CN106563470A - NiS2 nano-particle/g-C3N4 mesoporous nanosheet composite and preparation method thereof - Google Patents
NiS2 nano-particle/g-C3N4 mesoporous nanosheet composite and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002135 nanosheet Substances 0.000 title abstract 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 19
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910052755 nonmetal Inorganic materials 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 229910052976 metal sulfide Inorganic materials 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 238000005286 illumination Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 150000002171 ethylene diamines Chemical class 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 230000002079 cooperative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical class O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- -1 cleaning Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 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
- 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
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- 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
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention belongs to the technical field of material synthesis, and provides a NiS2 nano-particle/g-C3N4 mesoporous nanosheet composite and a preparation method thereof. NiS2 nano-particle loaded graphite type mesoporous C3N4 composite is synthesized with a simple one-step solvothermal method, and can be used for degrading Rhodamine B under the condition of visible light. The composite has the advantages of being green, environment-friendly and low in cost and adopting a simple preparation technology, and the prepared catalyst facilitates large-scale industrial production and has excellent photocatalytic activity and good environmental stability. Under the synergistic effect produced through compounding of the non-metal catalyst g-C3N4 and metal sulfide NiS2, and transmission of photo-induced electrons and holes can be substantially accelerated, so that visible light photocatalysis performance of the composite is remarkably improved.
Description
Technical field
The invention belongs to field of material synthesis technology, and in particular to NiS2Nano-particle/g-C3N4Meso-porous nano piece is combined
Material and preparation method thereof.
Background technology
In recent years, the environmental pollution and energy crisis faced by the mankind is increasingly serious, and current development and utilization solar energy is
Solve one of significant challenge of current crisis.From for the energy and environment remediation angle, with quasiconductor and its derived material as matchmaker
The photocatalysis technology of Jie can utilize the noxious substances such as cleaning, waste water and gas in continuable solar energy processing environment, by
It is widely considered to be the desirable route for solving the problems, such as current water body orgnic compound pollution.But in solar spectrum, ultraviolet light is only
Account for 5%, and the ratio of visible ray up to 43%, therefore, design and develop high performance visible light-responded catalysis material according to
It is old to be extremely important, and become the Main way of photocatalyst development.
Used as visible light-responded narrow band gap photocatalyst, which effectively can degrade organic nickel sulfide under visible light illumination
Pollutant, embody excellent photocatalytic activity, so as to be extensively studied and be used for the side such as photochemical catalytic oxidation environmental contaminants
Face.But the dispersion of nickel sulfide active component itself is relatively low and electronics rate of load condensate is high, therefore receives in terms of practical application
Significantly limit.However, carbonitride can band due to chemical stabilities such as its light, heat, suitably as non-metal optical catalyst
Have been a great concern with the performance such as visible light-responded.Graphite type carbon nitride nanometer sheet is loaded by nickel sulfide nanoparticles can
Effectively to make up the defect of nickel sulfide presence, while being the effective way for more preferably lifting its photocatalysis performance.Therefore, this
It is bright there is provided NiS2Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, it is intended in using carbonitride and sulfur
The formed cooperative effect that is combined for changing both nickel is carried out reinforced composite stability and promotes the quick of light induced electron and hole
Separate, so as to suppress the compound of photo-generated carrier, lift its photocatalytic activity.
The content of the invention
The present invention is intended to provide NiS2Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, the method
NiS is obtained by simple solvent-thermal method2Loaded mesoporous lamellar g-C of nano-particle3N4Composite.NiS prepared by the present invention2
Nano-particle/g-C3N4Meso-porous nano piece composite can be applicable to catalytic degradation rhodamine B under visible ray.
NiS2Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, specifically includes following steps：
（1）At room temperature, in proportion ground mesoporous carbonitride is added in ethylene glycol, ultrasonic disperse is disperseed
Liquid A；
（2）Nickel dichloride hexahydrate is added to into step（1）Dispersion liquid A in, be thoroughly mixed uniform, obtain mixed liquid B；
（3）Carbon bisulfide is slowly added in ethylenediamine, after reacting under magnetic agitation, is stopped stirring, is obtained mixed solution C；
（4）By step（3）In mixed solution C be dropwise slowly added to step（2）Mixed liquid B in, ultrasonic disperse, stop stirring
And after impregnating, be placed in loading stainless steel autoclave, constant temperature thermal response, reaction naturally cool to room temperature after terminating；
（5）By step（4）The precipitate centrifugation for obtaining, then uses dehydrated alcohol and distilled water wash respectively, is vacuum dried,
Obtain described NiS2Nano-particle/g-C3N4Meso-porous nano piece composite.
