CN105457662B - A kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material and preparation method thereof - Google Patents
A kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material and preparation method thereof Download PDFInfo
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- CN105457662B CN105457662B CN201510988976.9A CN201510988976A CN105457662B CN 105457662 B CN105457662 B CN 105457662B CN 201510988976 A CN201510988976 A CN 201510988976A CN 105457662 B CN105457662 B CN 105457662B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 64
- 239000007787 solid Substances 0.000 claims abstract description 61
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 235000019441 ethanol Nutrition 0.000 claims abstract description 27
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 31
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 20
- 239000012265 solid product Substances 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 13
- 238000001291 vacuum drying Methods 0.000 claims description 12
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 10
- 239000001358 L(+)-tartaric acid Substances 0.000 claims description 10
- 235000011002 L(+)-tartaric acid Nutrition 0.000 claims description 10
- FEWJPZIEWOKRBE-LWMBPPNESA-N L-(+)-Tartaric acid Natural products OC(=O)[C@@H](O)[C@H](O)C(O)=O FEWJPZIEWOKRBE-LWMBPPNESA-N 0.000 claims description 10
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 4
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 4
- -1 polytetrafluoroethylene Polymers 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 16
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 125000005909 ethyl alcohol group Chemical group 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000003643 water by type Substances 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 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 239000001048 orange dye Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002699 waste material Substances 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B01J35/33—
-
- B01J35/39—
Abstract
The present invention provides a kind of 3D bouquets structure BiOCl ZnFe2O4Composite photocatalyst material and its preparation, the present invention is using hydro-thermal method technology of preparing, first by a certain amount of Fe (NO3)3·9H2O solids and Zn (NO3)2·6H2O solids are added in deionized water, are stirred evenly, and add a certain amount of sodium hydroxide, are transferred in polytetrafluoroethylene (PTFE) in the reaction kettle in village, are reacted in 180 DEG C of baking ovens for 24 hours after being vigorously stirred a period of time, and product water and ethyl alcohol are dried in vacuo to obtain Zn after washing2Fe2O4Powder sample, then, by the Zn of preparation2Fe2O4Powder and BiCl3Solid, which is added in absolute ethyl alcohol, to be disperseed, and is added in after sodium hydroxide solution is mixed and is transferred in polytetrafluoroethylene (PTFE) in the reaction kettle in village, 4h is reacted in 160 DEG C of baking ovens, product water and ethyl alcohol are dried in vacuo to obtain 3D bouquet structure BiOCl Zn after washing2Fe2O4Composite photocatalyst material；The present invention structure flower-shaped 3D structure, visible lights catalyst system of class, the absorption region of visible ray is enhanced by forming heterojunction structure, and catalytic effect is much larger than the catalytic performance of each monomer.
Description
Technical field
The present invention relates to a kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material and its preparation belong to nano combined
Field of material preparation.
Background technology
Environmental pollution and energy shortage are the world today's two big main problems urgently to be resolved hurrily.Photocatalytic Oxidation With Semiconductors skill
Art has become environmental improvement and solar energy converts a very active research direction of field, because photocatalysis oxidation technique has
Efficiently, energy saving, nontoxic, contaminant degradation is thoroughly and the advantages that non-secondary pollution.
The metal composite oxide of spinel structure, it is special due to its structure, there are many performances, metallurgy, electronics,
The fields such as chemical industry all have been widely used, and can be used as magnetic material, absorbing material, sensing material, battery cathode material
With high temperature engineering material etc..BiOCl is ground in recent years as a kind of conductor photocatalysis material for having good photocatalytic activity
The highest attention for the person of studying carefully；BiOCl is indirect band-gap semiconductor, has the layer structure of height anisotropic, the two are apparent
Advantage can promote efficiently separating for light induced electron and hole, make it have preferable photocatalytic activity.
Some researches show that two kinds of semiconductor couplings can improve the photocatalysis quantum efficiency of certain semiconductor, pass through two kinds
Semiconductors coupling forms hetero-junctions, can utilize the complementarity of two kinds of semiconductor energy level structures, i.e. between two kinds of semi-conducting materials
Energy level difference efficiently separate charge, achieve the purpose that promote light induced electron and hole to detaching, shifting and transmit, so as to press down
Light induced electron processed and hole it is compound；Simultaneously it is also possible to increase the stability of semiconductor light-catalyst.
