CN109465037A - The magnetic CDs-MoS of micropollutants in a kind of degradation water2-Fe3O4The green synthesis method of catalysis material - Google Patents
The magnetic CDs-MoS of micropollutants in a kind of degradation water2-Fe3O4The green synthesis method of catalysis material Download PDFInfo
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- 230000015556 catabolic process Effects 0.000 title claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 17
- 238000001308 synthesis method Methods 0.000 title claims abstract description 6
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 45
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 28
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 11
- 239000008103 glucose Substances 0.000 claims abstract description 11
- 239000002135 nanosheet Substances 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 239000013049 sediment Substances 0.000 claims abstract description 6
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- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
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- 238000001291 vacuum drying Methods 0.000 claims description 2
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- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 238000004064 recycling Methods 0.000 abstract description 11
- 239000003651 drinking water Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 8
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- 238000007146 photocatalysis Methods 0.000 abstract description 5
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- 239000004065 semiconductor Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 6
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- 238000012512 characterization method Methods 0.000 description 5
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 241000446313 Lamella Species 0.000 description 3
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- 150000001875 compounds Chemical class 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
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- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- JNRLEMMIVRBKJE-UHFFFAOYSA-N 4,4'-Methylenebis(N,N-dimethylaniline) Chemical compound C1=CC(N(C)C)=CC=C1CC1=CC=C(N(C)C)C=C1 JNRLEMMIVRBKJE-UHFFFAOYSA-N 0.000 description 1
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention discloses a kind of magnetic CDs-MoS of micropollutants in degradation water2‑Fe3O4The green synthesis method of catalysis material.Method includes the following steps: (1) is by MoS2It is uniform with glucose mixed grinding, water is then added, after continuing grinding uniformly, washing, redisperse, centrifugation add water after collecting supernatant, obtain molybdenum disulfide nano sheet solution；(2) by MoS2Nanometer sheet solution is centrifuged and collects sediment, is re-dissolved in ethylene glycol, and FeCl is then added3•6H2O and NaAc reaction, is separated after cooling with magnet, then wash, dry, obtains magnetic CDs-MoS2‑Fe3O4Catalysis material.CDs-MoS of the invention2‑Fe3O4Catalysis material not only has high photocatalysis efficiency, but also can be carried out magnetic recovery recycling, solves the preparation and recycling problem of the catalytic degradation photochemical catalyst of micro- Organic Pollutants in current drinking water source.
Description
Technical field
The invention belongs to nanocatalyst preparation fields, and in particular to it is a kind of degradation water in micropollutants magnetic CDs-
MoS2-Fe3O4The green synthesis method of catalysis material.
Background technique
Since the stable water outlet of existing waterworks reduces, the micro-content organism type detected in raw water increases, perhaps
The presented micro- contamination characteristics in the water source of more drinking water.Organic dyestuff is widely used in weaving, the industries such as plastics and cosmetics.By
The dyestuff applied in its toxicity and antibiont degradability, industry will lead to the pollution at water source.Traditional micropollutants remove skill
Art mainly includes physical method, chemical method and bioanalysis, they not only cannot make pollutant obtain thorough mineralising, but also exist
The disadvantages of generating secondary pollution, processing cost high and poor selectivity.
In recent years, it is widely studied due to photocatalytic degradation improving efficiency and dropping the advantage of low cost aspect.
Photocatalysis technology almost can include stupid with all pairs of human bodies of catalytic degradation and the harmful part inorganic substances of environment and organic substance
Solid chlorinated aromatics including, which not only takes full advantage of nature resource abundant, such as the use of sunlight, neither unrestrained
Take resource, secondary pollution will not be caused, and improve reaction speed.Currently, being used for the photochemical catalyst master of photocatalytic degradation
If making semiconductor or new modified composite material, i.e., single photochemical catalyst and composite photocatalyst containing transistion metal compound
Agent.Single type catalyst mainly has TiO2, ZnO, Cds, WO3Deng.Composite photo-catalyst then has metal/semiconductor, metal-doped
Semiconductor, a variety of semiconductors couplings, the types such as transition metal complex.Light needed for the bandgap excitation of semiconductor light-catalyst
The difference of source, band gap size and energy leads to the difference of photocatalytic activity.Although some narrow-band semiconductor photochemical catalysts with it is visible
Light reaction, but optical instability and chemical instability due to its own and cannot act as good photochemical catalyst or individually
Using effect is poor.For example, iron oxide causes the slight erosion of anode to react, photocatalytic activity is not high；ZnO is unstable in water
It is fixed, Zn (OH) is formed in particle surface2；Metal sulfide becomes unstable under aqueous solution or illumination, can generate anodic attack
Reaction etc..So preparing convieniently synthesized, it has excellent performance and the strong photochemical catalyst of recuperability is still a problem.
