CN110102311B - Nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material and preparation method thereof - Google Patents

Nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material and preparation method thereof Download PDF

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CN110102311B
CN110102311B CN201910184629.9A CN201910184629A CN110102311B CN 110102311 B CN110102311 B CN 110102311B CN 201910184629 A CN201910184629 A CN 201910184629A CN 110102311 B CN110102311 B CN 110102311B
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郭莉
韩宣宣
张开来
王丹军
王婵
付峰
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Yanan University
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Abstract

The invention discloses a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material, which is prepared from Bi2WO6And Ni0.5Zn0.5Fe2O4Composition of, wherein Ni0.5Zn0.5Fe2O4And Bi2WO6The mass ratio of (A) to (B) is 1-4: 10. the invention also discloses a method for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material. The nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material has the advantages of wide visible light response range, high visible light catalytic activity, easiness in recovery through a magnetic separation technology and stable reusability.

Description

Nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material and preparation method thereof
Technical Field
The invention belongs to the technical field of composite material preparation methods, and particularly relates to a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material and a method for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material.
Background
Bismuth tungstate (Bi)2WO6) The Aurivillius type oxide is the Aurivillius type oxide with the simplest structure, the Bi6s orbital and the O2p orbital of the Aurivillius type oxide are hybridized to form a Valence Band (VB), and the W5d orbital of the Aurivillius type oxide forms a Conduction Band (CB). Since Bi2WO6Has a narrow forbidden band width (about 2.7eV), and can absorb part of visible light to be excitedTherefore, the photocatalyst has potential application value in the fields of environmental purification and new energy development, and becomes one of the photocatalysts widely researched at present. However, as a photocatalyst, Bi2WO6There are mainly three problems: firstly, photo-generated electrons/holes (e-/h +) are easy to recombine, and the separation efficiency is not high; secondly, the visible light absorption range is relatively narrow; III is Bi2WO6The photocatalyst has a problem that it is difficult to recycle the photocatalyst. The first two problems lead to Bi2WO6The visible light catalytic activity of the material is to be further improved, and the third problem causes the problem that the material has high cost in practical application as a photocatalytic material.
Spinel type ferrite (MFe)2O4And M ═ Ni, Zn, Co, Mg, Ca) has unique optical, electrical, and magnetic properties, has good application prospects in the fields of magnetic materials, dielectrics, superconduction, luminescence, catalysis, biology, medicine, and the like, is mainly used as a microwave absorber and a magnetic recording material at present, and application research as a photocatalytic material in the field of photocatalysis is still at the beginning. Spinel type nickel zinc ferrite (Ni)0.5Zn0.5Fe2O4) The photocatalyst has good absorption on visible light and magnetism, is easy to recover in a catalytic system through a magnetic separation technology, and has attracted attention in recent years when applied to the field of photocatalysis. However, the spinel-type nickel-zinc ferrite has a small forbidden band width, so that a photogenerated carrier is easy to compound, the oxidation and reduction capability of the photogenerated carrier is weak, the photocatalytic activity of the photogenerated carrier is usually low, and the spinel-type nickel-zinc ferrite is difficult to be practically applied as a photocatalytic material.
For Bi2WO6And Ni0.5Zn0.5Fe2O4As a problem of the photocatalyst, the commonly used modification strategies at present comprise metal/nonmetal element doping, precious metal surface deposition, semiconductor compounding and the like, wherein the semiconductor compounding can expand the spectral response range of the catalyst and improve the separation efficiency of a photon-generated carrier, and the photocatalyst is widely concerned as an efficient modification method. In addition, the solution of the recycling problem of the catalytic material has important significance for promoting the practical application of the photocatalytic material, and the photocatalytic material is commonly used at presentThe recovery method comprises the methods of filtration, centrifugation, magnetic separation and the like, wherein the magnetic separation is a research hotspot due to the characteristics of simple operation, high efficiency and the like.
