CN105457662A - 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and preparation method thereof - Google Patents
3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and preparation method thereof Download PDFInfo
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- CN105457662A CN105457662A CN201510988976.9A CN201510988976A CN105457662A CN 105457662 A CN105457662 A CN 105457662A CN 201510988976 A CN201510988976 A CN 201510988976A CN 105457662 A CN105457662 A CN 105457662A
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 24
- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 7
- 230000001699 photocatalysis Effects 0.000 title abstract description 10
- 238000007146 photocatalysis Methods 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 73
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 67
- 239000007787 solid Substances 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 235000019441 ethanol Nutrition 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims abstract 2
- 238000003756 stirring Methods 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 239000011941 photocatalyst Substances 0.000 claims description 26
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 25
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 18
- 239000012265 solid product Substances 0.000 claims description 17
- 238000013019 agitation Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 11
- 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
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 2
- -1 polytetrafluoroethylene Polymers 0.000 abstract 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 2
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 2
- 230000000694 effects Effects 0.000 abstract 1
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 abstract 1
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 206010013786 Dry skin Diseases 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 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
- 239000001048 orange dye Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 3
- 230000008901 benefit Effects 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
- 230000000593 degrading effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 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
- 239000011358 absorbing material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application 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
- 238000004134 energy conservation Methods 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
- NNGHIEIYUJKFQS-UHFFFAOYSA-L hydroxy(oxo)iron;zinc Chemical compound [Zn].O[Fe]=O.O[Fe]=O NNGHIEIYUJKFQS-UHFFFAOYSA-L 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention provides a 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and preparation thereof. By adopting a hydrothermal-method preparation process, firstly, a certain amount of Fe(NO3)3*9H2O solid and Zn(NO3)2*6H2O solid are added into de-ionized water and are uniformly stirred; then a certain amount of sodium hydroxide is added and is violently stirred for a period of time; then the mixture is transferred into a reaction kettle with a polytetrafluoroethylene lining, and reacts in a drying oven at 180 DEG C for 24 hours; a product is washed with water and ethanol, and then is dried in vacuum to obtain a Zn2Fe2O4 powder sample; then the prepared Zn2Fe2O4 powder and a BiCl3 solid are added into absolute ethyl alcohol to be dispersed, a sodium hydroxide solution is added and the materials are mixed and stirred; then the mixture is transferred into the reaction kettle with the polytetrafluoroethylene lining and reacts in a drying oven at 160 DEG C for 4 hours; and a product is washed with the water and the ethanol and then is dried in vacuum to obtain the 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material. According to the 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and the preparation thereof, a flower-shape-like 3D structured visible light catalyst system is constructed, an absorption range of visible light is enhanced through forming a heterojunction structure, and the catalysis effect is much better than the catalysis performance of each monomer.
Description
Technical field
The present invention relates to a kind of 3D bouquet structure BiOCl-ZnFe
2o
4composite photocatalyst material and preparation thereof, belong to Nano-composite materials field.
Background technology
Environmental pollution and energy shortage are the world today's two large subject matters urgently to be resolved hurrily.Photocatalytic Oxidation With Semiconductors technology has become a very active research direction of environmental improvement and solar energy converting field, because photocatalysis oxidation technique has efficient, energy-conservation, nontoxic, contaminant degradation thoroughly and the advantage such as non-secondary pollution.
The composite metal oxide of spinel structure, special due to its structure, there is a lot of performance, all have been widely used in fields such as metallurgy, electronics, chemical industry, can as magnetic material, absorbing material, sensing material, battery cathode material and high temperature engineering material etc.BiOCl, as a kind of conductor photocatalysis material having good photocatalytic activity, is subject to showing great attention to of researchers in recent years; BiOCl is indirect band-gap semiconductor, and have the layer structure of height anisotropic, these two clear superiorities can promote that light induced electron is separated with the effective of hole, make it have good photocatalytic activity.
