CN106629983B - Application of the molybdenum sulfide composite reactive Carbon Materials near infrared light catalysis denitrogenation - Google Patents
Application of the molybdenum sulfide composite reactive Carbon Materials near infrared light catalysis denitrogenation Download PDFInfo
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- CN106629983B CN106629983B CN201611242635.8A CN201611242635A CN106629983B CN 106629983 B CN106629983 B CN 106629983B CN 201611242635 A CN201611242635 A CN 201611242635A CN 106629983 B CN106629983 B CN 106629983B
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- ammonia nitrogen
- molybdenum sulfide
- carbon materials
- near infrared
- infrared light
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 31
- 238000006555 catalytic reaction Methods 0.000 title abstract description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 14
- 238000005286 illumination Methods 0.000 claims description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 229910001868 water Inorganic materials 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- -1 feature exist In Chemical compound 0.000 claims description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 3
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 3
- 229910018890 NaMoO4 Inorganic materials 0.000 claims 2
- 230000002745 absorbent Effects 0.000 claims 2
- 239000002250 absorbent Substances 0.000 claims 2
- 239000003610 charcoal Substances 0.000 claims 2
- 150000002500 ions Chemical class 0.000 claims 2
- 238000007789 sealing Methods 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 32
- 238000006731 degradation reaction Methods 0.000 abstract description 32
- 239000003054 catalyst Substances 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract 2
- 229910052961 molybdenite Inorganic materials 0.000 description 12
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 12
- 239000000243 solution Substances 0.000 description 8
- 230000031700 light absorption Effects 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- NXMWOOVRJPJOSH-UHFFFAOYSA-N C1(=CC=CC=C1)O.C1(=CC=CC=C1)O.[Cl] Chemical compound C1(=CC=CC=C1)O.C1(=CC=CC=C1)O.[Cl] NXMWOOVRJPJOSH-UHFFFAOYSA-N 0.000 description 1
- 241001125671 Eretmochelys imbricata Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/39—
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/14—NH3-N
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of application of molybdenum sulfide composite reactive Carbon Materials near infrared light catalysis denitrogenation, comprising: is N by ammonia nitrogen degradation using molybdenum sulfide composite reactive Carbon Materials as photochemical catalyst under the conditions of near infrared light2And H2O.The present invention has the function of molecular recognition and infrared photocatalytic degradation using manganese oxide composite reactive Carbon Materials as catalyst, to ammonia nitrogen, ammonia nitrogen can be degraded to N under near infrared light2And H2O can still make degradation rate > 90% of ammonia nitrogen after the catalyst repeats catalytic degradation ammonia nitrogen 5~10 times.
Description
Technical field
The present invention relates to a kind of molybdenum sulfide composite reactive Carbon Materials and its using near infrared light in catalytic degradation ammonia nitrogen
Using.
Background technique
It can solve environmental energy problem with the sun, utilize TiO originating from Fujishima in 19722Optoelectronic pole electrolysis water system
Hydrogen, subsequent Carey were reported in 1976 and are utilized TiO2The toxicity that more chlorine diphenol are eliminated in photochemical catalytic oxidation utilizes the sun from this
Can degrade environmental contaminants research rapidly become people research hot spot.But TiO2It can only utilize and account for solar energy 4% or so
Ultraviolet light, to TiO2It is doped and develops Fe2O3、WO3、Bi2WO6Equal new catalysts, although part is solved to visible
The Utilizing question of light, but account for the infrared light of solar energy nearly 50% it is still necessary to develop and use.
In recent years, two-dimensional material received the extensive concern of people due to its good optical and electrology characteristic.And close
The application aspect of infrared light, document only report MoS2Research for photo-thermal drug release treating cancer.Therefore, how to utilize
Infrared light also becomes the direction of industry research staff research.
Summary of the invention
The purpose of the present invention is to provide a kind of molybdenum sulfide composite reactive Carbon Materials answering near infrared light catalysis denitrogenation
With to overcome the shortcomings of present technology.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of molybdenum sulfide composite reactive Carbon Materials photocatalysis under near infrared light illumination condition
Purposes in degradation of ammonia nitrogen.
