CN110227525A - A kind of two dimension catalysis material and preparation method thereof and its application method - Google Patents
A kind of two dimension catalysis material and preparation method thereof and its application method Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 68
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 100
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims abstract description 42
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 32
- 239000006227 byproduct Substances 0.000 claims abstract description 31
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 29
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 claims abstract description 15
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 12
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 12
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
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- 230000002459 sustained effect Effects 0.000 claims abstract description 6
- 235000019441 ethanol Nutrition 0.000 claims description 31
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 25
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 17
- 238000005286 illumination Methods 0.000 claims description 16
- 238000005119 centrifugation Methods 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
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- 238000007146 photocatalysis Methods 0.000 claims description 11
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- 230000000052 comparative effect Effects 0.000 description 40
- VMXUWOKSQNHOCA-LCYFTJDESA-N ranitidine Chemical compound [O-][N+](=O)/C=C(/NC)NCCSCC1=CC=C(CN(C)C)O1 VMXUWOKSQNHOCA-LCYFTJDESA-N 0.000 description 31
- 229960000620 ranitidine Drugs 0.000 description 31
- UMFJAHHVKNCGLG-UHFFFAOYSA-N n-Nitrosodimethylamine Chemical compound CN(C)N=O UMFJAHHVKNCGLG-UHFFFAOYSA-N 0.000 description 20
- 230000003197 catalytic effect Effects 0.000 description 15
- 230000000694 effects Effects 0.000 description 14
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
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- 238000002835 absorbance Methods 0.000 description 4
- 230000033558 biomineral tissue development Effects 0.000 description 4
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- 238000011160 research Methods 0.000 description 4
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- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
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- 229910021389 graphene Inorganic materials 0.000 description 3
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
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- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910017435 S2 In Inorganic materials 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
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- 238000005530 etching Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- B01J35/39—
-
- B01J35/61—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention discloses a kind of two-dimentional catalysis material and preparation method thereof and its application methods, and wherein preparation method includes: by Ti3C2Powder is placed in ethanol solution, is centrifuged after fully dispersed to solution, takes upper layer suspension spare；Sodium molybdate and thiocarbamide are dissolved into Ti3C2In the suspension of ethanol solution, stirs evenly and fully dispersed, obtain mixed solution；Mixed solution is carried out to be heated to predetermined temperature sustained response a few hours, obtains reaction product；Reaction product is dried, grind, is filtered, two-dimentional catalysis material MoS is obtained2/Ti3C2.Composite photocatalyst material MoS made from preparation method of the invention2/Ti3C2It is by MoS2With Ti3C2It is combined, the compound specific surface area for increasing material of two kinds of two-dimensional materials, the heterojunction structure of formation substantially increases the photocatalytic activity of composite material, to obtain the MoS for capableing of efficient degradation nitrosamine disinfection by-products formation potential under visible light2/Ti3C2Composite material.
Description
Technical field
The present invention relates to Photocatalyst more particularly to a kind of two-dimentional catalysis material and preparation method thereof and
Its application method.
Background technique
Recently as the improvement of people's living standards, people are greatly improved to the attention rate of drinking water quality.
The water outlet of natural water factory generally requires to disinfect by chlorine or chloramination, however, some natural organic matter meetings in drinking water
The disinfection by-products for generating and being harmful to human health is reacted with disinfectant, wherein more representational is nitrosodimethylamine
(NDMA), because its height is carcinogenic, teratogenesis due to attract wide public concern.Nitrosamine disinfection by-products once generates, it is extremely difficult to it is removed,
So nitrosamine control will be set about from the control of precursor.It is wherein ranitidine than more typical nitrosamine precursor, it is
It is currently known the precursor for being easiest to generate NDMA in precursor.
In recent years, gradually increased using the research of Photocatalitic Technique of Semiconductor degradation of contaminant.Conductor photocatalysis purification
Technology becomes a kind of emerging depollution of environment technology because of its energy-efficient, environmentally protective advantage.So far, semiconductor
Photochemical catalyst has been applied successfully to multiple fields, including photocatalytically degradating organic dye, solar battery, photolysis water hydrogen
Deng.
Two-dimension nano materials are because of its unique layer structure and show unique physical property and chemical property, thus
Cause the great interest of researcher.Especially in photocatalysis field, two-dimensional material has unique structure, biggish specific surface
Long-pending, preferable crystal structure and active site abundant, are urged at the advantages that enhancing the separation rate of carrier in the light of organic dyestuff
Change the fields such as degradation and shows excellent performance.Two-dimentional photocatalyst material common at present mainly has: two-dimensional metallic oxidation
Object lamella, nano metal sulfide piece, carbonitride and transition metal carbonitrides etc..Molybdenum disulfide (MoS2), as one kind
Novel two-dimensional structure material has the structure similar with graphene.Suitable forbidden bandwidth can guarantee MoS2In visible light
The photocatalysis performance (visible light account for about sunshine gross energy 46%) of range.However, pure MoS2Photo-generate electron-hole pairs
Recombination rate it is high, photocatalysis performance is lower, these factors inhibit it in the application of photocatalysis field.
