CN111686777A - NiS-g-C3N4Method for preparing photocatalyst - Google Patents
NiS-g-C3N4Method for preparing photocatalyst Download PDFInfo
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- CN111686777A CN111686777A CN201911426775.4A CN201911426775A CN111686777A CN 111686777 A CN111686777 A CN 111686777A CN 201911426775 A CN201911426775 A CN 201911426775A CN 111686777 A CN111686777 A CN 111686777A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 41
- 239000000203 mixture Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 12
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 230000007935 neutral effect Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- IICCLYANAQEHCI-UHFFFAOYSA-N 4,5,6,7-tetrachloro-3',6'-dihydroxy-2',4',5',7'-tetraiodospiro[2-benzofuran-3,9'-xanthene]-1-one Chemical compound O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 IICCLYANAQEHCI-UHFFFAOYSA-N 0.000 description 6
- 229930187593 rose bengal Natural products 0.000 description 6
- 229940081623 rose bengal Drugs 0.000 description 6
- STRXNPAVPKGJQR-UHFFFAOYSA-N rose bengal A Natural products O1C(=O)C(C(=CC=C2Cl)Cl)=C2C21C1=CC(I)=C(O)C(I)=C1OC1=C(I)C(O)=C(I)C=C21 STRXNPAVPKGJQR-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
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- 238000002474 experimental method Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000000628 photoluminescence spectroscopy Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910000581 Yellow brass Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 201000011510 cancer Diseases 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification 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
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- 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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- 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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/36—Organic compounds containing halogen
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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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
Disclosure of the inventionNiS-g-C3N4A preparation method of a photocatalyst belongs to the technical field of photocatalysts. The method comprises the following steps: step (1): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and NiS, and stirring for 1h by using a magnetic stirrer; step (2): after stirring, adding a nickel nitrate solution with the volume concentration of 0.1M, and continuously stirring for 1 h; and (3): after stirring, adding a sodium sulfide solution with the volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture; and (4): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to dry at 60 ℃ overnight to obtain NiS-g-C3N4. NiS is introduced in the invention to construct NiS-g-C3N4The introduction of NiS accelerates the introduction of NiS-g-C3N4Thereby improving the redox ability and photocatalytic activity of the photocatalyst.
Description
Technical Field
The invention relates to the technical field of photocatalysts, in particular to a NiS-g-C photocatalyst3N4A preparation method of the photocatalyst.
Background
The photocatalyst is a general name of chemical substances capable of playing a role in catalysis under the excitation of photons, and is mainly applied to a plurality of advanced fields such as environmental purification, self-cleaning materials, advanced new energy, cancer medical treatment, high-efficiency antibiosis and the like.
The photocatalytic technique is one of the methods for eliminating environmental pollution by means of sunlight, and in the prior art, various visible-light-responsive oxide, sulfide and polymerized semiconductor photocatalysts are sequentially valued, such as BiVO4、Bi2MoO6、CdS、g-C3N4However, the photocatalytic activity of single-component semiconductor photocatalysts is limited by the high recombination rate of photoinduced electron-hole pairs and the low absorption capacity of visible light (less than 450nm), so that these semiconductor photocatalysts show unsatisfactory photoactivity, and therefore, in order to improve the photocatalytic activity of photocatalysts, a composite photocatalyst with stronger visible light photocatalytic performance is urgently needed to degrade environmental pollutants.
Disclosure of Invention
In order to solve the problems in the prior art, embodiments of the present invention provide a method for preparing a photocatalyst. The method bagComprises the following steps: step (1): 0.235g of g-C was weighed3N4Putting into a beaker, adding 50ml of deionized water and NiS, and stirring for 1h by using a magnetic stirrer; step (2): after stirring, adding a nickel nitrate solution with the volume concentration of 0.1M, and continuously stirring for 1 h; and (3): after stirring, adding a sodium sulfide solution with the volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture; and (4): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to be dried overnight at 60 ℃ to obtain NiS-g-C3N4。
Further, the mass of the NiS added in the step (1) is g-C3N40.5 to 2.0 percent of the mass.
Further, the mass of said NiS added in said step (1) is preferably said g-C3N40.5% of the mass.
Further, the volume of the nickel nitrate solution added in the step (2) is 0.125 mL-0.5 mL.
Further, the volume of the nickel nitrate solution added in the step (2) is preferably 0.125 mL.
Further, the volume of the sodium sulfide solution added in the step (3) is 0.15mL-0.6 mL.
