CN103816906A - Ni3B load carbon composite catalyst for hydrogen production by ammonia borane hydrolysis - Google Patents
Ni3B load carbon composite catalyst for hydrogen production by ammonia borane hydrolysis Download PDFInfo
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- CN103816906A CN103816906A CN201410056196.6A CN201410056196A CN103816906A CN 103816906 A CN103816906 A CN 103816906A CN 201410056196 A CN201410056196 A CN 201410056196A CN 103816906 A CN103816906 A CN 103816906A
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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
Abstract
A Ni3B load carbon composite catalyst for hydrogen production by ammonia borane hydrolysis is a composite catalyst prepared by loading a carbon source carrier with Ni3B active substance, the carbon source carrier is VulcanXC-72, the Ni3B active substance loaded on the carbon source carrier is a crystalline substance with the particle diameter being less than or equal to 10nm, the Ni3B load amount in the composite catalyst is 30-70wt%; a preparation method is as follows: using nickel chloride as a nickel salt, using potassium borohydride as a reduction agent, adding different proportions of a carbon source for synthesis in a tetraglycol solution. The advantages of the Ni3B load carbon composite catalyst are that: a carbon source material in the Ni3B load carbon composite catalyst has a high specific surface area, and can effectively disperse nanoparticles; the Ni3B active substance loaded on carbon has small particle size, large specific surface area and many catalytic active sites, and can significantly improve the activity of the catalyst; the Ni3B load carbon composite catalyst is synthesized in situ by a solution method, and has the advantages of being simple in process, low in cost, easy to implement, and convenient for large-scale popularization and application.
Description
Technical field
The present invention relates to hydrogen storage material field, particularly a kind of carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3b composite catalyst and preparation method thereof.
Background technology
Along with the development of human society, energy crisis and environmental pollution become the significant problem that the world today faces.People strive to find a kind of environmental friendliness, renewable new forms of energy that fuel value is high.Hydrogen Energy, as a kind of new cleaning fuel, has originate wide, caloric value advantages of higher, is considered to the new generation of green energy.But promoting the use of of Hydrogen Energy is still faced with two hang-ups, the safe and efficient of Hydrogen Energy produced and stored, and this has become the bottleneck of restriction Hydrogen Energy development.In recent years, the development of hydrogen storage material has obtained remarkable progress.In light hydrogen occluding material, ammonia borine has higher quality hydrogen-storage density (19.6wt%) and is more and more subject to people's concern, has become one of a kind of potential hydrogen storage material.
It is controlled and thorough that ammonia borane hydrolysis is put hydrogen methods, becomes one of study hotspot of people.But its water solution system is stable, catalyst-free Water Under liberation hydrogen is slow, and therefore, the key that in ammonia borine, hydrogen energy source is released makes to find a kind of desirable catalyst.Current research report shows, the catalyst that is applicable to the reaction of ammonia borane hydrolysis is mainly catalyst based and Ni, Co metal and compound thereof etc. of precious metals pt, referring to: J Power Sources, 2006,156:190-4; J Power Sources, 2006,163:364-70; Inorg Chem. 2007,46:788-94.Show significant catalytic activity although Pt is catalyst based, its cost is high, abundance is low, is difficult to realize industrialization, therefore finds the catalyst that a kind of cost low activity is high most important.
In non-precious metal catalyst, nickel-base catalyst has the advantages such as cost is low, toxicity is little, catalytic performance is good and causes people's concern.At present, some researchs show that nickel B catalyst has good catalytic activity, referring to: Int J Hydrogen Energy, 2012,37:327-34.Yao etc. once reported amorphous Ni
x b catalyzing hydrolysis ammonia borine, referring to: Int J Hydrogen Energy, 2008,33:2462-7.Kalidindi etc. once reported Ni-Ni
3b nano composite material is put hydrogen catalyst as catalysis ammonia borine, referring to: Int J Hydrogen Energy, 2010,35:10819-25; Phys Chem Chem Phys. 2009,11:770-5, has good catalytic activity.Through literature survey, Schaefer ZL etc. had once reported synthetic Ni in solution
3b is nanocrystalline and study its structure and magnetic, referring to: J Phys Chem C. 2008,112:19846-51.But about Ni
3the Ni of B and carbon load
3b did not also report for the research of catalyzing hydrolysis ammonia borine.