Disclosure of Invention
The invention aims to provide a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material, which solves the problems that the visible light catalytic activity of bismuth tungstate and the nickel-zinc ferrite is not high, and the bismuth tungstate is difficult to recycle.
The second purpose of the invention is to provide a method for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material, which is used for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material.
In order to achieve the first object, a first technical solution adopted by the present invention is:
a Ni-Zn ferrite/bismuth tungstate magnetic composite photocatalytic material is prepared from Bi2WO6And Ni0.5Zn0.5Fe2O4Composition of, wherein Ni0.5Zn0.5Fe2O4And Bi2WO6The mass ratio of (A) to (B) is 1-4: 10.
in order to achieve the second object, a second technical solution adopted by the present invention is:
a method for preparing a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material is implemented according to the following steps:
step 1: synthesis of Ni0.5Zn0.5Fe2O4The method specifically comprises the following steps:
step 1.1: mixing water and liquid polyethylene glycol to obtain a mixed liquid A;
step 1.2: firstly, Ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3Dissolving in the mixed liquid A, rapidly magnetically stirring for 100-140 min, and adding NH dropwise3·H2O, adjusting the pH value to 9-11, and finally continuing to perform rapid magnetic stirring for 20-60 min to obtain a mixed liquid B;
step 1.3: transferring the mixed liquid B into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying oven, and reacting for 3-8 h at 170-200 ℃ to obtain a mixture C;
step 1.4: naturally cooling the mixture C to room temperature, then carrying out magnetic separation to obtain a precipitate, sequentially carrying out water washing and alcohol washing on the precipitate, finally carrying out vacuum drying for 5-12 h at the temperature of 60-100 ℃, and grinding to obtain Ni0.5Zn0.5Fe2O4；
Step 2: synthesis of Ni0.5Zn0.5Fe2O4/Bi2WO6The method specifically comprises the following steps:
step 2.1: to Ni0.5Zn0.5Fe2O4Adding a hexadecyl trimethyl ammonium bromide aqueous solution, and performing ultrasonic dispersion for 10min-20min to obtain a mixture D;
step 2.2: adding Bi (NO) to the mixture D3)3·5H2Adding dilute nitric acid solution, magnetically stirring at room temperature for 20-50 min, and slowly adding Na dropwise after magnetic stirring2WO4·2H2O water solution, and finally stirring for 1-3 h by high-speed magnetic force to obtain a mixture E;
step 2.3: transferring the mixture E into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying box, and reacting for 4-9 h at the temperature of 140-180 ℃ to obtain a mixture F;
step 2.4: naturally cooling the mixture F to room temperature, then carrying out magnetic separation to obtain a precipitate, sequentially carrying out water washing and alcohol washing on the precipitate, finally carrying out vacuum drying for 5-12 h at the temperature of 60-100 ℃, and grinding to obtain Ni0.5Zn0.5Fe2O4/Bi2WO6。
The second technical scheme of the invention also has the following characteristics:
in said step 1.1: the volume ratio of water to liquid polyethylene glycol is 2: 1.
in said step 1.2, Ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3The mass ratio of (1): 1: 4, andand Fe (NO)3)3And the mass-to-volume ratio of the substances of water in step 1.1 is 3: 20 mol/L.
In the step 2.1, the concentration of the hexadecyl trimethyl ammonium bromide aqueous solution is 8.23mmol/L, Ni0.5Zn0.5Fe2O4The mass volume ratio of the ammonium bromide to the hexadecyl trimethyl ammonium bromide aqueous solution is 7: 3000 g/mL.
