CN116328794A - Preparation method and application of high-efficiency catalytic oxidation heterojunction material - Google Patents
Preparation method and application of high-efficiency catalytic oxidation heterojunction material Download PDFInfo
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 34
- 230000003647 oxidation Effects 0.000 title claims abstract description 32
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 51
- 229910002588 FeOOH Inorganic materials 0.000 claims abstract description 32
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002474 experimental method Methods 0.000 claims abstract description 11
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 11
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 11
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000012360 testing method Methods 0.000 claims abstract description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000004088 simulation Methods 0.000 claims abstract description 6
- 239000011734 sodium Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 57
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 51
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 50
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- 238000006243 chemical reaction Methods 0.000 claims description 30
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- 229910021641 deionized water Inorganic materials 0.000 claims description 25
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- 231100000719 pollutant Toxicity 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 230000001105 regulatory effect Effects 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
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- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
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- 239000007787 solid Substances 0.000 claims description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 19
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 4
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- 238000002386 leaching Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical class [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
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- 238000005984 hydrogenation reaction Methods 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B01J23/74—Iron group metals
- B01J23/745—Iron
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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Abstract
The invention relates to the technical field of heterojunction material synthesis, and discloses a preparation method of a high-efficiency catalytic oxidation heterojunction material, which comprises the following steps: s1: mixing, collecting 3-5g sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution; the invention also provides application of the high-efficiency catalytic oxidation heterojunction material as a catalyst for degradationThe test comprises the following steps: simulation light: and simulating visible light by using a 35W xenon lamp to perform a photocatalytic degradation experiment. The invention not only has higher oxidation-reduction potential (E0=2.5-3.1V), wider pH application range (3-9), stronger selectivity, but also can improve MoS 2 Actual application value of the delta-FeOOH/PMS/vis system in wastewater treatment.
Description
Technical Field
The invention relates to the technical field of heterojunction material synthesis, in particular to a preparation method and application of a high-efficiency catalytic oxidation heterojunction material.
Background
Along with the continuous progress of social development, we gradually pay attention to the water environment pollution phenomenon. As a common industrial wastewater, the printing and dyeing wastewater has the advantages of large discharge amount, high organic pollutant content, complex components, high chromaticity, toxicity, harm and difficult treatment. Direct emissions without treatment or mishandling can seriously destroy the ecological environment and threaten human health
At present, domestic and foreign wastewater treatment methods include a physical method, a biological method and an advanced oxidation method (AOPs). AOPs can effectively solve the above problems, including photocatalysis, electrochemistry, fenton-like, and the like. Based on sulfate radicals (SO 4 -) (E0=2.5 to 3.1V) heterogeneous photo-Fenton (Fenton) technology as one of the AOPs, which is SO compared to hydroxyl radical (. OH) 4 The advantages of having a higher redox potential, a longer half-life and a stronger selectivity, and a wide applicable pH range (15) are thus of great interest.
Molybdenum disulfide (MoS) 2 ) Because of its unique microstructure, it is widely used as electrode material for solar cell, battery, etc. and as promoter in the course of photocatalysis reaction. Related studies have shown that when MoS 2 The catalyst can be used for photocatalytic decomposition of water to prepare hydrogen or photocatalytic degradation of pollutants in combination with other semiconductors, can remarkably improve the activity of the catalyst, and can be used as a catalyst promoter in the photocatalytic reaction process instead of noble metal Pt due to abundant raw material sources and low cost.
delta-FeOOH is a polymorph of four known iron oxyhydroxides, which can be synthesized by rapid oxidation; has higher surface area; the catalyst has ferrimagnetism at room temperature, so that the catalyst can be recovered after the reaction; moreover, fe is one of the most abundant elements on the earth, and has sufficient raw materials and low price; thus, delta-FeOOH is an effective, environmentally friendly, low cost catalyst.
