CN107684914B - Magnetic Bi2MoO6/CuFe2O4Composite photocatalytic material and preparation method thereof - Google Patents
Magnetic Bi2MoO6/CuFe2O4Composite photocatalytic material and preparation method thereof Download PDFInfo
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- 229910002900 Bi2MoO6 Inorganic materials 0.000 title claims abstract description 33
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910016516 CuFe2O4 Inorganic materials 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 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 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract 3
- 238000004043 dyeing Methods 0.000 abstract 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- 238000011084 recovery Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000013329 compounding Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010034960 Photophobia Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- DXKGMXNZSJMWAF-UHFFFAOYSA-N copper;oxido(oxo)iron Chemical compound [Cu+2].[O-][Fe]=O.[O-][Fe]=O DXKGMXNZSJMWAF-UHFFFAOYSA-N 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 230000002349 favourable effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- 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
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8876—Arsenic, antimony or bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J35/33—
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- B01J35/39—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a magnetic Bi2MoO6/CuFe2O4The composite photocatalytic material and the preparation method thereof are as follows: adding Bi2MoO6Ultrasonically dispersing in deionized water, and adding Cu (NO)3)2·3H2O、Fe(NO3)3·9H2Placing O and disodium ethylene diamine tetraacetate in a water bath at 20-30 ℃ and stirring for 0.5-1 h to obtain a suspension A, adding urea to the suspension A, placing the suspension A in a water bath at 50-80 ℃ to react for 0.5-2 h to obtain a mixed suspension B, placing the mixed suspension B in a hydrothermal reaction kettle at 120-160 ℃, stirring to react for 1-8 h, filtering, washing and drying the obtained reaction mixed solution to obtain a solid, placing the solid in a muffle furnace to calcine at 400-700 ℃ for 1-3 h to obtain magnetic Bi with high catalytic activity2MoO6/CuFe2O4A composite photocatalytic material. The invention overcomes the defect of Bi2MoO6Has the defects of easy recombination of electron holes and poor recoverability, and prepares the magnetic Bi2MoO6/CuFe2O4The process of the composite photocatalytic material has the advantages of high efficiency and easy operation, and can replace TiO2And ZnO and the like are applied to photocatalytic purification of printing and dyeing wastewater, medical wastewater and heavy metal wastewater.
Description
(I) technical field
The invention relates to a preparation method of a recyclable photocatalytic material, and particularly relates to magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material and a preparation method thereof belong to the field of preparation and application of visible photocatalytic materials.
(II) background of the invention
Along with the development of social economy, the improvement of the living standard of people and the enhancement of health and environmental awareness, people have realized the importance of pollutant treatment, continuously explore new technologies and new methods for treating atmospheric pollution and water pollution, and the photocatalysis is considered by extensive researchers to be one of effective methods for solving the problems of atmospheric environment and water environment pollution. The photocatalysis technology can deeply react at room temperature and directly utilize sunlight as a light source for driving, is an ideal environment pollution treatment technology, and has wide application prospect and great social and economic benefits.
Currently, much research is conducted on traditional photocatalytic materials such as TiO2ZnO and the like have higher forbidden band width, so that the solar energy utilization rate is low (the ultraviolet radiation in sunlight is less than 5 percent), and therefore, the semiconductor photocatalytic material with visible light response activity attracts the attention of researchers and transfers the research direction to non-TiO2Series of visible light catalysts, e.g. with Bi2MoO6Is a typical bismuth-based visible light catalytic material and has a narrow forbidden band width Eg2.71eV, has the capability of degrading organic pollutants under visible light, has a unique electronic structure, can form a steep absorption edge in a visible light range, enables the formation and the flow of a cavity to be smoother by utilizing the reverse bond action between anions and cations, is favorable for the implementation of a photocatalytic reaction, and is expected to replace the traditional photocatalyst to become a new favorite in the field of organic sewage purification treatment.