Based on above analysis, bonded spinel stone structure ZnFe2O4With the respective advantage of BiOCl materials, hydro-thermal method is utilized to prepare 3D
Structure BiOCl-ZnFe2O4Composite photocatalyst material has very strong magnetism, is easily recycled；Meanwhile, it is capable to promote photoproduction
Electrons and holes inhibit light induced electron and compound, the catalytic under more advantageous visible ray in hole to detaching, shifting and transmit
Can, and stability enhances.
Invention content
Present invention aims at a kind of mild easy hydro-thermal method the preparation method has been used, a kind of 3D bouquets structure is obtained
BiOCl-ZnFe2O4Composite visible light catalysis material.The present invention structure flower-shaped 3D structure, visible lights catalyst system of class, passes through
The absorption region that heterojunction structure enhances visible ray is formed, catalytic effect is much larger than the catalytic performance of each monomer.
Technical scheme is as follows：
A kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material, which is characterized in that the amount ratio including substance is
4:1~1:2 BiOCl, ZnFe2O4, the ZnFe2O4Particle is wrapped in pattern as on 3D structure flower ball-shapeds BiOCl.
The 3D bouquet structures BiOCl-ZnFe2O4The preparation method of composite photocatalyst material, which is characterized in that including
Following steps：
(1) Fe (NO are weighed3)3·9H2O solids and Zn (NO3)2·6H2O solids are added to dissolving in deionized water and are mixed
Solution is closed, magnetic agitation is uniformly mixed；Add in L (+) tartaric acid solid thereto again, continuing stirring makes it fully react；Again to
Sodium hydrate solid is wherein added in, stirring makes it fully react；Mixed liquor is transferred in hydrothermal reaction kettle and is reacted, obtains solid
Product is washed with brand-new deionized water and ethyl alcohol, and vacuum drying obtains ZnFe2O4Powder；
(2) the preparation ZnFe in step (1) is weighed2O4Powder, BiCl3Solid, which is distributed in absolute ethyl alcohol, obtains suspension A,
It weighs NaOH solids and is dissolved in distilled water obtaining solution B, suspension A mix with solution B, stir after it is made fully to react, will mix
It closes liquid and is transferred in hydrothermal reaction kettle and react, obtain solid product, washed with brand-new deionized water and ethyl alcohol, vacuum drying obtains
BiOCl-ZnFe2O4Powder.
Further, in the step (1), the Fe (NO3)3·9H2O、Zn(NO3)2·6H2O, L (+) tartaric acid, hydrogen
The amount ratio of the substance of sodium oxide molybdena is 2:1:1:3.1, Fe (NO in mixed liquor3)3·9H2A concentration of 0.1g/mL of O.
Further, in the step (2), ZnFe2O4Powder and BiCl3The amount ratio of solid matter is 2:1~1:4,
BiCl3The amount of the substance of solid and NaOH solids is than 1:2.
Further, step (1) mixed liquor be transferred to the condition of reaction kettle for 180 DEG C~200 DEG C reaction 12h~
24h。
Further, the condition that step (2) mixed liquor is transferred to reaction kettle is 160 DEG C~180 DEG C reaction 3h~6h.
Further, the step (1), (2) vacuum drying are dry at less than 100 DEG C.
Further, brand-new deionized water and ethyl alcohol respectively wash three times wherein in step (1), (2).
The technological merit of the present invention：
Prepared composite photo-catalyst can promote light induced electron and hole to detaching, shifting and transmit in the present invention,
And inhibit light induced electron and compound, the catalytic performance under more advantageous visible ray in hole；Meanwhile it is prepared using hydro-thermal method used
Equipment is simple, does not need to high temperature, lower cost mass production, and agents useful for same is environmentally safe, and prepared catalysis
Agent has very ferromagnetism, is easily recycled.
Description of the drawings
BiOCl, ZnFe of Fig. 1 present invention2O4、BiOCl-ZnFe2O4Composite photo-catalyst XRD diagram.
BiOCl, ZnFe of Fig. 2 present invention2O4、BiOCl-ZnFe2O4The infrared figure of composite photo-catalyst Fourier.
BiOCl, BiOCl-ZnFe of Fig. 3 present invention2O4Composite photo-catalyst SEM schemes.
BiOCl, ZnFe2O4, BiOCl-ZnFe2O4 composite photo-catalyst light degradation design sketch of Fig. 4 present invention.