In carbonitride, MXenes has and graphene as a kind of two-dimensional layer material emerging in recent years
The features such as similar unique layer structure and good hydrophily, in the photocatalytic degradation field of organic dyestuff
Using.It is studied by multiple trial, in 2011, the researchers such as the Michael Naguib of Univ Drexel utilized HF acid
As etching agent, successfully by Ti most representative in MAX phase3AlC2In Al erode, obtained a kind of two-dimensional layer
Ti3C2Tx(T be-F ,-OH functional group) because it has the two-dimensional structure similar to graphene, and is being removed by MAX phase, therefore
It is named as MXene.Up to the present, it is known that MAX phase material have more than 70 kinds, one of the most common type is Ti3AlC2.Two
Dimension stratiform MXenes family has been used in the research of field of environmental pollution control.Wherein, Ti3C2As being a kind of novel two
Layer structure material is tieed up, there is the features such as good hydrophily, environment friendly and chemical stability, had been applied in absorption
In the application of degradating organic dye.However, by the Ti of two-dimensional layered structure3C2Material is as photochemical catalyst, for nitrous of degrading
So far there is not been reported for the research of amine disinfection by-products formation potential, especially that it is compound with other two-dimensional materials, and being used for can
Catalytic degradation behavior under light-exposed, does not there is research so far.
The disclosure of background above technology contents is only used for auxiliary and understands design and technical solution of the invention, not necessarily
The prior art for belonging to present patent application, no tangible proof show above content present patent application the applying date
In disclosed situation, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
It is low to the utilization rate of sunlight in water treatment applications to solve photocatalysis technology, to emerging present in water environment
Pollutant (PPCPs) catalytic degradation effect is bad, can not the technical bottlenecks such as mineralising, the present invention propose it is a kind of can in visible light region
New Two Dimensional composite photocatalyst material with efficient degradation disinfection by-products formation potential and preparation method thereof and its under visible light
Degradation application to nitrosamine disinfection by-products formation potential.
In order to achieve the above object, the invention adopts the following technical scheme:
The invention discloses a kind of preparation methods of two-dimentional catalysis material, comprising the following steps:
S1: by Ti3C2Powder is placed in ethanol solution, is centrifuged after fully dispersed to solution, takes upper layer suspension standby
With；
S2: sodium molybdate and thiocarbamide are dissolved into the Ti that step S1 is obtained3C2In the suspension of ethanol solution, stir evenly simultaneously
It is fully dispersed, obtain mixed solution；
S3: the mixed solution that step S2 is obtained being carried out to be heated to predetermined temperature sustained response a few hours, is obtained reaction and is produced
Object；
S5: reaction product being dried, grind, is filtered, and obtains two-dimentional catalysis material MoS2/Ti3C2。
Preferably, the preparation method further include: further include step S4 between step S3 and step S5: step S3 is obtained
To reaction product deionized water and ethyl alcohol be centrifuged, wash multipass；Further, the rate of the centrifugation step in step S4
For 8000~11000r/min, centrifugation time is 10~30min.
Preferably, the mass concentration of the ethanol solution in step S1 is 5~20%；Further, by Ti in step S13C2
Powder is placed in ethanol solution specifically according to obtained Ti3C2The concentration of ethanol solution is 0.5~2mg/ml Ti is added3C2Powder
End.
Preferably, the rate of the centrifugation step in step S1 is 7000~9000r/min, and centrifugation time is 10~30min；
Whipping step in step S2 uses 0.5~2h of magnetic agitation；Further, the dispersion steps difference in step S1 and step S2
Using ultrasonic disperse, wherein the ultrasonic disperse in step S1 is 50~200W using power, and the time is 0.5~3h；Step S2
In ultrasonic disperse using power be 100~300W, the time be 0.5~3h.
Preferably, according to Ti in step S23C2Quality account for MoS2And Ti3C2The 5~20% of gross mass are by predetermined quality
Sodium molybdate and thiocarbamide be dissolved into the Ti of the predetermined volume that step S1 is obtained3C2In the suspension of ethanol solution；Further, it walks
The ratio between amount of substance of sodium molybdate and thiocarbamide is 1:3~1:10 in rapid S2.
Preferably, 180~220 DEG C are heated in step S3 in heating stepses, reacts 12~36h.
Preferably, the temperature of the drying steps in step S5 is 60~90 DEG C, and drying time is 8~18h, filtration step tool
Body uses the screen to filtrate 3 times or more of 200~400 mesh.
The invention also discloses a kind of two-dimentional catalysis materials, are made using above-mentioned preparation method.
The invention also discloses a kind of application methods of above-mentioned two-dimentional catalysis material, by the two-dimentional catalysis material
Applied to photocatalytic degradation disinfection by-products formation potential containing nitrosamine.
