CN113000048A - MoS2Preparation method and application of Co-loaded nanoparticles - Google Patents
MoS2Preparation method and application of Co-loaded nanoparticles Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 27
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 27
- FTDUHBOCJSQEKS-UHFFFAOYSA-N borane;n-methylmethanamine Chemical compound B.CNC FTDUHBOCJSQEKS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000003054 catalyst Substances 0.000 claims description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 150000001868 cobalt Chemical class 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 150000001721 carbon Chemical class 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000006356 dehydrogenation reaction Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 238000006460 hydrolysis reaction Methods 0.000 description 17
- 230000007062 hydrolysis Effects 0.000 description 14
- 239000000725 suspension Substances 0.000 description 12
- YPTUAQWMBNZZRN-UHFFFAOYSA-N dimethylaminoboron Chemical compound [B]N(C)C YPTUAQWMBNZZRN-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000012267 brine Substances 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000011232 storage material Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
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- 238000004220 aggregation Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- WZMUUWMLOCZETI-UHFFFAOYSA-N azane;borane Chemical class B.N WZMUUWMLOCZETI-UHFFFAOYSA-N 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- B01J35/40—
-
- 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
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
-
- 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
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
-
- 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
- C01B2203/1082—Composition of support materials
-
- 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 discloses a MoS2The preparation and application of the Co-loaded nano-particles are characterized in that the particles are dispersed by stirring and ultrasound in the synthesis process of the particle material, and a reducing agent sodium borohydride is rapidly added under the ice bath condition, so that fine Co nano-particles are formed. The synthesis method has simple equipment requirement, rapid synthesis and no need of a stabilizer, and is a simple, convenient and green synthesis method. The nano particle has good catalytic selectivity for hydrolytic dehydrogenation of dimethyl ammonia borane, has good recoverable and recyclable performance, and can be used as a good economic catalystThe agent is used.
Description
Technical Field
The invention relates to a nano material used in the technical field of catalysis, in particular to a MoS2A preparation method and application of Co-loaded nanoparticles.
Background
In the 21 st century of rapid development of industry, energy acquisition from fossil fuels such as natural gas and petroleum is the main approach of us, but the reserves of fossil fuels are limited due to non-renewable energy, and the development of new clean energy is urgent. Hydrogen energy is one of the major breakthrough targets of researchers, has the advantages of high hydrogen storage density, light weight, harmless combustion products and the like, and is widely stored in chemical hydrogen storage materials.
In the chemical hydrogen storage material, the ammonia borane has the hydrogen storage amount of 19.8 wt%, can release hydrogen at room temperature under the action of a catalyst, and is one of the hydrogen storage materials with great potential. However, the ammonia borane is high in price at present, and is not beneficial to large-scale storage and preparation of hydrogen. The derivative of ammonia borane, namely dimethyl ammonia borane, has the advantages of relatively low price, stability at room temperature, convenience in storage and the like, and can also be used for preparing hydrogen.
The current hydrolysis research of dimethyl ammonia borane is mainly biased to dehydrogenation coupling in organic solvent tetrahydrofuran or toluene, and is less reactive in aqueous phase. In addition, noble metals are the main components in the reaction for catalyzing the hydrolysis, and complete non-noble metals are rarely used for the hydrolytic dehydrogenation of the substrate.
Disclosure of Invention
The invention provides a MoS2The Co-loaded nano-particles can show good catalytic selectivity and recyclability for dimethyl ammonia borane, and are a non-noble metal economical catalyst with excellent performance.
The technical scheme of the invention is that the MoS2The preparation method of the Co-loaded nanoparticle material comprises the following steps:
s1, MoS2Mixing with cobalt salt and water, performing ultrasonic treatment for 20-30, and stirring the solution in an ice bath environment for 1 h;
s2, adding NaBH4Dissolving with water, adding into the solution in S1 for reaction, and stirring for 1h in the reaction process, wherein the mixed reaction is carried out in an ice bath environment;
s3, after the reaction is finished, centrifuging, washing and vacuum drying are carried out to obtain MoS2Carrying Co nanoparticles.