In the step 2.2, the concentration of the dilute nitric acid solution is 4mol/L, and the volume ratio of the dilute nitric acid solution to the hexadecyl trimethyl ammonium bromide aqueous solution in the step 2.1 is 1: 18, Na2WO4·2H2The concentration of the O aqueous solution is 0.0207-0.0827g/mL, Na2WO4·2H2The volume ratio of the O aqueous solution to the dilute nitric acid solution is 12: 5, Bi (NO)3)3·5H2O and Na2WO4·2H2The mass ratio of O is 2: 1.
the invention has the beneficial effects that: the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material has the advantages of wide visible light response range, high visible light catalytic activity, easy recovery by a magnetic separation technology and stable reusability; the method for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material has the advantages of easily available raw materials, simple synthesis steps, mild conditions, good controllability, good dispersibility of the prepared product, difficult agglomeration and high purity.
Drawings
FIG. 1 shows pure Ni obtained in comparative example 10.5Zn0.5Fe2O410% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6X-ray powder diffractogram of (a);
FIG. 2 shows 10% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6Photoelectron Spectroscopy (XPS) full spectrum of (a);
FIG. 3 shows 10% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6Bi4f narrow scan spectrum;
FIG. 4 is an embodiment10% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6The W4f narrow scan spectrum of (a);
FIG. 5 shows 10% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6Narrow scan spectrum of O1 s;
FIG. 6 shows 10% Ni obtained in example 20.5Zn0.5Fe2O4/Bi2WO6Narrow scan spectra of Zn2p, Ni2p, and Fe2 p;
FIG. 7 shows pure Ni obtained in comparative example 10.5Zn0.5Fe2O4SEM photograph of (a);
FIG. 8 shows pure Bi obtained in comparative example 22WO6SEM photograph of (a);
FIG. 9 shows 5% Ni obtained in example 10.5Zn0.5Fe2O4/Bi2WO6SEM photograph of (a);
FIG. 10 shows 20% Ni obtained in example 40.5Zn0.5Fe2O4/Bi2WO6SEM photograph of (a);
FIG. 11 shows 60% Ni obtained in example 70.5Zn0.5Fe2O4/Bi2WO6SEM photograph of (a);
FIG. 12 shows pure Ni obtained in comparative examples 1 and 2, respectively0.5Zn0.5Fe2O4(NZTY) and pure Bi2WO6(BWO) and solid UV-Vis absorption spectra of 5% NZTY/BWO, 10% NZTY/BWO and 20% NZTY/BWO obtained in examples 1, 2 and 4, respectively;
FIG. 13 shows pure Ni obtained in comparative examples 1 and 2, respectively0.5Zn0.5Fe2O4(NZTY) and pure Bi2WO6(BWO) and a comparison graph of the concentration change of the 10% NZTY/BWO obtained in the example 2 in the process of degrading rhodamine B (RhB);
FIG. 14 shows pure Ni obtained in comparative examples 1 and 2, respectively0.5Zn0.5Fe2O4(NZTY) and pure Bi2WO6(BWO) and examples1-4, 6 and 7 respectively obtain 5% NZTY/BWO, 10% NZTY/BWO, 15% NZTY/BWO, 20% NZTY/BWO, 40% NZTY/BWO and 60% NZTY/BWO as photocatalysts, and the degradation rate of rhodamine B (RhB) is compared in 10min of illumination;
FIG. 15 is a graph comparing the 20% NZTY/BWO obtained in example 4 before and after recovery by magnetic separation;
FIG. 16 is a graph showing the comparison of the photocatalytic performance of 20% NZTY/BWO obtained in example 4 when it is used repeatedly 5 times.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments.
The invention relates to a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material, which is prepared from Bi2WO6And Ni0.5Zn0.5Fe2O4Composition of, wherein Ni0.5Zn0.5Fe2O4And Bi2WO6The mass ratio of (A) to (B) is 1-4: 10.
