CN112570000B - MoS 2 /ND/g-C 3 N 4 Composite material and preparation method thereof - Google Patents
MoS 2 /ND/g-C 3 N 4 Composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 3
- 239000000203 mixture Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002113 nanodiamond Substances 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 8
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 8
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 8
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 8
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000006303 photolysis reaction Methods 0.000 claims abstract description 4
- 230000015843 photosynthesis, light reaction Effects 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 6
- 238000001354 calcination Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
Images
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- B01J35/39—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1094—Promotors or activators
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a MoS 2 /ND/g‑C 3 N 4 The composite material and the preparation method thereof comprise the following steps: (1) cleaning and drying the nano-diamond; (2) the melamine, thiourea, metal chloride, nano diamond and ammonium molybdate are dissolved in absolute ethyl alcohol, heated and insulated for 10 to 24 hours at the temperature of 50 to 80 ℃, and naturally cooled to the room temperature; (3) grinding the mixture obtained in the step (2), putting the mixture into a tube furnace, calcining, and naturally cooling to room temperature; (4) dissolving the product obtained in the step (3) in water, filtering and cleaning after magnetic stirring, and drying to obtain MoS 2 /ND/g‑C 3 N 4 A composite material. The invention utilizes MoS 2 Instead of noble metal promoters to construct MoS 2 /ND/g‑C 3 N 4 The composite material has better activity of hydrogen production by photolysis of water without noble metal as a cocatalyst.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a MoS 2 /ND/g-C 3 N 4 A composite material and a preparation method thereof.
Background
Semiconductor photocatalytic technology can convert solar energy into new energy, such as hydrogen energy, by means of semiconductor materials. Plays an increasingly important role in the field of energy conservation. Graphite phase carbon nitride (g-C) 3 N 4 ) As a carbon-based material, the material has the characteristics of simple preparation, low cost, visible light response, easy structure adjustment and the like, and is favored by people. But practical application is limited due to easy recombination of photogenerated carriers and low visible light responsivity. Research shows that the strong light scattering effect of the nano-diamond (nanodiamond) enables the g-C to be in a high-speed mode 3 N 4 The visible light utilization efficiency of (D) is improved, however, ND/g-C 3 N 4 The activity of the photocatalytic hydrogen production of (a) is still not high, and noble metal promoters, such as platinum, are still required. The development of a photocatalyst which does not participate in a cocatalyst, is cheap and has high activity has certain significance.
Disclosure of Invention
The invention provides a MoS 2 /ND/g-C 3 N 4 The composite material and the preparation method solve the problem of ND/g-C in the prior art 3 N 4 The problem of low activity of photocatalytic hydrogen production is that MoS with better catalytic activity is utilized 2 Replacing the noble metal promoter.
The technical scheme for realizing the invention is as follows:
MoS 2 /ND/g-C 3 N 4 The preparation method of the composite material comprises the following steps:
(1) cleaning and drying the nano-diamond;
(2) the melamine, thiourea, metal chloride, nano diamond and ammonium molybdate are dissolved in absolute ethyl alcohol, heated and insulated for 10 to 24 hours at the temperature of 50 to 80 ℃, and naturally cooled to the room temperature;
(3) grinding the mixture obtained in the step (2), putting the mixture into a tube furnace, calcining, and naturally cooling to room temperature;
(4) and (4) dissolving the product obtained in the step (3) in water, filtering and cleaning after magnetic stirring, and drying to obtain the MoS2/ND/g-C3N4 composite material.
The nano-diamond of 5-10 nm is washed by deionized water, sulfuric acid and ethanol for a plurality of times in sequence, and then dried for 20-40 min at 410-450 ℃ in air atmosphere.
In the step (2), the mass ratio of melamine to thiourea to the metal chloride to the nano-diamond to the ammonium molybdate is 0.9: 0.7: 3: (0.001-0.005): (0.002-0.005).
In the step (2), the metal chloride is a mixture of KCl and LiCl, and the molar ratio of KCl to LiCl is 1: 1.
And (3) preserving the heat for 25-40min at 530-580 ℃ under nitrogen.
Dissolving the product obtained in the step (4) in water at 70-85 ℃, and magnetically stirring for 2 h.
The MoS 2 /ND/g-C 3 N 4 The composite material is of a nano-sheet porous structure.
The MoS 2 /ND/g-C 3 N 4 The composite material is applied to the hydrogen production by hydrolyzing water.
