CN107149940B - Preparation method of fluorine and nitrogen co-doped molybdenum disulfide - Google Patents
Preparation method of fluorine and nitrogen co-doped molybdenum disulfide Download PDFInfo
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- CN107149940B CN107149940B CN201710312767.1A CN201710312767A CN107149940B CN 107149940 B CN107149940 B CN 107149940B CN 201710312767 A CN201710312767 A CN 201710312767A CN 107149940 B CN107149940 B CN 107149940B
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 56
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 28
- 239000011737 fluorine Substances 0.000 title claims abstract description 26
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 title claims 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 claims abstract description 14
- 238000001291 vacuum drying Methods 0.000 claims abstract description 14
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 10
- 239000010935 stainless steel Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 13
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims description 5
- 239000011684 sodium molybdate Substances 0.000 claims description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 23
- 238000000034 method Methods 0.000 abstract description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 4
- 239000011733 molybdenum Substances 0.000 abstract description 4
- 239000011593 sulfur Substances 0.000 abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000005868 electrolysis reaction Methods 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- -1 ammonium fluoroborate Chemical compound 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000009029 wenxiao Substances 0.000 description 1
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Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/51—
Abstract
A preparation method of fluorine and nitrogen co-doped molybdenum disulfide mainly comprises the steps of sequentially adding a molybdenum source, a sulfur source, a nitrogen source and a fluorine source into a stainless steel reaction kettle according to a certain mass ratio, adding water, stirring for 10-30 minutes, wherein the filling amount is 60-80%, placing the mixture into the stainless steel reaction kettle for sealing, placing the mixture into a crucible furnace, heating at 250-450 ℃ for 6-24 hours, and taking out the mixture after the reaction kettle is naturally cooled to room temperature; and washing the mixture with absolute ethyl alcohol, dilute hydrochloric acid and distilled water for 3-6 times, filtering, and placing the obtained powder in a vacuum drying oven for vacuum drying at 60-100 ℃ for 6-24 hours. The method has the advantages of simple process, mild reaction conditions, no need of adding any surfactant, high repeatability and low cost, and the prepared fluorine and nitrogen co-doped molybdenum disulfide has excellent catalytic activity, shows excellent catalytic activity for hydrogen evolution in electrolyzed water under an acidic environment, and has good circulation stability.
Description
Technical Field
The invention relates to a preparation method of a catalyst for hydrogen production by water electrolysis.
Background
In the current society, fossil energy is the most important energy consumed globally, but due to limited reserves, the exhaustion of the fossil energy cannot be avoided along with continuous exploitation and use of human beings. Meanwhile, when fossil energy is not completely combusted, a large amount of greenhouse gases such as carbon dioxide and the like are generated, so that the greenhouse effect of the atmosphere is enhanced, a series of very serious problems such as global warming are caused, and polluted flue gas can be generated during combustion, and the global ecological environment is seriously threatened. In view of the above, the development of clean renewable energy is the direction of energy development in the future. Among the numerous energy carriers, hydrogen attracts a great deal of attention and is considered as a new energy source with the highest efficiency and cleanliness. This is because hydrogen not only has an extremely high energy density, but it forms only water during combustion, and is highly clean.
Wherein the hydrogen production by electrolyzing water shows wider application prospect. In the water electrolysis process, a proper catalyst is generally required to reduce the overpotential of the hydrogen evolution reaction and promote the hydrogen evolution reaction. Platinum group noble metals such as Pt, Pd, etc. are the most commonly used high-efficiency catalysts at present, but the wide application of the platinum group noble metals is greatly limited due to the high price of the platinum group noble metals. Recently, molybdenum disulfide, a two-dimensional material, has attracted much attention as a catalyst for hydrogen production by water electrolysis due to its unique physical and chemical properties.
Researches have shown that active sites of molybdenum disulfide are mainly concentrated at edges, the whole basal plane of the molybdenum disulfide is inert, WenXiao et al (adv. energy mater.2017,1602086) obtains higher catalytic performance of hydrogen production by electrolyzing water by doping molybdenum disulfide with nitrogen, but the whole basal plane is still inert, Hong L i et al (Nat Mater 15,48-53) activates the basal plane by increasing sulfur vacancy of the basal plane, so that the basal plane has catalytic activity, but needs to provide stretching force for the basal plane, has complex operation and is difficult to be widely applied.
Disclosure of Invention
The invention aims to provide a preparation method of fluorine and nitrogen co-doped molybdenum disulfide, which has the advantages of simple synthesis process, mild reaction conditions, high repeatability, activation of a large amount of inert basal planes and excellent catalytic activity of hydrogen production by water electrolysis. The invention prepares the catalyst with excellent catalytic activity for hydrogen production by electrolyzing water by a hydrothermal method mainly at a lower temperature without adding any surfactantFluorine and nitrogen co-doped molybdenum disulfide (hereinafter referred to as MoS)2-NF) in the presence of a catalyst.
