CN108455524A - A kind of application of transition metal carbide - Google Patents
A kind of application of transition metal carbide Download PDFInfo
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- CN108455524A CN108455524A CN201810048826.3A CN201810048826A CN108455524A CN 108455524 A CN108455524 A CN 108455524A CN 201810048826 A CN201810048826 A CN 201810048826A CN 108455524 A CN108455524 A CN 108455524A
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- Prior art keywords
- transition metal
- metal carbide
- ammonia
- ammonia borine
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- 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
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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
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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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
The invention discloses a kind of application of transition metal carbide, the transition metal carbide is reacted for ammonia borine decomposing hydrogen-production.Transition metal carbide in the present invention is prepared simply, and when for the reaction of ammonia borine decomposing hydrogen-production, reaction condition is mild.It is easy to operate, reproducible when transition metal carbide is reacted for ammonia borine decomposing hydrogen-production in the present invention, there is chemical economy；It is higher to the utilization ratio of light, it can be achieved that luminous energy is to chemical transformation of energy；The hydrogen of generation can alleviate environment and energy problem.
Description
Technical field
The present invention relates to ammonia borane hydrolysis De-hydrogen Technology fields.More particularly, to a kind of answering for transition metal carbide
With.
Background technology
Hydrogen, as a kind of energy carrier that cleaning is renewable, abundant, it is considered to be future substitutes traditional fossil energy reason
One of candidate energy thought, but due to its low boiling point under air conditions and density, this expectation is met in practical applications
It to many stubborn problems, including storage, transmits, release.Therefore exploitation safe and effective storage and release in a mild condition
The chemicals of hydrogen is required.
Ammonia borine, due to smaller molecular weight and higher hydrogen content, long-term stability, it is nontoxic the advantages that, be considered
It is competitive hydrogen storage chemicals.Currently, decomposing ammonia borine generates hydrogen in homogeneous molecular system, out-phase metal, gold
Belong to oxide, metal phosphorizing objects system makes progress.
In recent years, transition metal carbide, since its good electric conductivity and chemical stability are widely used to electricity and urge
Change in HER, however being but rarely reported for ammonia borine decomposition reaction.
Therefore, the application the present invention provides a kind of transition metal carbide in the reaction of ammonia borine decomposing hydrogen-production.
Invention content
It is an object of the present invention to provide a kind of applications of transition metal carbide.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of application of transition metal carbide, the transition metal carbide are reacted for ammonia borine decomposing hydrogen-production.This
Invention realizes Co by optimum synthesis strategy2C-material exposes the regulation and control of crystal face, makes it have excellent catalysis ammonia borine
The ability of molecule decomposing hydrogen-production.Before this, ammonia borine decomposing hydrogen-production reaction mainly utilizes noble metal or transiting metal oxidation
Object, phosphide, report of the transition metal carbide for the reaction are less.
Preferably, the ammonia borine decomposing hydrogen-production reaction includes the following steps：Under air-proof condition, by transition metal carbide
Aqueous dispersions and ammonia borine aqueous solution mix and carry out ammonia borine decomposing hydrogen-production and react.
Preferably, transition metal carbide Co2C.Compared to being reported before based on Co-TiC/C nano particles, Co2C
Preparation simple condition it is mild and decompose the efficient of ammonia borine.
Preferably, the Co2It is oleyl amine or polyhydroxy-alcohol that the surface of C, which has ligand, the ligand,.In the present invention, a side
These ligands of face participate in Co2The preparation of C, the Co that on the other hand these ligands can stably generate2C makes it avoid reuniting.
Preferably, the condition of ammonia borine decomposing hydrogen-production reaction is to be protected from light and heating condition or illumination and room temperature item
Part.In routine techniques, the reaction of ammonia borine decomposing hydrogen-production is a thermal response, and different rates can be realized under different heating condition
Decomposing hydrogen-production reacts, it is however generally that, temperature is higher, and rate is faster.And in the present invention, Co2C can not only meet the routine skill
Art, simultaneously because Co2C has good extinction characteristic, therefore the decomposition of ammonia borine only can be also realized under illumination condition, this is
The advantage of the present invention.In order to exclude the influence of extinction effect, we are in routine techniques, Co2It is strictly protected from light by C when heating.