Further, the volume of the sodium sulfide solution added in the step (3) is preferably 0.15 mL.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: NiS is introduced in the invention to construct NiS-g-C3N4The introduction of NiS accelerates the introduction of NiS-g-C3N4Thereby improving the redox ability and photocatalytic activity of the photocatalyst.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows a NiS-g-C according to an embodiment of the present invention3N4A flow chart of a preparation method of the photocatalyst;
FIG. 2 is g-C provided by the present invention3N4And NiS-g-C of different mass fractions3N4Degradation curve for rose bengal;
FIG. 3 is g-C provided by the present invention3N4And 0.5% -NiS-g-C3N4Fluorescence spectrum of (2).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example one
NiS-g-C3N4A method for preparing a photocatalyst, see fig. 1, comprising the steps of: step (1): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and NiS, and stirring for 1h by using a magnetic stirrer;
step (2): after stirring, adding a nickel nitrate solution with the volume concentration of 0.1M, and continuously stirring for 1 h;
and (3): after stirring, adding a sodium sulfide solution with the volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
and (4): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to dry at 60 ℃ overnight to obtain NiS-g-C3N4。
In addition, g-C3N4The (graphite phase carbon nitride) is a semiconductor material with excellent photoelectric characteristics, the unique forbidden band width of the semiconductor material can absorb the visible light wavelength in sunlight, the sunlight utilization of the photocatalytic material is extended to the visible light region, and a catalyst can be provided for a plurality of photodegradation and photoreduction reactions. g-C3N4The potential of the hydrogen-oxygen-hydrogen composite material can meet the requirements of decomposing water to generate hydrogen and the oxidation reduction of oxygen, and meets the requirements of photolysis water hydrogen production and photolysis water oxygen production. Due to g-C3N4The unique physical and chemical characteristics of the photocatalyst make the photocatalyst become a photocatalyst with wide application prospect and full potential. Due to g-C3N4Is sufficiently negative, g-C3N4The electrons on the CB have strong reducing capability and have great potential for dechlorination and degradation of pollutants. But the rapid recombination of the photo-generated electron-hole pairs greatly constrains the g-C3N4The photocatalytic reduction oxidation capability of (1). In g-C3N4The hydrogen bonds are found, and the fact that the material cannot be completely polymerized is proved, and meanwhile, a large number of defects are found on the surface of the material, which is considered to cause Lewis-base characteristics, so that the regeneration of electrons and holes on the surface of the material is accelerated, and the original promotion effect on photocatalytic degradation is reduced. Thus g-C3N4The photocatalyst is a very potential material in the aspects of decomposing water and degrading organic pollutants.
In addition, the NiS (nickel sulfide) crystal was yellow brass, and the powder was black. Density: 5.3-5.6g/mL, 25/4 ℃. Melting Point 797 ℃.
Example two
NiS-g-C3N4A method for preparing a photocatalyst, the method comprising the steps of:
a step (101): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and NiS with the mass ratio of 0.5%, and stirring for 1h by using a magnetic stirrer;
a step (102): after stirring, adding 0.125mL of nickel nitrate solution with volume concentration of 0.1M, and continuing stirring for 1 h;
step (103): after stirring, adding 0.15mL of sodium sulfide solution with volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
a step (104): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to dry at 60 ℃ overnight to obtain NiS-g-C3N4。
EXAMPLE III
NiS-g-C3N4A method for preparing a photocatalyst, the method comprising the steps of:
step (201): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and 1% of NiS by mass, and stirring for 1h by using a magnetic stirrer;
step (202): after stirring, adding 0.25mL of nickel nitrate solution with volume concentration of 0.1M, and continuing stirring for 1 h;
step (203): after stirring, adding 0.3mL of sodium sulfide solution with volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
a step (204): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to dry at 60 ℃ overnight to obtain NiS-g-C3N4。
Example four
NiS-g-C3N4A method for preparing a photocatalyst, the method comprising the steps of:
step (301): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and NiS with the mass ratio of 1.5%, and stirring for 1h by using a magnetic stirrer;
step (302): after stirring, adding 0.375mL of nickel nitrate solution with volume concentration of 0.1M, and continuing stirring for 1 h;
step (303): after stirring, adding 0.45mL of sodium sulfide solution with volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
step (304): the mixture was washed to neutrality by centrifugation using absolute ethanol and deionized water,then transferring the mixture to a culture dish and drying the culture dish at 60 ℃ overnight to obtain NiS-g-C3N4。
EXAMPLE five
NiS-g-C3N4A method for preparing a photocatalyst, the method comprising the steps of:
a step (401): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and 2% of NiS by mass, and stirring for 1h by using a magnetic stirrer;
step (402): after stirring, adding 0.5mL of nickel nitrate solution with volume concentration of 0.1M, and continuing stirring for 1 h;
step (403): after stirring, adding 0.6mL of sodium sulfide solution with volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
a step (404): centrifugally washing the mixture to neutrality by using absolute ethyl alcohol and deionized water, and then transferring the mixture to a culture dish to dry at 60 ℃ overnight to obtain NiS-g-C3N4。
Note that NiS-g-C prepared for the purpose of comparing examples of the present invention3N4In pure g-C3N4And 0.5% -NiS-g-C prepared in example3N4、1％-NiS-g-C3N4、1.5％-NiS-g-C3N4、2％-NiS-g-C3N4Degradation experiments of rose bengal under visible light irradiation, and g-C3N4And 0.5% -NiS-g-C3N4Performing fluorescence spectrum analysis:
firstly, a xenon lamp is used as a light source to carry out a photocatalytic degradation experiment, a filter with the wavelength of more than 420nm is used to filter out ultraviolet light, the external condition is to ensure that the temperature is not changed during the catalytic reaction, rose red solution with the concentration of 10mg/L and the volume of 45mL is used as a target degradation product, and the adding amount of the catalyst is 0.045 g. In order to ensure that adsorption equilibrium is achieved, dark reaction is carried out for 30min, and then light reaction is carried out, and points are sampled at fixed time. And centrifuging the sample after sampling, taking the supernatant, and performing ultraviolet test to obtain a visible light absorption spectrum.
