CN110711586B - Low-temperature preparation method of magnetic bismuth-containing iron oxide photocatalyst - Google Patents
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 32
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 89
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 62
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000005457 ice water Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000696 magnetic material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- YDADSACUMGYURZ-UHFFFAOYSA-N [O-2].[Fe+2].[Bi+3] Chemical compound [O-2].[Fe+2].[Bi+3] YDADSACUMGYURZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 3
- 229910000416 bismuth oxide Inorganic materials 0.000 abstract description 2
- 230000005684 electric field Effects 0.000 abstract description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 6
- 229940012189 methyl orange Drugs 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 230000009977 dual effect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000005293 ferrimagnetic effect Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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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
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
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Abstract
A low-temperature preparation method of a magnetic bismuth-containing iron oxide photocatalyst belongs to the technical field of preparation of magnetic photocatalyst materials. The invention aims to solve the problem of recycling of the existing bismuth-containing photocatalyst. The invention directly uses Bi (NO) by a solvothermal method 3 ) 3 Solution, Fe (NO) 3 ) 3 Solution and NaBH 4 The solution and NaOH aqueous solution are used for preparing the magnetic bismuth-containing iron oxide photocatalyst. The preparation method compounds bismuth and ferric oxide with photocatalysis effect to have magnetism, so that the photocatalyst can be recycled under the action of an external electric field, can be recycled, is environment-friendly and reduces the cost. The preparation method has the advantages of short preparation time and relatively low preparation temperature, and saves the preparation cost. The photocatalyst prepared by the invention has uniform microstructure, good photocatalytic stability and high magnetic permeability.
Description
Technical Field
The invention relates to a low-temperature preparation method of a magnetic bismuth-containing iron oxide photocatalyst, belonging to the technical field of preparation of magnetic photocatalyst materials.
Background
The magnetic material is a substance capable of directly or indirectly generating magnetism from transition elements such as iron, cobalt, nickel, and alloys thereof. Ferromagnetic substances and ferrimagnetic substances are ferromagnetic substances, and magnetic materials are generally called ferromagnetic substances and are functional materials with wide ancient and dual purposes. Modern magnetic materials have been widely used and play an important role in the traditional and emerging fields of electronics, computers, information communication, medical treatment, aerospace, automobiles, wind power and the like.
The photocatalysis technology is regarded as a high-efficiency and green technical method due to the advantages of few intermediate products, energy conservation, simple use process, no secondary pollution and the like. The metal bismuth is a photocatalyst applied to a photocatalytic technology, and can be recycled as a catalyst, so that the provision of a recyclable magnetic bismuth-containing photocatalyst is necessary.
Disclosure of Invention
The invention provides a low-temperature preparation method of a magnetic bismuth-containing iron oxide photocatalyst, aiming at solving the problem of recycling of the existing bismuth-containing photocatalyst.
The technical scheme of the invention is as follows:
a low-temperature preparation method of a magnetic bismuth-containing iron oxide photocatalyst comprises the following operation steps:
step 1, dissolving Bi (NO) by using ethylene glycol 3 ) 3 ·5H 2 O to obtain Bi (NO) with the mass fraction of 4.3% 3 ) 3 Solution of Fe (NO) dissolved in deionized water 3 ) 3 ·5H 2 O obtains 5 to 30 mass percent of Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solutions to prepare a reaction solution A;
step 2, dissolving NaBH by using deionized water 4 Obtaining NaBH with the mass fraction of 9 to 18.5 percent 4 Solution, then to NaBH 4 Adding 10% NaOH aqueous solution in mass fraction into the solution to obtain reaction solution B;
step 3, dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2-3 h, and obtaining a reaction solution C;
and 4, placing the reaction solution C in a reaction kettle, cooling to room temperature after the heating reaction is finished, centrifuging, removing supernate, drying and grinding to obtain the bismuth-containing iron oxide composite magnetic material.
Preferably: bi (NO) in said step 1 3 ) 3 Solution with Fe (NO) 3 ) 3 The volume ratio of the solution was 5: 1.
Preferably: and in the step 3, dropwise adding the reaction solution B into the reaction solution A under the ice-water bath condition.
Preferably: NaBH in the step 2 4 The volume ratio of the solution to the aqueous NaOH solution was 5: 1.
Preferably: the specific operation process of the step 4 is as follows: and (3) placing the reaction solution C into a reaction kettle, placing the reaction kettle into a box-type resistance heating furnace, preserving the temperature at 180 ℃ for 12-24 h to complete heating reaction, naturally cooling to room temperature, performing solid-liquid separation by using a centrifugal machine, removing supernatant, drying and grinding to obtain the bismuth iron oxide composite magnetic material.
Most preferably: the drying is carried out by using a forced air drying oven or a vacuum drying oven.