Preferably, it is described be protected from light and in heating condition heating temperature be 35~65 DEG C etc. in one kind, the present invention through largely
It is experimentally confirmed that heating temperature is higher, decomposition efficiency is also higher；The factors such as considering cost, in the temperature model that the present invention is given
It is more excellent to enclose interior effect；Further, in certain specific implementation modes of the present invention, for example, described be protected from light and in heating condition
Heating temperature is 35~45,45~65 DEG C etc..
Preferably, in the aqueous dispersions of the transition metal carbide transition metal carbide a concentration of 0.22~
1.52mg/mL；The present invention confirms that the concentration of transition metal carbide is bigger, and decomposition efficiency is higher through many experiments；Consider
The factors such as cost, effect is more excellent in the concentration range of the given transition metal carbide of the present invention；Further, in the present invention
Certain specific implementation modes in, for example, in the aqueous dispersions of the transition metal carbide transition metal carbide concentration
For 0.22~1.52mg/mL, 0.22~0.65mg/mL, 0.22~1.09mg/mL, 0.65~1.09mg/mL, 0.65~
1.52mg/mL, 1.09~1.52mg/mL etc.；It is highly preferred that when a concentration of 0.65mg/mL of transition metal carbide, unit matter
Measure Co2It is most that C generates hydrogen volume within the unit interval.
Preferably, a concentration of 1.62~16.2mol/L of the ammonia borine Ammonia In Aqueous Solution borine；The present invention is through a large amount of real
It issues after examination and approval now, decomposes a certain amount of ammonia borine, if its concentration is excessive, corresponding volume meeting very little, error can be bigger when measuring；
If concentration is too small, corresponding volume can be bigger, and the volume of injection generates larger mistake to the volume for generating hydrogen；In above-mentioned ammonia boron
In the concentration range of alkane, obtained result is more excellent.
Preferably, further include NaOH in the ammonia borine aqueous solution, a concentration of 2.5~25mol/L of wherein NaOH.This hair
Bright neutral and alkali condition is more advantageous to the decomposition of ammonia borine；The present invention has found through many experiments, in the concentration range of above-mentioned NaOH, obtains
The result arrived is more excellent.
Preferably, the volume ratio of the aqueous dispersions of the transition metal carbide and ammonia borine aqueous solution is 3：1~48：1；
Further, in certain specific implementation modes of the present invention, for example, the aqueous dispersions of the transition metal carbide and ammonia boron
The volume ratio of alkane aqueous solution is 3:1~23：1、23:1~48：1 etc.；It is highly preferred that the volume ratio is 23：1, the volume ratio
Under, one side Co2C can be very good to be disperseed, and on the other hand inject volume change caused by ammonia borine aqueous solution by syringe
Error to generating hydrogen volume can be ignored.
In addition, unless otherwise specified, any range recorded in the present invention includes any number between end value and end value
The arbitrary subrange that any number between value and end value or end value is constituted.
Beneficial effects of the present invention are as follows：
1, the transition metal carbide in the present invention is prepared simple, when for the reaction of ammonia borine decomposing hydrogen-production, reaction condition
Mildly.
2, easy to operate, reproducible when transition metal carbide is reacted for ammonia borine decomposing hydrogen-production in the present invention, tool
There is chemical economy.
3, high to the utilization ratio of light when transition metal carbide is reacted for ammonia borine decomposing hydrogen-production in the present invention, it can
Realize luminous energy to chemical transformation of energy.Due to Co2There is C good extinction characteristic, diffusing reflection to absorb spectrogram such as 4 institute of attached drawing
Show, under illumination condition, the reaction of ammonia borine decomposing hydrogen-production can be completed by absorbing luminous energy, luminous energy is realized and turn to chemical energy
Change.
4, when transition metal carbide is reacted for ammonia borine decomposing hydrogen-production in the present invention, the hydrogen of generation can alleviate environment
And energy problem.
Description of the drawings
Specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows Co in the present invention2The transmission electron microscope picture of C.
Fig. 2 shows Co in the present invention2The X-ray diffractogram of C.
Fig. 3 shows Co in the present invention2The X-ray photoelectron spectroscopic analysis figure of C.
Fig. 4 shows Co in the present invention2The diffusing reflection abosrption spectrogram of C.
Fig. 5 shows the H generated at 45 DEG C in the embodiment of the present invention 12Volume changes over time figure.
Fig. 6 shows the H generated under White LED illumination in the embodiment of the present invention 22Volume changes over time figure.
Fig. 7 shows in comparative example 1 of the present invention the H generated at 45 DEG C2Volume changes over time figure.
