CN112871213A - Bismuth ferrite composite photocatalytic material and preparation method thereof - Google Patents
Bismuth ferrite composite photocatalytic material and preparation method thereof Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 137
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 136
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002121 nanofiber Substances 0.000 claims abstract description 69
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000002105 nanoparticle Substances 0.000 claims abstract description 42
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 36
- 239000013110 organic ligand Substances 0.000 claims abstract description 17
- 150000003751 zinc Chemical class 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 43
- 239000000835 fiber Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- 238000010041 electrostatic spinning Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000013094 zinc-based metal-organic framework Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001523 electrospinning Methods 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 5
- 238000006557 surface reaction Methods 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 7
- 229960000907 methylthioninium chloride Drugs 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 5
- 229960000583 acetic acid Drugs 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 description 4
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 4
- 238000013032 photocatalytic reaction Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical compound C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
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- 239000011324 bead Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100001240 inorganic pollutant Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000004162 soil erosion Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
The invention belongs to the technical field of photocatalysis, and particularly relates to a bismuth ferrite composite photocatalytic material and a preparation method thereof. The preparation method of the bismuth ferrite composite photocatalytic material comprises the following steps: providing bismuth ferrite nanofibers; dissolving the bismuth ferrite nanofiber in a mixed solution containing zinc salt and imidazole organic ligands, and growing metal organic framework nano particles on the surface of the bismuth ferrite nanofiber to obtain the bismuth ferrite composite photocatalytic material. The bismuth ferrite composite photocatalytic material prepared by the preparation method can increase surface reaction active sites and improve photocatalytic activity, so that the bismuth ferrite composite photocatalytic material has better photocatalytic response and circulation stability characteristics under visible light and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to a bismuth ferrite composite photocatalytic material and a preparation method thereof.
Background
People also face the problems of environmental pollution and energy shortage when enjoying the benefits brought by modern industrial informatization. Among them, the ecological environment in which human beings live suffers from many phenomena such as soil erosion, garbage pollution, and excessive discharge of toxic and harmful pollutants. In the environmental protection measures, the traditional sewage treatment technologies such as physical and chemical methods, biochemical sedimentation methods, biological adsorption methods and the like have the defects of incomplete treatment, high treatment cost, secondary pollution in the treatment process and the like. With the discovery that the photocatalysis technology can effectively convert solar energy in nature into available chemical energy in the last 70 th century, people are continuously exploring how to utilize the continuous clean energy to be applied to environmental protection. The photocatalytic reaction is that a photocatalyst carries out oxidation-reduction reaction under the irradiation of sunlight to generate a series of active substances with strong oxidizing property. The photocatalytic technology decomposes various organic and inorganic pollutants in sewage into inorganic small molecules by active substances with strong oxidizing property generated by photocatalytic reaction. The application of the photocatalysis technology has the outstanding advantages of high efficiency, stability, no secondary pollution, reusable catalyst, suitability for degradation of various organic pollutants and the like.
In view of the above, bismuth ferrite is found to be a photocatalytic material capable of responding in visible light, but bismuth ferrite has the problems of few reactive active sites on the surface of the material and low separation efficiency of photon-generated carriers, thereby limiting the practical application of bismuth ferrite.
Therefore, the prior art is in need of improvement.
Disclosure of Invention
The invention aims to provide a bismuth ferrite composite photocatalytic material and a preparation method thereof, and aims to solve the technical problems of few reactive active sites on the surface of the existing bismuth ferrite and low separation efficiency of photon-generated carriers.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a bismuth ferrite composite photocatalytic material on the one hand, which comprises the following steps:
providing bismuth ferrite nanofibers;
dissolving the bismuth ferrite nanofiber in a mixed solution containing zinc salt and imidazole organic ligands, and growing metal organic framework nano particles on the surface of the bismuth ferrite nanofiber to obtain the bismuth ferrite composite photocatalytic material.
The invention also provides a bismuth ferrite composite photocatalytic material, which comprises bismuth ferrite nanofibers and metal-organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers.