Summary of the invention
The object of the invention is to for above-mentioned existing problems, a kind of carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis is provided
3b composite catalyst and preparation method thereof, this composite catalyst is the Ni of carbon load
3b, the carbon source material adding has higher specific area, effectively dispersing nanometer particle, utilization rate and the stability of raising active material; Load on the Ni on carbon
3b active material has that particle diameter is little, specific area is large, active site is many, thereby has increased substantially the catalytic activity of catalyst; Its preparation method technique is simple, with low cost, easy to implement, is convenient to large-scale promotion application.
Technical scheme of the present invention:
A kind of carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3b composite catalyst is carbon source carrier load Ni
3the composite catalyst of B active material composition, chemical formulation is Ni
3b/C, carbon source carrier is VulcanXC-72, loads on the Ni on carbon
3b active material is the crystalline state material of particle diameter≤10nm, Ni in composite catalyst
3the load capacity of B is 30-70wt%.
A kind of described carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3the preparation method of B composite catalyst, take VulcanXC-72 as carbon source, nickel chloride is nickel salt, take potassium borohydride as reducing agent, adds the carbon source of different proportion, synthetic in tetraethylene glycol solution, concrete preparation process is as follows:
1) under room temperature, nickel chloride and tetraethylene glycol solution are mixed and ultrasonic dissolution obtains the mixed solution of green transparent, in mixed solution, the concentration of nickel chloride is 0.03mol/L, in mixed solution, add VulcanXC-72, ultrasonic agitation becomes the mixed solution a of homogeneous, and the addition of VulcanXC-72 is according to Ni in composite catalyst
3the load capacity of B is determined;
2) in ice-water bath, excessive potassium borohydride is mixed with tetraethylene glycol solution and dissolved and obtain mixed solution b, in mixed solution b, the concentration of potassium borohydride is 0.62mol/L;
3) in argon gas, mixed solution a is warming up to 45 ℃, then mixed solution b is added in mixed solution a, after being warmed up to 280 ℃ under stirring, keep 5min, centrifugal while being down to room temperature, and with after ethanol washing 5 times in vacuum drying oven 60 ℃ dry, vacuum is-0.1MPa to make the carbon load Ni of a series of different loads amounts
3b composite catalyst.
Advantage of the present invention is: this carbon load Ni
3carbon source material in B composite catalyst has higher specific area, effectively dispersing nanometer particle, utilization rate and the stability of raising active material; Load on the Ni on carbon
3b active material has that particle diameter is little, specific area is large, active site is many, thereby has increased substantially the catalytic activity of catalyst, and at room temperature, the maximum hydrogen discharging rate of this composite catalyst catalysis ammonia borane hydrolysis can reach 1168 mL min
-1g
-1, the activation energy of reaction is minimum can be to 44.06 kJ mol
-1; This composite catalyst adopts solwution method original position synthetic, and technique is simple, with low cost, easy to implement, is convenient to large-scale promotion application.
Accompanying drawing explanation
Fig. 1 is the Ni of different loads amount
3the XRD figure of B/C.
Fig. 2-4th, load capacity is respectively 34.25wt%, 50.35wt%, the Ni of 67.90wt%
3b/C catalyst TEM figure.
Fig. 5 is that load capacity is 34.25wt%, 50.35wt%, the Ni of 67.90wt%
3b/C catalyst is the hydrogen discharging performance resolution chart of catalysis ammonia borane hydrolysis at room temperature.
Fig. 6-8th, load capacity is 34.25wt%, 50.35wt%, the Ni of 67.90wt%
3b/C catalyst is 25 ℃ of water-baths, and 35 ℃, 45 ℃, hydrogen discharging performance test and the activation energy resolution chart of catalysis ammonia borane hydrolysis at 55 ℃.
