CN107970960B - Preparation method of MoP, FeP and redox graphene three-phase composite material - Google Patents
Preparation method of MoP, FeP and redox graphene three-phase composite material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims abstract description 19
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 19
- 239000011733 molybdenum Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 8
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims 1
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 150000001875 compounds Chemical class 0.000 description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000011144 upstream manufacturing Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- -1 molybdenum phosphide compound Chemical class 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
-
- 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
- B01J37/28—Phosphorising
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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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
- 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
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Abstract
The preparation method of the three-phase composite material of the MoP, the FeP and the redox graphene is characterized in that ferric acetylacetonate and molybdenum acetylacetonate are loaded on the graphene oxide, the loaded graphene oxide is taken as a precursor, and then the precursor is phosphorized at high temperature in a short time to obtain the three-phase composite material of the MoP, the FeP and the redox graphene.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to a preparation method of a three-phase composite material of MoP, FeP and redox graphene and application of the three-phase composite material in the aspect of hydrogen production through electrocatalytic hydrolysis.
Background
The urgent need for clean and renewable energy sources has driven the search for catalysts for the production of hydrogen by electrolysis. Recently, Transition Metal Phosphides (TMPs) have been demonstrated to be highly active, highly stable HER catalysts and have faradaic efficiencies approaching 100% not only in strongly acidic solutions, but also in use in strongly basic and neutral media. A large number of researches show that the nanometer hybrid as the catalyst can combine the advantages of all components, and a synergistic effect is generated on a heterogeneous interface, so that the catalytic hydrogen production performance is greatly improved. The preparation of nanocomposites is therefore gaining increasing attention from researchers. However, the traditional preparation method of molybdenum phosphide is complicated, the required phosphorization temperature is higher (not less than 850 ℃) and the time is long (not less than 5h), the obtained molybdenum phosphide is basically sintered, and the catalytic activity is reduced. Therefore, the search for a suitable preparation method of molybdenum phosphide and molybdenum phosphide compound is very important. According to the invention, the three-phase composite material of MoP, FeP and redox graphene is prepared by utilizing the dispersion effect of the redox graphene.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of a three-phase composite material of MoP, FeP and redox graphene.
The preparation method of the MoP, FeP and redox graphene three-phase composite material adopts the following technical scheme:
a preparation method of a three-phase composite material of MoP, FeP and redox graphene comprises the steps of loading ferric acetylacetonate and molybdenum acetylacetonate on graphene oxide, taking the loaded material as a precursor, and carrying out high-temperature short-time phosphorization to obtain the three-phase composite material of MoP, FeP and redox graphene.
A preparation method of a three-phase composite material of MoP, FeP and redox graphene comprises the following steps:
(1) dissolving a certain amount of molybdenum acetylacetonate and iron acetylacetonate in a certain amount of ethanol, and then dispersing a certain amount of graphene oxide in the solution;
(2) taking part of the samples obtained in the step (1), and drying the samples in a drying oven at 80 ℃ to obtain a graphene oxide loaded iron acetylacetonate and molybdenum acetylacetonate composite material serving as a precursor;
(3) putting the sample obtained in the step (2) and a certain amount of sodium hypophosphite into a tubular furnace for phosphorization;
(4) the phosphorized sample is repeatedly washed with water and ethanol for several times and then dried.
Further, the adding proportion of the molybdenum acetylacetonate and the iron acetylacetonate in the step (1) is that the mass ratio is 1-2: 1-2.
Further, in the step (3), the phosphating temperature is 750-850 ℃, and the time of the phosphorus bloom is 1 h.
A preparation method of a three-phase composite material of MoP, FeP and redox graphene comprises the following steps: dissolving 150mg of iron acetylacetonate and 150mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, dispersing 100mg of graphene oxide into the solution, carrying out ultrasonic treatment for 30 minutes, transferring the solution into an oven at 80 ℃ for drying for 24 hours after ultrasonic treatment to obtain a compound precursor, cooling to room temperature, and collecting a product; 1.0g of sodium hypophosphite is placed on the upstream side of a tube furnace, 100mg of the compound precursor is placed on the downstream side of another porcelain boat, a sample is heated and insulated at the temperature of 750-850 ℃ for 0.5-1.5h at the heating speed of 3 ℃/min, and then the sample is naturally cooled to the room temperature under the protection of Ar 2.