Further, the cobalt salt in S1 is cobalt chloride hexahydrate, which reacts with MoS2And the mass ratio of water is 1.19:2: 200.
Further, the carrier MoS2Replacement by Fe3O4、AC、CeO2Or ZrO2The substitution amount was 1: 1.
Further, the time for mixing after adding water in S1 is 5min, and the time for ultrasonic treatment is 30 min.
Further, in S1 and S2, the stirring speed in the ice bath environment was 2400 r/min.
The invention also relates to the MoS prepared by the method2The particle size of the Co-loaded nano-particles is 10-70 nm.
The invention also relates to said MoS2The loaded Co nano-particles are used as a catalyst for hydrolyzing dimethyl ammonia borane to produce hydrogen. The catalyst has the advantages of high hydrolytic activity, good cyclability, economy, simple synthesis and the like.
The complete hydrolysis equation of the dimethyl ammonia borane is as follows:
Me2NHBH3+2H2O→Me2NH2BO2+3H2↑
in the application of the catalyst for hydrolyzing dimethyl ammonia borane to produce hydrogen, the catalyst has high catalytic selectivity, and the activation energy value is 58.31 KJ/mol. TOF values 5 minutes before the reaction can be calculated:
wherein t is 5min, mLH2The volume of hydrogen gas obtained in the reaction was 5 minutes.
Calculated TOF 2330mLH2·g-1·min-1。
The invention also has the following beneficial effects:
at present, for hydrogen production by hydrolysis of dimethyl ammonia borane, catalytic hydrolysis is mostly carried out by a noble metal catalyst, a bimetallic catalyst containing noble metal and the like, and the cost can be greatly reduced by using non-noble metal. Based on the current research, a method for producing hydrogen by hydrolyzing dimethyl ammonia borane only by using Co nanoparticles does not exist, and the Co nanoparticles can efficiently catalyze the dimethyl ammonia borane to produce hydrogen by hydrolyzing in a short time and can become a good substitute of a noble metal catalyst.
Hair brushObviously, the method has good effect on inhibiting the aggregation of the nano particles by reduction under the ice bath condition. The method generates the product of MoS2The size of the loaded Co nano-particles is 10-70 nm. Through simple low-temperature reduction, the method is simple and convenient to operate, has low equipment requirement, and has the advantages of environmental protection and economy.
Drawings
FIG. 1 is Co @ MoS2And MoS2XRD test pattern of (1).
FIG. 2 shows MoS2TEM images and particle size distribution of the loaded Co nanoparticles.
FIG. 3 is a graph showing the effect of substrate concentration on hydrolysis kinetics.
FIG. 4 is a graph of the effect of catalyst concentration on hydrolysis kinetics.
FIG. 5 is a graph of the effect of temperature on hydrolysis kinetics.
FIG. 6 is a graph showing the effect of sodium hydroxide concentration on hydrolysis kinetics.
Fig. 7 is a Co nanoparticle catalyst cycling performance test.
Fig. 8 is a graph of the effect on catalytic performance of Co nanoparticle loading with different carriers.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention should not be construed as being limited thereto.
Example 1:
preparing a nano material:
(1) a50 mL round bottom flask was charged with 200mg of MoS2Then 119mg of CoCl was added2·6H2O, finally adding 20mL of deionized water, and stirring for 5 min;
(2) carrying out ultrasonic treatment on the solution in the step (1) for 30 min;
(3) placing the solution in the step (2) in an ice bath environment and violently stirring for 1 h;
(4) weighing 293mg of NaBH4And dissolved in 1mL of deionized water;
(5) quickly injecting the solution in the step (4) into the solution in the step (3), and continuously and vigorously stirring for 1h in an ice bath;
(6) centrifuging and washing the solution in the step (5)Vacuum 60 ℃ drying and noted Co @ MoS2。
Fe was also prepared using the same method3O4，AC，CeO2，ZrO2Supported Co nanoparticles; are respectively marked as Co @ Fe3O4，Co@AC，Co@CeO2，Co@ZrO2。
Co@MoS2And MoS2The XRD test pattern of (A) is shown in FIG. 1. As can be seen from FIG. 1, Co @ MoS2Characteristic diffraction peak and MoS2The crystal face of Co is consistent, and no visible peak of the crystal face of Co exists, mainly because the nano particles are fine and do not form a good crystal form, so that no characteristic peak exists. We performed further TEM characterization and found that fine Co nanoparticles did form. As can be seen from FIG. 2, the dispersed morphology of the nanoparticles is located in MoS2Edge position, average particle size at 40.5 nm.