Preferably, the application method specifically includes: the two-dimentional catalysis material being placed in and sterilizes by-product containing nitrosamine
In the aqueous solution of object precursor, and illumination reaction is carried out under LED light；Further, containing the water-soluble of disinfection by-products formation potential
The concentration of liquid is 5~20mg/L, and the intensity of illumination of LED light is 10~50mW/cm2, the illumination reaction time is 0.5~2h.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention prepares two-dimentional catalysis material MoS2/Ti3C2Preparation method use hydro-thermal method, it is simple and easy, at
This is low, and synthesis condition is mild, is conducive to large-scale promotion.
(2) composite photocatalyst material MoS produced by the present invention2/Ti3C2It is by MoS2With Ti3C2It is combined, two kinds of two dimensions
Material cladding increases the specific surface area of material, and the heterojunction structure of formation substantially increases the photocatalytic activity of composite material,
The composite photocatalyst material has stronger optical absorption characteristics in visible region, natural light can be efficiently utilized, in visible region
Emerging pollutant (PPCPs) is catalytically decomposed in domain, solves the problems, such as that existing photochemical catalyst is not high to visible light utilization efficiency.
(3) two-dimentional catalysis material MoS produced by the present invention2/Ti3C2, thunder Buddhist nun can be catalytically decomposed in visible light region and replace
The PPCPs such as fourth, and effective mineralising can be reached, the mineralization rate in 1 hour can reach 41.81~73.58%, solves existing light and urges
The problems such as agent is low to high concentration (10mg/L) PPCPs degradation efficiency, mineralization rate is low.
(4) two-dimentional catalysis material MoS produced by the present invention2/Ti3C2In Ti3C2With good hydrophily, environment friend
The features such as good property and chemical stability, by MoS2With Ti3C2It is compound, it can use Ti3C2Biggish surface area is MoS2Growth mentions
For substrate, and MoS2The characteristic of semiconductor of variable band gap can also modify Ti3C2, the p-n heterojunction structure energy strengthening material of the two formation
The photocatalytic activity of material improves the degradation property of pollutant.
(5) two-dimentional catalysis material MoS produced by the present invention2/Ti3C2Under visible light to the PPCPs' such as ranitidine
NDMA formation potential can decline 82.92~97.99%, much higher than it has been reported that being a kind of safe and efficient water treatment technology.
In further embodiment, by adjusting MoS2And Ti3C2The adding proportion of two kinds of components can optimize obtained two
Tie up catalysis material MoS2/Ti3C2Under visible light to the degradation capability of nitrosamine disinfection by-products formation potential；Wherein in Ti3C2
Quality account for MoS2And Ti3C2Gross mass 5~20% when, MoS obtained2/Ti3C2By-product is sterilized to nitrosamine under visible light
The degradation capability of object precursor is more preferably.
Detailed description of the invention
Fig. 1 a is MoS made from comparative example 12Scanning electron microscope (SEM) photograph；
Fig. 1 b is Ti made from comparative example 23C2The scanning electron microscope (SEM) photograph of powder；
Fig. 1 c is two dimension catalysis material MoS made from Examples 1 to 52/Ti3C2Scanning electron microscope (SEM) photograph；
Fig. 2 a is MoS made from comparative example 12Transmission electron microscope picture；
Fig. 2 b is Ti made from comparative example 23C2The transmission electron microscope picture of powder；
Fig. 2 c is two dimension catalysis material MoS made from Examples 1 to 52/Ti3C2Transmission electron microscope picture；
Fig. 3 is MoS made from comparative example 12, Ti made from comparative example 23C2Powder and the difference of Examples 1 to 5 preparation
MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2Respectively for 10mg/L ranitidine in visible light
Under catalytic degradation effect figure；
Fig. 4 is MoS made from comparative example 12, Ti made from comparative example 23C2Powder and the difference of Examples 1 to 5 preparation
MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2The thunder Buddhist nun of degradation 10mg/L replaces under visible light respectively
The remineralization efficacy figure of fourth 60min；
Fig. 5 is MoS made from comparative example 12, Ti made from comparative example 23C2Powder and the difference of Examples 1 to 5 preparation
MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2The thunder Buddhist nun of degradation 10mg/L replaces under visible light respectively
NDMA before and after fourth generates gesture comparison diagram；
Fig. 6 is two-dimentional composite photocatalyst material MoS prepared by embodiment 42/Ti3C2Degradation 10mg/L is repeated under visible light
Ranitidine 5 times degradation effect figures.
Specific embodiment
Below against attached drawing and in conjunction with preferred embodiment, the invention will be further described.
The preferred embodiment of the present invention discloses a kind of preparation method of two-dimentional catalysis material, comprising the following steps:
S1: configuring certain density ethanol solution, weighs the Ti of certain mass3C2Powder is placed in ethanol solution, is sufficiently divided
Solution is centrifuged after dissipating, takes upper layer suspension spare；
Specifically, the concentration of ethanol solution is preferably 5~20%, and more preferably 10%；Weighed Ti3C2The quality of powder
Ti for 100mg, after dilution3C2The concentration of ethanol solution is 0.5~2mg/ml, more preferably 1mg/ml；What dispersion steps used
It is ultrasonic disperse, ultrasonic disperse is 50~200W using power, and the time is 0.5~3h；The centrifugation rate of centrifugation step is preferred
For 7000~9000r/min, centrifugation time is preferably 10~30min.