Further, the molybdenum sulfide composite reactive Carbon Materials include active carbon and 1wt%~10wt% molybdenum sulfide particle,
And the molybdenum sulfide is distributed in the activated carbon surface.
Further, the specific surface area of the molybdenum sulfide composite reactive Carbon Materials is 12-16m2/g。
Further, the partial size of the molybdenum sulfide composite reactive Carbon Materials is 4.0-5.6nm, and adjacent molybdenum sulfide interlamellar spacing is
0.54-0.7nm。
More preferred, the ammonia nitrogen includes NH3And/or NH4 +。
Further, the range of wavelengths lambda of the near infrared light is 780nm~2500nm.
The embodiment of the invention provides a kind of purification methods of ammonia nitrogen comprising: molybdenum sulfide composite reactive Carbon Materials are added
Enter the liquid-phase system containing ammonia nitrogen, and with liquid-phase system described near infrared light illumination, makes the ammonia nitrogen by photocatalytic degradation N2
And H2O。
Further, the mass ratio of the molybdenum sulfide composite reactive Carbon Materials and ammonia nitrogen is 100mg:5~50mg.
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included: the liquid phase containing ammonia nitrogen is waited for
Sample and molybdenum sulfide composite reactive Carbon Materials, which are mixed into, to be protected from light in device, and in the illumination window for being protected from light device
Place setting only near infrared light can be made to pass through optical filter, later with light source irradiate described in be protected from light device, make ammonia nitrogen quilt therein
Photocatalytic degradation is N2And H2O。
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included:
(1) Photoreactor and optical filter are provided, to guarantee to only have near infrared radiation to enter Photoreactor；
(2) sample to be tested and molybdenum sulfide composite reactive Carbon Materials are added in the Photoreactor in step (1), cover optical filtering
Piece, then it is placed in illumination under light source, sample to be tested described in different time sections is measured in the light absorption value of visible light wave range；
(3) according to formula: ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100% calculates ammonia nitrogen
Degradation rate.
Further, light absorption value of the sample to be tested at 554nm is measured.
Further, after the molybdenum sulfide composite reactive Carbon Materials repeat catalytic degradation ammonia nitrogen 5-10 times, the degradation of ammonia nitrogen
Rate is still > 90%.
Compared with prior art, the invention has the advantages that
(1) method of molybdenum sulfide composite reactive Carbon Materials catalytic degradation ammonia nitrogen of the invention, using near infrared light light by ammonia
Nitrogen degradation is N2And H2O, without adding extra oxidant, to reduce costs, and the catalyst repeats catalytic degradation ammonia
After nitrogen 5-10 times, the degradation rate of the ammonia nitrogen is still > 90%.
(2) method of molybdenum sulfide composite activated carbon catalytic degradation ammonia nitrogen of the invention, can benefit by molybdenum sulfide, active carbon etc.
With the near infrared light in sunlight, the utilization to solar energy is greatly improved, and preparation method of the invention is simple, condition is easy
Control.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in invention, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is the reaction mechanism figure in the embodiment of the present invention 1；
Fig. 2 is molybdenum sulfide (MoS in the embodiment of the present invention 12), active carbon (AC) and molybdenum sulfide composite activated carbon (AC-MoS2)
XRD diagram；
Fig. 3 is MoS in the embodiment of the present invention 12, AC and AC-MoS2Raman spectrogram；
Fig. 4 a- Fig. 4 d is MoS in the embodiment of the present invention 12, AC and AC-MoS2TEM figure, wherein Fig. 4 a is molybdenum sulfide
TEM figure, Fig. 4 b are the TEM figures of active carbon, and Fig. 4 c and Fig. 4 d are AC-MoS2TEM figure；
Fig. 5 is AC-MoS in the embodiment of the present invention 12The curve graph of ammonia nitrogen degradation rate after repeating 1-7 times.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to the accompanying drawing to specific reality of the invention
The mode of applying is described in detail.The example of these preferred embodiments is illustrated in the accompanying drawings.Shown in attached drawing and according to
The embodiments of the present invention of attached drawing description are only exemplary, and the present invention is not limited to these embodiments.
