-1488), there is no other miscellaneous peaks, explanations
The doping of Fe does not change Bi2O2CO3Crystal structure.
As shown in Figure 4, (010) diffraction maximum of 2 θ=30.2 ° is examined, is found in test example doped with Fe3+'s
Bi2O2CO3The peak of photochemical catalyst is relative to Bi conventional in comparative example2O2CO3The peak of photochemical catalyst, which has, a little to be deviated, this
It is due to Bi2O2CO3The big Bi3 of some radius in lattice+Ion is by the small Fe of radius3+Ion is substituted, and illustrates Fe3+From
Son enters Bi2O2CO3Lattice.
X-ray photoelectron spectroscopy analysis is carried out to test example, obtained Fig. 5 is the XPS High Resolution Spectrums of test example.
As shown in Figure 5, doped with Fe in test example3+Bi2O2CO3Two peaks of the Fe2p of photochemical catalyst, Fe2p3/2 exist
At 711.5eV, Fe2p1/2 is at 724eV, corresponding Fe3+Element chemistry state.Combination at its Fe2p3/2 peak can be apparent high
In Fe2O3Middle Fe3+Combination energy, again show that Fe3+Bi is substituted2O2CO3Bi in lattice3+。
UV-Vis DRS spectrum analysis is carried out to test example and comparative example, obtained Fig. 6 is test example and comparison
Outer-visible spectrogram that diffuses of example.
It will be appreciated from fig. 6 that Bi conventional in comparative example2O2CO3Photochemical catalyst does not absorb visible ray, and in test example doped with
Fe3+Bi2O2CO3Photochemical catalyst has apparent absorption between 400~600nm of wavelength, illustrates that the doping of Fe improves
Bi2O2CO3Absorption to visible ray.
The expression activitiy of degradation methyl orange is carried out to test example and comparative example, obtained Fig. 7 is test example and comparative example pair
The expression activitiy curve of methyl orange degradation.
As shown in Figure 7, Bi conventional in comparative example2O2CO3Photochemical catalyst almost non-degradable methyl orange after 2 hours, and
Doped with Fe in test example3+Bi2O2CO3Photochemical catalyst but degrades about 98% methyl orange, illustrates that the doping of Fe significantly carries
High Bi2O2CO3Visible light activity.
In conclusion the Fe doping Bi of the embodiment of the present invention2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3
Photochemical catalyst, by Fe3+Doping enters Bi2O2CO3Lattice in, Bi can be effectively improved2O2CO3Absorption to visible ray；Fe will be contained3 +Dopant be doped in alkali organic solvent solution, Fe3+In Bi2O2CO3Doping effect in lattice is good, the object of synthesis
The grain size of matter is small, large specific surface area.So as to effectively increase Bi2O2CO3Visible light photocatalysis active.
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 range 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, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of Fe adulterates Bi2O2CO3The preparation method of photochemical catalyst, which is characterized in that including：Fe will be contained3+Dopant molten
There are Bi (NO3)3And mixing in the alkali organic solvent solution of sodium citrate, hydro-thermal reaction is carried out under conditions of containing ammonium hydroxide.
2. preparation method according to claim 1, which is characterized in that the alkali organic solvent includes N, N- dimethyl methyls
Amide.
3. preparation method according to claim 1, which is characterized in that described to contain Fe3+Dopant be containing Fe3+It is inorganic
Salt；Preferably, to contain Fe3+Strong acid weak base salt；It is highly preferred that for Fe (NO3)3。
4. preparation method according to claim 1, which is characterized in that the mass concentration of the ammonium hydroxide is 25~35%；It is excellent
Selection of land is 25~30%；It is highly preferred that it is 28%.
5. according to Claims 1 to 4 any one of them preparation method, which is characterized in that the Bi (NO3)3, the citric acid
Sodium, the alkali organic solvent, it is described contain Fe3+Dopant and the ammonium hydroxide amount ratio be 0.8~1.2g：0.15~
0.45g：8~12ml：0.02g~0.15g：3~8ml.