Specific implementation mode
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.It will be appreciated by those skilled in the art that specifically described content is illustrative and be not restrictive below, it should not be with this
It limits the scope of the invention.
In the present invention, preparation method is then conventional method unless otherwise specified.Raw material used is equal unless otherwise instructed
It can be obtained from disclosed commercial sources, the percentage is mass percent unless otherwise specified.
Transition metal carbide Co in the present invention2C's prepares bibliography [CrystEngComm, 2014,16,8000] system
, specific experiment step includes：Weigh the anhydrous CoAc of 200mg2In two-mouth bottle, 15mL oleyl amines and 2mL 3-EG (three second are added
Glycol), 2.5h is heated to reflux at 290 DEG C, entire reaction process carries out under an ar atmosphere.Post-processing：5000rpm is centrifuged
5min discards clear liquid, and n-hexane is added and acetone washes black solid, until supernatant is colourless.Obtained solid is dried.It is logical
Transmission electron microscope TEM, XRD, XPS are crossed, diffusing reflection absorbs the Co to being prepared2C is characterized, as shown in Figs 1-4.It can from Fig. 1
Find out, the Co2C is laminated structure；Fig. 2 is Co2The XRD spectrum (PDF No.65-1457) of C, the ownership at each peak is as shown in the figure；Figure
3 be Co2The XPS figures of Co elements, wherein 778.7eV are attributed to the Co of carbonization in C；Fig. 4 is Co2The diffusing reflection of C absorbs collection of illustrative plates, can
Find out that it has good extinction characteristic within the scope of 200-2000nm.
Embodiment 1
In the case where being protected from light heating condition, wherein heating temperature is 45 DEG C, Co2C realizes that ammonia borine molecule decomposes, specific embodiment party
Method is as follows：Take the Co that 3mg is prepared2C solid powders add 4.6mL water ultrasonic disperses, are sealed after magneton is added and use masking foil
Package, is placed in oil bath.Put up drainage collection H2Device.100mg NaOH, 50mg ammonia borines are weighed respectively, and 200 μ are added
L water dissolutions squeeze into rapidly Co using syringe2In C, and immediately begin to timing, reading.
Fig. 5 is the H that the system is generated at 45 DEG C2Volume changes over time figure.It can be seen from the figure that generating H2Body
The growth of product at any time linearly increases trend, illustrates that catalyst has good stability in the system.
Embodiment 2
In illumination and under room temperature, Co2C realizes that ammonia borine molecule decomposes, and specific implementation method is as follows：3mg is taken to prepare
Obtained Co2C solid powders add 4.6mL water ultrasonic disperses, are sealed after magneton is added, are placed in illumination under White LED, put up
Drainage collection H2Device.100mg NaOH, 50mg ammonia borines are weighed respectively, and 200 μ L water dissolutions are added, it is rapid using syringe
Squeeze into Co2In C, and immediately begin to timing, reading.
Fig. 6 is the H that the system generates under White LED illumination2Volume changes over time figure.It is seen that having
When illumination, ammonia borine, which can occur to decompose completely within the time of 400s, releases H2, and when there is no light, then need the long period
It completes, illustrates that illumination can accelerate reaction and carry out.
Some embodiments
The concentration of transition metal carbide decomposes ammonia borine molecule in the aqueous dispersions of measurement transition metal carbide
It influences, i.e. method and step the difference is that only with embodiment 1 and change Co2The dosage of C solid powders, as shown in table 1：
The influence that the concentration of 1 transition metal carbide of table decomposes ammonia borine molecule
| Embodiment is numbered | Co2The dosage of C solid powders | As a result |
| 3 | 1mg | Hydrogen-producing speed is 2.23mL/mgmin |
| 4 | 5mg | Hydrogen-producing speed is 2.29mL/mgmin |
| 5 | 7mg | Hydrogen-producing speed is 2.38mL/mgmin |
Conclusion：The present invention pass through experimental studies have found that, be added Co2The increase of C powder qualities, the hydrogen-producing speed of system by
It is cumulative fast, and when catalyst amount increases to a certain amount of, the hydrogen-producing speed of system can decline.The present invention it has been investigated that
3mg is Co2The optimal dosage of C, hydrogen-producing speed 4.76mL/mgmin.