There are some researches show, two kinds of semiconductor couplings can improve the photocatalysis quantum efficiency of certain semiconductor, hetero-junctions is formed by two kinds of semiconductors coupling, the complementarity of two kinds of semiconductor energy level structures can be utilized, namely the effective separated charge of energy level difference between two kinds of semi-conducting materials, reach and promote light induced electron with hole to the object being separated, shifting and transmit, thus the compound in light induced electron and hole can be suppressed; Meanwhile, the stability of semiconductor light-catalyst may also be increased.
Based on above analysis, bonded spinel stone structure ZnFe
2o
4with BiOCl material advantage separately, hydro-thermal method is utilized to prepare 3D structure BiOCl-ZnFe
2o
4composite photocatalyst material, has very strong magnetic, is easy to recycle; Meanwhile, can promote that light induced electron and hole are to being separated, shifting and transmitting, and suppress the compound in light induced electron and hole, the catalytic performance under more favourable visible ray, and stability strengthens.
Summary of the invention
The object of the invention is to employ the easy hydro-thermal method preparation method of a kind of gentleness, obtains a kind of BiOCl-ZnFe of 3D bouquet structure
2o
4composite visible light catalysis material.The present invention builds class flower-shaped 3D structure, visible light catalyst system, and enhance the absorption region of visible ray by forming heterojunction structure, catalytic effect is much larger than the catalytic performance of each monomer.
Technical scheme of the present invention is as follows:
A kind of 3D bouquet structure BiOCl-ZnFe
2o
4composite photocatalyst material, is characterized in that, comprises amount of substance than BiOCl, the ZnFe for 4:1 ~ 1:2
2o
4, described ZnFe
2o
4it is on 3D structure flower ball-shaped BiOCl that particulate is wrapped in pattern.
Described 3D bouquet structure BiOCl-ZnFe
2o
4the preparation method of composite photocatalyst material, is characterized in that, comprises the following steps:
(1) Fe (NO is taken
3)
39H
2o solid and Zn (NO
3)
26H
2o solid joins in deionized water to dissolve and obtains mixed solution, and magnetic agitation mixes; Add L (+) tartaric acid solid more wherein, continue stirring and make it fully react; Add sodium hydrate solid wherein again, stir and make it fully react; Transferred in hydrothermal reaction kettle by mixed liquor and react, obtain solid product, with brand-new deionized water and ethanol washing, vacuum drying obtains ZnFe
2o
4powder;
(2) the preparation ZnFe in step (1) is taken
2o
4powder, BiCl
3suspension A is obtained in solid dispersal to absolute ethyl alcohol, take NaOH solid and to be dissolved in distilled water obtaining solution B, suspension A is mixed with solution B, after stirring makes it fully react, mixed liquor is transferred in hydrothermal reaction kettle and reacts, obtain solid product, with brand-new deionized water and ethanol washing, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Further, in described step (1), described Fe (NO
3)
39H
2o, Zn (NO
3)
26H
2the amount of substance of O, L (+) tartaric acid, NaOH is than being 2:1:1:3.1, Fe (NO in mixed liquor
3)
39H
2the concentration of O is 0.1g/mL.
Further, in described step (2), ZnFe
2o
4powder and BiCl
3the amount of solid matter is than being 2:1 ~ 1:4, BiCl
3solid compares 1:2 with the amount of substance of NaOH solid.
Further, the condition of reactor transferred to by described step (1) mixed liquor is 180 DEG C ~ 200 DEG C reaction 12h ~ 24h.
Further, the condition of reactor transferred to by described step (2) mixed liquor is 160 DEG C ~ 180 DEG C reaction 3h ~ 6h.
Further, described step (1), (2) vacuum drying are dry at lower than 100 DEG C.
Further, wherein step (1), (2) middle brand-new deionized water and ethanol respectively wash three times.