A preparation method of a three-phase composite material of MoP, FeP and redox graphene comprises the following steps: dissolving 100mg of iron acetylacetonate and 200mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, dispersing 100mg of graphene oxide into the solution, carrying out ultrasonic treatment for 30 minutes, transferring the solution into an oven at 80 ℃ for drying for 24 hours after ultrasonic treatment to obtain a compound precursor, cooling to room temperature, and collecting a product; 1.0g of sodium hypophosphite is placed on the upstream side of a tube furnace, 100mg of the compound precursor is placed on the downstream side of another porcelain boat, a sample is heated and insulated at the temperature of 750-850 ℃ for 0.5-1.5h at the heating speed of 3 ℃/min, and then the sample is naturally cooled to the room temperature under the protection of Ar 2.
A preparation method of a three-phase composite material of MoP, FeP and redox graphene comprises the following steps: dissolving 200mg of iron acetylacetonate and 100mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, dispersing 100mg of graphene oxide into the solution, carrying out ultrasonic treatment for 30 minutes, transferring the solution into an oven at 80 ℃ for drying for 24 hours after ultrasonic treatment to obtain a compound precursor, cooling to room temperature, and collecting a product; 1.0g of sodium hypophosphite is placed on the upstream side of a tube furnace, 100mg of the compound precursor is placed on the downstream side of another porcelain boat, a sample is heated and insulated at the temperature of 750-850 ℃ for 0.5-1.5h at the heating speed of 3 ℃/min, and then the sample is naturally cooled to the room temperature under the protection of Ar 2.
The composite material of MoP, FeP and redox graphene prepared by the invention can complete phosphorization in a short time at low temperature, and the addition of the redox graphene can effectively prevent the aggregation of phosphide particles. The MoP, FeP and redox graphene prepared by the method can be used as an electrocatalytic hydrogen production catalyst with excellent performance, and has high catalytic activity and good stability. The MoP, FeP and redox graphene prepared by the method can be synthesized in a large amount, expensive equipment is not needed, and the method can be widely used for electrocatalytic hydrogen production catalysts.
Drawings
Fig. 1 is an XRD analysis chart of MoP, FeP, and redox graphene.
Fig. 2 is a linear sweep voltammetry curve of electrocatalytic hydrogen production performance of a six-MoP, FeP, redox graphene three-phase composite material in a three-electrode test embodiment.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the drawings of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
According to the preparation method of the three-phase composite material of the MoP, the FeP and the redox graphene, iron acetylacetonate and molybdenum acetylacetonate are loaded on the graphene oxide, and then the three-phase composite material of the MoP, the FeP and the redox graphene is obtained through high-temperature short-time phosphorization by taking the iron acetylacetonate and the molybdenum acetylacetonate as precursors.
The invention provides a preparation method of a MoP, FeP and redox graphene three-phase composite material, which comprises the following steps:
1. dissolving a certain amount of molybdenum acetylacetonate and iron acetylacetonate in a certain amount of ethanol, and then dispersing a certain amount of graphene oxide in the solution. Preferably, the best preparation method is as follows: the addition ratio of the molybdenum acetylacetonate to the iron acetylacetonate is 1:1 (mass ratio).
2. And (3) putting part of samples obtained in the step (1) in an oven to dry at 80 ℃ to obtain the graphene oxide loaded iron acetylacetonate and molybdenum acetylacetonate composite material serving as a precursor.
3. Putting the sample obtained in the step 2 and a certain amount of sodium hypophosphite into a tubular furnace for phosphorization, preferably, the best preparation method is as follows: the phosphorization temperature is 800 ℃, and the phosphorization time is 1 h.
4. The phosphorized sample is repeatedly washed with water and ethanol for several times and then dried.
Compared with the existing MoP, the method has the advantages that the phosphorization is completed at a lower temperature (750-850 ℃) and in a shorter time (0.5-1.5h) to obtain the MoP and FeP redox graphene. The MoP, FeP and redox graphene material has excellent performance of hydrogen production by water electrolysis. When the material is attached to a rotating disk electrode at 0.3mg/cm2, the current density can reach 30mA/cm2 at an overpotential of 180 mV.
The specific embodiment is as follows:
fig. 1 shows XRD analysis patterns of MoP, FeP, and redox graphene.
The first embodiment is as follows: dissolving 150mg of iron acetylacetonate and 150mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, then dispersing 100mg of graphene oxide into the solution, carrying out ultrasonic treatment for 30 minutes, and transferring the solution into an oven at 80 ℃ for 24 hours to be dried after ultrasonic treatment, thereby obtaining a precursor of the compound. Then cooled to room temperature and the product was collected.