According to the preparation method of the bismuth ferrite composite photocatalytic material, metal organic framework nano particles grow on the surface of the bismuth ferrite nano fibers, and the uniform diameter of the bismuth ferrite nano fibers can enable the metal organic framework materials of spherical nano particles to be uniformly distributed on the surface, so that the bismuth ferrite composite photocatalytic material is free of accumulation and agglomeration and has a complete structure; and the metal organic framework nano-particle material has the characteristics of ordered porous structure, high specific surface area, adjustable appearance and strong chemical adsorption capacity, can increase the surface reaction active sites of the bismuth ferrite composite photocatalytic material and improve the photocatalytic activity when growing on the surface of the bismuth ferrite nano-fiber, thereby having better photocatalytic response and cycle stability characteristics under visible light and having good application prospect.
The bismuth ferrite composite photocatalytic material provided by the invention comprises bismuth ferrite nanofibers and metal organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers. The bismuth ferrite nanofiber structure can be uniformly combined with metal organic framework nanoparticles; and the metal organic framework nano-particle material has the characteristics of ordered porous structure, high specific surface area, adjustable morphology and strong chemical adsorption capacity, and can increase the surface reaction active sites of the bismuth ferrite composite photocatalytic material and improve the photocatalytic activity under the synergistic effect of the two materials, so that the metal organic framework nano-particle material has the characteristics of better photocatalytic response and circulation stability under visible light and has good application prospect.
Drawings
FIG. 1 is a scanning electron microscope picture of a bismuth ferrite composite Zif-8 nanofiber photocatalytic material provided by an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
On one hand, the embodiment of the invention provides a preparation method of a bismuth ferrite composite photocatalytic material, which comprises the following steps:
s01: providing bismuth ferrite nanofibers;
s02: dissolving the bismuth ferrite nanofiber in a mixed solution containing zinc salt and imidazole organic ligands, and growing metal organic framework nano particles on the surface of the bismuth ferrite nanofiber to obtain the bismuth ferrite composite photocatalytic material.
According to the preparation method of the bismuth ferrite composite photocatalytic material provided by the embodiment of the invention, the metal organic framework nano particles grow on the surface of the bismuth ferrite nano fibers, and the uniform diameter of the bismuth ferrite nano fibers can enable the metal organic framework materials of the spherical nano particles to be uniformly distributed on the surface, so that the bismuth ferrite composite photocatalytic material is free of accumulation and agglomeration and has a complete structure; and the metal organic framework nano-particle material has the characteristics of ordered porous structure, high specific surface area, adjustable appearance and strong chemical adsorption capacity, can increase the surface reaction active sites of the bismuth ferrite composite photocatalytic material and improve the photocatalytic activity when growing on the surface of the bismuth ferrite nano-fiber, thereby having better photocatalytic response and cycle stability characteristics under visible light and having good application prospect.
In the step S01, the preparation method of the bismuth ferrite nanofiber comprises:
s011, preparing a precursor solution containing bismuth nitrate, ferric nitrate and polyvinylpyrrolidone;
s012, passing the precursor solution through an electrostatic spinning device to obtain initial bismuth ferrite nano-fibers;
s013 annealing the initial bismuth ferrite nanofiber to obtain the bismuth ferrite nanofiber.
Through the electrostatic spinning technology, a bismuth ferrite nanofiber sample can be obtained.
Further, the preparation of the precursor solution comprises: pouring bismuth nitrate pentahydrate and ferric nitrate nonahydrate with equal molar quantity into deionized water and glacial acetic acid solution, and stirring for 1-2h on a magnetic stirrer until solute is completely dissolved; then evenly mixing with the solution of polyvinylpyrrolidone in dimethyl amide.
Further, the parameters of the electrospinning device include: the fiber collecting distance is 12-18cm, the spinning voltage is 13-19kV, the advancing speed is 0.1-0.5mL/h, the humidity is less than 40% rh, and the temperature is 0-40 ℃. The diameter of the prepared fiber is smaller when the fiber collecting distance is longer and the spinning voltage is higher, and if the humidity is too large, the nano fiber is difficult to form, and the spinning needle is easy to block when the environmental temperature is too high or too low; therefore, under the conditions, the bismuth ferrite nano-fiber with the diameter of 150-300nm can be better formed.