Research in recent years shows molybdenum disulfide (MoS2) it is expected to the semiconductor material that substituted for silicon becomes of new generation.As one kind
Most representative material, MoS in transition metal dichalcogenide2Due to its excellent electronics, optics and catalytic property and permitted
It is multi-field to cause great interest.Importantly, MoS2It is a kind of ideal visible light-responded photochemical catalyst, it can be more
Fully utilize sunlight.When removing the layer at one or limited quantity, two-dimensional MoS2Since indirect band gap transitions are straight
Tape splicing gap and so that photocatalysis performance is got a promotion.Chemical stripping and solvent-thermal process are to prepare MoS2The common method of nanometer sheet.
However in actual application, MoS2Nanometer sheet is easy to lead to its more inertia basal plane of active edge exposure due to accumulation,
Lead to the decline and forfeiture of catalytic activity.In addition, if powdered nano material will be by particle aggregation without modification appropriate
Influence, make its optics, electronics and catalytic performance reduce, the potential application which prevent it in photocatalytic degradation.Therefore,
Some strategies are dedicated to modifying MoS with active biomolecule2Or use MoS2It is compound to form heterojunction structure to re-assembly compound
Object.However, most methods are all limited to special equipment or toxic solvent, these are molten due to complicated step and preparation process
Agent is unsustainable and unfriendly to environment.
In addition, many studies have shown that, carbon quantum dot (CDs) can be used as the receptor or donor of light induced electron, have high
Photocatalysis potential.Compared with traditional semiconductor-quantum-point, CDs not only has nontoxicity and is readily synthesized, but also has only
Special optical property, biocompatibility, chemical inertness and the good solubility in polar solvent.It is utilized in addition, CDs has
Long wavelength and energy conversion up-conversion luminescence ability, this enable the photochemical catalyst based on CDs using visible optical radiation into
Row catalysis.However, recycling for simple CDs needs to carry out additional separating step after the reaction, which prevent they
Potentiality in practical application.MoS is modified using CDs as a result,2MoS can be promoted simultaneously2Resistant to aggregation ability and CDs repetition benefit
With performance, having an opportunity to play its cooperative ability makes its Photocatalytic Degradation Property be improved significantly.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the object of the present invention is to provide a kind of magnetism CDs-MoS2-Fe3O4
Catalysis material and its synthetic method be applied to degradation micropollutants.
The purpose of the present invention is achieved through the following technical solutions.
The magnetic CDs-MoS of micropollutants in a kind of light degradation drinking water2-Fe3O4Green synthesis method, including it is following
Step:
(1) preparation of molybdenum disulfide nano sheet solution: by MoS2It is uniform with glucose mixed grinding, water is then added, continues to grind
It after mill is uniform, is washed with water, is redispersed in water and is centrifugated, added water after collecting supernatant, obtain MoS2Nanometer sheet is molten
Liquid；
(2) CDs-MoS2-Fe3O4Preparation: the MoS that step (1) is obtained2Nanometer sheet solution is centrifuged and collects sediment, then weighs
It is newly dissolved in ethylene glycol, FeCl is then added under stiring3·6H2O and NaAc continues that after mixing evenly, mixture is shifted
It reacts into reaction kettle, after naturally cool to room temperature, is separated with magnet, be washed with water and wash to remove impurity, and is dry, obtain magnetic
CDs-MoS2-Fe3O4Catalysis material.
Preferably, in step (1), MoS2Mass ratio with glucose is 1:9-1:17.
Preferably, in step (1), MoS2Dosage with glucose is respectively 100-200 mg and 1.2-1.8 g, distillation
The additive amount of water is 0.6 mL.
Preferably, in step (1), the number of the washing is 3 times.
Preferably, in step (1), the condition of the centrifuge separation is that 2000-3000 rpm is centrifuged 20 min.
Preferably, in step (1), gained molybdenum disulfide nano sheet solution be stored in 4 DEG C it is spare.
Preferably, in step (2), the condition of the centrifugation is that 12000 rpm are centrifuged 30 minutes.
Preferably, in step (2), MoS2Nanometer sheet solution, FeCl3·6H2The mass ratio of O and NaAc is 1:5:3.3.