Sodium hypophosphite (1.0g) was placed on the upstream side of the tube furnace, the above compound precursor (100mg) was placed downstream in another porcelain boat, and the sample was heated at 750 ℃ for 0.5h at a rate of 3 ℃/min. Then naturally cooling to room temperature under the protection of Ar 2.
Example two: in the synthesis of a precursor: dissolving 100mg of iron acetylacetonate and 200mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, then dispersing 100mg of graphene oxide into the solution, carrying out ultrasonic treatment for 30 minutes, and transferring the solution into an oven at 80 ℃ for 24 hours to be dried after ultrasonic treatment to obtain a precursor of the compound. The other processing is the same as in embodiment one.
Example three: in the synthesis of a precursor: dissolving 200mg of iron acetylacetonate and 100mg of molybdenum acetylacetonate in 30ml of ethanol, carrying out ultrasonic treatment for 30 minutes, then dispersing 100mg of graphene oxide in the solution, carrying out ultrasonic treatment for 30 minutes, and transferring the solution to an oven at 80 ℃ for 24 hours to dry after ultrasonic treatment, thereby obtaining a precursor of the compound. The other processing is the same as in embodiment one.
Example four: the phosphating temperature was set to 800 ℃ and the other treatments were the same as in example one.
Example five: the phosphating temperature was set to 850 ℃ and the other processes were the same as in example one.
Example six: the phosphating temperature holding time is set to 1h, and other treatments are the same as in example four. As shown in fig. 2, a linear sweep voltammetry curve for testing the electrocatalytic hydrogen production performance of the three-phase composite material of MoP, FeP and redox graphene by using three electrodes is shown.
Example seven: the phosphating temperature holding time is set to 1.5h, and other treatments are the same as example four.
It should be understood that while the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein, and any combination of the various embodiments may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.
Claims (1)
1. A preparation method of a three-phase composite material of MoP, FeP and redox graphene is characterized by comprising the following steps:
(1) dissolving a certain amount of molybdenum acetylacetonate and iron acetylacetonate in a certain amount of ethanol, and then dispersing a certain amount of graphene oxide in the solution;
(2) taking part of the samples obtained in the step (1), and drying the samples in a drying oven at 80 ℃ to obtain a graphene oxide loaded iron acetylacetonate and molybdenum acetylacetonate composite material serving as a precursor;
(3) putting the sample obtained in the step (2) and a certain amount of sodium hypophosphite into a tubular furnace for phosphorization;
(4) repeatedly washing the phosphorized sample with water and ethanol for several times, and drying;
in the step (1), the addition ratio of the molybdenum acetylacetonate to the iron acetylacetonate is 1-2 by mass: 1-2;
in the step (3), the phosphating temperature is 750-850 ℃ and the phosphating time is 1 h.
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| CN108654659B (en) * | 2018-05-11 | 2019-04-02 | 重庆文理学院 | A kind of phosphating sludge/graphene composite nano material and preparation method thereof |
| CN111211309B (en) * | 2020-01-17 | 2021-12-07 | 上海应用技术大学 | Phosphorus-doped graphene-coated iron oxide composite material and preparation method and application thereof |
| CN113072044B (en) * | 2021-03-25 | 2022-06-21 | 安徽师范大学 | Core-shell structure FeP nano-chain, preparation method thereof and application thereof in battery |
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| CN104001529A (en) * | 2014-06-09 | 2014-08-27 | 东南大学 | Preparation method of load type transit metallic phosphide catalyst |
| CN105720278A (en) * | 2016-03-31 | 2016-06-29 | 华中科技大学 | High-efficiency multi-element transition metal phosphide hydrogen-evolution catalyst and preparation method thereof |
| CN105772041A (en) * | 2014-12-25 | 2016-07-20 | 中国科学院理化技术研究所 | Photocatalytic hydrogen production cocatalyst, photocatalytic system and hydrogen production method |
| CN107180944A (en) * | 2017-06-20 | 2017-09-19 | 大连理工常州研究院有限公司 | A kind of preparation method and applications of metal phosphide nano-particle |
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| CN104001529A (en) * | 2014-06-09 | 2014-08-27 | 东南大学 | Preparation method of load type transit metallic phosphide catalyst |
| CN105772041A (en) * | 2014-12-25 | 2016-07-20 | 中国科学院理化技术研究所 | Photocatalytic hydrogen production cocatalyst, photocatalytic system and hydrogen production method |
| CN105720278A (en) * | 2016-03-31 | 2016-06-29 | 华中科技大学 | High-efficiency multi-element transition metal phosphide hydrogen-evolution catalyst and preparation method thereof |
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