Step（1）In, the ultrasonic time is 0.5 ~ 1h；The mesoporous carbonitride is 0.01 ~ 0.2 with ethylene glycol amount ratio
g：20~30 mL.
Step（2）In, the Nickel dichloride hexahydrate and step（1）Middle carbonitride mass ratio is 0.15 ~ 0.4 g：0.01~
0.2 g。
Step（3）In, the Carbon bisulfide is 0.1 ~ 0.3 mL with ethylenediamine amount ratio：20 ~ 40 mL, magnetic agitation
Response time is 10 min.
Step（4）In, the ultrasonic disperse time is 2 ~ 5min, and dip time is 12 h；The temperature of constant temperature thermal response is
140 ~ 180 DEG C, constant temperature time is 18 ~ 24 h.
Step（5）In, the dehydrated alcohol and distilled water wash number of times are respectively 4 times；Vacuum drying temperature condition be 50 ~
60 DEG C, the time is 4 ~ 8 h.
NiS obtained in of the invention2Nano-particle/g-C3N4Meso-porous nano piece composite is used for catalysis drop under visible light
Solution rhodamine B.
Beneficial effects of the present invention are：
（1）NiS prepared by the present invention2Nano-particle/g-C3N4Meso-porous nano piece composite, its preparation process is simple, cost
Low, it is easy to large-scale industrial production, the heterojunction material has good environmental stability, is solving environmental pollution and the energy
There is good application prospect in terms of crisis.
（2）Suspension characteristic of the photocatalyst system in Photocatalytic Degradation Process effectively raises the utilization to light source
Rate.
（3）NiS2Nano-particle/g-C3N4Meso-porous nano piece composite can be used as the visible light photocatalysis of function admirable
Agent.g-C3N4With NiS2It is combined produced cooperative effect and not only improves the life-span that improve light induced electron and hole, promotes photoproduction
The transmission of electric charge, and effectively improve the stability of compound rear catalyst.Therefore, NiS2Nano-particle/g-C3N4Meso-porous nano
Piece composite considerably enhances degradation effect of the catalyst to organic dyestuff, has in photocatalysis practical application area wide
Prospect.
Description of the drawings
Fig. 1 is the XRD spectrum of the sample prepared by embodiment 1, with NiS2, g-C3N4XRD figure comparison diagram；
Fig. 2 is the transmission electron microscope picture of the sample prepared by embodiment 1, and A is g-C3N4Meso-porous nano piece, B are NiS2Nano-particle, C
For NiS2/g-C3N4Composite；
Fig. 3 be embodiment 1 prepared by concentration be under visible light illumination 5 mg/L rhodamine B photocatalytic degradation effect
Figure.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1：
Prepare NiS2Nano-particle/g-C3N4Meso-porous nano piece composite：
0.01g carbonitrides are added in 30 mL ethylene glycol, ultrasonic disperse 1h after stirring adds 0.237 g, six chloride hydrates
Nickel, is stirred uniform dispersion liquid A；By 0.15 mL CS2It is added dropwise in 26 mL ethylenediamines, 5 min of ultrasonic disperse is obtained
To dispersion liquid B；Dispersion liquid B is dropwise slowly added in dispersion liquid B, 2 ~ 5min of ultrasonic disperse, 12 h are stirred and impregnated in stopping, being put
In 100 mL stainless steel autoclaves, 180 DEG C of constant temp. heatings naturally cool to room temperature, respectively deionized water, nothing after 24 h of reaction
Water-ethanol respectively washing 4 times, are dried 8h, that is, obtain described NiS under the conditions of 60 DEG C of vacuum2Nano-particle/g-C3N4Meso-porous nano piece
Composite.
The material under visible light illumination, the rhodamine B of 150 min degradables 90%.