The MoS 2 /ND/g-C 3 N 4 The hydrogen yield of the composite material under the irradiation of visible light is 619.24 mu molh -1 。
The invention has the beneficial effects that: the invention utilizes MoS 2 Instead of noble metal promoters to construct MoS 2 /ND/g-C 3 N 4 The composite material has better activity of hydrogen production by photolysis of water without noble metal as a cocatalyst. Irradiating with visible light for 240 min without cocatalyst, MoS 2 /ND/g-C 3 N 4 The hydrogen production amount of (2) was 619.24. mu. molh -1 Is obviously higher than g-C 3 N 4 And MoS 2 /g-C 3 N 4 。
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 MoS of the sample of example 1 2 /ND/g-C 3 N 4 （MoS 2 3%) SEM image (a) and TEM image (b).
FIG. 2 is a graph comparing the hydrogen production rates of samples under visible light irradiation.
FIG. 3 shows the MoS sample 2 /ND/g-C 3 N 4 The cycle experimental diagram of hydrogen production by photolysis of water.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without inventive step, are within the scope of the present invention.
Example 1
MoS 2 /ND/g-C 3 N 4 The preparation method of the composite material comprises the following steps:
(1) commercially available nanodiamond purification at 5-10 nm: deionized water rinse multiple times-sulfuric acid rinse multiple times-ethanol rinse multiple times, and then heated to 420 ℃ for about 30min under an air atmosphere.
(2) Taking g-C 3 N 4 The precursor melamine and thiourea mixture (thiourea 0.912g, melamine 0.756 g), 3g KCl/LiCl (molar ratio is 49.4:50.6), a proper amount of nano-diamond 3mg and ammonium molybdate 3mg, and the above materials are mixed into 50mL of absolute ethanol. Then, the mixture was heated to 50 ℃ and incubated for 24 hours, and then allowed to cool to room temperature.
(3) The mixture obtained above was ground thoroughly in an agate mortar for 10 min. The mixture was then transferred to an alumina ceramic crucible and covered with a lid. Subsequently, the crucible containing the mixture was placed in a tube furnace, heated to 550 ℃ with nitrogen as a shielding gas, and held for 25 min. The heating rate is 5-10 ℃/min, and then the mixture is naturally cooled to the room temperature.
(4) The obtained product was dissolved in deionized water at 70 ℃ and magnetically stirred for 2h to remove excess salts. Then filtered and washed 3-5 times with deionized water. Then, the mixture was dissolved in deionized water and dried in a vacuum freeze dryer for 48 hours. Obtaining MoS 2 /ND/g-C 3 N 4 A composite material.
Example 2
MoS 2 /ND/g-C 3 N 4 The preparation method of the composite material comprises the following steps:
(1) commercially available 5-10 nm nanodiamond purification: deionized water rinse multiple times-sulfuric acid rinse multiple times-ethanol rinse multiple times, then heated at 410 ℃ for about 20min under air atmosphere.
(2) Taking g-C 3 N 4 The precursor melamine and thiourea mixture (thiourea 0.912g, melamine 0.756 g), 3g KCl/LiCl (molar ratio is 49.4:50.6), a proper amount of nano-diamond 3mg and ammonium molybdate 2mg, and 80mL of absolute ethanol is added into the materials. Then, the mixture was heated to 70 ℃ and incubated for 15 hours, and then allowed to cool to room temperature.
(3) The mixture obtained above was ground thoroughly in an agate mortar for 20 min. The mixture was then transferred to an alumina ceramic crucible and covered with a lid. Subsequently, the crucible containing the mixture was placed in a tube furnace, heated to 530 ℃ with nitrogen as a protective gas, and held for 40 min. The heating rate is 5-10 ℃/min, and then the mixture is naturally cooled to the room temperature.
(4) The obtained product was dissolved in deionized water at 80 ℃ and magnetically stirred for 2h to remove excess salts. Then filtered and washed 3-5 times with deionized water. Then, the mixture was dissolved in deionized water and dried in a vacuum freeze dryer for 48 hours. Obtaining MoS 2 Nano diamond/g-C 3 N 4 A composite material.
Example 3
MoS 2 /ND/g-C 3 N 4 The preparation method of the composite material comprises the following steps:
(1) commercially available 5-10 nm nanodiamond purification: deionized water rinse multiple times-sulfuric acid rinse multiple times-ethanol rinse multiple times, then heated at 450 ℃ for about 40min under air atmosphere.