S2: weighing the sodium molybdate and thiocarbamide of certain mass, is dissolved in the Ti that the step S1 of certain volume is obtained together3C2Second
In the suspension of alcoholic solution, stirs evenly and fully dispersed, obtain mixed solution；
Specifically, wherein according to Ti3C2Quality account for MoS2And Ti3C2The 5~20% of gross mass are by the molybdenum of predetermined quality
Sour sodium and thiocarbamide are dissolved into the Ti for the predetermined volume that step S1 is obtained3C2In the suspension of ethanol solution；In preferred scheme,
According to Ti3C2Quality account for MoS2And Ti3C2The sodium molybdate of predetermined quality and thiocarbamide are dissolved into step S1 by the 13% of gross mass
The Ti of obtained predetermined volume3C2In the suspension of ethanol solution.
Specifically, the ratio between amount of substance of sodium molybdate and thiocarbamide is 1:3~1:10, more preferably 1:5；Whipping step is preferred
Using 0.5~2h of magnetic agitation；For dispersion steps using ultrasonic disperse, ultrasonic disperse is 100~300W using power, when
Between be 0.5~3h.
S3: the mixed solution that step S2 is obtained being carried out to be heated to predetermined temperature sustained response a few hours, is obtained reaction and is produced
Object；
Specifically, the obtained mixed solution of step S2 is transferred in hydrothermal reaction kettle, heating reaction preferably 180~
220 DEG C, 12~36h is reacted, is more preferably reacted for 24 hours at 210 DEG C.
S4: reaction product deionized water and ethyl alcohol that step S3 is obtained being centrifuged, wash multipass, more to remove surface
Remaining impurity and organic matter；
Specifically, the centrifugation rate of centrifugation step is preferably 8000~11000r/min, and centrifugation time is preferably 10~
30min；Washing step preferably repeatedly 3 times or more.
S5: obtained reaction product being dried, grind, is filtered, and obtains two-dimentional catalysis material MoS2/Ti3C2。
Specifically, drying steps are to be placed in reaction product in the baking oven of certain temperature dry a few hours, preferred dry
Temperature is 60~90 DEG C, and drying time is 8~18h, dry 12h at more preferably 70 DEG C.Sample after drying is easy agglomeration, will
It is placed in agate mortar, is ground for several times repeatedly, arrives hetero-junctions sample MoS with 200~400 mesh screen filter 23s time2/
Ti3C2。
Another preferred embodiment of the invention discloses a kind of two-dimentional catalysis material, as uses above-mentioned preparation method system
The two-dimentional catalysis material MoS obtained2/Ti3C2。
Another preferred embodiment of the invention also discloses the above-mentioned two-dimentional catalysis material of one kind and drops applied to photocatalysis
The method for solving disinfection by-products formation potential, comprising: the two dimension catalysis material is placed in certain volume containing before disinfection by-products
In the aqueous solution of body object (ranitidine), start illumination reaction under the LED light of 25W, sample at regular intervals, with it is ultraviolet-
Visible spectrophotometer is tested its absorbance, and combined standard working curve, is calculated in aqueous solution at 314nm wavelength
The residual concentration of disinfection by-products formation potential (ranitidine).
Specifically, the volume of ranitidine aqueous solution is preferably 10-30ml, more preferably 20ml；Ranitidine concentration is excellent
It is selected as 5-20mg/L, more preferably 10mg/L；The intensity of illumination of the LED light of 25W is preferably 10-50mW/cm2, more preferably
30mW/cm2；The illumination reaction time is preferably 0.5-2h, more preferably 1h.
Following combination comparative examples and specific embodiment are to the preparation method of two-dimentional catalysis material of the invention and its can
The light-exposed lower degradation application to nitrosamine disinfection by-products formation potential is described further.
(the preparation MoS of comparative example 12Applied to photocatalytic degradation disinfection by-products formation potential):
(1) it weighs 0.242g sodium molybdate and 0.381g thiocarbamide is dissolved in 48ml ultrapure water, stir evenly, ultrasonic disperse.
(2) mixed solution is transferred in 50ml hydrothermal reaction kettle, is heated in 210 DEG C of Muffle furnace, sustained response 24
Hour.
(3) obtained product deionized water and ethyl alcohol are removed into the impurity of excess surface through high speed centrifugation, washing 3 times
Or organic matter.