the invention relates to a method for preparing the nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material, which is implemented according to the following steps:
step 1: synthesis of Ni0.5Zn0.5Fe2O4The method specifically comprises the following steps:
step 1.1: mixing water and liquid polyethylene glycol according to the volume ratio of 2:1 to obtain a mixed liquid A;
step 1.2: firstly, Ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3Dissolving in the mixed liquid A, rapidly magnetically stirring for 100-140 min, and adding NH dropwise3·H2O, adjusting the pH value to 9-11, and finally continuing to perform rapid magnetic stirring for 20-60 min to obtain a mixed liquid B; wherein Ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3The mass ratio of (1): 1: 4, and Fe (NO)3)3And the mass-to-volume ratio of the substances of water in step 1.1 is 3: 20 mol/L;
step 1.3: transferring the mixed liquid B into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying oven, and reacting for 3-8 h at 170-200 ℃ to obtain a mixture C;
step 1.4: naturally cooling the mixture C to room temperature, then carrying out magnetic separation to obtain a precipitate, sequentially carrying out water washing and alcohol washing on the precipitate, finally carrying out vacuum drying for 5-12 h at the temperature of 60-100 ℃, and grinding to obtain Ni0.5Zn0.5Fe2O4；
Step 2: synthesis of Ni0.5Zn0.5Fe2O4/Bi2WO6The method specifically comprises the following steps:
step 2.1: to Ni0.5Zn0.5Fe2O4Adding a hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 8.23mmol/L, and performing ultrasonic dispersion for 10min-20min to obtain a mixture D; wherein Ni0.5Zn0.5Fe2O4The mass volume ratio of the ammonium bromide to the hexadecyl trimethyl ammonium bromide aqueous solution is 7: 3000 g/mL;
step 2.2: adding Bi (NO) to the mixture D3)3·5H2O, adding dilute nitric acid solution with the concentration of 4mol/L, magnetically stirring at high speed for 20min to 50min at room temperature, and slowly dropping Na with the concentration of 0.0207 to 0.0827g/mL after the magnetic stirring at high speed is finished2WO4·2H2O water solution, and finally stirring for 1-3 h by high-speed magnetic force to obtain a mixture E; wherein the volume ratio of the dilute nitric acid solution to the hexadecyl trimethyl ammonium bromide aqueous solution in the step 2.1 is 1: 18, Na2WO4·2H2The volume ratio of the O aqueous solution to the dilute nitric acid solution is 12: 5, Bi (NO)3)3·5H2O and Na2WO4·2H2The mass ratio of O is 2: 1;
step 2.3: transferring the mixture E into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying box, and reacting for 4-9 h at the temperature of 140-180 ℃ to obtain a mixture F;
step 2.4: naturally cooling the mixture F to room temperature, then carrying out magnetic separation to obtain a precipitate, and sequentially carrying out water treatment on the precipitateWashing with alcohol, vacuum drying at 60-100 deg.C for 5-12 h, and grinding to obtain Ni0.5Zn0.5Fe2O4/Bi2WO6。
Example 1
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 2.9198g Bi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.9927g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 5% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 5% NZTY/BWO.
Example 2
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving in 10mL of water and 5mL of liquid polyethylene glycol (PEG-400)Adding into the mixed liquid, rapidly magnetically stirring for 120min, and adding NH dropwise3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 1.4599g Bi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.4964g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 10% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 10% NZTY/BWO.
Example 3
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 0.9733gBi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.3309g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 15% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 15% NZTY/BWO.
Example 4
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 0.7300gBi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.2482g of Na2WO4·2H2O is dissolved in 6mL of deionized water and then slowly dropped onStirring the mixture at high speed and magnetic force for 2h, then transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling the mixture to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, drying the precipitate at 80 ℃ in vacuum for 7h, and grinding the dried precipitate to obtain 20% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 20% NZTY/BWO.
Example 5
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 0.4866gBi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.1655g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 30% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 30% NZTY/BWO.
Example 6
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, and carrying out a hydrothermal reaction at 180 ℃ for 5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 0.3650gBi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.1241g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 40% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 40% NZTY/BWO.