Here, it should also be noted that, in order to avoid having obscured the present invention because of unnecessary details, in the accompanying drawings only
Show with closely related structure and/or processing step according to the solution of the present invention, and be omitted little with relationship of the present invention
Other details.
The embodiment of the invention provides a kind of molybdenum sulfide composite reactive Carbon Materials photocatalysis under near infrared light illumination condition
Purposes in degradation of ammonia nitrogen.
Further, the molybdenum sulfide composite reactive Carbon Materials include active carbon and 1wt%~10wt% molybdenum sulfide particle,
And the molybdenum sulfide is distributed in the activated carbon surface.
Further, the specific surface area of the molybdenum sulfide composite reactive Carbon Materials is 12-16m2/g。
Further, the partial size of the molybdenum sulfide composite reactive Carbon Materials is 4.0-5.6nm, and adjacent molybdenum sulfide interlamellar spacing is
0.54-0.7nm。
More preferred, the ammonia nitrogen includes NH3And/or NH4 +。
Further, the range of wavelengths lambda of the near infrared light is 780nm~2500nm.
The embodiment of the invention provides a kind of ammonia nitrogen purification methods comprising: molybdenum sulfide composite reactive Carbon Materials are added
Liquid-phase system containing ammonia nitrogen, and with liquid-phase system described near infrared light illumination, make the ammonia nitrogen by photocatalytic degradation N2With
H2O。
Further, the mass ratio of the molybdenum sulfide composite reactive Carbon Materials and ammonia nitrogen is 100mg:5~50mg.
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included: the liquid phase containing ammonia nitrogen is waited for
Sample and molybdenum sulfide composite reactive Carbon Materials, which are mixed into, to be protected from light in device, and in the illumination window for being protected from light device
Place setting only near infrared light can be made to pass through optical filter, later with light source irradiate described in be protected from light device, make ammonia nitrogen quilt therein
Photocatalytic degradation is N2And H2O。
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included:
(1) Photoreactor and optical filter are provided, to guarantee to only have near infrared radiation to enter Photoreactor；
(2) sample to be tested and molybdenum sulfide composite reactive Carbon Materials are added in the Photoreactor in step (1), cover optical filtering
Piece, then it is placed in illumination under light source, sample to be tested described in different time sections is measured in the light absorption value of visible light wave range；
(3) according to formula: ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100% calculates ammonia nitrogen
Degradation rate.
Further, light absorption value of the sample to be tested at 554nm is measured.
Further, after the molybdenum sulfide composite activated carbon repeats catalytic degradation ammonia nitrogen 5-10 times, the degradation rate of ammonia nitrogen still >
90%.
In one more preferred embodiment, a kind of ammonia nitrogen purification method is specifically included:
(1) Photoreactor and optical filter are provided, to guarantee to only have near infrared radiation to enter Photoreactor；
(2) sample to be tested and molybdenum sulfide composite activated carbon are added in the Photoreactor in step (1), covers optical filter,
It is placed in illumination under light source again, measures sample to be tested described in different time sections in the light absorption value of visible light wave range；
(3) according to formula: ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100% calculates ammonia nitrogen
Degradation rate.
Further, light absorption value of the sample to be tested at 554nm is measured.
Further, after the molybdenum sulfide composite activated carbon repeats catalytic degradation ammonia nitrogen 5-10 times, the degradation rate of ammonia nitrogen still >
85.4%.
Technology of the invention is further explained below in conjunction with drawings and examples.
Embodiment 1
(1)MoS2Preparation: take 1.21g Na2MoO4·2H2O (0.005mol), 1.60g CS (NH2)2(0.020mol)
In volume be 100mL beaker in, stirring until all dissolution, be then transferred in polytetrafluoroethylene (PTFE) inner sleeve, addition go from
Sub- water dissolves solid sufficiently and inner sleeve is placed in stainless steel outer sleeve cylinder to the 80% of total volume, seals, is heated to 200 DEG C,
Reaction 24 hours.Then sample is cooled down at room temperature, is washed with deionized, solable matter is removed.Obtained black
Solid dry 6h, the MoS of system in 40 DEG C of baking ovens2Semiconductor material.MoS2Unit cell is formed according to hexagonal symmetry stacking
, belong toSpace groupAccording to symmetry, MoS2Vibration mode with 4 Raman actives:E1g,
A1g.Referring to Fig. 3, it is located at 385cm-1And 408cm-1The Raman peaks at place are respectively belonging toAnd A1gVibration, this is further demonstrated that
Prepared sample is MoS2.A is the TEM figure of molybdenum sulfide referring to fig. 4.