The BiOCl-ZnFe of Fig. 5 present invention2O4Magnetic recovery figure after composite photo-catalyst reaction.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment the present invention is further illustrated, but protection scope of the present invention is simultaneously
It is without being limited thereto.
Embodiment 1：
(1) Fe (NO are weighed3)3·9H2O solid masses is 4.04g and Zn (NO3)2·6H2O solid masses is added in for 1.49g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 1.92g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 4.4g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Middle reaction obtains solid product afterwards for 24 hours, is respectively washed three times with brand-new deionized water and ethyl alcohol, and 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 1.0g, BiCl3Solid masses is distributed to for 1.58g
In 35mL absolute ethyl alcohols suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.4g, will be suspended
Liquid A is mixed with solution B, and stirring makes it fully react 30min, mixed liquor is transferred to after reacting 4h in 160 DEG C of reaction kettles and obtained
Solid product washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
As a control test, BiOCl white powders are prepared according to the generous method of preparation BiOCl white powders in step (2)：Claim
Take BiCl3Solid masses is distributed in 35mL absolute ethyl alcohols for 1.58g and obtains suspension A, and it is molten for 0.4g to weigh NaOH solid masses
Solution B is obtained in 30mL distilled water, suspension A is mixed with solution B, stirring makes it fully react 30min, and mixed liquor is shifted
Solid product is obtained after reacting 4h into 160 DEG C of reaction kettles, washs each washing three times with brand-new deionized water and ethyl alcohol, vacuum is done
It is dry to obtain BiOCl white powder samples.
The ZnFe that will be prepared in the present embodiment2O4Powder, BiOCl white powders, BiOCl-ZnFe2O4Powder is XRD respectively
Difraction spectrum, the XRD diagram of gained is as shown in Figure 1, BiOCl and ZnFe as seen from Figure 12O4Characteristic diffraction peak, and
BiOCl-ZnFe2O4BiOCl and ZnFe can be seen in composite photo-catalyst XRD spectrum simultaneously2O4Characteristic diffraction peak.
ZnFe obtained2O4Powder, BiOCl white powders, BiOCl-ZnFe2O4Powder does FTIR spectrum respectively
As shown in Fig. 2, BiOCl has obvious characteristic peak, ZnFe when velocity of wave is 1043 as seen from Figure 22O4Have when velocity of wave is 808 bright
Aobvious characteristic peak, BiOCl-ZnFe2O4It can clearly be seen that BiOCl and ZnFe in composite catalyst FT-IR collection of illustrative plates2O4Characteristic peak, i.e.,
There is obvious characteristic peak to have obvious characteristic peak when velocity of wave is 1043 again when velocity of wave is 808.
Fig. 1, Fig. 2 the result shows that 3D bouquets structure BiOCl-ZnFe of the present invention2O4The system of composite photocatalyst material
Preparation Method, which is made in product, contains BiOCl and ZnFe2O4。
The SEM of sample obtained is schemed as shown in figure 3, the SEM figures that Fig. 3 (a) is BiOCl are 3D flower ball-shapeds, and Fig. 3 (b) is
BiOCl-ZnFe2O4The SEM spectrum of composite photo-catalyst, it can be seen that many micrograined textures of outer layer covers are grown in flower ball-shaped
On BiOCl, BiOCl and ZnFe is further illustrated2O4Compound success.
BiOCl, ZnFe obtained in 0.1g the present embodiment are weighed respectively2O4、BiOCl-ZnFe2O4Composite photo-catalyst, profit
Photoactivation reaction instrument carries out degradation experiment, observes the catalytic action that three kinds of catalyst degrade to methyl orange dye with this, Fig. 4 is
The light degradation design sketch of the degradation methyl orange dye of different catalysts is added in, as seen from Figure 4 in methyl orange dye blank test
It is more stable under illumination, essentially unchangedization；ZnFe2O4The degradation rate for methyl orange dye of degrading is 13%；BiOCl degradation methyl oranges
The degradation rate of dyestuff is 57%；BiOCl-ZnFe2O4Composite photocatalyst for degrading rate is up to 89%；Illustrate prepared by the present invention
BiOCl-ZnFe2O4Composite photocatalyst for degrading effect is good.
The BiOCl-ZnFe that will be thrown in above-mentioned light degradation system using magnet2O4Composite photo-catalyst is useless after reaction
It is recycled in water shown in front and rear waste liquid transparency figure such as Fig. 5 (a), Fig. 5 (b), magnetic recovery COMPARATIVE CATALYST figure shown in fig. 5 is said
The bright BiOCl-ZnFe2O4Composite catalyst has preferable magnetic.