The Co nanoparticles are used for the kinetics of hydrogen production by hydrolysis of the hydrogen storage material dimethylaminoborane. The research is respectively carried out from the aspects of substrate concentration, catalyst concentration, reaction temperature, different carriers, different sodium hydroxide concentrations and cycle performance.
Example 2
The Co nanoparticles are applied to the dependence of the hydrogen production kinetics of dimethyl ammonia borane on the substrate concentration. The method comprises the following steps:
weighing 23mg of Co nanoparticles, adding magnetons, and adding 9mL of deionized water to obtain a suspension;
and (3) placing the suspension in a water bath kettle, wherein the rotating speed is 2400r/min, and the temperature is set to be 30 ℃. After the reactor was sealed with a plug of brine, 15.35/30.7/46.05/61.4mg (noted as 0.25/0.5/0.75/1mmol) of dimethylaminoborane, respectively, were charged into the reactor, and the hydrogen volume was recorded.
As shown in FIG. 3, the fitted slope of hydrolysis of dimethylaminoborane approaches 0, indicating that the relationship between the hydrolysis reaction and the substrate concentration is zero order reaction, and the dependence on the substrate concentration is not large.
Example 3
The Co nanoparticles are applied to the research on the dependence of the hydrogen production kinetics of dimethyl ammonia borane on the concentration of the catalyst. The method comprises the following steps:
(1) respectively weighing 13.8/23/32.2/41.4mg of Co nanoparticles (marked as 3%, 5%, 7% and 9%), adding magnetons, and adding 9mL of deionized water to obtain a suspension;
(2) and (3) placing the suspension in a water bath kettle, wherein the rotating speed is 2400r/min, and the temperature is set to be 30 ℃. After the reactor was sealed with a plug of brine, a metered amount of dimethylaminoborane, 61.4mg in the reactor, was injected and the recording of the hydrogen volume was started.
As shown in FIG. 4, the hydrolysis of dimethyl ammonia borane is fitted to a first order curve, which shows that the hydrolysis reaction is first order reaction relative to the catalyst concentration, and the higher the catalyst concentration, the faster the reaction rate.
Example 4
The application of Co nanoparticles to the dependence of the hydrogen production kinetics of dimethyl ammonia borane on temperature. The method comprises the following steps:
(1) weighing 23mg of Co nanoparticles, adding magnetons, and adding 9mL of deionized water to obtain a suspension;
(2) the suspension was placed in a water bath at 2400r/min and set at 25/30/35/40 ℃. After the reactor was sealed with a plug of brine, a metered amount of dimethylaminoborane, 61.4mg in the reactor, was injected and the recording of the hydrogen volume was started.
As shown in FIG. 5, the hydrolysis of dimethyl ammonia borane is fitted to a first order curve, which shows that the hydrolysis reaction is first order reaction with temperature, and the reaction rate is faster with higher temperature.
Example 5
The influence of the Co nanoparticles on the concentration of sodium hydroxide when applied to the hydrogen production kinetics of dimethyl ammonia borane. The method comprises the following steps:
(1) weighing 23mg of Co nanoparticles, adding magnetons, and adding 9mL of deionized water to obtain a suspension;
(2) and (3) placing the suspension in a water bath kettle, wherein the rotating speed is 2400r/min, and the temperature is set to be 30 ℃. After the reactor was sealed with a plug of brine, dimethylaminoborane containing varying sodium hydroxide concentrations were injected into the reactor, i.e., 61.4mg of dimethylaminoborane was dissolved in 1mL of a solution containing 4/8/12/16mg of sodium hydroxide (noted as 0.1/0.2/0.3/0.4M).