(2)AC-MoS2Preparation: weigh MoS2The active carbon ultrasonic disperse of the 5% of quality is in 10ml deionized water.It takes
1.21gNaMoO4·2H2O, 1.56g (NH2)2CS, in the beaker that volume is 100ml, stirring, will be upper up to all dissolutions
Two solution mixing are stated, stirs 1 hour, is then transferred in polytetrafluoroethylene (PTFE) inner sleeve, deionized water is added to total volume
80%, it dissolves solid sufficiently and inner sleeve is placed in stainless steel outer sleeve cylinder, seal, be heated to 200 DEG C, react 24 hours.So
Sample is cooled down at room temperature afterwards, is washed with deionized, solable matter is removed.Obtained black solid is in 40 DEG C of baking ovens
AC-MoS is made in middle dry 6h2Composite material.C and Fig. 4 d is AC-MoS referring to fig. 42TEM figure.
(3) photocatalysis is tested: being encased the wall of cup of a 100ml beaker with masking foil, to avoid ultraviolet light and visible light
It into reaction system, is covered on beaker mouth with λ > 780nm cut-off type optical filter, to guarantee to only have near infrared radiation to enter light
300W ultraviolet-visible light lamp is placed in above reactor by reactor.Certain density ammonia nitrogen solution is added in beaker, uses
NaHCO3-Na2CO3(0.1mol/L) buffer solution adjusts pH value, and a certain amount of catalyst is added into beaker, is placed under light source,
Magnetic stirrer, per the absorbance for measuring remaining ammonia nitrogen solution every other hour.1ml ammonia nitrogen solution is taken, 1.5ml Na Shi is added to try
Agent, 1ml potassium sodium tartrate solution are diluted to 50ml, measure the absorbance at 388nm with T1901 ultraviolet-uisible spectrophotometer,
The degradation rate of ammonia nitrogen is calculated with this.
Ammonia nitrogen degradation rate=(1-Ci/C0) × 100%=(1-Ai/A0) × 100%
In formula, C0For the initial concentration of ammonia nitrogen, A0For the absorbance of initial soln, CiFor the concentration of remaining ammonia nitrogen, AiIt is surplus
The absorbance of remaining ammonia nitrogen.
(4) stability of hybrid catalyst catalyst stability: is evaluated by multiple circulation experiment.AC-MoS2Catalysis
The degradation rate of agent continuous 7 catalytic degradation ammonia nitrogens under near infrared radiation.Therapy lasted 8h each time, in degradation knot each time
Shu Hou is washed to obtain catalyst, is then further continued for that the catalyst is recycled by centrifuge separation, deionized water.Referring to Fig. 5 institute
Show, in AC-MoS2After the 7 circulation degradations of catalyst photocatalytic degradation ammonia nitrogen, ammonia nitrogen removal frank is still 90% or more.
Ammonia nitrogen degradation is N using near infrared light light by the method for change molybdenum composite activated carbon catalytic degradation ammonia nitrogen of the invention2
And H2O, without adding extra oxidant, to reduce costs.
It should be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, its object is to allow be familiar with this
The personage of item technology cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all
Equivalent change or modification made by Spirit Essence according to the present invention, should be covered by the protection scope of the present invention.
