CN107519909A - Molybdenum disulfide quantum-dot modified graphite-like carbon nitrence, its preparation method and its application - Google Patents
Molybdenum disulfide quantum-dot modified graphite-like carbon nitrence, its preparation method and its application Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 56
- 239000002096 quantum dot Substances 0.000 title claims abstract description 45
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- 238000002604 ultrasonography Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000011941 photocatalyst Substances 0.000 claims description 9
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 7
- 229920004890 Triton X-100 Polymers 0.000 claims description 7
- 239000013504 Triton X-100 Substances 0.000 claims description 7
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 6
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 229940051250 hexylene glycol Drugs 0.000 claims description 3
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims description 3
- 239000011684 sodium molybdate Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229910052961 molybdenite Inorganic materials 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910019934 (NH4)2MoO4 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910015221 MoCl5 Inorganic materials 0.000 description 1
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 after mixing Chemical compound 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 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 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Optics & Photonics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of molybdenum disulfide quantum-dot modified graphite-like carbon nitrence, its preparation method and its application, is the carbon nitrence using nanometer class molybdenum disulfide quantum dot modification two-dimensional layered structure；The content of molybdenum disulfide quantum dot is 1wt%~10wt%, and surplus is carbon nitrence.Preparation method is：(1) soluble molybdenum salt and sulfide and hydrazine, pass through hydro-thermal reaction molybdenum disulfide quantum dot；(2) the g C for synthesizing solid-phase sintering3N4It is distributed to molybdenum disulfide quantum dot in microemulsion, MoS is synthesized using the method for micro emulsion ultrasound2QDs/g‑C3N4Composite, higher photocatalysis efficiency.Cost is cheap, technique is simple.
Description
Technical field
The present invention relates to field of nanometer material technology, specifically a kind of quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide can
See composition, preparation and the application of light photochemical catalyst.
Background technology
Widely studied because of its unique structure and excellent performance using graphene as the two-dimensional layer material of representative
With concern, it is with a wide range of applications in environment and energy field.The g-C of class graphene-structured3N4Because of its special semiconductor
Feature (energy gap Eg=2.7eV), there is absorption in visible region, and with good chemical stability and by the general of people
All over concern, it is widely used in organic reaction, degradating organic dye, photolysis water hydrogen as novel metalloid catalysis material
Etc. in all kinds of catalytic reactions.
However, g-C3N4In actual applications still by photo-generated carrier low separation efficiency, it is seen that light utilization efficiency is low, compares table
The puzzlement for the shortcomings of area is small, thus limit its application in photocatalysis field.In reality, g-C3N4Generally effect one
Co-catalyst or composite catalyst are used for the enhancing of traditional catalysis material performance, and we are in Chinese invention patent carbon nitrence/carbon
Sour silver/silver bromide tri compound nano material (CN106378170A) and g-C3N4-TiO2Composite mesoporous visible-light photocatalyst
(CN105618097A) by adding g-C in3N4Realize the lifting of photocatalysis performance.Quanta point material strengthens g-C3N4Light is urged
The content for changing performance even has no report.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of quantum-dot modified graphite-like carbon of molybdenum disulfide
Nitrence, its preparation method and its application.The composite nano materials yield that cost is cheap, technique is simple, obtains is high, has higher
Photocatalysis efficiency.
Above-mentioned purpose is achieved by the following technical solution：
A kind of quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, it is using nanometer class molybdenum disulfide quantum dot modification two dimension
Carbon nitrence (the g-C of layer structure3N4)；The weight/mass percentage composition of molybdenum disulfide quantum dot is 1%~10%, and surplus is carbon nitrence.
It is preferred that the weight/mass percentage composition of molybdenum disulfide quantum dot is 7%, because addition is 7% composite photocatalyst
Agent has more preferably excellent photocatalysis performance.
The preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, comprises the following steps：
(1) preparation of molybdenum disulfide quantum dot：Soluble molybdenum salt is dissolved in deionized water respectively with sulfide, after mixing,
Hydrazine is added, MoS is synthesized by hydro-thermal reaction2Quantum dot, reaction temperature are 260-320 DEG C, reaction time 9-18h；
Soluble molybdenum salt and the mol ratio of sulfide are 1:2-1:2.2；
The volume ratio of hydrazine and deionized water is 1:10-1:4；
Molybdenum salt is ammonium molybdate, sodium molybdate or molybdenum pentachloride (MoCl5)；Sulfide is vulcanized sodium, potassium sulfide or thiocarbamide；
(2) preparation of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide：The g-C that solid-phase sintering is synthesized3N4With step
(1) prepare gained molybdenum disulfide quantum dot to be distributed in microemulsion, MoS is synthesized using the method for micro emulsion-ultrasound2QDs/g-C3N4
Composite photocatalyst material.
The addition of molybdenum disulfide quantum dot is 1wt%~10wt%.
