CN110182759A - Bamboo-like carbon nano tubes load MgH2Nano-particles reinforcement hydrogen storage material and preparation method thereof - Google Patents
Bamboo-like carbon nano tubes load MgH2Nano-particles reinforcement hydrogen storage material and preparation method thereof Download PDFInfo
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
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Abstract
The invention discloses a kind of bamboo-like carbon nano tubes to load MgH2The preparation method of nano-particles reinforcement hydrogen storage material, comprising: (1), by bamboo-like carbon nano tubes with the n-heptane solution of dibutylmagnesium mix, be evaporated under inert atmosphere protection;(2), obtained sample is reacted at a temperature of hydrogen and 180~200 DEG C, obtains bamboo-like carbon nano tubes load MgH2Nano-particles reinforcement system;(3), bamboo-like carbon nano tubes are loaded into MgH2Nano-particles reinforcement system applies High Voltage, obtains the bamboo-like carbon nano tubes load MgH with high hydrogen-storage density2Nano-particles reinforcement hydrogen storage material.The present invention is using the bamboo-like carbon nano tubes of major diameter, thin pipe wall and high-specific surface area as MgH2Confinement carrier improves the load factor and hydrogen storage property of composite material;And by the method for subsequent high pressure compression, the synthesis hydrogen-storage density of composite material is significantly improved, preparation method is simple, and the composite material hydrogen storage property of preparation is excellent, can be widely applied to the directions such as mobile power source and fuel cell.
Description
Technical field
The invention belongs to hydrogen storage material fields, and in particular to a kind of bamboo-like carbon nano tubes load MgH of high hydrogen-storage density2
Nano particle composite material and preparation method thereof.
Background technique
Magnesium-base hydrogen storage material because its resource abundant, cheap price, nontoxic and pollution-free and higher theoretical hydrogen storage content by
To extensive concern, it is considered as one of the hydrogen storage material of most development potentiality.
But its thermodynamic stability is higher, causes its hydrogen discharging temperature high (400 DEG C of >), dynamic performance poor, far from
Meet the requirement for practical application.Currently, improving MgH2The main method of hydrogen storage property has alloying, catalytic modification and receives
Riceization etc., wherein nanosizing can improve suction hydrogen desorption kinetics performance by reducing particle size greatly.
Nanometer confinement is by MgH2One of important method of nanosizing not only can effectively be inhibited using mesoporous framework material
Particle is grown up, and nano particle is formed, and the reunion of particle can also be prevented in cyclic process, and then improve nanometer confinement system
Stable circulation performance.
CN104649229A, which is disclosed, a kind of prepares a nanometer method for confinement magnesium-base hydrogen storage material, it is characterised in that: such
Hydrogen storage material is magnesium hydride (MgH2) be supported in mesoporous framework material nano duct, the mesoporous framework material is mesoporous
One of carbon, carbon gel, carbon nanotubes, mesoporous silicon SBA-15, metal-organic framework.Pass through dibutylmagnesium (MgBu2)
It is impregnated with mesoporous framework material, utilizes high temperature and pressure by MgBu in a high pressure reaction kettle2It is replaced as being supported on mesoporous framework material
MgH inside and outside nano pore hole2, then the MgH that will be supported on outside duct with pentane2It washes away, is made through dry.
Nanometer confinement MgH made from this kind of method2At room temperature can hydrogen release, with excellent suction hydrogen desorption kinetics and
Hydrogen release thermodynamics.
But current nanometer confinement system MgH2Load factor it is universal lower (30wt.%-70 wt.%), reduce
The quality hydrogen-storage density and volume hydrogen-storage density of compound system, are difficult to meet the requirement of on-vehicle fuel.
Summary of the invention
The problems such as present invention is low for current magnesium-base nano confinement system load factor, hydrogen-storage density is low and poor circulation,
Propose a kind of bamboo-like carbon nano tubes load MgH2The preparation method of nano-particles reinforcement hydrogen storage material, with Bamboo-shaped carbon nanometer
Pipe is as MgH2Confinement carrier;And by the method for high pressure compression, the hydrogen-storage density of compound system is improved.The method of the present invention process
Simply, reaction is easy to control.
The present invention is achieved in the following ways:
A kind of bamboo-like carbon nano tubes load MgH2The preparation method of nano-particles reinforcement hydrogen storage material, comprising:
Step 1 mixes bamboo-like carbon nano tubes with the n-heptane solution of dibutylmagnesium, is evaporated under inert atmosphere protection;
Sample in step 1 is reacted 2~4h by step 2 at a temperature of hydrogen and 180~200 DEG C, is obtained Bamboo-shaped carbon and is received
Mitron loads MgH2Nano-particles reinforcement system;
Bamboo-like carbon nano tubes are loaded MgH by step 32Nano-particles reinforcement system applies High Voltage on press machine, obtains
MgH is loaded to the bamboo-like carbon nano tubes with high hydrogen-storage density2Nano-particles reinforcement hydrogen storage material.