The specific embodiment
Embodiment 1:
A kind of described carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3the preparation method of B composite catalyst, concrete preparation process is as follows:
1) under room temperature, in round-bottomed flask, nickel chloride and tetraethylene glycol solution are mixed and ultrasonic dissolution obtains the mixed solution of green transparent, in mixed solution, the concentration of nickel chloride is 0.03mol/L, presses Ni in mixed solution
3the load capacity of B is that 34.25wt% adds corresponding VulcanXC-72, and ultrasonic agitation becomes the mixed solution a of homogeneous;
2) in ice-water bath, excessive potassium borohydride is mixed with tetraethylene glycol solution and dissolved and obtain mixed solution b, in mixed solution b, the concentration of potassium borohydride is 0.62mol/L;
3) in argon gas, mixed solution a is warming up to 45 ℃, then mixed solution b is added in mixed solution a, keep 5min after being warmed up to 280 ℃ under stirring, centrifugal while being down to room temperature, and with after ethanol washing 5 times in vacuum drying oven 60 ℃ dry, vacuum is-0.1MPa to make carbon load Ni
3b composite catalyst.
This carbon load Ni
3the XRD of B composite catalyst schemes as shown in Figure 1; TEM schemes as shown in Figure 2.
Through XRD analysis and elementary analysis, the catalyst of preparation is Ni
3b/C, Ni
3b load capacity is 34.25wt%.
Embodiment 2:
A kind of described carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3the preparation method of B composite catalyst, concrete preparation process is substantially the same manner as Example 1, difference be step 1) in mixed solution by Ni
3the load capacity of B is that 50.35wt% adds corresponding VulcanXC-72.
This carbon load Ni
3the XRD of B composite catalyst schemes as shown in Figure 1; TEM schemes as shown in Figure 3.
Through XRD analysis and elementary analysis, the catalyst of preparation is Ni
3b/C, Ni
3b load capacity is 50.35wt%.
Embodiment 3:
A kind of described carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3the preparation method of B composite catalyst, concrete preparation process is substantially the same manner as Example 1, difference be step 1) in mixed solution by Ni
3the load capacity of B is that 67.90wt% adds corresponding VulcanXC-72.
This carbon load Ni
3the XRD of B composite catalyst schemes as shown in Figure 1; TEM schemes as shown in Figure 4.
Through XRD analysis and elementary analysis, the catalyst of preparation is Ni
3b/C, Ni
3b load capacity is 67.90wt%.
Composite catalyst prepared by embodiment 1-3 is to the test of ammonia borane hydrolysis hydrogen discharging performance and activation energy test.
Composite catalyst prepared by embodiment 1-3 is catalysis ammonia borane hydrolysis respectively, measure its reaction rate and activation energy: get 40mg ammonia borine and be placed in 25mL round-bottomed flask bottom, at 25 ℃, 35 ℃, 45 ℃, 55 ℃ of water-baths, add 8mL distilled water, under stirring condition, add 10mgNi
3b/C catalyst, catalysis ammonia borane hydrolysis, measures hydrogen desorption capacity with drainage.
Fig. 5 is that load capacity is 34.25wt%, 50.35wt%, the Ni of 67.90wt%
3b/C catalyst is the hydrogen discharging performance resolution chart of catalysis ammonia borane hydrolysis at room temperature.As calculated, under room temperature, load capacity is the Ni of 34.25wt%, 50.35wt%, 67.90wt%
3the hydrogen discharging rate of B/C catalyst ammonia borane hydrolysis is respectively 1168.0,692.3,665.2 mL min
-1g
-1, the Ni that wherein load capacity is 34.25wt%
3the hydrogen discharging rate maximum of B/C catalysis ammonia borane hydrolysis.
Fig. 6-8th, load capacity is 34.25wt%, 50.35wt%, the Ni of 67.90wt%
3b/C catalyst is 25 ℃ of water-baths, and 35 ℃, 45 ℃, hydrogen discharging performance test and the activation energy resolution chart of catalysis ammonia borane hydrolysis at 55 ℃.The Ni that wherein load capacity is 67.90wt%
3the activation energy of B/C catalysis ammonia borane hydrolysis reaction is minimum, is 44.06 kJ/mol.
In sum, the prepared carbon supported catalyst Ni of the present invention
3the crystal structure of B/C has XRD to characterize; In catalyst, phosphorus content is by elemental analysis; The pattern of element is characterized by TEM; The catalytic performance of catalyst and the activation energy of reaction characterize by putting hydrogen test; Pressure is standard atmospheric pressure, and temperature is 25-55 ℃.