However, Bi2MoO6The liquid phase reaction has the defects of difficult separation and recovery and difficult recycling, and the main reason is that the powdery Bi2MoO6The particles are fine, difficult to settle and easy to run off. And CuFe2O4(Eg2.0eV) is a magnetic photocatalytic material with visible light sensitivity, has the advantages of simple preparation process and strong magnetism, but Bi2MoO6Or CuFe2O4When used alone, the rate of recombination of photo-generated electrons and holes is high, so that Bi is added2MoO6And CuFe2O4The composite material is expected to replace the traditional photocatalyst to become a new favorite in the field of magnetic recyclable photocatalysts by carrying out semiconductor compounding.
Disclosure of the invention
Aiming at the existing Bi2MoO6Has the defects of high photon-hole recombination rate and poor recyclabilityProvide a magnetic Bi2MoO6/CuFe2O4The composite photocatalytic material and the preparation method thereof are used for making up for the defects.
The invention is realized by the following technical scheme:
magnetic Bi2MoO6/CuFe2O4The preparation method of the composite photocatalytic material comprises the following steps:
(1) adding Bi2MoO6Ultrasonically dispersing in deionized water, and adding Cu (NO)3)2·3H2O、Fe(NO3)3·9H2Placing O and disodium ethylene diamine tetraacetate (EDTA-2Na) in a water bath at the temperature of 20-30 ℃, and stirring for 0.5-1 h to obtain a suspension A; the Bi2MoO6With Cu (NO)3)2·3H2O、Fe(NO3)3·9H2The mass ratio of the O to the disodium ethylene diamine tetraacetate is 1: 0.604-2.416: 2.02-8.08: 0.005-0.02;
(2) adding urea into the suspension A obtained in the step (1), and placing the suspension A in a water bath at the temperature of 50-80 ℃ for reaction for 0.5-2 h to obtain a mixed suspension B; the suspension A is added with Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.3-0.6: 1;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at the temperature of 120-160 ℃, stirring and reacting for 1-8 hours, filtering, washing and drying the obtained reaction mixed solution to obtain a solid, and calcining the obtained solid to obtain magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
Further, in the step (1), the addition amount of the deionized water and the Bi are2MoO6The mass ratio of (A) to (B) is 1: 0.016-0.04.
Further, in the step (1), Bi is preferably used2MoO6With Cu (NO)3)2·3H2O、 Fe(NO3)3·9H2The mass ratio of the O to the ethylene diamine tetraacetic acid disodium is 1: 0.604-1.208: 2.02-4.04: 0.005-0.01.
Further, in the step (2), the suspension A is added with Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.4-0.6: 1.
Further, in the step (3), the hydrothermal reaction temperature of the mixed suspension B is preferably 120-130 ℃, and the reaction time is preferably 2-3 hours.
And further, in the step (3), the calcining process is to place the obtained solid in a muffle furnace to calcine at 400-700 ℃ for 1-3 h to obtain the magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
Furthermore, the method specifically comprises the following steps:
(1) adding Bi2MoO6Ultrasonically dispersing in deionized water, and adding Cu (NO)3)2·3H2O、Fe(NO3)3·9H2Placing the O and the disodium ethylene diamine tetraacetate into a water bath at the temperature of 20-30 ℃, and stirring for 0.5-1 h to obtain a suspension A; the Bi2MoO6With Cu (NO)3)2·3H2O、 Fe(NO3)3·9H2The mass ratio of the O to the disodium ethylene diamine tetraacetate is 1: 0.604-1.208: 2.02-4.04: 0.005-0.01; the addition amount of the deionized water and the Bi2MoO6The mass ratio of (A) to (B) is 1: 0.016-0.02;
(2) adding urea into the suspension A obtained in the step (1), and placing the suspension A in a water bath at the temperature of 50-80 ℃ for reaction for 0.5-2 h to obtain a mixed suspension B; the suspension A is added with Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.4-0.6: 1;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at the temperature of 120-130 ℃, stirring for reaction for 2-3 hours, filtering, washing and drying the obtained reaction mixed solution to obtain a solid, and placing the obtained solid in a muffle furnace to calcine at the temperature of 400-700 ℃ for 1-3 hours to obtain magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
Compared with the prior art, the invention has the beneficial effects that:
the technology adopts a hydrothermal-calcining combined method, avoids the defects of high precipitation speed and serious agglomeration caused by using alkaline precipitants such as NaOH, ammonia water and the like in the traditional composite material preparation process, and adopts Bi2MoO6/CuFe2O4Compounding, Bi can be increased2MoO6Magnetic recoverability and catalytic activity. The magnetic Bi prepared by the invention has strong magnetism and high photocatalytic activity2MoO6/CuFe2O4The composite photocatalytic material can replace the traditional photocatalyst TiO2ZnO, etc. are applied to the purification treatment of industrial and domestic sewage.