Embodiment 2：
(1) Fe (NO are weighed3)3·9H2O solid masses is 4.04g and Zn (NO3)2·6H2O solid masses is added in for 1.49g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 1.92g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 4.4g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Middle reaction obtains solid product afterwards for 24 hours, is respectively washed three times with brand-new deionized water and ethyl alcohol, and 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 0.5g, BiCl3Solid masses is distributed to for 1.58g
In 35mL absolute ethyl alcohols suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.4g, will be suspended
Liquid A is mixed with solution B, and stirring makes it fully react 30min, mixed liquor is transferred to after reacting 4h in 160 DEG C of reaction kettles and obtained
Solid product washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
Embodiment 3：
(1) Fe (NO are weighed3)3·9H2O solid masses is 4.04g and Zn (NO3)2·6H2O solid masses is added in for 1.49g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 1.92g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 4.4g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Solid product is obtained after middle reaction 12h, is respectively washed three times with brand-new deionized water and ethyl alcohol, 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 0.5g, BiCl3Solid masses is distributed to for 1.58g
In 35mL absolute ethyl alcohols suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.4g, will be suspended
Liquid A is mixed with solution B, and stirring makes it fully react 30min, mixed liquor is transferred to after reacting 4h in 160 DEG C of reaction kettles and obtained
Solid product washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
Embodiment 4
(1) Fe (NO are weighed3)3·9H2O solid masses is 4.04g and Zn (NO3)2·6H2O solid masses is added in for 1.49g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 1.92g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 4.4g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Solid product is obtained after middle reaction 12h, is respectively washed three times with brand-new deionized water and ethyl alcohol, 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 0.5g, BiCl3Solid masses is distributed to for 1.58g
In 35mL absolute ethyl alcohols suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.4g, will be suspended
Liquid A is mixed with solution B, and stirring makes it fully react 30min, mixed liquor is transferred to after reacting 3h in 160 DEG C of reaction kettles and obtained
Solid product washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
Embodiment 5
(1) Fe (NO are weighed3)3·9H2O solid masses is 4.04g and Zn (NO3)2·6H2O solid masses is added in for 1.49g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 1.92g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 4.4g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Solid product is obtained after middle reaction 12h, is respectively washed three times with brand-new deionized water and ethyl alcohol, 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 0.5g, BiCl3Solid masses is distributed to for 0.79g
In 35mL absolute ethyl alcohols suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.2g, will be suspended
Liquid A is mixed with solution B, and stirring makes it fully react 30min, mixed liquor is transferred to after reacting 4h in 160 DEG C of reaction kettles and obtained
Solid product washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
Embodiment 6
(1) Fe (NO are weighed3)3·9H2O solid masses is 2.02g and Zn (NO3)2·6H2O solid masses is added in for 0.75g
Into 40mL deionized waters, dissolving obtains mixed solution, and magnetic agitation is uniformly mixed；It is slowly added to L (+) tartaric acid thereto again
Solid 0.96g is slowly added to after finishing, and continuing stirring makes it fully react；It is slowly added to NaOH solid 2.2g thereto again,
Increase magnetic agitation rotating speed, continuing stirring makes it fully react 30min, stirs evenly；Mixed liquor is transferred to 180 DEG C of reaction kettles
Solid product is obtained after middle reaction 12h, is respectively washed three times with brand-new deionized water and ethyl alcohol, 60 DEG C of vacuum is dried to obtain ZnFe2O4Powder
End.
(2) the preparation ZnFe in step (1) is weighed2O4Powder quality 1g, BiCl3Solid masses is distributed to 35mL for 0.79g
In absolute ethyl alcohol suspension A, weigh NaOH solid masses and be dissolved in 30mL distilled water obtaining solution B for 0.4g, by suspension A with
Solution B mixes, and stirring makes it fully react 30min, mixed liquor is transferred in 160 DEG C of reaction kettles after reacting 3h and obtains solid production
Object washs each washing three times with brand-new deionized water and ethyl alcohol, and vacuum drying obtains BiOCl-ZnFe2O4Powder.
The embodiment is the preferred embodiments of the present invention, but present invention is not limited to the embodiments described above, not
Away from the present invention substantive content in the case of, those skilled in the art can make it is any it is conspicuously improved, replace
Or modification all belongs to the scope of protection of the present invention.