As shown in fig. 6, the sodium hydroxide solution can effectively promote the hydrolysis kinetics of dimethyl ammonia borane, when the concentration of sodium hydroxide reaches 0.2M, the promoting effect is the greatest, and the reaction rate is negligibly improved by increasing the concentration of sodium hydroxide.
Example 6
The Co nano particles are applied to the hydrogen production dynamics pair circulation performance test of dimethyl ammonia borane. The method comprises the following steps:
(1) weighing 23mg of Co nanoparticles, adding magnetons, and adding 9mL of deionized water to obtain a suspension;
(2) and (3) placing the suspension in a water bath kettle, wherein the rotating speed is 2400r/min, and the temperature is set to be 30 ℃. After the reactor was sealed with a plug of brine, a metered amount of dimethylaminoborane, 61.4mg in the reactor, was injected and the recording of the hydrogen volume was started.
(3) After the reaction was complete, a further charge of 61.4mg of dimethylaminoborane was added to the reactor and the hydrogen volume was recorded again. This step was repeated up to 5 times.
As shown in fig. 7, as the number of times of catalysis increases, the hydrogen production rate is slightly slowed down, but the catalyst activity is still high, and the cycle performance of the Co nanoparticles is good.
Example 7
The Co nano particles are applied to the influence of the hydrogen production kinetics of dimethyl ammonia borane on different carriers. The method comprises the following steps:
(1) weighing 23mg of Co nanoparticles, adding magnetons, and adding 9mL of deionized water to obtain a suspension;
(2) and (3) placing the suspension in a water bath kettle, wherein the rotating speed is 2400r/min, and the temperature is set to be 30 ℃. After the reactor was sealed with a plug of brine, a metered amount of dimethylaminoborane, 61.4mg in the reactor, was injected and the recording of the hydrogen volume was started.
As shown in FIG. 8, the support can have important significance for Co nano-scale, and the catalytic activity of different supports can be seen as Co @ MoS2>Co@ZrO2>Co@CeO2>Co@AC>Co@Fe3O4。Co@MoS2The main reason for having the highest catalytic activity can be attributed to the strong interaction between the support and the Co nanoparticles.
Claims (8)
1. MoS2The preparation method of the Co-loaded nanoparticle material is characterized by comprising the following steps of:
s1, MoS2Mixing with cobalt salt and water, performing ultrasonic treatment for 20-30min, and stirring the solution in ice bath environment for 1 h;
s2, adding NaBH4Dissolving with water, adding into the solution in S1 for reaction, and stirring for 1h in the reaction process, wherein the mixed reaction is carried out in an ice bath environment;
s3, after the reaction is finished, centrifuging, washing and vacuum drying are carried out to obtain MoS2Carrying Co nanoparticles.
2. The method of claim 1, wherein: the cobalt salt in S1 is cobalt chloride hexahydrate, which reacts with MoS2And the mass ratio of water is 1.19:2: 200.
3. The method of claim 1, wherein: mixing the carrier MoS2Replacement by Fe3O4Activated carbon, CeO2Or ZrO2The substitution amount was 1: 1.
4. The method of claim 1, wherein: the water is added into the S1, the mixing time is 5min, and the ultrasonic treatment time is 30 min.
5. The method of claim 1, wherein: the stirring speed in the ice bath environment in S1 and S2 was 2400 r/min.
6. MoS prepared by the method of any of claims 1 to 52The particle size of the Co-loaded nano-particles is 10-70 nm.
7. The MoS of claim 62The loaded Co nano-particles are used as a catalyst for hydrolyzing dimethyl ammonia borane to produce hydrogen.
8. Use according to claim 7, characterized in that: the activation energy value was 58.31 KJ/mol.
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Citations (3)
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| CN111377479A (en) * | 2020-03-20 | 2020-07-07 | 苏州科技大学 | Application of nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production |
| CN112387290A (en) * | 2020-10-26 | 2021-02-23 | 三峡大学 | Fe3O4Preparation method and application of supported metal nanoparticles |
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| CN111377481A (en) * | 2020-03-20 | 2020-07-07 | 苏州科技大学 | Application of cobalt-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production |
| CN111377479A (en) * | 2020-03-20 | 2020-07-07 | 苏州科技大学 | Application of nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production |
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