FIG. 2 is g-C3N4And NiS-g-C of different mass fractions3N4Degradation curves for rose bengal, as can be seen in the figure, g-C3N4，0.5％-NiS-g-C3N4，1％-NiS-g-C3N4，1.5％-NiS-g-C3N4，2％-NiS-g-C3N4The degradation efficiency of rose bengal is 63%, 98%, 79%, 53% and 50%, respectively, and the result shows that the degradation efficiency of rose bengal is 0.5% -NiS-g-C3N4The highest degradation efficiency of rose bengal indicates that 0.5% -NiS-g-C3N4Has good stability.
In addition, the transport and recombination processes of the photo-generated electron-hole pairs were tested by photoluminescence spectroscopy (PL). FIG. 3 is g-C3N4And 0.5% -NiS-g-C3N4PL spectrum of (2). As can be seen in the figure, g-C3N4And 0.5% -NiS-g-C3N4Is located at 465nm, which is associated with recombination of photo-generated electron-hole pairs. For g-C3N4Has stronger emission intensity due to high combination rate of electron-hole pairs. However, when an appropriate amount of NiS is introduced, 0.5% -NiS-g-C3N4Shows lower emission intensity, indicating 0.5% -NiS-g-C3N4Has a binding ratio of electron-hole pairs of less than g-C3N4. That is, the introduction of NiS accelerates by 0.5% -NiS-g-C3N4The separation of charges in (2) is favorable for improving the photocatalytic activity.
It is worth to say that NiS is introduced in the invention, and NiS-g-C is constructed3N4The introduction of NiS accelerates the introduction of NiS-g-C3N4Thereby improving the redox ability and photocatalytic activity of the photocatalyst.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. NiS-g-C3N4A method for preparing a photocatalyst, the method comprising: step (1): 0.235g of g-C was weighed3N4Putting the mixture into a beaker, adding 50mL of deionized water and NiS, and stirring for 1h by using a magnetic stirrer;
step (2): after stirring, adding a nickel nitrate solution with the volume concentration of 0.1M, and continuously stirring for 1 h;
and (3): after stirring, adding a sodium sulfide solution with the volume concentration of 0.1M, and stirring at normal temperature overnight to obtain a mixture;
and (4): and (3) centrifugally washing the mixture to be neutral by using absolute ethyl alcohol and deionized water while stirring, and then transferring the mixture to a culture dish to be dried overnight at 60 ℃ to obtain NiS-g-C3N 4.
2. NiS-g-C according to claim 13N4The preparation method of the photocatalyst is characterized in that the mass of the NiS added in the step (1) is g-C3N40.5 to 2.0 percent of the mass.
3. NiS-g-C according to claim 23N4The preparation method of the photocatalyst is characterized in that the mass of the NiS added in the step (1) is preferably g-C3N40.5% of the mass.
4. NiS-g-C according to claim 13N4The preparation method of the photocatalyst is characterized in that the volume of the nickel nitrate solution added in the step (2) is 0.125-0.5 mL.
5. NiS-g-C according to claim 43N4The preparation method of the photocatalyst is characterized in that the volume of the nickel nitrate solution added in the step (2) is preferably 0.125 mL.
6. NiS-g-C according to claim 13N4The preparation method of the photocatalyst is characterized in that the volume of the sodium sulfide solution added in the step (3) is 0.15mL-0.6 mL.
7. NiS-g-C according to claim 63N4The method for preparing the photocatalyst is characterized in that the volume of the sodium sulfide solution added in the step (3) is preferably 0.15 mL.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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