Further, the conditions of the annealing treatment include: heating to 380-420 ℃ at the heating rate of 2-10 ℃/min, such as 400 ℃, and then preserving the heat for 2-4 h; when the annealing temperature is too low, the polyvinylpyrrolidone in the fiber is not completely decomposed, and the annealing temperature is too high, the fiber is easy to generate recrystallization phenomenon to cause the fiber to be in a bead shape, so the crystallization effect of the annealing condition is better. Before annealing treatment, drying the initial bismuth ferrite nano-fiber for 12-24h at 70-80 ℃; this allows for better removal of acetic acid and dimethyl amide from the original fiber.
In step S02, dissolving the bismuth ferrite nanofiber in a mixed solution containing a zinc salt and an imidazole organic ligand, and growing metal-organic framework nanoparticles on the surface of the bismuth ferrite nanofiber comprises:
s021, preparing a zinc salt solution and an imidazole organic ligand solution;
s022, mixing the zinc salt solution and the imidazole organic ligand solution to obtain a mixed solution;
s023, adding the bismuth ferrite nano-fiber into the mixed solution, sequentially carrying out magnetic stirring and ultrasonic treatment, and then carrying out drying treatment.
The metal organic framework has the characteristics of ordered porous structure, high specific surface area, adjustable appearance, strong chemical adsorption capacity and the like, and the embodiment of the invention designs that composite metal organic framework nano particles are grown on the surface of the bismuth ferrite nano fiber and can be obtained by combining the steps of an electrostatic spinning technology and an ultrasonic crystallization method. The performance detection of the bismuth ferrite composite photocatalytic material proves that the bismuth ferrite nanofiber composite metal organic framework nano-particles have more excellent photocatalytic performance.
Further, the zinc salt solution can be a zinc nitrate solution, and the imidazole organic ligand solution can be a 2-methylimidazole solution. Further, growing the zinc-based metal organic framework nano-particles according to the molar ratio of bismuth ferrite of the bismuth ferrite nano-fibers to the imidazole organic ligand of 1.3-1.8: 1. (further, the time of the magnetic stirring is 10-15min, under the condition, the bismuth ferrite nano-fiber is fully dispersed in the mixed solution, further, the time of the ultrasonic treatment is 0.5-1h, under the condition, the metal organic framework nano-particle can be better grown, further, the temperature of the drying treatment is 70-80 ℃, and the time is 12-24h, under the condition, the solvent can be better volatilized, and a dried finished product is obtained The zinc-based metal organic framework nano-particles with small particle size increase the specific surface area and improve the catalytic active sites.
On the other hand, the embodiment of the invention also provides a bismuth ferrite composite photocatalytic material, which comprises bismuth ferrite nanofibers and metal-organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers.
The bismuth ferrite composite photocatalytic material provided by the embodiment of the invention comprises bismuth ferrite nanofibers and metal-organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers. The bismuth ferrite nanofiber structure can be uniformly combined with metal organic framework nanoparticles; and the metal organic framework nano-particle material has the characteristics of ordered porous structure, high specific surface area, adjustable morphology and strong chemical adsorption capacity, and can increase the surface reaction active sites of the bismuth ferrite composite photocatalytic material and improve the photocatalytic activity under the synergistic effect of the two materials, so that the metal organic framework nano-particle material has the characteristics of better photocatalytic response and circulation stability under visible light and has good application prospect.
Specifically, the bismuth ferrite composite photocatalytic material catalyzes and removes methylene blue under a visible light source.
Specifically, the bismuth ferrite composite photocatalytic material is composed of bismuth ferrite nanofibers and metal organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers.
Specifically, the bismuth ferrite nanofiber is a bismuth ferrite electrostatic spinning fiber, and the diameter of the bismuth ferrite nanofiber is 150-300 nm; the metal organic framework nano-particles are zinc-based metal organic framework nano-particles, the particle size of the metal organic framework nano-particles is 30-100nm, the metal organic framework nano-particles with the particle size are combined on the surface of the bismuth ferrite nano-fiber, and the bismuth ferrite nano-fiber has the advantages of uniform appearance, small particle size, large specific surface area and more catalytic active sites.
Further, the metal organic framework nano-particles are prepared from zinc salt and imidazole organic ligands, and specifically, the composite proportion of the bismuth ferrite nano-fibers and the metal organic framework nano-particles is formed according to the molar ratio of the bismuth ferrite nano-fibers to the imidazole organic ligands used as raw materials for preparing the zinc-based metal organic framework nano-particles being 1.3-1.8: 1. The proportion can ensure that the zinc-based metal organic framework nano particles can uniformly grow on the surface of the bismuth ferrite nano fiber.