The technical scheme of the invention is as follows:
(1) the method comprises the following steps of sequentially adding a molybdenum source, a sulfur source, a nitrogen source and a fluorine source into a stainless steel reaction kettle according to the mass ratio of 1: 2-5.7: 0.57: 2, adding water, controlling the filling amount of the reaction kettle to be 60-80% by controlling the molar ratio of the molybdenum source to the water to be 1: 1785-.
(2) Placing the stainless steel reaction kettle in the step (1) in a crucible furnace, heating for 6-24 hours at 250-450 ℃, and taking out the mixture after the reaction kettle is naturally cooled to room temperature;
(3) and (3) washing the mixture obtained in the step (2) with absolute ethyl alcohol, dilute hydrochloric acid (0.5 mol/L) and distilled water for 3-6 times in sequence, filtering, and placing the obtained powder in a vacuum drying oven with the vacuum degree of-1 Mpa for vacuum drying at the temperature of 60-100 ℃ for 6-24 hours to obtain the petal-shaped fluorine and nitrogen co-doped molybdenum disulfide with excellent electrolytic water hydrogen evolution catalytic activity.
Compared with the prior art, the invention has the following advantages:
1. the fluorine and nitrogen codoped molybdenum disulfide can be prepared at a lower temperature, the CVD equipment and high-temperature conditions required by conventional doping are avoided, the reaction conditions are mild, the preparation process is simplified, and the repeatability is high.
2. The prepared fluorine and nitrogen codoped molybdenum disulfide has a good petal-shaped ball shape, and the doping of fluorine and nitrogen enables the electron transmission capability of the material to be strong, and a large amount of inert basal planes to be activated, so that the material has excellent catalytic activity for hydrogen evolution in water electrolysis and good cycling stability.
3. Any surfactant is not required to be added in the synthesis process, so that the post-treatment step of removing the surfactant is avoided, the operation process is simple, and the cost is reduced.
4. Can be produced in large scale and realize industrialization.
Drawings
FIG. 1 shows MoS obtained in example 1 of the present invention2-scanning electron microscopy of NF.
FIG. 2 shows MoS obtained in example 1 of the present invention2NF at 0.5MH2SO4A linear scanning diagram for hydrogen production by water electrolysis of solution.
FIG. 3 is a MoS prepared according to example 1 of the present invention2-energy spectrum of NF.
FIG. 4 shows MoS obtained in example 2 of the present invention2High-power transmission electron microscopy images of NF.
FIG. 5 shows MoS obtained in example 3 of the present invention2Pore size distribution plot of NF.
FIG. 6 shows MoS obtained in example 4 of the present invention2Transmission electron microscopy of NF.
FIG. 7 shows MoS obtained in example 5 of the present invention2-NFd at 0.5M H2SO4And (3) a time-current diagram for producing hydrogen by electrolyzing water with the solution.
Example 1
Sequentially adding 0.35 g of sodium molybdate, 2 g of thiourea, 0.7 g of ammonium fluoride and 45ml of water into a stainless steel reaction kettle with the volume of 75ml, stirring for 30 minutes, and sealing, wherein the filling amount is 60%; then the reaction kettle is placed in a crucible furnace, heated for 6 hours at 350 ℃, and then taken out after the reaction kettle is naturally cooled to room temperature. And washing the mixture with absolute ethyl alcohol, 0.5 mol/L diluted hydrochloric acid and distilled water for 6 times, filtering, and then placing the mixture in a vacuum drying oven with the vacuum degree of-1 Mpa for vacuum drying at 70 ℃ for 12 hours to obtain the fluorine and nitrogen co-doped molybdenum disulfide with excellent catalytic activity for hydrogen production by electrolyzing water.
As shown in fig. 1, it can be clearly seen that the fluorine and nitrogen co-doped molybdenum disulfide is in the shape of a petal sphere, and the petal sphere is formed by stacking sheets.
As shown in FIG. 2, it can be seen that the synthesized fluorine and nitrogen co-doped molybdenum disulfide has excellent performance of hydrogen production by electrolyzing water in an acidic solution, and the initial reaction potential is-110 mV
As shown in fig. 3, it can be clearly seen that nitrogen, fluorine, molybdenum and sulfur are present in the doped molybdenum disulfide, and the nitrogen and fluorine are successfully doped.
Example 2
Sequentially adding 0.35 g of sodium molybdate, 2 g of thioacetamide, 0.7 g of ammonium fluoride and 45ml of water into a stainless steel reaction kettle with the volume of 75ml, stirring for 30 minutes, and sealing, wherein the filling amount is 60%; then the reaction kettle is placed in a crucible furnace, heated for 12 hours at 450 ℃, and then taken out after the reaction kettle is naturally cooled to room temperature. And washing the mixture with absolute ethyl alcohol, 0.5 mol/L diluted hydrochloric acid and distilled water for 3 times, filtering, and then placing the mixture in a vacuum drying oven with the vacuum degree of-1 Mpa for vacuum drying at the temperature of 60 ℃ for 24 hours to obtain the fluorine and nitrogen co-doped molybdenum disulfide with excellent catalytic activity for hydrogen production by electrolyzing water.