Research has shown that Fe/Mo double-active site catalyst has practical application value. However, less research is conducted on the activation of PMS system by Mo/Fe catalyst under visible light, and the prepared MoS 2 /δ-FeOOH(MoS 2 delta-FeOOH) heterojunction material reduces the leaching problem of metal ions, and the magnetic material is convenient to recycle, thereby being beneficial to saving cost and providing a new solution for the field of activating PMS degradation pollutants by using visible light as a catalyst.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method and application of a high-efficiency catalytic oxidation heterojunction material, and the prepared MoS 2 The delta-FeOOH heterojunction material reduces the leaching problem of metal ions, and the magnetic material is convenient to recycle, thereby contributing to cost saving. In addition, the cocatalyst MoS 2 The introduction of the Fe/Mo double active sites realizes that the degradation efficiency of pollutants is obviously improved in a PMS/vis system.
(II) technical scheme
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of a high-efficiency catalytic oxidation heterojunction material comprises the following steps:
s1: mixing, collecting 3-5g sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution;
s2: drying, namely slowly transferring the mixed solution in the step S1 into a 100ml reaction kettle, and preserving heat for 24 hours at 180 ℃ in a forced air drying box to perform a synthesis reaction;
s3: obtaining MoS 2 After the reaction is finished, naturally cooling to room temperature, removing the mixed solution, respectively cleaning for 3 times by using absolute ethyl alcohol and deionized water, and finallyDrying in a drying oven at 60deg.C for 10 hr, and agate grinding to obtain black powder (MoS) 2 ；
S4: stirring and weighing 50mgMoS 2 The powder is placed in a beaker filled with 100m deionized water, and is subjected to ultrasonic treatment for 30min to obtain solution A;
s5: dissolving, adding 0.5-5g of ferrous ammonium sulfate (Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O) dissolving in 50ml deionized water to obtain solution B;
s6: naOH was added, and after the sonication in S4 was completed, 5ml of NaOH solution was added to the A solution and stirred for 10min to produce negatively charged MoS 2 The particles are solution C;
s7: regulatory structure will contain 5-20wt% MoS 2 Fe of (2) 2+ Solution B was slowly poured into solution C, followed by the addition of 2ml H 2 O 2 (30%), the final pH value is regulated to 12 by rapidly oxidizing and synthesizing delta-FeOOH firmly attached to the surface of molybdenum disulfide, and the morphology and structure of the catalyst are regulated and controlled;
s8: obtaining a catalyst, stirring for 10min, standing for aging for 3h, centrifuging the material, alternately cleaning with deionized water and absolute ethyl alcohol for 3-6 times, and vacuum drying at 60 ℃ for 12h to obtain MoS 2 delta-FeOOH heterojunction catalyst.
Further, in the step S1, ethylene glycol is used as a solvent, and sodium molybdate and thiourea are used as a Mo source and an S source.
On the basis of the scheme, the solvothermal synthesis temperature in the S2 is controlled at 180 ℃, and the reaction time is 24 hours.
As a still further scheme of the invention, the volume ratio of the ionized water to the absolute ethyl alcohol in the S3 is 1:1.
Further, the ultrasonic treatment in the step S4 is carried out for 30min to enable MoS 2 The powder was well dispersed and the reaction environment was at room temperature.
On the basis of the scheme, the concentration of NaOH in the S6 is 2mol/L, and the addition of the NaOH in the S6 ensures MoS 2 The surface is negatively charged.
As a still further aspect of the present invention, in S7H 2 O 2 Is added to provide Fe 2+ The ph=12 in S7 can regulate the morphology and structure of the catalyst.
Further, the aging for 3 hours in S8 is favorable for firmly attaching delta-FeOOH to MoS 2 Is a surface of the substrate.
The invention also provides application of the high-efficiency catalytic oxidation heterojunction material, which is used as a catalyst for degradation test, and comprises the following steps:
simulation light: selecting a 35W xenon lamp to simulate visible light for a photocatalytic degradation experiment;
and (3) preparing pollutants: 2ml of RhB solution (1 g/L) is diluted in 100ml of deionized water, namely the concentration of pollutants is 20mg/L;
stirring: placing the beaker in a constant-temperature heating magnetic stirrer, and maintaining the reaction temperature at 25+/-1 ℃;
adsorption analysis: weighing 0.3g/L of catalyst, dispersing in the pollutant solution, and stirring for 30min after light-shielding treatment to achieve adsorption-analysis balance experiment;
adding an oxidant: placing the preheated 35W xenon lamp above a beaker, and simultaneously adding 1mmol/L PMS oxidant solution;
sampling: 4mL of the solution was aspirated every 5min with 10mL syringe and filtered through a 0.45um aqueous filter to 1mLNaNO 2 (0.2M) quencher in a sample vial;
the result is obtained: a certain amount of filtrate was loaded through a quartz cuvette and different concentrations of RhB were tested using an ultraviolet-visible spectrophotometer at a wavelength of 554 nm.