Prepare monomer NiS2：
0.237 g Nickel dichloride hexahydrates are added in 30 mL ethylene glycol, are stirred uniformly, are added 0.15mL CS2, surpass
Sound disperses 5 min, is subsequently added into 26 mL ethylenediamines, after mix homogeneously reactant liquor is proceeded in 100 mL stainless steel autoclaves,
180 DEG C of constant temp. heatings, naturally cool to room temperature after 24 h of reaction, and deionized water, dehydrated alcohol are respectively washed 4 times respectively, vacuum 60
8 h are dried under the conditions of DEG C, you can be prepared into simple NiS2。
Except containing NiS in the material of result sign synthesis in Fig. 12, also contain g-C3N4；
In Fig. 2, TEM results show simple g-C3N4Exist with mesoporous lamellar form, NiS2Monomer is deposited in the form of Cubic
, composite TEM figures it can be seen that NiS2Nano-particle is equably supported on g-C3N4On meso-porous nano piece；
Fig. 3 is monomer NiS2And g-C3N4And g-C3N4/NiS2The activity experiment figure of rhodamine B degradation.Can be significantly from figure
It was observed that, NiS2Nano-particle/g-C3N4The degradation rate of meso-porous nano piece composite is apparently higher than simple NiS2And g-
C3N4。
Embodiment 2：
0.1 g carbonitrides are added in 20 mL ethylene glycol, 0.5 h of ultrasonic disperse after stirring, add the hydration chlorine of 0.18 g six
Change nickel, be stirred uniform dispersion liquid A；By 0.2 mL CS2It is added dropwise in 20 mL ethylenediamines, 5 min of ultrasonic disperse is obtained
To dispersion liquid B；Dispersion liquid B is dropwise slowly added in dispersion liquid B, 2 ~ 5min of ultrasonic disperse, 12 h are stirred and impregnated in stopping, being put
In 100 mL stainless steel autoclaves, 180 DEG C of constant temp. heatings naturally cool to room temperature, respectively deionized water, nothing after 18 h of reaction
Water-ethanol respectively washing 4 times, are dried 10 h, that is, obtain described NiS under the conditions of 60 DEG C of vacuum2Nano-particle/g-C3N4Meso-porous nano
Piece composite.The material under visible light illumination, the rhodamine B of 150 min degradables 79%.
Embodiment 3：
0.15 g carbonitrides are added in 25 mL ethylene glycol, 1 h of ultrasonic disperse after stirring, add the hydration chlorine of 0.32 g six
Change nickel, be stirred uniform dispersion liquid A；By 0.26 mL CS2It is added dropwise in 40 mL ethylenediamines, 5 min of ultrasonic disperse,
Obtain dispersion liquid B；Dispersion liquid B is dropwise slowly added in dispersion liquid B, 2 ~ 5min of ultrasonic disperse, 12h is stirred and impregnated in stopping,
Be placed in 100 mL stainless steel autoclaves, 180 DEG C of constant temp. heatings, after 12 h of reaction, naturally cool to room temperature, respectively deionized water,
Dehydrated alcohol respectively washing 4 times, are dried 4 h, that is, obtain described NiS under the conditions of 60 DEG C of vacuum2Nano-particle/g-C3N4It is mesoporous to receive
Rice piece composite.The material under visible light illumination, the rhodamine B of 150 min degradables 87%.
Embodiment 4：
0.2 g carbonitrides are added in 28 mL ethylene glycol, 1 h of ultrasonic disperse after stirring adds 0.24 g, six chloride hydrates
Nickel, is stirred uniform dispersion liquid A；By 0.18 mL CS2It is added dropwise in 24 mL ethylenediamines, 5 min of ultrasonic disperse is obtained
To dispersion liquid B；Dispersion liquid B is dropwise slowly added in dispersion liquid B, 2 ~ 5min of ultrasonic disperse, 12 h are stirred and impregnated in stopping, being put
In 100 mL stainless steel autoclaves, 180 DEG C of constant temp. heatings naturally cool to room temperature, respectively deionized water, nothing after 20 h of reaction
Water-ethanol respectively washing 4 times, are dried 6 h, that is, obtain described NiS under the conditions of 60 DEG C of vacuum2Nano-particle/g-C3N4Meso-porous nano
Piece composite.The material under visible light illumination, the rhodamine B of 150 min degradables 83%.
