CN106395742A - Hydrogen storage composite material MgH2-Ni-rGO and method for preparing same - Google Patents
Hydrogen storage composite material MgH2-Ni-rGO and method for preparing same Download PDFInfo
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- CN106395742A CN106395742A CN201611003669.1A CN201611003669A CN106395742A CN 106395742 A CN106395742 A CN 106395742A CN 201611003669 A CN201611003669 A CN 201611003669A CN 106395742 A CN106395742 A CN 106395742A
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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
- C01B3/0005—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
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- Y02E60/32—Hydrogen storage
Abstract
The invention belongs to the technical field of hydrogen storage materials, and particularly discloses a hydrogen storage composite material MgH2-Ni-rGO and a method for preparing the same. The hydrogen storage composite material and the method have the advantages that the problem that MgH2 is used as a hydrogen storage material and is high in hydrogen storage capacity (7.6 wt.%H2) but application of the MgH2 is constrained due to the high hydrogen release temperature (higher than 380 DEG C) of the MgH2 can be solved by the aid of the hydrogen storage composite material and the method; Ni nano-particles and MgH2 nano-particles are loaded on graphene by the aid of solvothermal processes, the hydrogen release performance of MgH2 is improved under catalytic effects and nano-crystallization effects jointly, accordingly, 4.6 wt.% of high-purity hydrogen can be released by the prepared composite material MgH2-Ni-rGO at the temperature of 300 DEG C within 30 min, and the hydrogen storage composite material prepared by the aid of the method is a perfect hydrogen storage composite material.
Description
Technical field
The invention belongs to hydrogen storage material technical field, a kind of specifically new composite for hydrogen storage MgH2- Ni-rGO and its system
Preparation Method.
Background technology
The going deep into of fast development with national economy and Process of Urbanization Construction, energy problem is outstanding day by day, and is made at present
Fossil energy is not only seriously polluted, and is non-renewable resources, so, in the urgent need to finding, one kind is sustainable to be made the mankind
With and free of contamination clean energy resource.Hydrogen is a kind of pollution-free(Its combustion product is water), there is high fuel value(1.4×108J/
Kg)Renewable and clean energy resource, be the optimal carrier of the energy.But at present because the density of hydrogen is all very low with condensation temperature,
Very big difficulty is had using high-pressure gaseous tank and low temperature liquid tank such conventional storage mode.So, find safe and convenient
Solid-state hydrogen storage mode becomes current study hotspot [1].Solid-state hydrogen storage mode volume hydrogen storage capability is high, without high pressure and heat-insulated
Container, security be good, no explosion danger, and conventional solid-state hydrogen storage material has metal hydride, complex hydrides, nano material
Deng.
MgH2As one kind of light metal hydride, not only there is high gravimetric energy density(7.6wt.%H2)And volume energy
Amount surface density(110kg/m3), and cheap and can be recycled, it is a kind of good solid-state hydrogen storage material.But,
Due to being commercialized MgH2Hydrogen discharging temperature is high(400 DEG C of >), hydrogen desorption kineticses greatly limit its use, institute the shortcomings of slow
To pass through MgH2Be combined [2] with material with carbon element, MgH is reduced using chemical synthesis process2The methods such as particle size [3], all become
Current study hotspot.The advantages of Graphene is due to its unique lamellar structure, lightweight, good chemical stability is wide
General as various carriers, using Graphene as carrier, carried metal nano particle, as catalyst, can effectively reduce
MgH2Hydrogen discharging temperature, but be substantially at present and catalyst and MgH realized using ball-milling method2Physical mixed [4].The present invention opens
Invasive employing solvent-thermal method loads Ni nano particle and MgH on Graphene simultaneously2Nano particle, passes through catalytic action simultaneously
Come jointly to MgH with nanosizing effect2Hydrogen discharging performance improved, this material, at 300 DEG C, can release in 30min
The high-purity hydrogen of 4.6 wt.%.
Bibliography:
[1] Takimoto, M., Hou, Z.Nature2006,443, 400-401
[2] Zlotea C., Oumellal Y., Hwang SJ., Ghimbeu CM., Latroche M.,J. Phys. Chem. C,2015, 119, 18091-18098
[3] Jeon KJ., Moon HR., Ruminski AM., Kisielowski C., Bardhan R., Urban
J.,Nature Materials, 2011, 10, 286-290
[4] Liu G., Wang YJ., Qiu FY., Jiao LF., Yuan HT.,J. Mater. Chem., 2012,
22, 22542-22549.
Content of the invention
It is an object of the invention to provide a kind of new and effective composite for hydrogen storage MgH2- Ni-rGO and preparation method thereof, should
Material can discharge the high-purity hydrogen of 4.6 wt. % in 30 min at 300 DEG C, can be used as a kind of potential hydrogen storage material.