(III) beneficial effects
Compared with the prior art, the invention provides a preparation method and application of a high-efficiency catalytic oxidation heterojunction material, and the preparation method has the following beneficial effects:
1. MoS in the present invention 2 The delta-FeOOH heterojunction can excite the interconversion between Fe (II) and Fe (III) and between Mo (IV) and Mo (VI), PMS is taken as an electron acceptor, and the photo-generated electrons and the active component Mo (IV) on the surface of the catalyst are effectively activated, so that the recombination of photo-generated electron-hole pairs is effectively inhibited, and the catalyst has the advantages ofThe high oxidation-reduction potential (E0=2.5-3.1V) has a wider pH application range (3-9) and stronger selectivity.
2. The invention not only considers the high-efficiency catalytic performance of the catalyst, but also fully considers the cost of a reaction system and the environment-friendly aspect by carrying out catalytic oxidation under visible light, thereby improving MoS 2 Actual application value of the delta-FeOOH/PMS/vis system in wastewater treatment.
3. The heterojunction structure and the visible light introduction in the invention have strong oxidizing capability to the difficult degradation pollutant and good removing effect.
Drawings
FIG. 1 is MoS 2 delta-FeOOH and MoS 2 Degradation effect of dye RhB in PMS/vis system without catalyst;
FIG. 2 is a MoS prepared 2 SEM image of photoelectrodes;
FIG. 3 is a MoS prepared 2 Schematic of the delta-FeOOH reaction;
FIG. 4 is a schematic flow chart of a method for preparing a high-efficiency catalytic oxidation heterojunction material
FIG. 5 shows a high efficiency catalytic oxidation MoS 2 Schematic flow structure diagram of degradation test by using delta-FeOOH heterojunction material as catalyst.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1 to 5, a method for preparing a high-efficiency catalytic oxidation heterojunction material includes the following steps:
s1: mixing, taking 3g of sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution;
s2: drying, namely slowly transferring the mixed solution in the step S1 into a 100ml reaction kettle, and preserving heat for 24 hours at 180 ℃ in a forced air drying box to perform a synthesis reaction;
s3: obtaining MoS 2 Naturally cooling to room temperature after the reaction is finished, removing the mixed solution, respectively cleaning for 3 times by using absolute ethyl alcohol and deionized water, finally placing the mixed solution in a drying oven at 60 ℃ for drying for 10 hours, and carrying out agate grinding on the obtained black solid to obtain black powder which is MoS 2 ；
S4: stirring and weighing 50mgMoS 2 The powder is placed in a beaker filled with 100m deionized water, and is subjected to ultrasonic treatment for 30min to obtain solution A;
s5: dissolving, 4.189g of ferrous ammonium sulfate (Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O) dissolving in 50ml deionized water to obtain solution B;
s6: naOH was added, and after the sonication in S4 was completed, 5ml of NaOH solution was added to the A solution and stirred for 10min to produce negatively charged MoS 2 The particles are solution C;
s7: regulatory structure will contain 20wt% mos 2 Fe of (2) 2+ Solution B was slowly poured into solution C, followed by the addition of 2ml H 2 O 2 (30%), the final pH value is regulated to 12 by rapidly oxidizing and synthesizing delta-FeOOH firmly attached to the surface of molybdenum disulfide, and the morphology and structure of the catalyst are regulated and controlled;
s8: obtaining a catalyst, stirring for 10min, standing for aging for 3h, centrifuging the material, alternately cleaning with deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 60 ℃ for 12h to obtain MoS 2 Delta-FeOOH heterojunction catalyst, moS 2 The delta-FeOOH heterojunction can excite the mutual conversion between Fe (II) and Fe (III) and between Mo (IV) and Mo (VI), PMS is used as an electron acceptor, the photogenerated electrons and the active component Mo (IV) on the surface of the catalyst are effectively activated, so that the recombination of the photogenerated electron-hole pairs is effectively inhibited, the high redox potential (E0=2.5-3.1V) is realized, the wide pH application range (3-9) is realized, and the high selectivity is realized.