Further, the bismuth ferrite composite photocatalytic material is prepared by the preparation method of the bismuth ferrite composite photocatalytic material.
In one embodiment, the preparation method of the bismuth ferrite composite photocatalytic material comprises the following steps:
(1) weighing 1-5mmol of bismuth nitrate pentahydrate and equimolar ferric nitrate nonahydrate, pouring into a beaker filled with 4-5mL of deionized water and 3-5mL of glacial acetic acid solution, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
(2) weighing 0.8-1g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into a beaker filled with 10-12mL of dimethylformamide, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
(3) transferring the solution in the step (2) into the beaker in the step (1), and stirring for 6-12h on a magnetic stirrer until the solution is completely and uniformly mixed;
(4) transferring the precursor solution to a 20mL injector of an electrostatic spinning device, setting the fiber collection distance of the device to be 12-18cm, setting the spinning voltage to be 13-19kV, setting the advancing speed to be 0.1-0.5mL/h, controlling the humidity to be less than 40% rh and the temperature to be 0-40 ℃, and finally spinning a primary bismuth ferrite fiber sample;
(5) drying the primary bismuth ferrite fiber obtained in the step (4) in a drying box at 70-80 ℃ for 12-24 h;
(6) putting the dried sample obtained in the step (5) into a muffle furnace for annealing treatment, and setting the heating rate to be 2-10 ℃/min; keeping the temperature for 2-4h, and finally collecting to obtain bismuth ferrite fibers;
(7) weighing 1-2mmol of 2-methylimidazole, adding into a beaker filled with 14.3mL of methanol, and stirring for 1-2h in a magnetic stirrer until the 2-methylimidazole is completely dissolved;
(8) dispersing 1-2mmol of zinc nitrate hexahydrate in a beaker filled with methanol solution with the same volume, and stirring for 1-2 hours in a magnetic stirrer until the zinc nitrate hexahydrate is completely dissolved;
(9) pouring the solution in the step (7) into the beaker in the step (8), and stirring for 0.5-1h in a magnetic stirrer until the solution is uniformly mixed;
(10) adding 2-3mmol of bismuth ferrite fiber into the solution obtained in the step (9), stirring for 10-15min in a magnetic stirrer until the mixture is uniform, and transferring ultrasonic treatment for 0.5-1h to form a suspension;
(11) and (4) centrifugally washing the suspension obtained in the step (10), washing with methanol to obtain a sample, drying the sample in a drying oven at 70-80 ℃ for 12-24h, and collecting the sample to obtain the final sample.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
A bismuth ferrite composite Zif-8 photocatalytic material is prepared by the following steps:
step S01: weighing 1-5mmol of bismuth nitrate pentahydrate and equimolar ferric nitrate nonahydrate, pouring into a beaker filled with 4-5mL of deionized water and 3-5mL of glacial acetic acid solution, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
step S02: weighing 0.8-1g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into a beaker filled with 10-12mL of dimethylformamide, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
step S03: transferring the solution obtained in the step S02 to a beaker obtained in the step S01, and stirring the solution on a magnetic stirrer for 6 to 12 hours until the solution is completely and uniformly mixed;
step S04: transferring the precursor solution to a 20mL injector of an electrostatic spinning device, setting the fiber collection distance of the device to be 12-18cm, setting the spinning voltage to be 13-19kV, setting the advancing speed to be 0.1-0.5mL/h, controlling the humidity to be less than 40% rh and the temperature to be 0-40 ℃, and finally spinning a primary bismuth ferrite fiber sample;
step S05: drying the primary bismuth ferrite fiber obtained in the step S04 in a drying box at 70-80 ℃ for 12-24 h;
step S06: annealing the dried sample obtained in the step S05 in a muffle furnace, and setting the heating rate to be 2-10 ℃/min; keeping the temperature for 2-4h, and finally collecting to obtain bismuth ferrite fibers;
step S07: weighing 1-2mmol of 2-methylimidazole, adding into a beaker filled with 14.3mL of methanol, and stirring for 1-2h in a magnetic stirrer until the 2-methylimidazole is completely dissolved;
step S08: dispersing 1-2mmol of zinc nitrate hexahydrate in a beaker filled with methanol solution with the same volume, and stirring for 1-2 hours in a magnetic stirrer until the zinc nitrate hexahydrate is completely dissolved;
step S09: pouring the solution obtained in the step S07 into the beaker obtained in the step S08, and stirring the solution for 0.5 to 1 hour in a magnetic stirrer until the solution is uniformly mixed;
step S10: adding 2-3mmol of bismuth ferrite fiber into the solution obtained in the step S09, stirring for 10-15min in a magnetic stirrer until the mixture is uniform, and transferring ultrasonic treatment for 0.5-1h to form suspension;
step S011: and (3) centrifugally washing the suspension obtained in the step (S11), wherein a washing solution adopts methanol, a sample obtained after washing is dried in a drying oven at 70-80 ℃ for 12-24h, a final sample is obtained by collection, a scanning electron microscope picture is shown in figure 1, and zinc-based metal organic framework nano particles are uniformly combined on the surface of the bismuth ferrite nano fiber.