Claims (2)
1. the carbon load Ni for the hydrogen manufacturing of ammonia borane hydrolysis
3b composite catalyst, is characterized in that: be carbon source carrier load Ni
3the composite catalyst of B active material composition, chemical formulation is Ni
3b/C, carbon source carrier is VulcanXC-72, loads on the Ni on carbon
3b active material is the crystalline state material of particle diameter≤10nm, Ni in composite catalyst
3the load capacity of B is 30-70wt%.
2. one kind as claimed in claim 1 for the carbon load Ni of ammonia borane hydrolysis hydrogen manufacturing
3the preparation method of B composite catalyst, is characterized in that: take VulcanXC-72 as carbon source, nickel chloride is nickel salt, take potassium borohydride as reducing agent, adds the carbon source of different proportion, synthetic in tetraethylene glycol solution, concrete preparation process is as follows:
1) under room temperature, nickel chloride and tetraethylene glycol solution are mixed and ultrasonic dissolution obtains the mixed solution of green transparent, in mixed solution, the concentration of nickel chloride is 0.03mol/L, in mixed solution, add VulcanXC-72, ultrasonic agitation becomes the mixed solution a of homogeneous, and the addition of VulcanXC-72 is according to Ni in composite catalyst
3the load capacity of B is determined;
2) in ice-water bath, excessive potassium borohydride is mixed with tetraethylene glycol solution and dissolved and obtain mixed solution b, in mixed solution b, the concentration of potassium borohydride is 0.62mol/L;
3) in argon gas, mixed solution a is warming up to 45 ℃, then mixed solution b is added in mixed solution a, after being warmed up to 280 ℃ under stirring, keep 5min, centrifugal while being down to room temperature, and with after ethanol washing 5 times in vacuum drying oven 60 ℃ dry, vacuum is-0.1MPa to make the carbon load Ni of a series of different loads amounts
3b composite catalyst.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990465A (en) * | 2014-06-17 | 2014-08-20 | 江西师范大学 | Ni-CeO2@graphene composite nano catalyst used for preparing hydrogen by ammonia borane hydrolysis of ammonia borane and preparation method of catalyst |
| CN104275204A (en) * | 2014-09-15 | 2015-01-14 | 河南科技大学 | Loaded catalyst for hydrolyzing ammonia borane to release hydrogen and preparation method of loaded catalyst |
| CN106140166A (en) * | 2016-06-29 | 2016-11-23 | 苏州大学 | A kind of loaded catalyst, preparation method and applications |
| CN107159214A (en) * | 2017-06-22 | 2017-09-15 | 桂林电子科技大学 | A kind of porous active carbon material load cobalt nanometer particle material and its preparation method and application |
| CN111569933A (en) * | 2020-06-22 | 2020-08-25 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| CN112827492A (en) * | 2021-01-07 | 2021-05-25 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
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| CN1044602A (en) * | 1989-01-30 | 1990-08-15 | 天津大学 | Resin-carried diboride nickel catalyst and preparation thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990465A (en) * | 2014-06-17 | 2014-08-20 | 江西师范大学 | Ni-CeO2@graphene composite nano catalyst used for preparing hydrogen by ammonia borane hydrolysis of ammonia borane and preparation method of catalyst |
| CN104275204A (en) * | 2014-09-15 | 2015-01-14 | 河南科技大学 | Loaded catalyst for hydrolyzing ammonia borane to release hydrogen and preparation method of loaded catalyst |
| CN106140166A (en) * | 2016-06-29 | 2016-11-23 | 苏州大学 | A kind of loaded catalyst, preparation method and applications |
| CN106140166B (en) * | 2016-06-29 | 2019-02-01 | 苏州大学 | A kind of loaded catalyst, preparation method and applications |
| CN107159214A (en) * | 2017-06-22 | 2017-09-15 | 桂林电子科技大学 | A kind of porous active carbon material load cobalt nanometer particle material and its preparation method and application |
| CN111569933A (en) * | 2020-06-22 | 2020-08-25 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| CN111569933B (en) * | 2020-06-22 | 2021-08-03 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| WO2021258425A1 (en) * | 2020-06-22 | 2021-12-30 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst and preparation method therefor and application thereof |
| CN112827492A (en) * | 2021-01-07 | 2021-05-25 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
| CN112827492B (en) * | 2021-01-07 | 2023-11-10 | 苏州大学 | Preparation method of catalyst for catalyzing ammonia borane hydrolysis |
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Application publication date: 20140528 |