Example 7
Step 1: 0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10 by O, continuously stirring for 30min, transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 180 DEG C5 h; after the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain Ni0.5Zn0.5Fe2O4Written as NZTY;
step 2: 0.1050g of Ni were weighed0.5Zn0.5Fe2O4Adding into 45mL CTAB water solution with concentration of 8.23mmol/L and ultrasonic dispersing for 30min, adding 0.2433gBi (NO)3)3·5H2O, then adding 2.5mL of dilute nitric acid solution with the concentration of 4mol/L, and magnetically stirring at high speed for 30min at room temperature; 0.0828g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dropping the dissolved O into the mixture, magnetically stirring at a high speed for 2h, transferring the mixture into a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water, washing with alcohol, vacuum-drying at 80 ℃ for 7h, and grinding to obtain 60% Ni0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is denoted as 60% NZTY/BWO.
Comparative example 1
0.1091g of Ni (NO) were weighed out separately3)2，0.1115g Zn(NO3)2And 0.6060g of Fe (NO)3)3Dissolving the mixture in a mixed liquid consisting of 10mL of water and 5mL of liquid polyethylene glycol (PEG-400), rapidly stirring for 120min by magnetic force, and then dropwise adding NH3·H2Adjusting the pH value to 10, continuously stirring for 30min, and transferring the obtained mixed liquid to a 50mL stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 180 ℃ for 5 h. After the hydrothermal reaction is finished, naturally cooling to room temperature, carrying out magnetic separation, washing the obtained precipitate with water and alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain pure Ni0.5Zn0.5Fe2O4It is referred to as NZTY.
Comparative example 2
0.7300g Bi (NO) were weighed out3)3·5H2O, added to 45mL of an aqueous CTAB solution having a concentration of 8.23mmol/L, followed by 2.5mL of a 4mol concentrationL dilute nitric acid solution, and magnetically stirring at high speed for 30min at room temperature. 0.2482g of Na2WO4·2H2Dissolving O in 6mL of deionized water, slowly dripping into the mixed liquid, magnetically stirring at high speed for 2h, transferring to a 100mL high-pressure reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction at 160 ℃ for 6h, naturally cooling to room temperature, performing centrifugal separation, washing the obtained precipitate with water, washing with alcohol, vacuum drying at 80 ℃ for 7h, and grinding to obtain pure Bi2WO6Photocatalytic material, denoted BWO.
As shown in FIG. 1, it can be seen that each diffraction peak position of the sample synthesized in comparative example 1 completely coincided with that of the standard card (JCPDS No.8-0234), indicating that the sample has a cubic spinel structure of Ni0.5Zn0.5Fe2O4(ii) a Diffraction peaks of the sample obtained in example 2 at 28.3 °, 32.8 °, 32.9 °, 47.0 °, 47.1 °, 55.8 °, 58.5 °, 68.7 °, 75.9 ° and 78.5 ° respectively correspond to orthorhombic Bi2WO6(131), (200), (002), (260), (202), (331), (262), (400), (103) and (204) (JCPDS No.39-0256), and the remaining diffraction peaks correspond to the cubic spinel structure Ni0.5Zn0.5Fe2O4The sample obtained in example 2 is described as being made of orthorhombic Bi2WO6And cubic phase spinel structure Ni0.5Zn0.5Fe2O4Composed and no hetero-peak appears, indicating that the sample purity is higher.