Comparative example
A bismuth ferrite nanofiber photocatalytic material is prepared by the following steps:
step S01: weighing 1-5mmol of bismuth nitrate pentahydrate and equimolar ferric nitrate nonahydrate, pouring into a beaker filled with 4-5mL of deionized water and 3-5mL of glacial acetic acid solution, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
step S02: weighing 0.8-1g of polyvinylpyrrolidone, adding the polyvinylpyrrolidone into a beaker filled with 10-12mL of dimethylformamide, and stirring for 1-2h on a magnetic stirrer until the solute is completely dissolved;
step S03: transferring the solution obtained in the step S02 to a beaker obtained in the step S01, and stirring the solution on a magnetic stirrer for 6 to 12 hours until the solution is completely and uniformly mixed;
step S04: transferring the precursor solution to a 20mL injector of an electrostatic spinning device, setting the fiber collection distance of the device to be 12-18cm, setting the spinning voltage to be 13-19kV, setting the advancing speed to be 0.1-0.5mL/h, controlling the humidity to be less than 40% rh and the temperature to be 0-40 ℃, and finally spinning a primary bismuth ferrite fiber sample;
step S05: drying the primary bismuth ferrite fiber obtained in the step S04 in a drying box at 70-80 ℃ for 12-24 h;
step S06: annealing the dried sample obtained in the step S05 in a muffle furnace, and setting the heating rate to be 2-10 ℃/min; keeping the temperature for 2-4h, and finally collecting to obtain the bismuth ferrite fiber.
Performance testing
The photocatalytic degradation effect experiment is carried out on the photocatalytic materials of the embodiment 1 and the comparative example, and the specific steps are as follows:
20mg of each of the photocatalytic materials of example 1 and comparative example was dispersed in 80mL of a methylene blue solution having a concentration of 20mg/L, and the photocatalyst surface and dye adsorption were equilibrated by stirring for 30min in a dark reaction. Then a 300W xenon lamp (lambda is more than or equal to 420nm) is turned on to simulate sunlight to carry out photocatalytic reaction, the photocatalytic reaction is carried out at normal temperature and normal pressure, a 300W xenon lamp (lambda is more than or equal to 420nm) is selected as a light source, and sampling analysis is carried out every 20 min. The absorbance of the methylene blue solution was measured with an ultraviolet-visible spectrophotometer at a wavelength of 664 nm. The degradation rate of the photocatalyst was calculated according to the formula [1- (initial concentration-end concentration)/initial concentration ] x 100%, and the 130min degradation results are shown in table 1 below.
TABLE 1
| Sample (I) | Comparative example | Example 1 |
| Degradation rate of methylene blue | 30.8％ | 83.7％ |
As can be seen from table 1 above, in example 1, compared with the comparative example, the degradation rate of the bismuth ferrite composite nanofiber photocatalytic material prepared in example 1 to methylene blue in a methylene blue solution is significantly improved. Therefore, the photodegradation capability of the prepared bismuth ferrite composite photocatalytic material is remarkably improved.