Microemulsion is Triton X-100, hexylene glycol, normal heptane triplex mixture system, volume ratio 1：1-2：1-
2；Or the triplex mixture system of Triton X-100, hexanol, normal heptane, volume ratio 1：1-2：1-2.
The quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide is used as visible light catalyst, applied to having engine dyeing in organic wastewater
The degraded of organic pollution in material, phenols, antibiotic, the degraded of heavy metal ion and air.
The present invention synthesizes the high quantum-dot modified graphite-like carbon nitrence of photocatalysis performance molybdenum disulfide using easy technique can
See light photochemical catalyst, catalytic performance is better than pure molybdenum disulfide and carbon nitrence, and the efficiency of degradation of organic substances improves 2-3 times, light
Catalysis time 8-15min.Therefore there is important application in the fields such as photocatalysis, air-sensitive, sewage disposal, is expected to be used for advising greatly
The industrial production of mould.
Brief description of the drawings
Fig. 1 is MoS made from the embodiment of the present invention 12QDs/g-C3N4The XRD and XPS spectrum figure of composite photo-catalyst.Fig. 1 a
For the XRD spectrum of product, it was demonstrated that MoS2QDs/g-C3N4G-C in compound be present3N4(100) and (002) diffraction maximum, MoS2's
(006) diffraction maximum, and with standard g-C3N4Card (JCPDF 87-1526) and standard MoS2Card (JCPDF 37-1492) is relative
Should, it was demonstrated that the formation of combination product.Fig. 1 b are MoS2QDs/g-C3N4The full spectrograms of XPS of composite, further demonstrate sample
Mo, S, C, N element presence in product.
Fig. 2 is pure molybdenum disulfide quantum dot (MoS2QDs, Fig. 2 a), g-C3N4(Fig. 2 b) and MoS2QDs/g-C3N4Compound
The TEM collection of illustrative plates of (Fig. 2 c).It can be seen that MoS2QDs is evenly dispersed into g-C3N4The surface of nanometer sheet.
Fig. 3 is MoS made from the embodiment of the present invention 12QDs/g-C3N4The curve line of photocatalyst for degrading song rhodamine B.
MoS2QDs addition is respectively 1,5%, 7%, 10%.Fig. 3 a are different MoS2The composite photocatalyst for degrading RhB of QDs contents
Photocatalysis result, its have preferable photocatalysis performance, particularly addition for 7% composite photo-catalyst have it is more preferably excellent
Performance.Fig. 3 b MoS2Quantum-dot modified g-C3N4With MoS2Nanometer sheet is modified g-C3N4(MoS2NS-g-C3N4) photocatalysis drop
RhB comparison diagram is solved, it can be seen that MoS2Quantum-dot modified composite photo-catalyst has more excellent performance, 10min
Degradation rate is up to 98%.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention can also pass through it
Its scheme for not departing from the technology of the present invention feature describes, therefore all within the scope of the present invention or in the equivalent scope of the invention
Change be included in the invention.
All reagents of the present invention are commercial product, can pass through commercially available approach and obtain.
Embodiment 1：
The preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, comprises the following steps：
(1) by 0.22g (NH4)2MoO4With 0.4g CH4N2S is dissolved in 40mL deionized water, adds 1.5ml N2H4,
After being completely dissolved, continue to stir 30min, then mixed liquor is transferred in 50mL stainless steel cauldron, be placed in vacuum drying chamber
In in 260 DEG C be incubated 9h, be cooled to room temperature.After reaction product is centrifuged, respectively with deionized water and absolute ethyl alcohol repeatedly
Washing, finally 80 DEG C of dry 10h obtain the powder product of grey black, i.e. molybdenum disulfide quantum dot under vacuum
(MoS2QDs)。
(2) 0.1g g-C are weighed again3N420mL is dissolved in be mixed by Triton X-100, hexanol, normal heptane
(volume ratio 1 in microemulsion:1:1), after ultrasonic disperse 10h, MoS is added2After QDs (1%-10%) continues ultrasonic 24h afterwards,
Washed repeatedly with deionized water and absolute ethyl alcohol, finally 60 DEG C of dry 12h obtain MoS under vacuum2QDs/g-C3N4It is compound
Nano material.
Embodiment 2：
The preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, comprises the following steps：
(1) by 0.2g Na2MoO4With 0.45g Na2S is dissolved in 40mL deionized water, adds 2ml N2H4, it is completely molten
Xie Hou, continue to stir 30min, then mixed liquor is transferred in 50mL stainless steel cauldron, be placed in vacuum drying chamber in 280
DEG C insulation 14h, be cooled to room temperature.After reaction product is centrifuged, washed repeatedly with deionized water and absolute ethyl alcohol respectively, most
80 DEG C of dry 10h obtain the powder product of grey black, i.e. molybdenum disulfide quantum dot under vacuum afterwards.