(4) product is placed in drying 12h hours in the baking oven at 70 DEG C, then places it in and grinds number in agate mortar
It is secondary, the screen to filtrate 3 times, MoS of the partial size less than 100 μm can be obtained2。
(5) by MoS obtained2Applied to photocatalytic degradation disinfection by-products formation potential: by MoS2Certain volume is placed in contain
In the aqueous solution of disinfection by-products formation potential (ranitidine), start illumination reaction under the LED light of 25W, at regular intervals
Sampling, with ultraviolet-visible spectrophotometer at 314nm wavelength, tests its absorbance, and combined standard working curve, calculates
The residual concentration of ranitidine in aqueous solution is obtained, as a result sees Fig. 3.
(the preparation Ti of comparative example 23C2Powder application is in photocatalytic degradation disinfection by-products formation potential):
(1) parent Ti3AlC2The synthesis of powder: Ti powder, TiC powder, Al powder are mixed with the molar ratio weighing of 1.0:2.0:1.2
It closes, then weighs mixing, abrasive media (zirconium oxide ballstone) and ball-milling additive (anhydrous second according to the mass ratio of 1.0:3.0:1.0
Alcohol) and be placed in polytetrafluoro configuration ethylene ball grinder, adjusting revolving speed in a planetary ball mill is 350r/min, ball milling duration
For 4h, uniform mixing is finally obtained and in 40 DEG C of drying in baking oven；After drying, it is sintered using vacuum non-pressure sintering method,
Then powder is further refined through high-energy ball milling, prepares Ti3AlC2Powder.
(2)Ti3C2The synthesis of powder: firstly, weighing 5gTi3AlC2Powder is slowly added into 80ml40%HF acid solution
In, then at room temperature, control revolving speed is 1200rmp, and magnetic agitation continues to bring it about corrosion reaction for 24 hours, after reaction
It is cleaned with deionized water, until the pH=5 or 6 of the supernatant after centrifugation, then uses washes of absolute alcohol 5 times, later will
Gained is deposited in 40 DEG C of baking ovens and dries for 24 hours, then places it in agate mortar and grind for several times, the screen to filtrate 3 times, finally obtains
The Ti of organ shape3C2Powder.
(3) by Ti obtained3C2Powder application is in photocatalytic degradation disinfection by-products formation potential: by Ti3C2Powder is placed in
In aqueous solution of the certain volume containing disinfection by-products formation potential (ranitidine), start illumination reaction under the LED light of 25W, often
It is sampled every a period of time, with ultraviolet-visible spectrophotometer at 314nm wavelength, tests its absorbance, and combined standard works
Curve is calculated the residual concentration of ranitidine in aqueous solution, as a result sees Fig. 3.
Embodiment 1 (prepares two-dimentional catalysis material MoS2/Ti3C2Applied to photocatalytic degradation disinfection by-products formation potential):
(1) ethanol water for configuring 100ml10%, takes 100mgTi3C2Powder is placed in ethanol solution, ultrasonic disperse 3
Hour, Ti at this time3C2The concentration of ethanol solution is 1mg/ml, after 100W ultrasonic disperse 3 hours, by solution 8000r/min high speed from
After heart 20min, take centrifuge tube upper layer suspension spare.
(2) it weighs 0.242g sodium molybdate and 0.381g thiocarbamide is dissolved in the above-mentioned Ti of 1.21ml3C2The upper layer of ethanol solution suspends
It in liquid, stirs evenly, ultrasonic disperse.
(3) mixed solution is transferred in 50ml hydrothermal reaction kettle, is heated in 210 DEG C of Muffle furnace, sustained response 24
Hour.
(4) obtained product deionized water and ethyl alcohol are removed into the impurity of excess surface through high speed centrifugation, washing 3 times
Or organic matter.
(5) product is placed in drying 12h hours in the baking oven at 70 DEG C, then places it in and grinds number in agate mortar
It is secondary, the screen to filtrate 3 times, the MoS of uniform particle sizes can be obtained2/Ti3C2Powder, wherein Ti3C2Quality account for MoS2And Ti3C2Total matter
The 0.75% of amount.
(6) by two-dimentional catalysis material MoS obtained2/Ti3C2Applied to photocatalytic degradation disinfection by-products formation potential: will
MoS2/Ti3C2It is placed in aqueous solution of the certain volume containing disinfection by-products formation potential (ranitidine), under the LED light of 25W
Start illumination reaction, samples at regular intervals, with ultraviolet-visible spectrophotometer at 314nm wavelength, test its extinction
Degree, and combined standard working curve, are calculated the residual concentration of ranitidine in aqueous solution, as a result see Fig. 3.
Embodiment 2:
Difference with embodiment 1 is only that Ti in step (2)3C2The volume of ethanol solution is 4.84ml, MoS obtained2/
Ti3C2Ti in powder3C2Quality account for MoS2And Ti3C2The 2.9% of gross mass.
Embodiment 3:
Difference with embodiment 1 is only that Ti in step (2)3C2The volume of ethanol solution is 9.68ml, MoS obtained2/
Ti3C2Ti in powder3C2Quality account for MoS2And Ti3C2The 5.7% of gross mass.