Dibutylmagnesium is dissolved in heptane, and general commercial dibutylmagnesium is directly dissolved with heptane, forms the heptane of dibutylmagnesium
Solution, it is preferable that bamboo-like carbon nano tubes and dibutylmagnesium mass ratio are 1:3~5 in the step 1.
Preferably, hydrogen pressure is 80~150bar in the step 2.
Preferably, the step 3 mesohigh is 700~1000MPa by force.
After applying HIGH PRESSURE TREATMENT, bamboo-like carbon nano tubes load MgH2Nano-particles reinforcement hydrogen storage material volume substantially subtracts
Small, the volume hydrogen-storage density of compound system significantly improves.
The preparation method of the bamboo-like carbon nano tubes, comprising:
Step A: dicyandiamide and nitrate are added to absolute ethanol, and stir lower back flow reaction;
Step B: carbon material is added, and the reaction was continued;
Step C: being evaporated solution, and obtained powder is warming up to 800~1200 DEG C under nitrogen atmosphere, 1~3h is roasted, after cooling
Obtain bamboo-like carbon nano tubes.
The bamboo-like carbon nano tubes that the present invention obtains are relatively large in diameter about 100nm, and relatively thin tube wall is about 8 carbon-coatings, and interior
There is unique spacer structure in portion.
Nitrate is nickel nitrate, ferric nitrate or cobalt nitrate in the step A.
Preferably, the molar ratio of dicyandiamide and nitrate is 3~5:1 in the step A.
Carbon material is active carbon, graphite or acetylene black in the step B, and the molar ratio with dicyandiamide is 6~10:25.
Carbon nanotube synthesized by design according to the program has unique Bamboo-shaped pattern, and caliber is big, tube wall is thin,
Be conducive to carbon nano tube surface nano particle is dispersed in load.
Heating rate is 2~5 DEG C/min in the step C.
Bamboo-like carbon nano tubes of the invention have the characteristics that major diameter, thin pipe wall and high-specific surface area, can load height
The MgH of mass ratio2Nano particle, and effectively inhibit growing up and reuniting for particle, improve the suction hydrogen release power of composite hydrogen storage material
And cycle performance.
By High Voltage compaction treatment, the volume hydrogen-storage density of composite hydrogen storage material is doubled and redoubled, and dynamic performance
Without obvious decaying, this is because unique bamboo joint structure inside carbon nanotube, plays a supporting role in HIGH PRESSURE TREATMENT process, energy
Original microscopic appearance is preferably maintained, and then maintains the hydrogen storage property of composite material.
The present invention also provides above-mentioned bamboo-like carbon nano tubes to load MgH2Nano-particles reinforcement hydrogen storage material preparation method
The bamboo-like carbon nano tubes load MgH being prepared2Nano-particles reinforcement hydrogen storage material, can be widely applied to mobile power source and combustion
Expect the directions such as battery.
Detailed description of the invention
Fig. 1 is (a) TEM and (b) HRTEM figure of bamboo-like carbon nano tubes prepared by embodiment 1;
Fig. 2 is that bamboo-like carbon nano tubes prepared by embodiment 1 load MgH2(a) TEM and (b) of nano-particles reinforcement system
SAED figure;
Fig. 3 is that bamboo-like carbon nano tubes prepared by embodiment 1 load MgH2Nano-particles reinforcement system (a) compacting before with
(b) photo after being compacted;
Fig. 4 is that bamboo-like carbon nano tubes prepared by embodiment 1 load MgH2Nano-particles reinforcement hydrogen storage material is inhaled hydrogen release and is followed
Ring performance curve;
Fig. 5 is that bamboo-like carbon nano tubes prepared by embodiment 1 load MgH2Nano-particles reinforcement hydrogen storage material HIGH PRESSURE TREATMENT
(a) 300 DEG C of isothermal dehydrogenations and 300 DEG C of (b), the 80bar isothermal of front and back inhale hydrogen curve.