Technological merit of the present invention:
Composite photo-catalyst prepared in the present invention can promote that light induced electron and hole are to being separated, shifting and transmitting, and suppresses the compound in light induced electron and hole, the catalytic performance under more favourable visible ray; Meanwhile, adopt hydro-thermal method to prepare equipment used simple, do not need high temperature, lower cost is produced in a large number, and agents useful for same environmentally safe, and prepared catalyst has very ferromagnetism, is easy to reclaim.
Accompanying drawing explanation
Fig. 1 BiOCl, ZnFe of the present invention
2o
4, BiOCl-ZnFe
2o
4composite photo-catalyst XRD schemes.
Fig. 2 BiOCl, ZnFe of the present invention
2o
4, BiOCl-ZnFe
2o
4the infrared figure of composite photo-catalyst Fourier.
Fig. 3 BiOCl, BiOCl-ZnFe of the present invention
2o
4composite photo-catalyst SEM schemes.
Fig. 4 BiOCl, ZnFe2O4, BiOCl-ZnFe2O4 composite photo-catalyst of the present invention light degradation design sketch.
Fig. 5 BiOCl-ZnFe of the present invention
2o
4magnetic recovery figure after composite photo-catalyst reaction.
Detailed description of the invention
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
Embodiment 1:
(1) Fe (NO is taken
3)
39H
2o solid masses is 4.04g and Zn (NO
3)
26H
2o solid masses be 1.49g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 1.92g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 4.4g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 24h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 1.0g, BiCl
3solid masses is that 1.58g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 4h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Test in contrast, according to the generous legal system of preparation BiOCl white powder in step (2) for BiOCl white powder: take BiCl
3solid masses is that 1.58g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 4h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl white powder samples.
By the ZnFe prepared in the present embodiment
2o
4powder, BiOCl white powder, BiOCl-ZnFe
2o
4powder does XRD difraction spectrum respectively, and the XRD of gained schemes as shown in Figure 1, BiOCl and ZnFe as seen from Figure 1
2o
4characteristic diffraction peak, and at BiOCl-ZnFe
2o
4biOCl and ZnFe can be seen in composite photo-catalyst XRD collection of illustrative plates simultaneously
2o
4characteristic diffraction peak.
Obtained ZnFe
2o
4powder, BiOCl white powder, BiOCl-ZnFe
2o
4powder does FTIR spectrum as shown in Figure 2 respectively, and BiOCl has obvious characteristic peak when velocity of wave is 1043 as seen from Figure 2, ZnFe
2o
4obvious characteristic peak is had, BiOCl-ZnFe when velocity of wave is 808
2o
4obviously BiOCl and ZnFe can be seen in composite catalyst FT-IR collection of illustrative plates
2o
4not only characteristic peak, has obvious characteristic peak when velocity of wave is 808 but also has obvious characteristic peak when velocity of wave is 1043.
The result of Fig. 1, Fig. 2 shows 3D bouquet structure BiOCl-ZnFe of the present invention
2o
4the preparation method of composite photocatalyst material obtains in product containing BiOCl and ZnFe
2o
4.
As shown in Figure 3, Fig. 3 (a) is the SEM figure of BiOCl is 3D flower ball-shaped to the SEM figure of obtained sample, and Fig. 3 (b) is BiOCl-ZnFe
2o
4the SEM collection of illustrative plates of composite photo-catalyst, can see that a lot of micrograined texture growth of outer layer covers is on flower ball-shaped BiOCl, further illustrates BiOCl and ZnFe
2o
4compound success.
Take BiOCl, ZnFe obtained in 0.1g the present embodiment respectively
2o
4, BiOCl-ZnFe
2o
4composite photo-catalyst, light-catalyzed reaction instrument is utilized to carry out degradation experiment, the catalytic action that three kinds of catalyst degrade to methyl orange dye is observed with this, Fig. 4 is the light degradation design sketch of the degraded methyl orange dye adding different catalysts, more stable under illumination in methyl orange dye blank test as seen from Figure 4, basic no change; ZnFe
2o
4the degradation rate of degraded methyl orange dye is 13%; The degradation rate of BiOCl degraded methyl orange dye is 57%; BiOCl-ZnFe
2o
4composite photocatalyst for degrading rate is up to 89%; BiOCl-ZnFe prepared by the present invention is described
2o
4composite photocatalyst for degrading effect is good.