Claims (8)
1.NiS2Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, it is characterised in that including following step
Suddenly：
（1）At room temperature, in proportion ground mesoporous carbonitride is added in ethylene glycol, ultrasonic disperse is disperseed
Liquid A；
（2）Nickel dichloride hexahydrate is added to into step（1）Dispersion liquid A in, be thoroughly mixed uniform, obtain mixed liquid B；
（3）Carbon bisulfide is slowly added in ethylenediamine, after reacting under magnetic agitation, is stopped stirring, is obtained mixed solution C；
（4）By step（3）In mixed solution C be dropwise slowly added to step（2）Mixed liquid B in, ultrasonic disperse, stop stirring
And after impregnating, be placed in loading stainless steel autoclave, constant temperature thermal response, reaction naturally cool to room temperature after terminating；
（5）By step（4）The precipitate centrifugation for obtaining, then uses dehydrated alcohol and distilled water wash respectively, is vacuum dried,
Obtain described NiS2Nano-particle/g-C3N4Meso-porous nano piece composite.
2. NiS according to claim 12Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, its
It is characterised by, step（1）In, the ultrasonic time is 0.5 ~ 1h；The mesoporous carbonitride and ethylene glycol amount ratio be 0.01 ~
0.2 g：20~30 mL.
3. NiS according to claim 12Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, its
It is characterised by, step（2）In, the Nickel dichloride hexahydrate and step（1）Middle carbonitride mass ratio is 0.15 ~ 0.4 g：0.01~
0.2 g。
4. NiS according to claim 12Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, its
It is characterised by, step（3）In, the Carbon bisulfide is 0.1 ~ 0.3 mL with ethylenediamine amount ratio：20 ~ 40 mL, magnetic agitation
Response time is 10 min.
5. NiS according to claim 12Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, its
It is characterised by, step（4）In, the ultrasonic disperse time is 2 ~ 5min, and dip time is 12 h；The temperature of constant temperature thermal response is
140 ~ 180 DEG C, constant temperature time is 18 ~ 24 h.
6. NiS according to claim 12Nano-particle/g-C3N4Meso-porous nano piece composite and preparation method thereof, its
It is characterised by, step（5）In, the dehydrated alcohol and distilled water wash number of times are respectively 4 times；Vacuum drying temperature condition is 50
~ 60 DEG C, the time is 4 ~ 8 h.
7.NiS2Nano-particle/g-C3N4Meso-porous nano piece composite, it is characterised in that the NiS2/g-C3N4Composite
It is the NiS according to any one of claim 1 ~ 62Nano-particle/g-C3N4The preparation method of meso-porous nano piece composite
Obtain.
8. NiS according to claim 72Nano-particle/g-C3N4Meso-porous nano piece composite is used to urge under visible light
Change rhodamine B degradation.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107892284A (en) * | 2017-11-28 | 2018-04-10 | 铜仁学院 | A kind of NiS/C3N4Binary complex and its methods for making and using same |
| CN107930671A (en) * | 2017-12-06 | 2018-04-20 | 福州大学 | A kind of ternary metal sulfide/graphite phase carbon nitride composite photocatalyst material and its preparation method and application |
| CN108067280A (en) * | 2017-11-23 | 2018-05-25 | 江南大学 | A kind of preparation method of nickel sulfide/class graphene carbon nitrogen compound composite catalyst |
| CN109835937A (en) * | 2017-11-29 | 2019-06-04 | 中国科学院大连化学物理研究所 | Nano metal sulfide piece and its preparation derived from metal organic framework compound |
| CN110368979A (en) * | 2019-08-08 | 2019-10-25 | 南京邮电大学 | A kind of tubulose g-C3N4/CuS/Cu2S nanocomposite and its preparation method and application |
| CN111129490A (en) * | 2019-12-06 | 2020-05-08 | 中国科学院过程工程研究所 | Single-phase NiS2Large-scale preparation method of powder |
| CN111905788A (en) * | 2020-07-11 | 2020-11-10 | 吉林化工学院 | NiSe/g-C3N4Preparation method and application of photocatalyst |