Some embodiments
What the amount ratio of the aqueous dispersions and ammonia borine aqueous solution that measure transition metal carbide decomposed ammonia borine molecule
It influences, i.e., method and step keeps total volume constant with embodiment 1, the difference is that only the water for changing transition metal carbide
The volume ratio of dispersion liquid and ammonia borine aqueous solution, as shown in table 2：
The shadow that the aqueous dispersions of 2 transition metal carbide of table and the volume ratio of ammonia borine aqueous solution decompose ammonia borine molecule
It rings
Conclusion：The present invention pass through experimental studies have found that, the volume ratio of transition metal carbide aqueous dispersions and ammonia Borane solution
Within the scope of preferred value of the present invention, system production hydrogen result has no significant difference.
Some embodiments
The influence that heating temperature decomposes ammonia borine molecule is measured, i.e. method and step the difference is that only with embodiment 1
Change heating temperature, as shown in table 3：
The influence that 3 heating temperature of table decomposes ammonia borine molecule
Conclusion：The present invention pass through experimental studies have found that, in preferred range of the present invention, with temperature raising system produce
Hydrogen rate is obviously improved.The factors such as considering cost, effect is more excellent within the scope of the given temperature of the present invention.
Comparative example 1
Ammonia borine molecule decomposes, and specific steps the difference is that only with embodiment 1, by Co2C solid powders replace with
CuCo/C powder prepares reference literature method [Applied Catalysis B:Environmental,2016,180,
121], Fig. 7 is the H that the system decomposes AB generations at 45 DEG C2Volume changes with time figure.It can be seen from the figure that this is urged
Agent decomposes AB and generates H2, with the extension of time, H2Volume is slowly increased, however system only produces within the time of 30min
Less than 12mL H2, illustrate the inefficient of system.
Conclusion：Under the same conditions, CuCo/C decomposes AB and generates H2When heating 30min, system produces about 12mL H2,
And Co in the present invention2AB completions can be decomposed to give off 100mL H by C in 4min2, illustrate Co of the present invention2C efficiency is far above CuCo/
C。
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (10)
1. a kind of application of transition metal carbide, which is characterized in that the transition metal carbide decomposes system for ammonia borine
Hydrogen reacts.
2. application according to claim 1, which is characterized in that the ammonia borine decomposing hydrogen-production reaction includes the following steps：
Under air-proof condition, the aqueous dispersions of transition metal carbide mix with ammonia borine aqueous solution to carry out ammonia borine decomposing hydrogen-production anti-
It answers.
3. application according to claim 1, which is characterized in that the transition metal carbide is Co2C。
4. application according to claim 3, which is characterized in that the Co2It is oleyl amine that the surface of C, which has ligand, the ligand,
Or polyhydroxy-alcohol.
5. application according to claim 2, which is characterized in that the condition of ammonia borine decomposing hydrogen-production reaction be protected from light and
Heating condition or illumination and room temperature condition.
6. application according to claim 2, which is characterized in that it is described be protected from light and in heating condition heating temperature be 35~65
℃。
7. application according to claim 2, which is characterized in that transition gold in the aqueous dispersions of the transition metal carbide
Belong to a concentration of 0.2~1.4mg/mL of carbide.
8. application according to claim 2, which is characterized in that a concentration of the 1.62 of the ammonia borine Ammonia In Aqueous Solution borine
~16.2mol/L.
9. application according to claim 2, which is characterized in that further include NaOH in the ammonia borine aqueous solution, wherein
A concentration of 2.5~25mol/L of NaOH.
10. application according to claim 2, which is characterized in that the aqueous dispersions and ammonia boron of the transition metal carbide
The volume ratio of alkane aqueous solution is 3：1~48：1.
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Cited By (3)
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| CN110498392A (en) * | 2018-05-18 | 2019-11-26 | 中国科学院理化技术研究所 | A kind of photocatalytic system and its application |
| CN112079332A (en) * | 2020-09-18 | 2020-12-15 | 北京大学 | Method for preparing hydrogen by directly inducing solid ammonia borane through photo-thermal method |
| CN113385206A (en) * | 2021-06-11 | 2021-09-14 | 河南理工大学 | High-efficiency hydrogen production catalyst under strong interaction of metal carriers and preparation method |
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| CN110498392A (en) * | 2018-05-18 | 2019-11-26 | 中国科学院理化技术研究所 | A kind of photocatalytic system and its application |
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| CN113385206A (en) * | 2021-06-11 | 2021-09-14 | 河南理工大学 | High-efficiency hydrogen production catalyst under strong interaction of metal carriers and preparation method |
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