Embodiment 4:
Difference with embodiment 1 is only that Ti in step (2)3C2The volume of ethanol solution is 24.2ml, MoS obtained2/
Ti3C2Ti in powder3C2Quality account for MoS2And Ti3C2The 13.1% of gross mass.
Embodiment 5:
Difference with embodiment 1 is only that Ti in step (2)3C2The volume of ethanol solution is 36.3ml, MoS obtained2/
Ti3C2Ti in powder3C2Quality account for MoS2And Ti3C2The 18.5% of gross mass.
It is following respectively by MoS made from comparative example 12, Ti made from comparative example 23C2Prepared by powder and Examples 1 to 5
Different MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2, for disinfection by-products presoma --- thunder Buddhist nun
It is characterized for the catalytic degradation performance of fourth under visible light.
It is as shown in Figure 1a MoS made from comparative example 12Scanning electron microscope (SEM) photograph, as shown in Figure 1 b for made from comparative example 2
Ti3C2The scanning electron microscope (SEM) photograph of powder is as illustrated in figure 1 c two dimension catalysis material MoS made from Examples 1 to 52/Ti3C2Sweep
Retouch electron microscope；It is as shown in Figure 2 a MoS made from comparative example 12Transmission electron microscope picture, as shown in Figure 2 b for made from comparative example 2
Ti3C2The transmission electron microscope picture of powder is as shown in Figure 2 c two dimension catalysis material MoS made from Examples 1 to 52/Ti3C2It is saturating
Penetrate electron microscope.It can be seen that MoS made from comparative example 1 from Fig. 1 a and Fig. 2 a2The diameter of layer structure is about 0.5-1 μm, slightly
Reunite；It can be seen that Ti made from comparative example 2 from Fig. 1 b and Fig. 2 b3C2Powder layer structure is clearly demarcated, and it is flat to can be used as crystal growth
Platform template；It can be seen that from Fig. 1 c and Fig. 2 c by hydro-thermal reaction, stratiform MoS2Nanometer sheet is in Ti3C2Grow above, formed compared with
Uniform compound two-dimensional layered structure MoS2/Ti3C2。
As shown in figure 3, being MoS made from comparative example 12, Ti made from comparative example 23C2Powder and Examples 1 to 5 preparation
Different MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2Exist respectively for the ranitidine of 10mg/L
Catalytic degradation effect figure under visible light.From figure 3, it can be seen that the photocatalysis of ranitidine drops in comparative example 1 and comparative example 2
Solution effect is poor, and the degradation efficiency of 1h is respectively 17% and 33%, illustrates that the independent photocatalytic degradation thunder Buddhist nun of two kinds of two-dimensional materials replaces
Fourth has no positive effect；And Examples 1 to 5 the result shows that difference MoS2/Ti3C2The composite photocatalyst material of mass ratio has
There is a degree of photocatalysis performance, the effect compared to comparative example 1,2 is obviously improved；It is real wherein in photocatalytic degradation 1h
Apply the MoS of the preparation of example 3~52/Ti3C2Photocatalytic degradation efficiency it is all higher (85% or more), and 4 highest of embodiment, close to
90%.
As shown in figure 4, being MoS made from comparative example 12, Ti made from comparative example 23C2Powder and Examples 1 to 5 preparation
Different MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2Degrade 10mg/L's under visible light respectively
The remineralization efficacy figure of ranitidine 60min.
Test method: by MoS made from comparative example 12, Ti made from comparative example 23C2Powder and Examples 1 to 5 preparation
Two-dimentional optic catalytic composite material MoS2/Ti3C2Solution recycling after illumination 1h respectively, uses 0.22 μm of syringe filters mistake
After filter, it is put into and detects remaining total organic carbon (TOC) content in total organic carbon analyzer, then will measure numerical value and initial thunder Buddhist nun
The ratio between TOC content value for fourth solution is used as light-catalysed mineralization rate (percentage).
Figure 4, it is seen that comparative example 1 and comparative example 2 are poor for the photocatalytic degradation remineralization efficacy of ranitidine,
The mineralization rate of 1h is respectively 26.14% and 16.53%, embodiment 1-5's statistics indicate that, different MoS2/Ti3C2Mass ratio is answered
After light combination catalysis material is for the photocatalytic degradation of ranitidine, a degree of mineralising is had occurred in ranitidine solution, than
The effect of comparative example 1,2 is obviously improved；It is similar with Fig. 3, with MoS2/Ti3C2Ti in composite photo-catalyst3C2Ratio
Improve, remineralization efficacy increase, in photocatalytic degradation 60min, wherein embodiment 3~5 prepare MoS2/Ti3C2Mass ratio is answered
The mineralising of light combination catalysis material is all higher (59% or more), and 4 highest of embodiment, is 73.58%.
As shown in figure 5, being MoS made from comparative example 12, Ti made from comparative example 23C2Powder and Examples 1 to 5 preparation
Different MoS2/Ti3C2The two-dimentional optic catalytic composite material MoS of mass ratio2/Ti3C2Degrade 10mg/L's under visible light respectively
NDMA before and after ranitidine generates gesture comparison diagram.