FIG. 2 shows that the sample synthesized in example 2 contains Bi, W, O, and C, wherein the C can be attributed to the C contamination source of the instrument itself; FIGS. 3-6 are high resolution spectra of Bi4f, W4f, O1s, Zn2p, Ni2p and Fe2p, respectively. In FIG. 3, the peaks with binding energies of 159.09eV and 164.14eV are assigned to Bi4f5/2And Bi4f7/2Indicating the existence of a + 3-valent Bi element; as can be seen from FIG. 4, the W element has two photoelectron peaks with different energy positions, and the peaks with the binding energies of 35.40eV and 37.74eV respectively correspond to W4f7/2And W4f5/2Comparing the energy state with the standard value to determine that the W element has a valence of + 6; as can be seen from FIG. 5, the peak of O1s on the surface of the sample is more complex, broader and asymmetric, and is subject to peak separationThe obtained peak values are 530.08eV and 532.5eV, which are respectively attributed to lattice oxygen and surface hydroxyl oxygen; FIG. 6 shows that, by comparison with the standard values, it is possible to determine that the Ni and Zn elements exist in the +2 valence state and the Fe element exists in the +3 valence state;
FIG. 7 shows that Ni obtained in comparative example 1 can be seen0.5Zn0.5Fe2O4The shape is irregular; FIG. 8 shows that pure Bi obtained in comparative example 2 can be seen2WO6The size is uniform, and the appearance is approximately regular; as can be seen from FIGS. 7 to 10, 20% Ni was obtained in example 4 of FIG. 100.5Zn0.5Fe2O4/Bi2WO6Is composed of regular Bi2WO6And irregular Ni0.5Zn0.5Fe2O4The particles are compounded, and the dispersion degree is higher; as can be seen from the combination of FIGS. 8 to 11, depending on Ni in the samples0.5Zn0.5Fe2O4Increased content of Bi in the sample2WO6The morphology gradually disappeared.
As shown in FIG. 12, it can be seen that Bi obtained in comparative example 22WO6Has an absorption edge of about 430 nm; pure Ni obtained in comparative example 10.5Zn0.5Fe2O4Strong absorption in the whole ultraviolet-visible light range; ni synthesized in examples 1, 2 and 40.5Zn0.5Fe2O4/Bi2WO6Composite photocatalytic material and Bi obtained in comparative example 22WO6The absorption is enhanced within the range of 400-700 nm, and the absorption edge is red-shifted, which shows that Ni0.5Zn0.5Fe2O4Remarkably broaden Bi2WO6The visible light response range of (a);
ni obtained by the production method of the present invention0.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material degrades rhodamine B wastewater to show the photocatalytic performance of the rhodamine B wastewater.
The specific experimental process is as follows: 20mg/L of rhodamine B (RhB) aqueous solution is prepared to be used as a simulated pollutant for carrying out photocatalytic activity evaluation. 0.1g of catalyst was added toThe quartz reactor containing 250mL RhB solution was placed in a photochemical reactor and magnetic stirring was started in the dark for 30min to disperse the catalyst sample uniformly while allowing the model contaminants to reach adsorption/desorption equilibrium on its surface. A500W metal halide lamp (a JB420 filter is added to filter light below 420 nm) is used as a visible light source. Sampling every 10min, carrying out magnetic separation, centrifuging for 10min by a high-speed centrifuge at 8000r/min, taking the supernatant, measuring the absorbance of the supernatant at the maximum absorption wavelength, and measuring the concentration change by a photometry so as to evaluate the photocatalytic activity of the catalyst. As can be seen from FIG. 13, the composite photocatalytic material obtained in example 2 contains 10% Ni0.5Zn0.5Fe2O4/Bi2WO6The photocatalytic activity is obviously higher than that of pure Ni obtained in comparative example 10.5Zn0.5Fe2O4And pure Bi obtained in comparative example 22WO6(ii) a As can be seen from FIG. 14, Bi2WO6And Ni0.5Zn0.5Fe2O4The visible light catalytic activity of the composite material can be obviously improved by compounding, and the improvement of the activity is related to the mass ratio of the two in the composite photocatalytic material, when Ni is used0.5Zn0.5Fe2O4Is Bi2WO6When the mass is 10-40%, the visible light catalytic activity of the obtained composite photocatalytic material is higher.
As shown in FIG. 15, it can be seen that 20% Ni was obtained in example 40.5Zn0.5Fe2O4/Bi2WO6The composite photocatalytic material is easy to recover by a magnetic separation technology;
as shown in FIG. 16, it can be seen that 20% Ni obtained in example 4 was used repeatedly 5 times0.5Zn0.5Fe2O4/Bi2WO6The reduction of the photocatalytic activity is not obvious, which shows that the reusability of the material is stable.