Preferably, in step (2), FeCl3·6H2The dosage of O and NaAc is respectively 0.1 g and 0.66g.
Preferably, in step (2), the time of the reaction is 12 hours.
Preferably, in step (2), the drying is 60 DEG C of vacuum drying.
The case where the present invention is based on micro- Organic Pollutants of drinking water source, the degradation for inventing a kind of organic pollutant are magnetic
CDs-MoS2-Fe3O4Catalysis material, mainly for molybdenum disulfide because easily aggregation causes catalytic activity to reduce with carbon quantum dot not
The problem of easily recycling, removes using glucose assisted milling and modifies MoS2, by MoS2Make glucose de- in situ on surface
Water quickly to prepare the CDs-MoS of CDs modification2-Fe3O4Nano-complex.This simple method synthesizes lamella with can be convenient
MoS2Nanometer sheet, and glucose can be made in MoS2Surface forms the carbonyl-functionalized CDs with strong binding force, generates efficient
Collaboration-catalytic action altogether.In addition, Fe3O4Introducing provide not only effective Magneto separate and the recycling of photochemical catalyst, Er Qieyou
In with MoS2It forms heterojunction structure and further promotes photocatalytic activity.The CDs-MoS of the method preparation2-Fe3O4Nanometer is multiple
Closing object not only has high photocatalysis efficiency, but also can be carried out magnetic recovery recycling, solves micro- in current drinking water source
The preparation and recycling problem of the catalytic degradation photochemical catalyst of Organic Pollutants.
Compared with prior art, the present invention has the advantage that
(1) this simple method of the present invention synthesizes MoS with can be convenient2Nanometer sheet, and by solvent thermal process, one kettle way is fast
The CDs-MoS of speed preparation multilayered structure2-Fe3O4Nano-complex is not necessarily to many more manipulations.
(2) material prepared by the present invention is with MoS2Nanometer sheet is as carrier, by CDs and Fe3O4It is compound simultaneously, reach weight
Purpose is recycled again, solves the problems, such as that CDs recycles cumbersome difficulty.
(3) MoS2Strong absorption efficiency and CDs and Fe in visible-range3O4Synergistic effect, further improve
Its Photocatalytic Degradation Property.
(4) catalysis material prepared by the present invention has fabulous catalytic activity, adds in the material of only 25 μ g/ ml
Under amount, 96.8% is up to for the degradation rate of drinking water Methylene Blue.
(5) catalysis material prepared by the present invention shows excellent reusability by magnetic separation, at 4 times
It repeats after recycling, the degradation efficiency of drinking water Methylene Blue is remained to reach 94.5%.
Detailed description of the invention
Fig. 1 a, Fig. 1 b are MoS in embodiment 1 and embodiment 2 respectively2The scanning electron microscope (SEM) photograph of nanometer sheet.
Fig. 2 a, Fig. 2 b, Fig. 2 c are embodiment 3, CDs-MoS in embodiment 4 and embodiment 5 respectively2-Fe3O4Scanning electron microscope
Figure.
Fig. 3 is blocky MoS2, MoS2Nanometer sheet and CDs-MoS2-Fe3O4The light of organic extracts from water methylene blue is urged
Change degradation curve figure.
Fig. 4 is CDs-MoS2-Fe3O4Recycle huge profit degradation organic extracts from water curve graph.
Specific experiment mode
Implementation of the invention is further described below in conjunction with example and attached drawing, but embodiments of the present invention are not limited to
This.
Embodiment 1
The preparation of molybdenum disulfide nano sheet: 150 mg MoS are weighed respectively2With 2.5 g glucose in mortar, and carry out 10
Min is tentatively ground.Later, 0.6 mL distilled water is added in mortar, continues to grind 2 h.After grinding, carried out three times with water
Washing.Finally, material is dispersed in water and 3000 rpm is used to be centrifuged 20 min, collect supernatant and is dissolved in 100 mL surely, protect
Be stored in 4 DEG C it is spare.MoS2The yield of nanometer sheet is 8%.Scanning electron microscope characterization result shows that its lamella is relatively thin, but part is accumulated
It is unstripped, there is good peeling effect (see Fig. 1 a).
Embodiment 2
The preparation of molybdenum disulfide nano sheet: 150 mg MoS are weighed respectively2With 1.4 g glucose in mortar, and carry out 10
Min is tentatively ground.Later, 0.6 mL distilled water is added in mortar, continues to grind 2 h.After grinding, carried out three times with water
Washing.Finally, material is dispersed in water and 3000 rpm is used to be centrifuged 20 min, collect supernatant and is dissolved in 100 mL surely, protect
Be stored in 4 DEG C it is spare.MoS2The yield of nanometer sheet is 21%.Scanning electron microscope characterization result shows that its lamella is very thin, is uniformly dispersed, has
Extraordinary peeling effect (see Fig. 1 b).