In the invention, in particular, glycol is used as a solvent in S1, sodium molybdate and thiourea are used as Mo sources and S sources, the solvothermal synthesis temperature in S2 is controlled at 180 ℃, the reaction time is 24h, the volume ratio of ionized water to absolute ethyl alcohol in S3 is 1:1, and ultrasonic treatment is carried out for 30min in S4 to lead MoS to be obtained 2 The powder is fully dispersed, the reaction environment is carried out at room temperature, the concentration of NaOH in S6 is 2mol/L, and the addition of NaOH in S6 ensures MoS 2 The surface is negatively charged, H in S7 2 O 2 Is added to provide Fe 2+ The pH=12 in S7 can regulate the shape and structure of the catalyst, and the aging for 3 hours in S8 is favorable for firmly attaching delta-FeOOH to MoS 2 Is a surface of the substrate.
The invention also provides application of the high-efficiency catalytic oxidation heterojunction material, which is used as a catalyst for degradation test, and comprises the following steps:
simulation light: selecting a 35W xenon lamp to simulate visible light for a photocatalytic degradation experiment;
and (3) preparing pollutants: 2ml of RhB solution (1 g/L) is diluted in 100ml of deionized water, namely the concentration of pollutants is 20mg/L;
stirring: placing the beaker in a constant-temperature heating magnetic stirrer, and maintaining the reaction temperature at 25+/-1 ℃;
adsorption analysis: weighing 0.3g/L of catalyst, dispersing in the pollutant solution, and stirring for 30min after light-shielding treatment to achieve adsorption-analysis balance experiment;
adding an oxidant: placing the preheated 35W xenon lamp above a beaker, and simultaneously adding 1mmol/L PMS oxidant solution;
sampling: 4mL of the solution was aspirated every 5min with 10mL syringe and filtered through a 0.45um aqueous filter to 1mLNaNO 2 (0.2M) quencher in a sample vial;
the result is obtained: the quartz cuvette is used for loading a certain amount of filtrate, the ultraviolet-visible spectrophotometer is used for testing different concentrations of RhB under the wavelength of 554nm, and the catalytic oxidation is carried out under the visible light, so that not only the high-efficiency catalytic performance of the catalyst is considered, but also the cost of a reaction system and the environment-friendly formula are fully consideredFlour with improved MoS 2 Actual application value of the delta-FeOOH/PMS/vis system in wastewater treatment.
Example 2
Referring to fig. 1 to 5, a method for preparing a high-efficiency catalytic oxidation heterojunction material includes the following steps:
s1: mixing, taking 4g of sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution;
s2: drying, namely slowly transferring the mixed solution in the step S1 into a 100ml reaction kettle, and preserving heat for 24 hours at 180 ℃ in a forced air drying box to perform a synthesis reaction;
s3: obtaining MoS 2 Naturally cooling to room temperature after the reaction is finished, removing the mixed solution, respectively cleaning for 3 times by using absolute ethyl alcohol and deionized water, finally placing the mixed solution in a drying oven at 60 ℃ for drying for 10 hours, and carrying out agate grinding on the obtained black solid to obtain black powder which is MoS 2 ；
S4: stirring and weighing 50mgMoS 2 The powder is placed in a beaker filled with 100m deionized water, and is subjected to ultrasonic treatment for 30min to obtain solution A;
s5: 1.984g of ferrous ammonium sulfate (Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O) dissolving in 50ml deionized water to obtain solution B;
s6: naOH was added, and after the sonication in S4 was completed, 5ml of NaOH solution was added to the A solution and stirred for 10min to produce negatively charged MoS 2 The particles are solution C;
s7: regulatory structure will contain 10wt% mos 2 Fe of (2) 2+ Solution B was slowly poured into solution C, followed by the addition of 2ml H 2 O 2 (30%), the final pH value is regulated to 12 by rapidly oxidizing and synthesizing delta-FeOOH firmly attached to the surface of molybdenum disulfide, and the morphology and structure of the catalyst are regulated and controlled;
s8: obtaining a catalyst, stirring for 10min, standing for aging for 3h, centrifuging the material, alternately cleaning with deionized water and absolute ethyl alcohol for 5 times, and vacuum drying at 60 ℃ for 12h to obtain MoS 2 Delta-FeOOH heterojunction catalyst, moS 2 The delta-FeOOH heterojunction can excite the mutual conversion between Fe (II) and Fe (III) and between Mo (IV) and Mo (VI), PMS is used as an electron acceptor, the photogenerated electrons and the active component Mo (IV) on the surface of the catalyst are effectively activated, so that the recombination of the photogenerated electron-hole pairs is effectively inhibited, the high redox potential (E0=2.5-3.1V) is realized, the wide pH application range (3-9) is realized, and the high selectivity is realized.