Use the BiOCl-ZnFe that magnet will be thrown in above-mentioned light degradation system
2o
4composite photo-catalyst is from the waste liquid transparency figure before and after reclaiming waste water after reaction as shown in Fig. 5 (a), Fig. 5 (b), and the magnetic recovery COMPARATIVE CATALYST shown in Fig. 5 schemes described BiOCl-ZnFe is described
2o
4composite catalyst has good magnetic.
Embodiment 2:
(1) Fe (NO is taken
3)
39H
2o solid masses is 4.04g and Zn (NO
3)
26H
2o solid masses be 1.49g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 1.92g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 4.4g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 24h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 0.5g, BiCl
3solid masses is that 1.58g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 4h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Embodiment 3:
(1) Fe (NO is taken
3)
39H
2o solid masses is 4.04g and Zn (NO
3)
26H
2o solid masses be 1.49g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 1.92g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 4.4g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 12h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 0.5g, BiCl
3solid masses is that 1.58g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 4h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Embodiment 4
(1) Fe (NO is taken
3)
39H
2o solid masses is 4.04g and Zn (NO
3)
26H
2o solid masses be 1.49g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 1.92g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 4.4g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 12h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 0.5g, BiCl
3solid masses is that 1.58g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 3h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Embodiment 5
(1) Fe (NO is taken
3)
39H
2o solid masses is 4.04g and Zn (NO
3)
26H
2o solid masses be 1.49g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 1.92g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 4.4g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 12h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 0.5g, BiCl
3solid masses is that 0.79g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.2g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 4h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Embodiment 6
(1) Fe (NO is taken
3)
39H
2o solid masses is 2.02g and Zn (NO
3)
26H
2o solid masses be 0.75g join in 40mL deionized water dissolve obtain mixed solution, magnetic agitation mixes; Slowly add L (+) tartaric acid solid 0.96g more wherein, slowly add complete after, continue stirring make it fully react; Slowly add NaOH solid 2.2g wherein again, increase magnetic agitation rotating speed, continue stirring and make it fully react 30min, stir; Obtain solid product after mixed liquor being transferred to 180 DEG C of reaction kettle for reaction 12h, respectively wash three times with brand-new deionized water and ethanol, vacuum 60 DEG C of dryings obtain ZnFe
2o
4powder.
(2) the preparation ZnFe in step (1) is taken
2o
4powder quality 1g, BiCl
3solid masses is that 0.79g to be distributed in 35mL absolute ethyl alcohol to obtain suspension A, taking NaOH solid masses is that 0.4g to be dissolved in 30mL distilled water obtaining solution B, suspension A is mixed with solution B, stirring makes it fully react 30min, solid product is obtained after mixed liquor being transferred to 160 DEG C of reaction kettle for reaction 3h, wash each washing three times by brand-new deionized water and ethanol, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.
Claims (8)
1. a 3D bouquet structure BiOCl-ZnFe
2o
4composite photocatalyst material, is characterized in that, comprises amount of substance than BiOCl, the ZnFe for 4:1 ~ 1:2
2o
4, described ZnFe
2o
4it is on 3D flower ball-shaped BiOCl that particulate is wrapped in pattern.