(2) 0.1g g-C are weighed again3N420mL is dissolved in be mixed by Triton X-100, hexylene glycol, normal heptane
Microemulsion in, its volume ratio be 1:1:After 2, ultrasonic disperse 10h, MoS is added2After continuing ultrasonic 24h after QDs 7%, use
Deionized water and absolute ethyl alcohol wash repeatedly, and finally 60 DEG C of dry 12h obtain MoS under vacuum2QDs/g-C3N4It is compound to receive
Rice material.
Embodiment 3：
The preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, comprises the following steps：
(1) by 0.3g MoCl5With 0.5g K2S is dissolved in 40mL deionized water, adds 3ml N2H4, it is completely dissolved
Afterwards, continue to stir 30min, then mixed liquor is transferred in 50mL stainless steel cauldron, be placed in vacuum drying chamber in 320 DEG C
18h is incubated, is cooled to room temperature.After reaction product is centrifuged, washed repeatedly with deionized water and absolute ethyl alcohol respectively, finally
80 DEG C of dry 10h obtain the powder product of grey black, i.e. molybdenum disulfide quantum dot under vacuum.
0.1g g-C are weighed again3N4Be dissolved in 20mL by Triton X-100, alcohol, normal heptane mix it is micro-
In emulsion, its volume ratio is 1:2:After 1, ultrasonic disperse 10h, MoS is added2After continuing ultrasonic 24h after QDs 7%, spend from
Sub- water and absolute ethyl alcohol wash repeatedly, and finally 60 DEG C of dry 12h obtain MoS under vacuum2QDs/g-C3N4Composite Nano material
Material.
Claims (7)
1. a kind of quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide, it is characterised in that repaiied using nanometer class molybdenum disulfide quantum dot
Adorn the carbon nitrence of two-dimensional layered structure；The weight/mass percentage composition of molybdenum disulfide quantum dot is 1%~10%, and surplus is carbon nitrence.
2. the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide described in claim 1, it is characterised in that molybdenum disulfide quantum dot
Weight/mass percentage composition be 7%, surplus is carbon nitrence.
3. the preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide described in claim 1, it is characterised in that including
Following steps：
(1) preparation of molybdenum disulfide quantum dot：Soluble molybdenum salt is dissolved in deionized water respectively with sulfide, after mixing, is added
Hydrazine, 260 DEG C of -320 DEG C of reaction 9-18h, MoS is synthesized by hydro-thermal reaction2Quantum dot；
(2) preparation of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide：The g-C that solid-phase sintering is synthesized3N4Made with step (1)
Standby gained molybdenum disulfide quantum dot is distributed in microemulsion, and MoS is synthesized using the method for micro emulsion-ultrasound2QDs/g-C3N4Complex light
Catalysis material.
4. the preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide according to claim 3, it is characterised in that
In step (1), described molybdenum salt is ammonium molybdate, sodium molybdate or molybdenum pentachloride, and sulfide is vulcanized sodium, potassium sulfide or thiocarbamide.
5. the preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide according to claim 3, it is characterised in that
In step (2), microemulsion is Triton X-100, hexylene glycol, normal heptane triplex mixture system, volume ratio 1：1-2：
1-2；Or the triplex mixture system of Triton X-100, hexanol, normal heptane, volume ratio 1：1-2：1-2.
6. the preparation method of the quantum-dot modified graphite-like carbon nitrence of molybdenum disulfide described in claim 3, it is characterised in that step
(1) in, the mol ratio of soluble molybdenum salt and sulfide is 1:2-1:2.2；The volume ratio of hydrazine and deionized water is 1:10-1:4；
The weight/mass percentage composition of molybdenum disulfide quantum dot is 1wt%~10wt% in step (2).
7. the purposes of the quantum-dot modified graphite-like carbon nitrence photocatalyst of molybdenum disulfide described in claim 1.
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| CN109174149A (en) * | 2018-08-13 | 2019-01-11 | 江苏大学 | A kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material and preparation method thereof |
| CN110252349A (en) * | 2019-07-11 | 2019-09-20 | 福州大学 | A kind of original position light deposition preparation CdS@MoS2The preparation method of composite photo-catalyst |
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| CN103614143A (en) * | 2013-11-28 | 2014-03-05 | 天津大学 | Preparation method of ferroferric oxide@silicon dioxide@zinc selenide fluorescent magnetic nanometer particles |
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| CN103614143A (en) * | 2013-11-28 | 2014-03-05 | 天津大学 | Preparation method of ferroferric oxide@silicon dioxide@zinc selenide fluorescent magnetic nanometer particles |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174149A (en) * | 2018-08-13 | 2019-01-11 | 江苏大学 | A kind of visible-light response type MoS2/GO/g-C3N4Tri compound catalysis material and preparation method thereof |
| CN110252349A (en) * | 2019-07-11 | 2019-09-20 | 福州大学 | A kind of original position light deposition preparation CdS@MoS2The preparation method of composite photo-catalyst |
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Application publication date: 20171229 |