| CN112064142A (en) * | 2020-08-21 | 2020-12-11 | 西安工程大学 | Nickel sulfide-graphite phase carbon nitride heterojunction photocatalyst fiber and preparation method thereof |
| CN113600220A (en) * | 2021-06-23 | 2021-11-05 | 宁夏大学 | Carbon nitride high-load dispersion NiS photocatalytic degradation material and preparation method thereof |
| CN114177928A (en) * | 2021-12-27 | 2022-03-15 | 吉林大学 | Composite photocatalyst Bi @ H-TiO with visible light response2/B-C3N4Preparation method and application thereof |
| CN114452986A (en) * | 2020-11-09 | 2022-05-10 | 湖南大学 | Grass-shaped carbon nitride/flower-shaped nickel sulfide composite material and preparation method and application thereof |
-
2016
- 2016-11-14 CN CN201610999187.XA patent/CN106563470A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| CHENGZHANG ZHU，ET.AL.: "Fabrication of noble-metal-free NiS2/g-C3N4 hybrid photocatalysts with visible light-responsive photocatalytic activities", 《RES CHEM INTERMED》 * |
| LISHA YIN，ET.AL.: "Enhanced visible-light-driven photocatalytic hydrogen generation over g-C3N4 through loading the noble metal-free NiS2 cocatalyst", 《RSC ADVANCES》 * |
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| CN108067280A (en) * | 2017-11-23 | 2018-05-25 | 江南大学 | A kind of preparation method of nickel sulfide/class graphene carbon nitrogen compound composite catalyst |
| CN107892284A (en) * | 2017-11-28 | 2018-04-10 | 铜仁学院 | A kind of NiS/C3N4Binary complex and its methods for making and using same |
| CN109835937B (en) * | 2017-11-29 | 2021-09-17 | 中国科学院大连化学物理研究所 | Metal sulfide nanosheet derived from metal organic framework compound and preparation method thereof |
| CN109835937A (en) * | 2017-11-29 | 2019-06-04 | 中国科学院大连化学物理研究所 | Nano metal sulfide piece and its preparation derived from metal organic framework compound |
| CN107930671A (en) * | 2017-12-06 | 2018-04-20 | 福州大学 | A kind of ternary metal sulfide/graphite phase carbon nitride composite photocatalyst material and its preparation method and application |
| CN110368979A (en) * | 2019-08-08 | 2019-10-25 | 南京邮电大学 | A kind of tubulose g-C3N4/CuS/Cu2S nanocomposite and its preparation method and application |
| CN110368979B (en) * | 2019-08-08 | 2022-04-22 | 南京邮电大学 | Tubular g-C3N4/CuS/Cu2S nano composite material and preparation method and application thereof |
| CN111129490A (en) * | 2019-12-06 | 2020-05-08 | 中国科学院过程工程研究所 | Single-phase NiS2Large-scale preparation method of powder |
| CN111905788A (en) * | 2020-07-11 | 2020-11-10 | 吉林化工学院 | NiSe/g-C3N4Preparation method and application of photocatalyst |
| CN112064142A (en) * | 2020-08-21 | 2020-12-11 | 西安工程大学 | Nickel sulfide-graphite phase carbon nitride heterojunction photocatalyst fiber and preparation method thereof |
| CN112064142B (en) * | 2020-08-21 | 2023-01-24 | 西安工程大学 | Nickel sulfide-graphite phase carbon nitride heterojunction photocatalyst fiber and preparation method thereof |
| CN114452986A (en) * | 2020-11-09 | 2022-05-10 | 湖南大学 | Grass-shaped carbon nitride/flower-shaped nickel sulfide composite material and preparation method and application thereof |
| CN113600220A (en) * | 2021-06-23 | 2021-11-05 | 宁夏大学 | Carbon nitride high-load dispersion NiS photocatalytic degradation material and preparation method thereof |
| CN113600220B (en) * | 2021-06-23 | 2023-11-07 | 宁夏大学 | High-load dispersion NiS photocatalytic degradation material of carbon nitride and preparation method thereof |
| CN114177928A (en) * | 2021-12-27 | 2022-03-15 | 吉林大学 | Composite photocatalyst Bi @ H-TiO with visible light response2/B-C3N4Preparation method and application thereof |
| CN114177928B (en) * | 2021-12-27 | 2023-10-03 | 吉林大学 | Composite photocatalyst Bi@H-TiO with visible light response 2 /B-C 3 N 4 Preparation method and application thereof |
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