The invention has the following beneficial effects: the invention utilizes the solvothermal method to prepare the magnetic bismuth-containing iron oxide photocatalyst, has the advantages of short preparation time and relatively low preparation temperature, and saves the preparation cost. The photocatalyst prepared by the method has magnetism by compounding bismuth and ferric oxide with photocatalysis, can be recycled under the action of an external electric field, can be recycled, and reduces the cost while being environment-friendly. The photocatalyst prepared by the invention has uniform microstructure, good photocatalytic stability and high magnetic permeability.
Drawings
FIG. 1 is an SEM photograph of embodiment 1;
FIG. 2 is a hysteresis loop of a magnetic bismuth-containing iron oxide photocatalyst made in accordance with the present application;
FIG. 3 is a graph of the photocatalytic efficiency of magnetic bismuth-containing iron oxide photocatalysts made according to the present application;
fig. 4 is an SEM photograph of elemental bismuth.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
Embodiment mode 1: preparation of magnetic bismuth-containing iron oxide photocatalyst (i)
(1) 2.4g of Bi (NO) were dissolved in 50ml of ethylene glycol solvent 3 ) 3 ·5H 2 O to Bi (NO) 3 ) 3 Solution 0.5g Fe (NO) dissolved in 50ml deionized water 3 ) 3 ·5H 2 O to Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solution in an ice water bath to prepare a reaction solution A;
(2) 0.902g of NaBH was dissolved using 10ml of deionized water 4 Obtaining NaBH 4 Solution, then to NaBH 4 Adding 0.095g of NaOH aqueous solution with the mass fraction of 2% into the solution to obtain reaction solution B;
(3) dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2 hours, so as to obtain a reaction solution C;
(4) and (3) placing the reaction solution C into a reaction kettle, placing the reaction kettle into a box-type resistance heating furnace, preserving the temperature for 12 hours at 180 ℃ to complete heating reaction, naturally cooling to room temperature, performing solid-liquid separation by using a centrifugal machine, removing supernatant, washing powder with water and alcohol for three times, drying by using an air blast drying oven, and grinding to obtain the magnetic bismuth-containing iron oxide photocatalyst (i).
Embodiment mode 2: preparation of magnetic bismuth-containing iron oxide photocatalyst (ii)
(1) 2.4g of Bi (NO) were dissolved in 50ml of ethylene glycol solvent 3 ) 3 ·5H 2 O to Bi (NO) 3 ) 3 Solution 1g of Fe (NO) dissolved in 50ml of deionized water 3 ) 3 ·5H 2 O to Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solution in an ice water bath to prepare a reaction solution A;
(2) 1.092g of NaBH was dissolved using 10ml of deionized water 4 Obtaining NaBH 4 Solution, then to NaBH 4 Adding NaOH with the mass of 0.115g into the solution2% NaOH aqueous solution to obtain a reaction solution B;
(3) dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2 hours, so as to obtain a reaction solution C;
(4) and (3) placing the reaction solution C into a reaction kettle, placing the reaction kettle into a box-type resistance heating furnace, preserving the temperature at 180 ℃ for 12h to complete heating reaction, naturally cooling to room temperature, performing solid-liquid separation by using a centrifugal machine, removing supernatant, washing powder with water and alcohol for three times, drying by using an air blast drying oven, and grinding to obtain the magnetic bismuth-containing iron oxide photocatalyst (ii).
Embodiment mode 3: preparation of magnetic bismuth-containing iron oxide photocatalyst (iii)
(1) 2.4g of Bi (NO) were dissolved in 50ml of ethylene glycol solvent 3 ) 3 ·5H 2 O to Bi (NO) 3 ) 3 Solution 2g of Fe (NO) dissolved in 50ml of deionized water 3 ) 3 ·5H 2 O to Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solution in an ice water bath to prepare a reaction solution A;
(2) 1.472g of NaBH dissolved in 10ml of deionized water 4 Obtaining NaBH 4 Solution, then to NaBH 4 Adding NaOH aqueous solution with the mass fraction of 2% and the mass of 0.155g of NaOH into the solution to obtain reaction solution B;
(3) dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2 hours, so as to obtain a reaction solution C;
(4) and (3) placing the reaction solution C into a reaction kettle, placing the reaction kettle into a box-type resistance heating furnace, preserving the temperature for 12 hours at 180 ℃ to complete heating reaction, naturally cooling to room temperature, performing solid-liquid separation by using a centrifugal machine, removing supernatant, washing powder with water and alcohol for three times, drying by using an air blast drying oven, and grinding to obtain the magnetic bismuth-containing iron oxide photocatalyst (iii).