(2) Taking g-C 3 N 4 The precursor melamine and thiourea mixture (thiourea 0.912g, melamine 0.756 g), 3g KCl/LiCl (molar ratio is 49.4:50.6), a proper amount of nano-diamond 5mg and ammonium molybdate 5mg, and the above materials are mixed into 100mL of absolute ethanol. Then, the mixture was heated to 80 ℃ and incubated for 10 hours, and then allowed to cool to room temperature.
(3) The mixture obtained above was ground thoroughly in an agate mortar for 30 min. The mixture was then transferred to an alumina ceramic crucible and covered with a lid. Subsequently, the crucible containing the mixture was placed in a tube furnace, heated to 580 ℃ with nitrogen as a shielding gas, and kept for 25 min. The heating rate is 5-10 ℃/min, and then the mixture is naturally cooled to the room temperature.
(4) The obtained product was dissolved in deionized water at 85 ℃ and magnetically stirred for 2h to remove excess salts. Then filtered and washed 3-5 times with deionized water. Then, the mixture was dissolved in deionized water and dried in a vacuum freeze dryer for 48 hours. Obtaining MoS 2 Nano diamond/g-C 3 N 4 A composite material.
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 (6)
1. MoS 2 /ND/g-C 3 N 4 The preparation method of the composite material is characterized by comprising the following steps:
(1) cleaning and drying the nano-diamond;
(2) the melamine, thiourea, metal chloride, nano diamond and ammonium molybdate are dissolved in absolute ethyl alcohol, heated and insulated for 10 to 24 hours at the temperature of 50 to 80 ℃, and naturally cooled to the room temperature; the mass ratio of the melamine to the thiourea to the metal chloride to the nano-diamond to the ammonium molybdate is 0.9: 0.7: 3: (0.001-0.005): (0.002-0.005); the metal chloride is a mixture of KCl and LiCl, and the molar ratio of KCl to LiCl is 1: 1;
(3) grinding the mixture obtained in the step (2), putting the mixture into a tube furnace, preserving the heat for 25-40min at 530-580 ℃ under nitrogen, and naturally cooling to room temperature;
(4) dissolving the product obtained in the step (3) in water, filtering and cleaning after magnetic stirring, and drying to obtain MoS 2 /ND/g-C 3 N 4 A composite material.
2. The MoS of claim 1 2 /ND/g-C 3 N 4 The preparation method of the composite material is characterized by comprising the following steps: the nano-diamond of 5-10 nm is washed by deionized water, sulfuric acid and ethanol for a plurality of times in sequence, and then dried for 20-40 min at 410-450 ℃ in air atmosphere.
3. The MoS of claim 1 2 /ND/g-C 3 N 4 The preparation method of the composite material is characterized by comprising the following steps: dissolving the product obtained in the step (4) in water at 70-85 ℃, and magnetically stirring for 2 h.
4. MoS prepared by the preparation method according to any one of claims 1 to 3 2 /ND/g-C 3 N 4 A composite material characterized by: the MoS 2 /ND/g-C 3 N 4 The composite material is of a nano-sheet porous structure.
5. The MoS of claim 4 2 /ND/g-C 3 N 4 A material characterized by: the MoS 2 /ND/g-C 3 N 4 The composite material is applied to hydrogen production by photolysis of water.
6. The MoS of claim 5 2 /ND/g-C 3 N 4 A material characterized by: the MoS 2 /ND/g-C 3 N 4 The hydrogen yield of the composite material under the irradiation of visible light is 619.24 mu molh -1 。
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| WO2016193464A1 (en) * | 2015-06-05 | 2016-12-08 | Centre National De La Recherche Scientifique | Production of dihydrogen with nanodiamond-supported photocatalyst |
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| CN104492470A (en) * | 2015-01-09 | 2015-04-08 | 江苏大学 | Preparation method of graphite type carbon nitride photocatalytic material |
| CN105772055A (en) * | 2016-04-06 | 2016-07-20 | 东莞理工学院 | Preparation method for carbon nitride visible-light-induced photocatalyst |
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| MoS_2/g-C_3N_4复合催化剂的制备及CdSe量子点敏化产氢性能研究;吴朝军等;《材料导报》;20170525;第167-172页 * |
| 氮化碳/碳复合光催化剂及其光解水产氢性能;曹煜祺等;《江苏理工学院学报》;20200415(第02期);第15-21页 * |
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