Embodiment 3
The preparation of molybdenum disulfide nano sheet is the same as embodiment 2.CDs-MoS2-Fe3O4Preparation: 40ml(0.5mg/mL) is ground
The MoS arrived2Nanometer sheet solution is centrifuged 30 minutes with 12000 rpm and collects sediment, then is re-dissolved in 40mL ethylene glycol.
Then under stiring by 0.05 g FeCl3·6H2O and 0.33 g NaAc are slowly added in suspension.Continue stirring 30 minutes
Afterwards, mixture is transferred in reaction kettle and is reacted 12 hours at 200 DEG C.After naturally cool to room temperature, is separated and be made with magnet
Product, and be washed with deionized for several times to remove impurity, be finally dried in vacuo in 60 DEG C.Scanning electron microscope characterization result can be with
See apparent sandwich lamellar structure, surface uniform load nano particle, but its load capacity is insufficient, may influence its catalytic effect
(see Fig. 2 a).
Embodiment 4
The preparation of molybdenum disulfide nano sheet is the same as embodiment 2.CDs-MoS2-Fe3O4Preparation: 40ml(0.5mg/mL) is ground
The MoS arrived2Nanometer sheet solution is centrifuged 30 minutes with 12000 rpm and collects sediment, then is re-dissolved in 40mL ethylene glycol.
Then under stiring by 0.2 g FeCl 3•6H 2O and 1.32 g NaAc are slowly added in suspension.Continue stirring 30 minutes
Afterwards, mixture is transferred in reaction kettle and is reacted 12 hours at 200 DEG C.After naturally cool to room temperature, is separated and be made with magnet
Product, and be washed with deionized for several times to remove impurity, be finally dried in vacuo in 60 DEG C.Scanning electron microscope characterization result can be with
See apparent sandwich lamellar structure, surface uniform load nano particle, but its load capacity is excessive, may shield the MoS at center2
Nanometer sheet influences its catalytic effect (see Fig. 2 b).
Embodiment 5
The preparation of molybdenum disulfide nano sheet is the same as embodiment 2.CDs-MoS2-Fe3O4Preparation: 40ml(0.5mg/mL) is ground
The MoS arrived2Nanometer sheet solution is centrifuged 30 minutes with 12000 rpm and collects sediment, then is re-dissolved in 40mL ethylene glycol.
Then under stiring by 0.1 g FeCl3·6H2O and 0.66 g NaAc are slowly added in suspension.After continuing stirring 30 minutes,
Mixture is transferred in reaction kettle and is reacted 12 hours at 200 DEG C.After naturally cool to room temperature, obtained produce is separated with magnet
Object, and be washed with deionized for several times to remove impurity, finally it is dried in vacuo in 60 DEG C.Scanning electron microscope characterization result can see
Complete sandwich lamellar structure, area load nano particle size is appropriate, is evenly distributed, can play good heterojunction structure (see
Fig. 2 c).
Embodiment 6
The preparation of molybdenum disulfide nano sheet is the same as embodiment 2.CDs-MoS2-Fe3O4Preparation with embodiment 5.Photocatalytic degradation methylene
Base indigo plant dyestuff: using 300W xenon lamp and AM1.5G optical filter as irradiation source, simulate 1 sun light intensity, passes through drinking water of degrading
The test bulk MoS of Methylene Blue2, MoS2Nanometer sheet and CDs-MoS2-Fe3O4Catalytic degradation organic extracts from water energy
Power.Containing 1 mL MB solution (2 × 10-3Mol/L), 20 mL sample bottles of the fresh NaOH solution of 1 mL (0.01 mol/L)
In be separately added into the blocky MoS of 0.5 mg2, MoS2Nanometer sheet and CDs-MoS2-Fe3O4As catalyst.Obtain the dyestuff such as Fig. 3
Degradation curve, catalytic effect CDs-MoS2-Fe3O4>MoS2Nanometer sheet > bulk MoS2, CDs-MoS2-Fe3O4Catalysis degradation modulus energy
Reach 96.8%.