As shown in fig. 4, it can be seen that the fluorine and nitrogen co-doped molybdenum disulfide has discontinuous crystal lattices and disconnected crystal lattices, and provides active sites for hydrogen production by water electrolysis.
Example 3
Sequentially adding 0.35 g of ammonium molybdate, 0.7 g of thiourea, 0.7 g of ammonium fluoroborate and 45ml of water into a stainless steel reaction kettle with the volume of 75ml, stirring for 10 minutes, and sealing, wherein the filling amount is 60%; then the reaction kettle is placed in a crucible furnace, heated for 12 hours at 350 ℃, and then taken out after the reaction kettle is naturally cooled to room temperature. And washing the mixture with absolute ethyl alcohol, 0.5 mol/L diluted hydrochloric acid and distilled water for 5 times, filtering, and then placing the mixture in a vacuum drying oven with the vacuum degree of-1 Mpa for vacuum drying at 70 ℃ for 24 hours to obtain the fluorine and nitrogen co-doped molybdenum disulfide with excellent electrolytic water evolution hydrogen catalytic activity.
As shown in fig. 5, it can be seen that the fluorine and nitrogen co-doped molybdenum disulfide has a microscopic mesoporous structure, and provides an ion rapid transmission channel for the hydrogen production process by water electrolysis.
Example 4
0.35 g of sodium molybdate, 2 g of L-cysteine, 0.2 g of ammonium fluoride and 45ml of water are sequentially added into a stainless steel reaction kettle with the volume of 75ml, stirred for 20 minutes, sealed and filled with 60 percent, then the reaction kettle is placed in a crucible furnace, heated for 24 hours at 350 ℃, then the mixture is taken out after the reaction kettle is naturally cooled to room temperature, and the mixture is sequentially washed for 5 times by absolute ethyl alcohol, 0.5 mol/L dilute hydrochloric acid and distilled water, filtered and then placed in a vacuum drying oven with the vacuum degree of-1 Mpa and dried for 6 hours at 100 ℃ in vacuum, thus obtaining the fluorine and nitrogen co-doped molybdenum disulfide with excellent electrolytic water hydrogen evolution catalytic activity.
As shown in fig. 6, it can be clearly seen that the fluorine and nitrogen co-doped molybdenum disulfide is formed by stacking sheets.
Example 5
Sequentially adding 0.35 g of sodium molybdate, 1.6 g of sulfur powder, 0.5 g of ammonium fluoride and 60ml of water into a stainless steel reaction kettle with the volume of 75ml, stirring for 30 minutes, and sealing, wherein the filling amount is 80%; then the reaction kettle is placed in a crucible furnace, heated for 24 hours at the temperature of 250 ℃, and then taken out after the reaction kettle is naturally cooled to the room temperature. And washing the mixture with absolute ethyl alcohol, 0.5 mol/L diluted hydrochloric acid and distilled water for 4 times, filtering, and then placing the mixture in a vacuum drying oven with the vacuum degree of-1 Mpa for vacuum drying at 70 ℃ for 12 hours to obtain the fluorine and nitrogen co-doped molybdenum disulfide with excellent electrolytic water evolution hydrogen catalytic activity.
As shown in fig. 7, it can be clearly seen that the current of the fluorine and nitrogen co-doped molybdenum disulfide has only slight decay within 30000s, indicating that the molybdenum disulfide has good long cycle performance.
Claims (1)
1. A preparation method of fluorine and nitrogen co-doped molybdenum disulfide is characterized by sequentially adding 0.35 g of sodium molybdate, 2 g of thiourea, 0.7 g of ammonium fluoride and 45m of L water into a stainless steel reaction kettle with the volume of 75m L, stirring for 30 minutes, sealing, wherein the filling amount is 60%, then placing the reaction kettle into a crucible furnace, heating for 6 hours at 350 ℃, then taking out a mixture after the reaction kettle is naturally cooled to room temperature, sequentially washing the mixture for 6 times with absolute ethyl alcohol, 0.5 mol/L diluted hydrochloric acid and distilled water, filtering, and then placing the mixture into a vacuum drying oven to be dried for 12 hours at 70 ℃ in vacuum, thus obtaining the fluorine and nitrogen co-doped molybdenum disulfide with excellent electrolytic water hydrogen production catalytic activity.
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CN111282582A (en) * | 2020-03-19 | 2020-06-16 | 苏州楚捷新材料科技有限公司 | Preparation method of foam nickel-based catalyst for hydrogen production by water electrolysis |
CN113451139B (en) * | 2021-06-23 | 2022-05-03 | 复旦大学 | Method for carrying out p-type doping on TMDCs based on PTFE and semiconductor |
CN114369848B (en) * | 2022-02-11 | 2023-05-09 | 苏州阳池科技有限公司 | Preparation and application of heteroatom doped molybdenum disulfide nanocomposite |
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