(IV) description of the drawings
FIG. 1 shows magnetic Bi prepared in example 2 of the present invention2MoO6/CuFe2O4Magnetic recovery diagram of composite photocatalytic material.
FIG. 2 shows magnetic Bi prepared in example 2 of the present invention2MoO6/CuFe2O4XRD pattern of the composite photocatalytic material.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1
(1) 1g of bismuth molybdate was weighed and ultrasonically dispersed in 50ml of deionized water, and 0.604g of Cu (NO) was added3)2·3H2O、2.02g Fe(NO3)3·9H2O and 0.005g of disodium ethylene diamine tetraacetate are put in a water bath at the temperature of 20 ℃ and stirred for 0.5h to obtain a suspension A;
(2) weighing 1.5g of urea, adding the urea into the mixed solution obtained in the step (1), and stirring the urea in a water bath at 50 ℃ for 0.5h to obtain a mixed suspension B;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at 120 ℃, stirring for reaction for 1h, filtering, washing and drying to obtain a solid, and placing the obtained solid in a muffle furnace to calcine at 400 ℃ for 3h to obtain the magnetic Bi with high catalytic activity2MoO6/CuFe2O4A composite photocatalytic material.
Example 2
(1) 0.8g of bismuth molybdate was weighed out and dispersed in 50ml of deionized water by ultrasonic, and 1.208g of Cu (NO) was added3)2·3H2O、4.04g Fe(NO3)3·9H2O and 0.01g of disodium ethylene diamine tetraacetate are placed in a water bath at the temperature of 30 ℃ and stirred for 1 hour to obtain a suspension A;
(2) weighing 2g of urea, adding the urea into the mixed solution obtained in the step (1), and stirring the urea in a water bath at 80 ℃ for 2 hours to obtain a mixed suspension B;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at 130 ℃, stirring for 8 hours, filtering, washing and drying to obtain a solid, placing the obtained solid in a muffle furnace, and calcining at 600 ℃ for 2 hours to obtain the magnetic Bi with high catalytic activity2MoO6/CuFe2O4A composite photocatalytic material.
Example 3
(1) 1.8g of bismuth molybdate was weighed and ultrasonically dispersed in 50ml of deionized water, followed by addition of 2.416g of Cu (NO)3)2·3H2O、8.08g Fe(NO3)3·9H2O and 0.02g of disodium ethylene diamine tetraacetate are placed in a water bath at the temperature of 20 ℃ and stirred for 0.5h to obtain a suspension A;
(2) weighing 8.05g of urea, adding the urea into the mixed solution obtained in the step (1), and stirring the urea in a water bath at 70 ℃ for 1 hour to obtain a mixed suspension B;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at 160 ℃, stirring for reaction for 2 hours, filtering, washing and drying to obtain a solid, and placing the obtained solid in a muffle furnace to calcine at 700 ℃ for 2 hours to obtain the magnetic Bi with high catalytic activity2MoO6/CuFe2O4A composite photocatalytic material.
Performance test experiment
50mL of Methylene Blue (MB) solution having an initial concentration of 4mg/L was put into a photocatalytic reaction quartz tube, and 0.08g of magnetic Bi prepared in example was weighed2MoO6/CuFe2O4Composite photocatalytic materialAdding into the MB solution, irradiating for 8h under visible light of a xenon lamp, testing the concentration of the residual MB in the solution by a spectrophotometer, calculating the degradation rate (%) of the MB, and recovering Bi by a permanent magnetic field2MoO6/CuFe2O4And (4) calculating the magnetic recovery yield (%) of the composite photocatalytic material. The results of the experiment are shown in table 1.