6. preparation method according to claim 5, which is characterized in that the Bi (NO3)3, the sodium citrate, the alkali
Property organic solvent, it is described contain Fe3+Dopant and the ammonium hydroxide amount ratio be 0.9~1.1g：0.25~0.35g：9~
11ml：0.05g~0.15g：4~6ml.
7. preparation method according to claim 6, which is characterized in that the Bi (NO3)3, the sodium citrate, the alkali
Property organic solvent, it is described contain Fe3+Dopant and the ammonium hydroxide amount ratio be 0.97g：0.3g：10ml：0.1g：5ml.
8. preparation method according to claim 1, which is characterized in that the reaction temperature of hydro-thermal reaction is 170~190 DEG C,
Reaction time is 8~12h；Preferably, reaction temperature is 175~185 DEG C, and the reaction time is 9~11h；It is highly preferred that reaction temperature
It is 170 DEG C to spend, reaction time 10h.
9. preparation method according to claim 8, which is characterized in that washing and drying are further included after hydro-thermal reaction；It is preferred that
Ground, dry drying temperature are 55~65 DEG C, and drying time is 7~9h；It is highly preferred that drying temperature is 60 DEG C, drying time
For 8h.
10. Fe made from a kind of claim 1~9 any one of them preparation method adulterates Bi2O2CO3Photochemical catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810077487.1A CN108212187B (en) | 2018-01-26 | 2018-01-26 | Fe doped Bi2O2CO3Preparation method of photocatalyst and Fe-doped Bi2O2CO3Photocatalyst and process for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810077487.1A CN108212187B (en) | 2018-01-26 | 2018-01-26 | Fe doped Bi2O2CO3Preparation method of photocatalyst and Fe-doped Bi2O2CO3Photocatalyst and process for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108212187A true CN108212187A (en) | 2018-06-29 |
| CN108212187B CN108212187B (en) | 2021-02-19 |
Family
ID=62669129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810077487.1A Expired - Fee Related CN108212187B (en) | 2018-01-26 | 2018-01-26 | Fe doped Bi2O2CO3Preparation method of photocatalyst and Fe-doped Bi2O2CO3Photocatalyst and process for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108212187B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110575841A (en) * | 2019-09-11 | 2019-12-17 | 哈尔滨理工大学 | Novel photocatalyst material for degrading methylene blue light and preparation method thereof |
| CN112774706A (en) * | 2021-01-31 | 2021-05-11 | 湖南科技大学 | Bismuth oxycarbonate/sepiolite composite photocatalyst and preparation method thereof |
| CN112844410A (en) * | 2021-01-29 | 2021-05-28 | 武汉理工大学深圳研究院 | Preparation method and application of nickel ion modified bismuth oxysulfide photocatalyst |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101204648A (en) * | 2006-12-20 | 2008-06-25 | 中国科学院金属研究所 | Method for preparing photocatalyst doping with mesopore nanometer titanium oxide |
| CN103253714A (en) * | 2013-05-28 | 2013-08-21 | 江苏科技大学 | Method for preparing chalcopyrite type CuInxFe(1-x)S2 nano crystals through Fe doping |
| CN103464138A (en) * | 2013-08-15 | 2013-12-25 | 陕西科技大学 | Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof |
| CN104190397A (en) * | 2014-07-21 | 2014-12-10 | 浙江大学 | High specific surface area metal doped oxide hollow nanosphere and preparation method thereof |
| CN105749945A (en) * | 2016-03-16 | 2016-07-13 | 湖北文理学院 | Fe(III)/Bi2O2CO3 photocatalyst preparation method |
-
2018
- 2018-01-26 CN CN201810077487.1A patent/CN108212187B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101204648A (en) * | 2006-12-20 | 2008-06-25 | 中国科学院金属研究所 | Method for preparing photocatalyst doping with mesopore nanometer titanium oxide |
| CN103253714A (en) * | 2013-05-28 | 2013-08-21 | 江苏科技大学 | Method for preparing chalcopyrite type CuInxFe(1-x)S2 nano crystals through Fe doping |
| CN103464138A (en) * | 2013-08-15 | 2013-12-25 | 陕西科技大学 | Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof |
| CN104190397A (en) * | 2014-07-21 | 2014-12-10 | 浙江大学 | High specific surface area metal doped oxide hollow nanosphere and preparation method thereof |
| CN105749945A (en) * | 2016-03-16 | 2016-07-13 | 湖北文理学院 | Fe(III)/Bi2O2CO3 photocatalyst preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 强小丹等: ""Fe3+掺杂Bi2MoO6光催化剂的合成及其活性研究"", 《应用化工》 * |
| 穆劲等: "《高等无机化学》", 31 July 2007 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110575841A (en) * | 2019-09-11 | 2019-12-17 | 哈尔滨理工大学 | Novel photocatalyst material for degrading methylene blue light and preparation method thereof |
| CN112844410A (en) * | 2021-01-29 | 2021-05-28 | 武汉理工大学深圳研究院 | Preparation method and application of nickel ion modified bismuth oxysulfide photocatalyst |
| CN112774706A (en) * | 2021-01-31 | 2021-05-11 | 湖南科技大学 | Bismuth oxycarbonate/sepiolite composite photocatalyst and preparation method thereof |
| CN112774706B (en) * | 2021-01-31 | 2023-10-24 | 湖南科技大学 | Bismuth oxide carbonate/sepiolite composite photocatalyst and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108212187B (en) | 2021-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108212187A (en) | Fe adulterates Bi2O2CO3Preparation method and Fe the doping Bi of photochemical catalyst2O2CO3Photochemical catalyst | |
| CN105935594B (en) | A kind of bismuth oxyiodide/nitrogen mixes graphene composite photocatalyst and preparation method thereof | |
| CN105148966B (en) | Carbon quantum dot grafted hydroxyapatite photocatalysis material preparation method | |
| CN102320662A (en) | Cesium tungsten bronze powder and preparation method thereof | |
| Zhang et al. | Novel La-doped Bi 2 WO 6 photocatalysts with enhanced visible-light photocatalytic activity | |
| CN104801292B (en) | A kind of preparation method of zinc-oxide nano hollow ball/graphene composite material | |
| CN101993043A (en) | Visible light photocatalyst of BiOBr micro sphere and preparation method thereof | |
| CN103420414B (en) | Solvothermal preparation method of bismuth trioxide microspheres and application thereof | |
| CN106215958A (en) | A kind of preparation method of the catalysis material of reusable edible | |
| CN106944074B (en) | A kind of visible-light response type composite photo-catalyst and its preparation method and application | |
| CN101791548A (en) | Visible light catalyst BiVO4 and preparation method thereof | |
| CN107774294A (en) | A kind of novel photochemical catalyst K g C3N4And its prepare and apply | |
| CN105384193A (en) | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst | |
| CN103111335B (en) | Ionic crystal type visible-light-induced photocatalyst based on Dawson type poly-tungstate and preparation method thereof | |
| CN108993538A (en) | A kind of preparation method of rhenium disulfide nanometer sheet/titanium dioxide nanofiber composite photocatalyst material | |
| CN105032397A (en) | Method for synthesizing bismuth vanadate photocatalyst through starch self-combustion | |
| CN106582722A (en) | Composite photocatalysis system, and preparation method and application thereof | |
| CN107597134A (en) | A kind of preparation method of Cu doping BiVO4 porous nanotube photochemical catalysts | |
| Zhao et al. | Synthesis of bismuth oxyiodide/kaolinite composite with enhanced photocatalytic activity | |
| CN113663685B (en) | Synthesis method and photocatalytic application of broadband composite photocatalyst | |
| CN103785425B (en) | A kind of flower-shaped Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst and application | |
| CN111054413A (en) | Ternary composite multi-effect photocatalyst and preparation method thereof | |
| CN106881118B (en) | A kind of method of ion-exchange synthesis heterojunction photocatalyst | |
| CN109382088A (en) | SnO2/ α~Bi2O3/ β~Bi2O3Composite material and preparation method | |
| CN103769175A (en) | Preparation method and application of composite photocatalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210219 Termination date: 20220126 |