Test method: by MoS made from comparative example 12, Ti made from comparative example 23C2Powder and Examples 1 to 5 preparation
Two-dimentional optic catalytic composite material MoS2/Ti3C2Solution recycling after illumination 1h respectively, it is molten with the ranitidine of initial concentration
Liquid (being denoted as control group) is diluted to 100 times together, then respectively takes 18ml, is separately added into the monochloro amine solution 2ml of 140mg/L, and 20 DEG C
Lower shading culture for 24 hours, after filtering later using 0.22 μm of syringe filters, is put into Liquid chromatography-tandem mass spectrometry combination analysis instrument
(LC-MS/MS) the remaining ranitidine concentration of detection in.
As shown in Figure 5, MoS made from comparative example 12, Ti made from comparative example 23C2Prepared by powder and Examples 1 to 5
Different MoS2/Ti3C2After the ranitidine solution 1h that degrades, NDMA generates gesture and drops respectively the composite photocatalyst material of mass ratio
As low as 33.94%, 52.88%, 17.08%, 12.59%, 10.65%, 2.01% and 3.05%；Examples 1 to 5 is relative to right
The effect of ratio 1~2 obviously gets a promotion, and wherein the effect of embodiment 3~5 is relatively preferable (reducing 89% or more), and
The effect of embodiment 4 is best, and the NDMA before and after the ranitidine for the 10mg/L that degrades under visible light generates gesture and reduces
97.99%.Show MoS prepared by embodiment 42/Ti3C2The method that composite material is used for photocatalytic degradation ranitidine, Neng Gouyou
The formation potential of effect control NDMA, reduces the generation risk of NDMA.
Fig. 6 is two-dimentional composite photocatalyst material MoS prepared by embodiment 42/Ti3C2Degradation 10mg/L is repeated under visible light
Ranitidine 5 times degradation effect figures.
Test method: two-dimentional optic catalytic composite material MoS prepared by embodiment 42/Ti3C2That recycles after illumination 1h answers
Condensation material successively uses deionized water and 95% ethanol washing, be placed in vacuum drying oven drying, then rejoins and newly takes
20ml concentration is in the ranitidine aqueous solution of 10mg/L, and the illumination 1h under the LED light of 25W, every 10min is sampled 3 times, with purple
Outside-visible spectrophotometer tests its absorbance, and combined standard working curve, corresponding water is calculated at wavelength 314nm
The residual concentration of ranitidine in sample.It is repeated 5 times according to above-mentioned steps, and tests and record related data respectively, result is such as
Shown in Fig. 6.
From fig. 6 it can be seen that during 5 reuses, the MoS of the preparation of embodiment 42/Ti3C2Composite photocatalyst
Material remains excellent visible light photocatalytic degradation performance, final removal effect of the ranitidine after 5 circulations in aqueous solution
Rate maintains 94.1% or more, shows that the composite material may be reused, and property retention is constant, has good stabilization
Property.
Two-dimentional catalysis material MoS is prepared in above-described embodiment 1~52/Ti3C2During, it can be using hydrofluoric acid
The means of this strong acid corrosion removing, prepare the Ti with two-dimensional layered structure first3C2Nano material (namely according to comparison
Ti made from the preparation method of example 23C2Powder), the MoS then as matrix, with same two-dimensional sheet2(can also be according to
MoS made from the preparation method of comparative example 12) compound；MoS is prepared using hydro-thermal method in the preferred embodiment of the present invention2/Ti3C2It is multiple
Condensation material, the compound specific surface area for increasing material of two kinds of two-dimensional materials, the heterojunction structure of formation can greatly improve compound
The photocatalytic activity of material.Meanwhile the adding proportion of two kinds of components is adjusted, in a particular embodiment, also advanced optimize two
Tie up catalysis material MoS2/Ti3C2Under visible light to the degradation capability of nitrosamine disinfection by-products formation potential；Wherein exist
Ti3C2Quality account for MoS2And Ti3C2Gross mass 5~20% when, MoS obtained2/Ti3C2Nitrosamine is sterilized under visible light
The degradation capability of by-product precursor more preferably, and Ti3C2Quality account for MoS2And Ti3C2Gross mass 13% when its effect it is best.