TABLE 1 results of the detection analysis of the samples of the examples
| Sample name | MB degradation Rate (%) | Magnetic recovery (%) |
| Example 1 | 93.2 | 96.5 |
| Example 2 | 96.8 | 98.3 |
| Example 3 | 91.7 | 95.4 |
As shown by the MB degradation rate (%) and the magnetic recovery rate (%) of the samples in the examples 1 to 3 in the table 1, the samples in the examples 1 to 3 have the MB degradation rate of more than 90% and the magnetic recovery rate of more than 95%, which indicates that the samples in the examples 1 to 3 have excellent photocatalytic and recycling performances.
Claims (7)
1. Magnetic Bi2MoO6/CuFe2O4The preparation method of the composite photocatalytic material is characterized by comprising the following steps:
(1) adding Bi2MoO6Ultrasonically dispersing in deionized water, and adding Cu (NO)3)2·3H2O、Fe(NO3)3·9H2Placing the O and the disodium ethylene diamine tetraacetate into a water bath at the temperature of 20-30 ℃, and stirring for 0.5-1 h to obtain a suspension A; the Bi2MoO6With Cu (NO)3)2·3H2O、Fe(NO3)3·9H2The mass ratio of the O to the disodium ethylene diamine tetraacetate is 1: 0.604-2.416: 2.02-8.08: 0.005-0.02;
(2) adding urea into the suspension A obtained in the step (1), and placing the suspension A in a water bath at the temperature of 50-80 ℃ for reaction for 0.5-2 h to obtain a mixed suspension B; the suspension A is prepared by adding Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.3-0.6: 1;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at the temperature of 120-160 ℃, stirring and reacting for 1-8 hours, filtering, washing and drying the obtained reaction mixed solution to obtain a solid, and calcining the obtained solid to obtain magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
2. The method of claim 1, wherein: in the step (1), the addition amount of the deionized water and the Bi are2MoO6The mass ratio of (A) to (B) is 1: 0.016-0.04.
3. The method of claim 1, wherein: in the step (1), the Bi2MoO6With Cu (NO)3)2·3H2O、Fe(NO3)3·9H2The mass ratio of the O to the disodium ethylene diamine tetraacetate is 1: 0.604-1.208: 2.02-4.04: 0.005-0.01.
4. The method of claim 1, wherein the method further comprises the step of removing the solvent from the mixtureThe method comprises the following steps: in the step (2), the suspension A is added with Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.4-0.6: 1.
5. The method of claim 1, wherein: in the step (3), the hydrothermal reaction temperature of the mixed suspension B is 120-130 ℃, and the reaction time is 2-3 h.
6. The method of claim 1, wherein: in the step (3), the calcining process is to place the obtained solid in a muffle furnace to calcine for 1-3 hours at 400-700 ℃ to obtain the magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
7. The method of claim 1, wherein: the method is specifically carried out according to the following steps:
(1) adding Bi2MoO6Ultrasonically dispersing in deionized water, and adding Cu (NO)3)2·3H2O、Fe(NO3)3·9H2Placing the O and the disodium ethylene diamine tetraacetate into a water bath at the temperature of 20-30 ℃, and stirring for 0.5-1 h to obtain a suspension A; the Bi2MoO6With Cu (NO)3)2·3H2O、Fe(NO3)3·9H2The mass ratio of the O to the disodium ethylene diamine tetraacetate is 1: 0.604-1.208: 2.02-4.04: 0.005-0.01; the addition amount of the deionized water and the Bi2MoO6The mass ratio of (A) to (B) is 1: 0.016-0.02;
(2) adding urea into the suspension A obtained in the step (1), and placing the suspension A in a water bath at the temperature of 50-80 ℃ for reaction for 0.5-2 h to obtain a mixed suspension B; the suspension A is prepared by adding Cu (NO)3)2·3H2The mass ratio of the mass of the O to the mass of the urea is 0.4-0.6: 1;
(3) placing the mixed suspension B obtained in the step (2) in a hydrothermal reaction kettle at the temperature of 120-130 ℃, stirring and reacting for 2-3 hours, filtering, washing and drying the obtained reaction mixed solution to obtain the productCalcining the obtained solid in a muffle furnace at 400-700 ℃ for 1-3 h to obtain magnetic Bi2MoO6/CuFe2O4A composite photocatalytic material.
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