Specific embodiment
The invention will be further described With reference to embodiment:
Embodiment 1:
(1) 24mmol dicyandiamide and 6mmol nickel nitrate are added in the dehydrated alcohol of 250mL respectively, with 500r/min's
Rate magnetic agitation, and 5h is heated at 78 DEG C in a manner of condensing reflux;
(2) active carbon of 8mmol is added in step (1) solution, the reaction was continued for 24 hours;
(3) solution in step (2) is evaporated, obtained powder is transferred in tube furnace, is warming up under nitrogen atmosphere
1000 DEG C, and 2h is kept the temperature, it is cooled to room temperature to obtain bamboo-like carbon nano tubes;
(4) bamboo-like carbon nano tubes are mixed with dibutylmagnesium (being dissolved in heptane) according to 1:3.3 mass ratio, in inert atmosphere
Under protection, solvent evaporated;
(5) sample in step (4) is reacted into 2h at the hydrogen pressure of 80bar and 200 DEG C, obtains bamboo-like carbon nano tubes
Load MgH2Nano-particles reinforcement system;
(6) MgH is loaded to bamboo-like carbon nano tubes using press machine2Nano-particles reinforcement system pressurization 750MPa, and protect
10min is pressed, the bamboo-like carbon nano tubes load MgH with high hydrogen-storage density is obtained2Nano-particles reinforcement hydrogen storage material.
As shown in Figure 1, being synthesized bamboo-like carbon nano tubes, it is relatively large in diameter about 100nm, tube wall relatively thin about 8
A carbon-coating, and there is unique spacer structure in inside.
As shown in Fig. 2, loading MgH for synthesized bamboo-like carbon nano tubes2Nano-particles reinforcement system, carbon nanotube table
The MgH in face2Particle is uniformly dispersed, and size is smaller, about 15-20nm.
As shown in figure 3, loading MgH for bamboo-like carbon nano tubes2The pattern comparison of nano-particles reinforcement system compacting front and back
Scheme, volume substantially reduces after HIGH PRESSURE TREATMENT, and the volume hydrogen-storage density of compound system is improved from 16.01 to 65.90g/L.
As shown in figure 4, loading MgH for bamboo-like carbon nano tubes2Nano-particles reinforcement hydrogen storage material inhales hydrogen release cycle performance
Curve shows excellent stable circulation performance, and hydrogen release capacity and dynamics are inhaled in cyclic process without apparent decaying.
As shown in figure 5, loading MgH for bamboo-like carbon nano tubes2Nano-particles reinforcement hydrogen storage material is before and after HIGH PRESSURE TREATMENT
Isothermal hydrogen storage property remain to maintain its original suction hydrogen desorption kinetics performance, before HIGH PRESSURE TREATMENT after HIGH PRESSURE TREATMENT
It compares, has no apparent decaying.
Embodiment 2:
(1) 25mmol dicyandiamide and 5mmol cobalt nitrate are added in the dehydrated alcohol of 250mL respectively, with 500r/min's
Rate magnetic agitation, and 5h is heated at 78 DEG C in a manner of condensing reflux;
(2) active carbon of 10mmol is added in step (1) solution, the reaction was continued for 24 hours;
(3) solution in step (2) is evaporated, obtained powder is transferred in tube furnace.It is warming up under nitrogen atmosphere
1200 DEG C, and 1h is kept the temperature, it is cooled to room temperature to obtain bamboo-like carbon nano tubes;
(4) bamboo-like carbon nano tubes are mixed with dibutylmagnesium (being dissolved in heptane) according to the mass ratio of 1:3.5, in indifferent gas
Under atmosphere protection, solvent evaporated;
(5) sample in step (4) is reacted into 3h at the hydrogen pressure of 120bar and 180 DEG C, obtains bamboo-like carbon nano tubes
Load MgH2Nano-particles reinforcement system;
(6) MgH is loaded to bamboo-like carbon nano tubes using press machine2Nano-particles reinforcement system pressurization 800MPa, and protect
10min is pressed, the bamboo-like carbon nano tubes load MgH with high hydrogen-storage density is obtained2Nano-particles reinforcement hydrogen storage material.
Embodiment 3:
(1) 24mmol dicyandiamide and 8mmol ferric nitrate are added in the dehydrated alcohol of 250mL respectively, with 500r/min's
Rate magnetic agitation, and 5h is heated at 78 DEG C in a manner of condensing reflux;
(2) graphite of 10mmol is added in step (1) solution, the reaction was continued for 24 hours;
(3) solution in step (2) is evaporated, obtained powder is transferred in tube furnace.It is warming up under nitrogen atmosphere
1000 DEG C, and 1h is kept the temperature, it is cooled to room temperature to obtain bamboo-like carbon nano tubes;
(4) bamboo-like carbon nano tubes are mixed with dibutylmagnesium (n-heptane solution) according to the mass ratio of 1:4, in inert atmosphere
Under protection, solvent evaporated;
(5) sample in step (4) is reacted into 2h at the hydrogen pressure of 100bar and 200 DEG C, obtains bamboo-like carbon nano tubes
Load MgH2Nano-particles reinforcement system;
(6) MgH is loaded to bamboo-like carbon nano tubes using press machine2Nano-particles reinforcement system pressurization 850MPa, and protect
10min is pressed, the bamboo-like carbon nano tubes load MgH with high hydrogen-storage density is obtained2Nano-particles reinforcement hydrogen storage material.