2. 3D bouquet structure BiOCl-ZnFe according to claim 1
2o
4the preparation method of composite photocatalyst material, is characterized in that, comprises the following steps:
Take Fe (NO
3)
39H
2o solid and Zn (NO
3)
26H
2o solid joins in deionized water to dissolve and obtains mixed solution, and magnetic agitation mixes; Add L (+) tartaric acid solid more wherein, continue stirring and make it fully react; Add sodium hydrate solid wherein again, stir and make it fully react; Transferred in hydrothermal reaction kettle by mixed liquor and react, obtain solid product, with brand-new deionized water and ethanol washing, vacuum drying obtains ZnFe
2o
4powder;
Take the preparation ZnFe in step (1)
2o
4powder, BiCl
3suspension A is obtained in solid dispersal to absolute ethyl alcohol, take NaOH solid and to be dissolved in distilled water obtaining solution B, suspension A is mixed with solution B, after stirring makes it fully react, mixed liquor is transferred in hydrothermal reaction kettle and reacts, obtain solid product, with brand-new deionized water and ethanol washing, vacuum drying obtains BiOCl-ZnFe
2o
4powder.
3. 3D bouquet structure BiOCl-ZnFe according to claim 2
2o
4the preparation method of composite photocatalyst material, is characterized in that, in described step (1), and described Fe (NO
3)
39H
2o, Zn (NO
3)
26H
2the amount of substance of O, L (+) tartaric acid, NaOH is than being 2:1:1:3.1, Fe (NO in mixed liquor
3)
39H
2the concentration of O is 0.1g/mL.
4. the preparation method of 3D bouquet structure BiOCl-ZnFe2O4 composite photocatalyst material according to claim 1, is characterized in that, in described step (2), and ZnFe
2o
4powder and BiCl
3the amount of solid matter is than comparing 1:2 for 2:1 ~ 1:4, BiCl3 solid with the amount of substance of NaOH solid.
5. 3D bouquet structure BiOCl-ZnFe according to claim 2
2o
4the preparation method of composite photocatalyst material, is characterized in that, the condition that reactor transferred to by described step (1) mixed liquor is 180 DEG C ~ 200 DEG C reaction 12h ~ 24h.
6. 3D bouquet structure BiOCl-ZnFe according to claim 2
2o
4the preparation method of composite photocatalyst material, is characterized in that, the condition that reactor transferred to by described step (2) mixed liquor is 160 DEG C ~ 180 DEG C reaction 3h ~ 6h.
7. 3D bouquet structure BiOCl-ZnFe according to claim 2
2o
4the preparation method of composite photocatalyst material, is characterized in that, described step (1), (2) vacuum drying are dry at lower than 100 DEG C.
8. 3D bouquet structure BiOCl-ZnFe according to claim 2
2o
4the preparation method of composite photocatalyst material, is characterized in that, wherein step (1), (2) brand-new deionized water and ethanol respectively wash three times.
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| CN111715277A (en) * | 2020-06-22 | 2020-09-29 | 江南大学 | Easily-recycled magnetic visible-light-driven photocatalyst and preparation method thereof |
| CN111889063A (en) * | 2020-09-01 | 2020-11-06 | 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 |
| CN113441141A (en) * | 2021-06-29 | 2021-09-28 | 辽宁大学 | BiOBr/MgFe2O4Catalyst, preparation method and application thereof |
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Cited By (10)
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| CN110038598A (en) * | 2019-03-27 | 2019-07-23 | 平顶山学院 | A kind of manufacturing method and its application of zinc ferrite/molybdenum disulfide composite photocatalyst material |
| CN111672523A (en) * | 2020-06-08 | 2020-09-18 | 陕西工业职业技术学院 | Three-dimensional ZnFe2O4/BiOCl (001) composite photocatalyst and preparation method thereof |
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| CN111715277B (en) * | 2020-06-22 | 2021-06-25 | 江南大学 | Easily-recycled magnetic visible-light-driven photocatalyst and preparation method thereof |
| CN111889063A (en) * | 2020-09-01 | 2020-11-06 | 福州大学 | BiOCl adsorbent, preparation method and application thereof in room temperature desulfurization |
| 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 |
| CN113441141A (en) * | 2021-06-29 | 2021-09-28 | 辽宁大学 | BiOBr/MgFe2O4Catalyst, preparation method and application 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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| CN105457662B (en) | 2018-06-26 |
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