Claims (8)
1.3D bouquet structures BiOCl-ZnFe2O4The preparation method of composite photocatalyst material, which is characterized in that include the following steps：
（1）Weigh Fe (NO3)3·9H2O solids and Zn (NO3)2·6H2O solids be added in deionized water dissolving obtain mixing it is molten
Liquid, magnetic agitation are uniformly mixed；Add in L (+) tartaric acid solid thereto again, continuing stirring makes it fully react；Again thereto
Sodium hydrate solid is added in, stirring makes it fully react；Mixed liquor is transferred in hydrothermal reaction kettle and is reacted, obtains solid production
Object is washed with brand-new deionized water and ethyl alcohol, and vacuum drying obtains ZnFe2O4Powder；
（2）Weigh step（1）In preparation ZnFe2O4Powder, BiCl3Solid, which is distributed in absolute ethyl alcohol, obtains suspension A, weighs
NaOH solids, which are dissolved in distilled water, obtains solution B, suspension A is mixed with solution B, after stirring makes it fully react, by mixed liquor
It is transferred in hydrothermal reaction kettle and reacts, obtain solid product, washed with brand-new deionized water and ethyl alcohol, vacuum drying obtains
BiOCl-ZnFe2O4Powder.
2. 3D bouquets structure BiOCl-ZnFe according to claim 12O4The preparation method of composite photocatalyst material, it is special
Sign is, the step（1）In, the Fe (NO3)3·9H2O、Zn(NO3)2·6H2O, the object of L (+) tartaric acid, sodium hydroxide
The amount ratio of matter is 2:1:1:3.1, Fe (NO in mixed liquor3)3·9H2A concentration of 0.1g/mL of O.
3. the preparation method of 3D bouquets structure BiOCl-ZnFe2O4 composite photocatalyst materials according to claim 1, special
Sign is, the step（2）In, ZnFe2O4Powder and BiCl3The amount ratio of solid matter is 2:1~1:4, BiCl3 Solid and NaOH
The amount of the substance of solid is than 1:2.
4. 3D bouquets structure BiOCl-ZnFe according to claim 12O4The preparation method of composite photocatalyst material, it is special
Sign is, the step（1）Mixed liquor is transferred to the condition of reaction kettle as 180 DEG C ~ 200 DEG C reaction 12h ~ for 24 hours.
5. 3D bouquets structure BiOCl-ZnFe according to claim 12O4The preparation method of composite photocatalyst material, it is special
Sign is, the step（2）The condition that mixed liquor is transferred to reaction kettle is 160 DEG C ~ 180 DEG C reaction 3h ~ 6h.
6. 3D bouquets structure BiOCl-ZnFe according to claim 12O4The preparation method of composite photocatalyst material, it is special
Sign is, the step（1）、（2）Vacuum drying is dry at less than 100 DEG C.
7. 3D bouquets structure BiOCl-ZnFe according to claim 12O4The preparation method of composite photocatalyst material, it is special
Sign is, wherein step（1）、（2）Brand-new deionized water and ethyl alcohol respectively wash three times.
8. 3D bouquet structures BiOCl-ZnFe prepared by a kind of any one of claim 1-7 preparation methods2O4Complex light is urged
Change material, which is characterized in that the amount ratio including substance is 4:1~1:2 BiOCl, ZnFe2O4, the ZnFe2O4Particle is wrapped in
Pattern is on 3D flower ball-shapeds BiOCl.
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| CN111672523B (en) * | 2020-06-08 | 2023-03-31 | 陕西工业职业技术学院 | Three-dimensional ZnFe 2 O 4 /BiOCl (001) composite photocatalyst and preparation method thereof |
| CN111715277B (en) * | 2020-06-22 | 2021-06-25 | 江南大学 | Easily-recycled magnetic visible-light-driven photocatalyst and preparation method thereof |
| CN111889063B (en) * | 2020-09-01 | 2021-09-28 | 福州大学 | BiOCl adsorbent, preparation method and application thereof in room temperature desulfurization |
| CN113145143A (en) * | 2021-02-26 | 2021-07-23 | 西南交通大学 | ZnFe2O4BiOBr photocatalytic composite material and preparation method thereof |
| CN113441141B (en) * | 2021-06-29 | 2023-09-08 | 辽宁大学 | BiOBr/MgFe 2 O 4 Catalyst, preparation method and application thereof |
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