Claims (2)

1. The magnetic composite photocatalytic Ni-Zn ferrite/bismuth tungstate material is prepared with Bi2WO6And Ni0.5Zn0.5Fe2O4Composition of, wherein Ni0.5Zn0.5Fe2O4And Bi2WO6The mass ratio of (A) to (B) is 1-4: 10.
2. a method for preparing a nickel-zinc ferrite/bismuth tungstate magnetic composite photocatalytic material is characterized by comprising the following steps of:
step 1: synthesis of Ni0.5Zn0.5Fe2O4The method specifically comprises the following steps:
step 1.1: mixing water and liquid polyethylene glycol to obtain a mixed liquid A; the volume ratio of water to liquid polyethylene glycol is 2:1
Step 1.2: firstly, Ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3Dissolving in the mixed liquid A, rapidly magnetically stirring for 100-140 min, and adding NH dropwise3·H2O, adjusting the pH value to 9-11, and finally continuing to perform rapid magnetic stirring for 20-60 min to obtain a mixed liquid B; ni (NO)3)2、Zn(NO3)2And Fe (NO)3)3The mass ratio of (1): 1: 4, and Fe (NO)3)3And the mass-to-volume ratio of the substances of water in step 1.1 is 3: 20 mol/L;
step 1.3: transferring the mixed liquid B into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying oven, and reacting for 3-8 h at 170-200 ℃ to obtain a mixture C;
step 1.4: naturally cooling the mixture C to room temperature, then carrying out magnetic separation to obtain a precipitate, sequentially carrying out water washing and alcohol washing on the precipitate, finally carrying out vacuum drying for 5-12 h at the temperature of 60-100 ℃, and grinding to obtain Ni0.5Zn0.5Fe2O4；
Step 2: synthesis of Ni0.5Zn0.5Fe2O4/Bi2WO6The method specifically comprises the following steps:
step 2.1: to Ni0.5Zn0.5Fe2O4Adding hexadecyl trimethyl ammonium bromide aqueous solution and carrying out ultrasonic dispersion 10min-20min to obtain a mixture D; the concentration of the hexadecyl trimethyl ammonium bromide aqueous solution is 8.23mmol/L, Ni0.5Zn0.5Fe2O4The mass volume ratio of the ammonium bromide to the hexadecyl trimethyl ammonium bromide aqueous solution is 7: 3000g/mL
Step 2.2: adding Bi (NO) to the mixture D3)3·5H2Adding dilute nitric acid solution, magnetically stirring at room temperature for 20-50 min, and slowly adding Na dropwise after magnetic stirring2WO4·2H2O water solution, and finally stirring for 1-3 h by high-speed magnetic force to obtain a mixture E; the concentration of the dilute nitric acid solution is 4mol/L, and the volume ratio of the dilute nitric acid solution to the hexadecyl trimethyl ammonium bromide aqueous solution in the step 2.1 is 1: 18, Na2WO4·2H2The concentration of the O aqueous solution is 0.0207-0.0827g/mL, Na2WO4·2H2The volume ratio of the O aqueous solution to the dilute nitric acid solution is 12: 5, Bi (NO)3)3·5H2O and Na2WO4·2H2The mass ratio of O is 2: 1;
step 2.3: transferring the mixture E into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the stainless steel high-pressure reaction kettle into an electric heating constant-temperature air blast drying box, and reacting for 4-9 h at the temperature of 140-180 ℃ to obtain a mixture F;
step 2.4: naturally cooling the mixture F to room temperature, then carrying out magnetic separation to obtain a precipitate, sequentially carrying out water washing and alcohol washing on the precipitate, finally carrying out vacuum drying for 5-12 h at the temperature of 60-100 ℃, and grinding to obtain Ni0.5Zn0.5Fe2O4/Bi2WO6。
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