Embodiment mode 4: preparation of magnetic bismuth-containing iron oxide photocatalyst (iiii)
(1) 2.4g of a solution of 2.4g in 50ml of ethylene glycol solventBi(NO 3 ) 3 ·5H 2 O to Bi (NO) 3 ) 3 Solution 3g of Fe (NO) dissolved in 50ml of deionized water 3 ) 3 ·5H 2 O to Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solution in an ice water bath to prepare a reaction solution A;
(2) 1.852g of NaBH dissolved in 10ml of deionized water 4 Obtaining NaBH 4 Solution, then to NaBH 4 Adding NaOH aqueous solution with the mass fraction of 2% and the mass of 0.195g of NaOH into the solution to obtain reaction solution B;
(3) dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2 hours, so as to obtain a reaction solution C;
(4) and (3) placing the reaction solution C into a reaction kettle, placing the reaction kettle into a box-type resistance heating furnace, preserving the temperature for 12 hours at 180 ℃ to complete heating reaction, naturally cooling to room temperature, performing solid-liquid separation by using a centrifugal machine, removing supernatant, washing powder with water and alcohol for three times, drying by using an air blast drying oven, and grinding to obtain the magnetic bismuth-containing iron oxide photocatalyst (iiii).
A scanning electron microscope test was performed on the magnetic bismuth-containing iron oxide photocatalyst (i) obtained in embodiment 1 to obtain an SEM photograph as shown in fig. 1. As can be seen from the comparison of the SEM photographs of the elemental bismuth in fig. 1 and 4, the magnetic bismuth-containing iron oxide photocatalyst (i) prepared in embodiment 1 uniformly grows iron oxide on the flaky bismuth.
As shown in fig. 2, the results of the measurement of the high-precision hysteresis loop of the magnetic bismuth-containing iron oxide photocatalysts (i), (ii), (iii) and (iiii) obtained in embodiments 1, 2, 3 and 4, respectively, using a hysteresis loop measuring instrument, are shown in fig. 2, and it can be seen from fig. 2 that the hysteresis loops of the photocatalysts (i), (ii), (iii) and (iiii) are narrow and steep, the magnetization process is nearly reversible, the hysteresis loss is small, the magnetic permeability is high, and the low coercive force magnetic induction strengths are 9.923T, 133.139T, 70.32T and 7.997T, respectively. These results show that as the content of iron oxide increases, the magnetic properties of the composite material increase and then decrease, and the photocatalytic effect also gradually decreases as the content of iron oxide increases.
A photocatalytic efficiency test experiment was performed on the magnetic bismuth-containing iron oxide photocatalyst (i) prepared in embodiment 1, and the specific experimental procedure was to add the prepared composite material to 100ml of methyl orange with a concentration of 30mg/L, magnetically stir the mixture under the irradiation of visible light, centrifuge 5ml of the solution every half hour, and measure the absorbance of the methyl orange using a spectrophotometer, and the test results are shown in fig. 3. As can be seen from FIG. 3, after 30 minutes of photocatalysis, the degradation of the material to methyl orange is obvious, which is the combined action of bismuth degradation of methyl orange and iron oxide adsorption of methyl orange, and the degradation efficiency of the material to methyl orange tends to be stable after 30 minutes.
Claims (2)
1. A low-temperature preparation method of a magnetic bismuth-containing iron oxide photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1, dissolving Bi (NO) by using ethylene glycol 3 ) 3 ·5H 2 O to obtain Bi (NO) with the mass fraction of 4.3% 3 ) 3 Solution of Fe (NO) dissolved in deionized water 3 ) 3 ·5H 2 O obtains 5 to 30 mass percent of Fe (NO) 3 ) 3 A solution; then Bi (NO) 3 ) 3 Solution and Fe (NO) 3 ) 3 Mixing the solutions to prepare a reaction solution A;
bi (NO) in said step 1 3 ) 3 Solution with Fe (NO) 3 ) 3 The volume ratio of the solution is 5: 1;
step 2, dissolving NaBH by using deionized water 4 Obtaining NaBH with the mass fraction of 9 to 18.5 percent 4 Solution, then to NaBH 4 Adding 10% NaOH aqueous solution in mass fraction into the solution to obtain reaction solution B;
NaBH in the step 2 4 The volume ratio of the solution to the NaOH aqueous solution is 5: 1;
step 3, dropwise adding the reaction solution B into the reaction solution A while stirring, wherein the dropwise adding stirring time is 2-3 h, and obtaining a reaction solution C;
the process of dropwise adding the reaction solution B into the reaction solution A to obtain the reaction solution C in the step 3 is carried out under the ice-water bath condition;
and 4, placing the reaction solution C in a reaction kettle, preserving the temperature at 180 ℃ for 12-24 hours to complete the heating reaction, cooling to room temperature after the heating reaction is completed, performing solid-liquid separation by using a centrifugal machine, discarding supernatant, drying and grinding to obtain the bismuth iron oxide composite magnetic material.
2. The method of claim 1, wherein the method comprises the steps of: the drying is carried out by using a forced air drying oven or a vacuum drying oven.
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Inventor after: Jin Xinxin Inventor after: Li Xiaoyue Inventor before: Li Xiaoyue Inventor before: Jin Xinxin |