Embodiment 7
The preparation of molybdenum disulfide nano sheet is the same as embodiment 2.CDs-MoS2-Fe3O4Preparation with embodiment 5.CDs-MoS2-Fe3O4
Recycling huge profit is used: being used 300W xenon lamp and AM1.5G optical filter as irradiation source, is simulated 1 sun light intensity, is drunk by degradation
The test bulk MoS of water Methylene Blue2, MoS2Nanometer sheet and CDs-MoS2-Fe3O4Catalytic degradation organic extracts from water
Ability.Containing 1 mL MB solution (2 × 10-3Mol/L), 20 mL samples of the fresh NaOH solution of 1 mL (0.01 mol/L)
The CDs-MoS of 0.5 mg is separately added into bottle2-Fe3O4As catalyst.After reaction, pass through external magnetic field quick separating and collection
Then catalyst is rinsed with a large amount of water.It will be followed for the second time in the mixture of the catalyst redisperse of recycling to new reactant
Ring utilizes, and identical program is carried out in subsequent circulation.Degradation effect is detected using ultraviolet spectrophotometry.Every time
It is independent catalysis in, with the progress of catalysis, UV absorption obviously weakens, and catalytic effect is significant.Due in recycling for material
Material has certain loss slightly, and catalytic effect has faint decline, but its CDs-MoS after circulation 4 times2-Fe3O4Catalysis drop
Solution rate, which remains to be maintained at 94.5%(, sees Fig. 4).
Claims (9)
1. the magnetic CDs-MoS of micropollutants in a kind of degradation water2-Fe3O4The green synthesis method of catalysis material, feature
It is, comprising the following steps:
(1) preparation of molybdenum disulfide nano sheet solution: by MoS2It is uniform with glucose mixed grinding, water is then added, continues to grind
It after uniformly, is washed with water, is redispersed in water and is centrifugated, added water after collecting supernatant, obtain MoS2Nanometer sheet solution；
(2) CDs-MoS2-Fe3O4Preparation: the MoS that step (1) is obtained2Nanometer sheet solution is centrifuged and collects sediment, then weighs
It is newly dissolved in ethylene glycol, FeCl is then added under stiring3·6H2O and NaAc continues that after mixing evenly, mixture is shifted
It reacts into reaction kettle, after naturally cool to room temperature, is separated with magnet, be washed with water and wash to remove impurity, and is dry, obtain magnetic
CDs-MoS2-Fe3O4Catalysis material.
2. the method according to claim 1, wherein in step (1), MoS2Mass ratio with glucose is 1:
9-1:17。
3. the method according to claim 1, wherein the condition of the centrifuge separation is 2000- in step (1)
3000 rpm are centrifuged 20 min.
4. the method according to claim 1, wherein the condition of the centrifugation is 12000 rpm in step (2)
Centrifugation 30 minutes.
5. the method according to claim 1, wherein in step (2), FeCl3·6H2The mass ratio of O and NaAc is
1:6.6。
6. the method according to claim 1, wherein in step (2), FeCl3·6H2O and NaAc amount ranges point
It Wei not 0.05-0.2g and 0.33-1.32g.
7. the method according to claim 1, wherein the temperature of the reaction is 200 DEG C in step (2).
8. the method according to claim 1, wherein the time of the reaction is 12 hours in step (2).
9. the method according to claim 1, wherein the drying is 60 DEG C of vacuum drying in step (2).
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| CN110444409A (en) * | 2019-07-24 | 2019-11-12 | 长安大学 | A kind of CQDs-MoS2- ZnS composite material, preparation method and application |
| CN111992229A (en) * | 2020-08-24 | 2020-11-27 | 广西师范大学 | Fe2O3-CoSe2Preparation method of @ Se oxygen evolution electrocatalyst |
| CN113457706A (en) * | 2021-06-23 | 2021-10-01 | 江苏大学 | Synthesis of N-BiOBr/CQDs/Fe by pollutant template element filling strategy3O4And applications thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110444409A (en) * | 2019-07-24 | 2019-11-12 | 长安大学 | A kind of CQDs-MoS2- ZnS composite material, preparation method and application |
| CN110444409B (en) * | 2019-07-24 | 2021-08-13 | 长安大学 | CQDs-MoS2-ZnS composite material, preparation method and application |
| CN111992229A (en) * | 2020-08-24 | 2020-11-27 | 广西师范大学 | Fe2O3-CoSe2Preparation method of @ Se oxygen evolution electrocatalyst |
| CN113457706A (en) * | 2021-06-23 | 2021-10-01 | 江苏大学 | Synthesis of N-BiOBr/CQDs/Fe by pollutant template element filling strategy3O4And applications thereof |
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