To sum up, the present invention uses easy technique, and having prepared under visible light being capable of efficient degradation nitrosamine disinfection pair
The MoS of product precursor object2/Ti3C2Composite material, the composite material is in industrial wastewater, sanitary wastewater, drink water purifying field
Disinfection by-products formation potential there is good degradation efficiency (to the catalysis degradation modulus of ranitidine up to 90% or more in 1h),
Therefore there is important application in the fields such as photocatalysis, sewage treatment, be expected to be used for large-scale industrial production.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those skilled in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, several equivalent substitute or obvious modifications can also be made, and performance or use is identical, all answered
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of two dimension catalysis material, which comprises the following steps:
S1: by Ti3C2Powder is placed in ethanol solution, is centrifuged after fully dispersed to solution, takes upper layer suspension spare；
S2: sodium molybdate and thiocarbamide are dissolved into the Ti that step S1 is obtained3C2In the suspension of ethanol solution, stir evenly and abundant
Dispersion, obtains mixed solution；
S3: the mixed solution that step S2 is obtained is carried out to be heated to predetermined temperature sustained response a few hours, obtains reaction product；
S5: reaction product being dried, grind, is filtered, and obtains two-dimentional catalysis material MoS2/Ti3C2。
2. preparation method according to claim 1, which is characterized in that further include: it is also wrapped between step S3 and step S5
It includes step S4: reaction product deionized water and ethyl alcohol that step S3 is obtained being centrifuged, wash multipass；Further, step
The rate of centrifugation step in S4 is 8000~11000r/min, and centrifugation time is 10~30min.
3. preparation method according to claim 1, which is characterized in that the mass concentration of the ethanol solution in step S1 is 5
~20%；Further, by Ti in step S13C2Powder is placed in ethanol solution specifically according to obtained Ti3C2Ethanol solution
Concentration is 0.5~2mg/ml Ti is added3C2Powder.
4. preparation method according to claim 1, which is characterized in that the rate of the centrifugation step in step S1 be 7000~
9000r/min, centrifugation time are 10~30min；Whipping step in step S2 uses 0.5~2h of magnetic agitation；Further,
Ultrasonic disperse is respectively adopted in dispersion steps in step S1 and step S2, and wherein the ultrasonic disperse in step S1 is using power
50~200W, time are 0.5~3h；The power that uses of ultrasonic disperse in step S2 is 100~300W, and the time is 0.5~3h.
5. preparation method according to claim 1, which is characterized in that according to Ti in step S23C2Quality account for MoS2With
Ti3C2The sodium molybdate of predetermined quality and thiocarbamide are dissolved into predetermined volume that step S1 is obtained by the 5~20% of gross mass
Ti3C2In the suspension of ethanol solution；Further, the ratio between amount of substance of sodium molybdate and thiocarbamide is 1:3~1 in step S2:
10。
6. preparation method according to claim 1, which is characterized in that be heated to 180~220 in heating stepses in step S3
DEG C, react 12~36h.
7. preparation method according to claim 1, which is characterized in that the temperature of the drying steps in step S5 is 60~90
DEG C, drying time is 8~18h, and filtration step specifically uses the screen to filtrate 3 times of 200~400 mesh or more.
8. a kind of two dimension catalysis material, which is characterized in that be made using the described in any item preparation methods of claim 1 to 7.
9. a kind of application method of two-dimentional catalysis material according to any one of claims 8, which is characterized in that by the two-dimentional photocatalysis
Material is applied to photocatalytic degradation disinfection by-products formation potential containing nitrosamine.
10. application method according to claim 9 characterized by comprising be placed in the two-dimentional catalysis material and contain
In the aqueous solution of nitrosamine disinfection by-products formation potential, and illumination reaction is carried out under LED light；Further, the by-product containing disinfection
The concentration of the aqueous solution of object precursor is 5~20mg/L, and the intensity of illumination of LED light is 10~50mW/cm2, the illumination reaction time
For 0.5~2h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110918108A (en) * | 2019-12-02 | 2020-03-27 | 镇江市高等专科学校 | MXene composite nano material and preparation method and application thereof |
| CN116328803A (en) * | 2023-03-11 | 2023-06-27 | 中南民族大学 | Preparation method and application of CdS@Ti3C2MXene-MoS 2 ternary composite catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532015A (en) * | 2016-12-27 | 2017-03-22 | 天津大学 | MoS2 inserted-layer Ti3C2 lithium ion battery negative electrode material and preparation method thereof |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN109772454A (en) * | 2019-02-28 | 2019-05-21 | 清华大学深圳研究生院 | Photocatalysis membrana and preparation method thereof and degradation application to disinfection by-products formation potential |
-
2019
- 2019-07-04 CN CN201910601053.1A patent/CN110227525A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106532015A (en) * | 2016-12-27 | 2017-03-22 | 天津大学 | MoS2 inserted-layer Ti3C2 lithium ion battery negative electrode material and preparation method thereof |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN109772454A (en) * | 2019-02-28 | 2019-05-21 | 清华大学深圳研究生院 | Photocatalysis membrana and preparation method thereof and degradation application to disinfection by-products formation potential |
Non-Patent Citations (1)
| Title |
|---|
| YUTING WU: "MoS2-Nanosheet-Decorated 2D Titanium Carbide (MXene) as High-Performance Anodes for Sodium-Ion Batteries", 《CHEMELECTROCHEM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110918108A (en) * | 2019-12-02 | 2020-03-27 | 镇江市高等专科学校 | MXene composite nano material and preparation method and application thereof |
| CN116328803A (en) * | 2023-03-11 | 2023-06-27 | 中南民族大学 | Preparation method and application of CdS@Ti3C2MXene-MoS 2 ternary composite catalyst |
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