In the invention, in particular, glycol is used as a solvent in S1, sodium molybdate and thiourea are used as Mo sources and S sources, the solvothermal synthesis temperature in S2 is controlled at 180 ℃, the reaction time is 24h, the volume ratio of ionized water to absolute ethyl alcohol in S3 is 1:1, and ultrasonic treatment is carried out for 30min in S4 to lead MoS to be obtained 2 The powder is fully dispersed, the reaction environment is carried out at room temperature, the concentration of NaOH in S6 is 2mol/L, and the addition of NaOH in S6 ensures MoS 2 The surface is negatively charged, H in S7 2 O 2 Is added to provide Fe 2+ The pH=12 in S7 can regulate the shape and structure of the catalyst, and the aging for 3 hours in S8 is favorable for firmly attaching delta-FeOOH to MoS 2 Is a surface of the substrate.
The invention also provides application of the high-efficiency catalytic oxidation heterojunction material, which is used as a catalyst for degradation test, and comprises the following steps:
simulation light: selecting a 35W xenon lamp to simulate visible light for a photocatalytic degradation experiment;
and (3) preparing pollutants: 2ml of RhB solution (1 g/L) is diluted in 100ml of deionized water, namely the concentration of pollutants is 20mg/L;
stirring: placing the beaker in a constant-temperature heating magnetic stirrer, and maintaining the reaction temperature at 25+/-1 ℃;
adsorption analysis: weighing 0.3g/L of catalyst, dispersing in the pollutant solution, and stirring for 30min after light-shielding treatment to achieve adsorption-analysis balance experiment;
adding an oxidant: placing the preheated 35W xenon lamp above a beaker, and simultaneously adding 1mmol/L PMS oxidant solution;
sampling: sucking 4mL of the solution with 10mL needle tube every 5min, and filtering with 0.45um water filter headWith 1mLNaNO 2 (0.2M) quencher in a sample vial;
the result is obtained: the quartz cuvette is used for loading a certain amount of filtrate, the ultraviolet-visible spectrophotometer is used for testing different concentrations of RhB under the wavelength of 554nm, and the catalytic oxidation is carried out under the visible light, so that the high-efficiency catalytic performance of the catalyst is considered, the cost of a reaction system and the environment-friendly aspect are fully considered, and the MoS is improved 2 Actual application value of the delta-FeOOH/PMS/vis system in wastewater treatment.
Example 3
Referring to fig. 1 to 5, a method for preparing a high-efficiency catalytic oxidation heterojunction material includes the following steps:
s1: mixing, taking 5g of sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution;
s2: drying, namely slowly transferring the mixed solution in the step S1 into a 100ml reaction kettle, and preserving heat for 24 hours at 180 ℃ in a forced air drying box to perform a synthesis reaction;
s3: obtaining MoS 2 Naturally cooling to room temperature after the reaction is finished, removing the mixed solution, respectively cleaning for 3 times by using absolute ethyl alcohol and deionized water, finally placing the mixed solution in a drying oven at 60 ℃ for drying for 10 hours, and carrying out agate grinding on the obtained black solid to obtain black powder which is MoS 2 ；
S4: stirring and weighing 50mgMoS 2 The powder is placed in a beaker filled with 100m deionized water, and is subjected to ultrasonic treatment for 30min to obtain solution A;
s5: dissolving, 0.883g of ferrous ammonium sulfate (Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O) dissolving in 50ml deionized water to obtain solution B;
s6: naOH was added, and after the sonication in S4 was completed, 5ml of NaOH solution was added to the A solution and stirred for 10min to produce negatively charged MoS 2 The particles are solution C;
s7: regulatory structure will contain 5wt% mos 2 Fe of (2) 2+ Slowly pour solution B intoTo solution C, 2ml of H were then added 2 O 2 (30%), the final pH value is regulated to 12 by rapidly oxidizing and synthesizing delta-FeOOH firmly attached to the surface of molybdenum disulfide, and the morphology and structure of the catalyst are regulated and controlled;
s8: obtaining a catalyst, stirring for 10min, standing for aging for 3h, centrifuging the material, alternately cleaning with deionized water and absolute ethyl alcohol for 6 times, and vacuum drying at 60 ℃ for 12h to obtain MoS 2 Delta-FeOOH heterojunction catalyst, moS 2 The delta-FeOOH heterojunction can excite the mutual conversion between Fe (II) and Fe (III) and between Mo (IV) and Mo (VI), PMS is used as an electron acceptor, the photogenerated electrons and the active component Mo (IV) on the surface of the catalyst are effectively activated, so that the recombination of the photogenerated electron-hole pairs is effectively inhibited, the high redox potential (E0=2.5-3.1V) is realized, the wide pH application range (3-9) is realized, and the high selectivity is realized.