In addition, a repeated experiment is performed on the photocatalytic degradation effect of the common bismuth ferrite fiber and the bismuth ferrite composite photocatalytic material prepared in example 1 on a methylene blue solution, and the photocatalyst prepared in each example is tested three times (83.7%, 82.6%, and 82.0% respectively) according to the test method described in the performance test, and the test results show that: the photocatalytic effect of the composite photocatalyst prepared in example 1 is not obviously reduced after three times of repeated tests. Therefore, the bismuth vanadate composite photocatalyst prepared by the method provided by the embodiment of the invention has stable performance, and therefore, the bismuth ferrite composite photocatalyst material provided by the embodiment of the invention has practical application significance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of a bismuth ferrite composite photocatalytic material is characterized by comprising the following steps:
providing bismuth ferrite nanofibers;
dissolving the bismuth ferrite nanofiber in a mixed solution containing zinc salt and imidazole organic ligands, and growing metal organic framework nano particles on the surface of the bismuth ferrite nanofiber to obtain the bismuth ferrite composite photocatalytic material.
2. The preparation method of the bismuth ferrite composite photocatalytic material as claimed in claim 1, wherein the step of dissolving the bismuth ferrite nanofiber in a mixed solution containing zinc salt and imidazole organic ligands, and the step of growing metal organic framework nanoparticles on the surface of the bismuth ferrite nanofiber comprises:
preparing a zinc salt solution and an imidazole organic ligand solution;
mixing the zinc salt solution and the imidazole organic ligand solution to obtain a mixed solution;
and adding the bismuth ferrite nano-fiber into the mixed solution, sequentially carrying out magnetic stirring and ultrasonic treatment, and then carrying out drying treatment.
3. The preparation method of the bismuth ferrite composite photocatalytic material as recited in claim 2,
the molar ratio of the bismuth ferrite nano-fiber to the imidazole organic ligand is 1.3-1.8: 1; and/or the presence of a gas in the gas,
the magnetic stirring time is 10-15 min; and/or the presence of a gas in the gas,
the ultrasonic treatment time is 0.5-1 h; and/or the presence of a gas in the gas,
the drying treatment temperature is 70-80 ℃, and the drying treatment time is 12-24 h.
4. The preparation method of the bismuth ferrite composite photocatalytic material as recited in any one of claims 1 to 3, wherein the preparation method of the bismuth ferrite nanofiber comprises the following steps:
preparing a precursor solution containing bismuth nitrate, ferric nitrate and polyvinylpyrrolidone;
enabling the precursor solution to pass through an electrostatic spinning device to obtain initial bismuth ferrite nanofibers;
annealing the initial bismuth ferrite nanofiber to obtain the bismuth ferrite nanofiber.
5. The method for preparing the bismuth ferrite composite photocatalytic material as recited in claim 4, wherein the parameters of the electrospinning device comprise: the fiber collecting distance is 12-18cm, the spinning voltage is 13-19kV, the advancing speed is 0.1-0.5mL/h, the humidity is less than 40% rh, and the temperature is 0-40 ℃.
6. The method for preparing the bismuth ferrite composite photocatalytic material as recited in claim 5, wherein the annealing conditions comprise: heating to 380-420 ℃ at the heating rate of 2-10 ℃/min, and then preserving the heat for 2-4 h.
7. The bismuth ferrite composite photocatalytic material is characterized by comprising bismuth ferrite nanofibers and metal organic framework nanoparticles combined on the surfaces of the bismuth ferrite nanofibers.
8. The bismuth ferrite composite photocatalytic material of claim 7, wherein the bismuth ferrite nanofibers are bismuth ferrite electrospun fibers; and/or the presence of a gas in the gas,
the metal organic framework nano-particles are zinc-based metal organic framework nano-particles.
9. The bismuth ferrite composite photocatalytic material as recited in claim 7, wherein the diameter of the bismuth ferrite nanofiber is 150-300 nm; and/or the particle size of the metal organic framework nano-particles is 30-100 nm; and/or the presence of a gas in the gas,
the metal organic framework nano-particles are prepared from zinc salt and imidazole organic ligands, and the molar ratio of bismuth ferrite to the imidazole organic ligands in the bismuth ferrite nano-fibers is 1.3-1.8: 1.
10. The bismuth ferrite composite photocatalytic material of claim 7, wherein the bismuth ferrite composite photocatalytic material is prepared by the method for preparing the bismuth ferrite composite photocatalytic material of any one of claims 1 to 6.
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