Claims (4)
1. purposes of the molybdenum sulfide composite reactive Carbon Materials under near infrared light illumination condition in photocatalytic degradation ammonia nitrogen, feature exist
In, molybdenum sulfide composite reactive Carbon Materials the preparation method is as follows:
Take 1.21g Na2MoO4·2H2O, 1.60g CS (NH2)2In the beaker that volume is 100mL, stirring is until all molten
Solution, is then transferred in polytetrafluoroethylene (PTFE) inner sleeve, and deionized water is added to the 80% of total volume, dissolves solid sufficiently inner sleeve
Cylinder is placed in stainless steel outer sleeve cylinder, is sealed, and is heated to 200 DEG C, is reacted 24 hours, is then cooled down sample at room temperature, spend
Ion water washing, solable matter is removed, and molybdenum sulfide is made in obtained black solid dry 6h in 40 DEG C of baking ovens；
5% active carbon ultrasonic disperse of molybdenum sulfide quality is weighed in 10ml deionized water, takes 1.21g NaMoO4·2H2O,
1.56g(NH2)2CS, in the beaker that volume is 100ml, stirring mixes above-mentioned two solution until all dissolutions, stirs
1 hour, be then transferred in polytetrafluoroethylene (PTFE) inner sleeve, deionized water be added to the 80% of total volume, make solid sufficiently dissolve by
Inner sleeve is placed in stainless steel outer sleeve cylinder, and sealing is heated to 200 DEG C, is reacted 24 hours, is then cooled down sample at room temperature,
It is washed with deionized, solable matter is removed, it is multiple that molybdenum sulfide is made in obtained black solid dry 6h in 40 DEG C of baking ovens
Close absorbent charcoal material；
The ammonia nitrogen includes NH3And/or NH4 +, the range of wavelengths lambda of the near infrared light is 780nm~2500nm.
2. a kind of ammonia nitrogen purification method, characterized by comprising: the liquid containing ammonia nitrogen is added in molybdenum sulfide composite reactive Carbon Materials
Phase system, and with liquid-phase system described near infrared light illumination, make the ammonia nitrogen by photocatalytic degradation N2And H2O；
Wherein, the molybdenum sulfide composite reactive Carbon Materials the preparation method is as follows:
Take 1.21g Na2MoO4·2H2O, 1.60g CS (NH2)2In the beaker that volume is 100mL, stirring is until all molten
Solution, is then transferred in polytetrafluoroethylene (PTFE) inner sleeve, and deionized water is added to the 80% of total volume, dissolves solid sufficiently inner sleeve
Cylinder is placed in stainless steel outer sleeve cylinder, is sealed, and is heated to 200 DEG C, is reacted 24 hours, is then cooled down sample at room temperature, spend
Ion water washing, solable matter is removed, and molybdenum sulfide is made in obtained black solid dry 6h in 40 DEG C of baking ovens；
5% active carbon ultrasonic disperse of molybdenum sulfide quality is weighed in 10ml deionized water, takes 1.21g NaMoO4·2H2O,
1.56g(NH2)2CS, in the beaker that volume is 100ml, stirring mixes above-mentioned two solution until all dissolutions, stirs
1 hour, be then transferred in polytetrafluoroethylene (PTFE) inner sleeve, deionized water be added to the 80% of total volume, make solid sufficiently dissolve by
Inner sleeve is placed in stainless steel outer sleeve cylinder, and sealing is heated to 200 DEG C, is reacted 24 hours, is then cooled down sample at room temperature,
It is washed with deionized, solable matter is removed, it is multiple that molybdenum sulfide is made in obtained black solid dry 6h in 40 DEG C of baking ovens
Close absorbent charcoal material；
The ammonia nitrogen includes NH3And/or NH4 +, the range of wavelengths lambda of the near infrared light is 780nm~2500nm.
3. ammonia nitrogen purification method as claimed in claim 2, it is characterised in that: the molybdenum sulfide composite reactive Carbon Materials and ammonia nitrogen
Mass ratio be 100mg:5~50mg.
4. ammonia nitrogen purification method as claimed in claim 2, characterized by comprising: by the liquid phase sample to be tested containing ammonia nitrogen with
Molybdenum sulfide composite reactive Carbon Materials, which are mixed into, to be protected from light in device, and is arranged only at the illumination window for being protected from light device
The optical filter that near infrared light can be made to pass through, later with light source irradiate described in be protected from light device, drop ammonia nitrogen therein by photocatalysis
Solution is N2And H2O。
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