In the invention, in particular, glycol is used as a solvent in S1, sodium molybdate and thiourea are used as Mo sources and S sources, the solvothermal synthesis temperature in S2 is controlled at 180 ℃, the reaction time is 24h, the volume ratio of ionized water to absolute ethyl alcohol in S3 is 1:1, and ultrasonic treatment is carried out for 30min in S4 to lead MoS to be obtained 2 The powder is fully dispersed, the reaction environment is carried out at room temperature, the concentration of NaOH in S6 is 2mol/L, and the addition of NaOH in S6 ensures MoS 2 The surface is negatively charged, H in S7 2 O 2 Is added to provide Fe 2+ The pH=12 in S7 can regulate the shape and structure of the catalyst, and the aging for 3 hours in S8 is favorable for firmly attaching delta-FeOOH to MoS 2 Is a surface of the substrate.
The invention also provides application of the high-efficiency catalytic oxidation heterojunction material, which is used as a catalyst for degradation test, and comprises the following steps:
simulation light: selecting a 35W xenon lamp to simulate visible light for a photocatalytic degradation experiment;
and (3) preparing pollutants: 2ml of RhB solution (1 g/L) is diluted in 100ml of deionized water, namely the concentration of pollutants is 20mg/L;
stirring: placing the beaker in a constant-temperature heating magnetic stirrer, and maintaining the reaction temperature at 25+/-1 ℃;
adsorption analysis: weighing 0.3g/L of catalyst, dispersing in the pollutant solution, and stirring for 30min after light-shielding treatment to achieve adsorption-analysis balance experiment;
adding an oxidant: placing the preheated 35W xenon lamp above a beaker, and simultaneously adding 1mmol/L PMS oxidant solution;
sampling: 4mL of the solution was aspirated every 5min with 10mL syringe and filtered through a 0.45um aqueous filter to 1mLNaNO 2 (0.2M) quencher in a sample vial;
the result is obtained: the quartz cuvette is used for loading a certain amount of filtrate, the ultraviolet-visible spectrophotometer is used for testing different concentrations of RhB under the wavelength of 554nm, and the catalytic oxidation is carried out under the visible light, so that the high-efficiency catalytic performance of the catalyst is considered, the cost of a reaction system and the environment-friendly aspect are fully considered, and the MoS is improved 2 Actual application value of the delta-FeOOH/PMS/vis system in wastewater treatment.