Claims (10)
1. a kind of bamboo-like carbon nano tubes load MgH2The preparation method of nano-particles reinforcement hydrogen storage material, comprising:
Step 1 mixes bamboo-like carbon nano tubes with the n-heptane solution of dibutylmagnesium, is evaporated under inert atmosphere protection;
Sample in step 1 is reacted 2~4h by step 2 at a temperature of hydrogen and 180~200 DEG C, obtains bamboo-like carbon nano tubes
Load MgH2Nano-particles reinforcement system;
Bamboo-like carbon nano tubes are loaded MgH by step 32Nano-particles reinforcement system applies High Voltage on press machine, is had
There is the bamboo-like carbon nano tubes load MgH of high hydrogen-storage density2Nano-particles reinforcement hydrogen storage material.
2. bamboo-like carbon nano tubes according to claim 1 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, bamboo-like carbon nano tubes and dibutylmagnesium mass ratio are 1:3~5 in the step 1.
3. bamboo-like carbon nano tubes according to claim 1 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, hydrogen pressure is 80~150bar in the step 2.
4. bamboo-like carbon nano tubes according to claim 1 or 3 load MgH2The preparation side of nano-particles reinforcement hydrogen storage material
Method, which is characterized in that step 3 mesohigh is 700~1000MPa by force.
5. bamboo-like carbon nano tubes according to claim 1 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, the preparation method of the bamboo-like carbon nano tubes, comprising:
Step A: dicyandiamide and nitrate are added to absolute ethanol, and stir lower back flow reaction;
Step B: carbon material is added, and the reaction was continued;
Step C: being evaporated solution, and obtained powder is warming up to 800~1200 DEG C under nitrogen atmosphere, roasts 1~3h, obtains after cooling
Bamboo-like carbon nano tubes.
6. bamboo-like carbon nano tubes according to claim 5 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, nitrate is nickel nitrate, ferric nitrate or cobalt nitrate in the step A.
7. bamboo-like carbon nano tubes according to claim 5 or 6 load MgH2The preparation side of nano-particles reinforcement hydrogen storage material
Method, which is characterized in that the molar ratio of dicyandiamide and nitrate is 3~5:1 in the step A.
8. bamboo-like carbon nano tubes according to claim 5 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, carbon material is active carbon, graphite or acetylene black in the step B, the molar ratio with dicyandiamide is 6~10:
25。
9. bamboo-like carbon nano tubes according to claim 5 load MgH2The preparation method of nano-particles reinforcement hydrogen storage material,
It is characterized in that, heating rate is 2~5 DEG C/min in the step C.
10. any bamboo-like carbon nano tubes load MgH according to claim 1~92Nano-particles reinforcement hydrogen storage material
The bamboo-like carbon nano tubes that preparation method is prepared load MgH2Nano-particles reinforcement hydrogen storage material.
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CN111137851A (en) * | 2020-01-09 | 2020-05-12 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
CN113363450A (en) * | 2021-07-01 | 2021-09-07 | 齐鲁工业大学 | Preparation method of carbon nano tube coated high-nickel ternary cathode composite material |
CN115744814A (en) * | 2022-09-28 | 2023-03-07 | 重庆大学 | Gamma-MoC/VN restricted domain catalyzed MgH2 nano composite hydrogen storage material and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111137851A (en) * | 2020-01-09 | 2020-05-12 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
CN111137851B (en) * | 2020-01-09 | 2021-05-14 | 浙江大学 | Light metal borohydride/carbon-loaded nano vanadium trioxide composite hydrogen storage material and preparation method thereof |
CN113363450A (en) * | 2021-07-01 | 2021-09-07 | 齐鲁工业大学 | Preparation method of carbon nano tube coated high-nickel ternary cathode composite material |
CN115744814A (en) * | 2022-09-28 | 2023-03-07 | 重庆大学 | Gamma-MoC/VN restricted domain catalyzed MgH2 nano composite hydrogen storage material and preparation method thereof |
CN115744814B (en) * | 2022-09-28 | 2024-05-10 | 重庆大学 | Gamma-MoC/VN (gamma-MoC/VN) domain-limited catalysis MgH2 nano composite hydrogen storage material and preparation method thereof |
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