In this description, it should be noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (9)
1. The preparation method of the high-efficiency catalytic oxidation heterojunction material is characterized by comprising the following steps of:
s1: mixing, collecting 3-5g sodium molybdate (Na 2 MoO 4 ·2H 2 O) and thiourea (CH) 4 N 2 S) dissolving in glycol solvent, and stirring ultrasonically for 30min to obtain mixed solution;
s2: drying, namely slowly transferring the mixed solution in the step S1 into a 100ml reaction kettle, and preserving heat for 24 hours at 180 ℃ in a forced air drying box to perform a synthesis reaction;
s3: obtaining MoS 2 Naturally cooling to room temperature after the reaction is finished, removing the mixed solution, respectively cleaning for 3 times by using absolute ethyl alcohol and deionized water, finally placing the mixed solution in a drying oven at 60 ℃ for drying for 10 hours, and carrying out agate grinding on the obtained black solid to obtain black powder which is MoS 2 ；
S4: stirring and weighing 50mgMoS 2 The powder is placed in a beaker filled with 100m deionized water, and is subjected to ultrasonic treatment for 30min to obtain solution A;
s5: dissolving, adding 0.5-5g of ferrous ammonium sulfate (Fe (NH) 4 ) 2 (SO 4 ) 2 ·6H 2 O) dissolving in 50ml deionized water to obtain solution B;
s6: naOH was added, and after the sonication in S4 was completed, 5ml of NaOH solution was added to the A solution and stirred for 10min to produce negatively charged MoS 2 The particles are solution C;
s7: regulatory structure will contain 5-20wt% MoS 2 Fe of (2) 2+ Solution B was slowly poured into solution C, followed by the addition of 2ml H 2 O 2 (30%), the final pH value is regulated to 12 by rapidly oxidizing and synthesizing delta-FeOOH firmly attached to the surface of molybdenum disulfide, and the morphology and structure of the catalyst are regulated and controlled;
s8: obtaining a catalyst, stirring for 10min, standing for aging for 3h, centrifuging the material, alternately cleaning with deionized water and absolute ethyl alcohol for 3-6 times, and vacuum drying at 60 ℃ for 12h to obtain MoS 2 delta-FeOOH heterojunction catalyst.
2. The method for preparing the high-efficiency catalytic oxidation heterojunction material according to claim 1, wherein ethylene glycol is used as a solvent, and sodium molybdate and thiourea are used as a Mo source and an S source in S1.
3. The method for preparing a high-efficiency catalytic oxidation heterojunction material according to claim 1, wherein the solvothermal synthesis temperature in the step S2 is controlled at 180 ℃ and the reaction time is 24h.
4. The method for preparing a high-efficiency catalytic oxidation heterojunction material according to claim 1, wherein the volume ratio of ionized water to absolute ethyl alcohol in the S3 is 1:1.
5. The method for preparing a high efficiency catalytic oxidation heterojunction material as claimed in claim 1, wherein said ultrasonic treatment in S4 is carried out for 30min to make MoS 2 The powder was well dispersed and the reaction environment was at room temperature.
6. The method for preparing a high-efficiency catalytic oxidation heterojunction material as claimed in claim 1, wherein the concentration of NaOH in S6 is 2mol/L, and the addition of NaOH in S6 enables MoS to be obtained 2 The surface is negatively charged.
7. The method for preparing a high efficiency catalytic oxidation heterojunction material as claimed in claim 1, wherein H in S7 2 O 2 Is added to provide Fe 2+ The ph=12 in S7 can regulate the morphology and structure of the catalyst.
8. The method for preparing a high-efficiency catalytic oxidation heterojunction material as claimed in claim 1, wherein 3h aging in S8 is favorable for firmly attaching delta-FeOOH to MoS 2 Is a surface of the substrate.
9. The application of the high-efficiency catalytic oxidation heterojunction material as a catalyst for degradation test comprises the following steps:
simulation light: selecting a 35W xenon lamp to simulate visible light for a photocatalytic degradation experiment;
and (3) preparing pollutants: 2ml of RhB solution (1 g/L) is diluted in 100ml of deionized water, namely the concentration of pollutants is 20mg/L;
stirring: placing the beaker in a constant-temperature heating magnetic stirrer, and maintaining the reaction temperature at 25+/-1 ℃;
adsorption analysis: weighing 0.3g/L of catalyst, dispersing in the pollutant solution, and stirring for 30min after light-shielding treatment to achieve adsorption-analysis balance experiment;
adding an oxidant: placing the preheated 35W xenon lamp above a beaker, and simultaneously adding 1mmol/L PMS oxidant solution;
sampling: 4mL of the solution was aspirated every 5min with 10mL syringe and filtered through a 0.45um aqueous filter to 1mLNaNO 2 (0.2M) quencher in a sample vial;
the result is obtained: a certain amount of filtrate was loaded through a quartz cuvette and different concentrations of RhB were tested using an ultraviolet-visible spectrophotometer at a wavelength of 554 nm.
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