The composite for hydrogen storage MgH that the present invention provides2The preparation method of-Ni-rGO, comprises the following steps that:
(1)Graphene oxide(GO)Preparation;
(2)Ni(OH)2Prepared by-GO:Using hydro-thermal method, by graphene oxide(GO)、C4H5O6Ni·4H2O, cetyl front three
Base ammonium bromide, hexamethylenetetramine mix in aqueous, and then in water heating kettle, heating response generates Ni (OH)2-GO;
(3)The preparation of Ni-rGO:By Ni (OH)2- GO calcines generation NiO-GO in atmosphere;Finally in H2-N2Middle calcining reduction becomes
Ni-rGO;
(4)MgH2The preparation of-Ni-rGO:Ni-rGO is added in hexamethylene with di-t-butyl magnesium, in H2Protection is lower to pass through solvent
Thermal response, that is, generate MgH2-Ni-rGO.
Step of the present invention(1)Operating process be:Weigh 2-2.5 g native graphite to pour in there-necked flask, add 100-
150 mL concentration are 65% HNO3, then it is slowly added to, at ice-water bath keeps 0 DEG C, the H that 100-150 mL concentration is 98%2SO4,
8-15 g KMnO is added after stirring 1-2 h4, it is warming up to 30-40 DEG C of reaction 2-3 h, then be warming up to 70-90 DEG C of reaction 1-2 h;
Add 300-500 mL distilled water diluting concentrated acid to obtain brown colloidal material after being cooled to room temperature, add the 35% of 30-50 mL
H2O2And the 10% HCl cleaning of 100-150 mL, obtain brown yellow solution;Centrifugation is washed to neutrality;Air drying at 50-60 DEG C
Obtain graphene oxide.
Step of the present invention(2)Operating process be:Weigh 0.09-0.10 g C4H5O6Ni·4H2O, 0.07-0.08 g ten
Six alkyl trimethyl ammonium bromides, 0.10-0.14 g hexamethylenetetramine are added in 40 mL distilled water, stir;Separately take
160-180 mg GO in 40 mL water, ultrasonic 2-4 h, then by two kinds of solution mix and blend 10-20 min, put into poly- after mixing
In tetrafluoroethene reactor, then it is placed in baking oven and to react 4-6 h at 120 DEG C -130 DEG C.Washed with distilled water centrifugation after having reacted
Wash 4-6 time, Ni (OH) after being dried, is obtained2-GO.
Step of the present invention(3)Operating process be:Take a certain amount of Ni (OH)2- GO is placed in tube furnace, in air atmosphere
Under rise to 350-360 DEG C with the heating rate of 2 DEG C/min-3 DEG C/min, at this temperature be incubated 2-4 h, be sintered into NiO-GO;
Again in H2-N2Rise to 400-420 DEG C with the heating rate of 2 DEG C/min-3 DEG C/min in gaseous mixture, be incubated 2-4 at this temperature
H, is reduced into Ni-rGO.
Step of the present invention(4)Operating process be:The Ni-rGO first claiming 20-30 mg adds in autoclave, adds
35-45 mL hexamethylene, 1.4-1.8 mL dibutylmagnesium, add 3-4 MPa H2, ultrasonic 30-40 min, stir 1-2 h,
React 20-24 h in 200-220 DEG C of oil bath, after having reacted, vacuumize 10-12 h at 75-85 DEG C and remove solvent, that is, be obtained
MgH2-Ni-rGO.
The present invention has the following aspects remarkable advantage:
1st, synthetic method is unique novel;
2nd, technique is not high to equipment requirement, it is easy to accomplish;
3rd, moderate cost.
Brief description
Fig. 1 GO, Ni-rGO and MgH2The XRD spectra of-Ni-rGO, wherein GO(Black line), Ni-rGO(Red line), MgH2-
Ni-rGO(Green line).
The TEM figure of Fig. 2 raw material and product.Wherein a)GO, b)Ni(OH)2- GO, c)Ni-rGO, d)MgH2-Ni-rGO.
Hydrogen desorption isotherms figure at 280 DEG C and 300 DEG C for Fig. 3 product.
Specific embodiment
Further illustrate the present invention below by embodiment.
Embodiment 1:
(1)The preparation of graphene oxide GO
Weigh 2 g native graphites to pour in there-necked flask, add the HNO that 100 mL concentration are 65%3, then keep 0 in ice-water bath
It is slowly added to the H that 100 mL concentration are 98% at DEG C2SO4, after stirring 1 h, add 10 g KMnO4, it is warming up to 35 DEG C of reaction 2 h,
It is warming up to 75 DEG C of reaction 1 h again;500 mL distilled water diluting concentrated acids are added to obtain brown colloidal material after being cooled to room temperature, then
Add 35% H of 40 mL2O2And 100 mL 10% HCl cleaning, obtain brown yellow solution;Centrifugation is washed to neutrality;50-60 ℃
Lower air drying obtains graphene oxide;
(2)Ni(OH)2Prepared by-GO
By 0.09 g C4H5O6Ni·4H20th, 0.07 g cetyl trimethylammonium bromide, 0.1 g hexamethylenetetramine are dissolved in
In 40 mL deionized waters, separately weigh 160 mg GO ultrasonic 2 h in 40 mL deionized waters, then will both mix and blends 10
As in ptfe autoclave after min, react 4 h at 120 DEG C, after having reacted, deionized water centrifuge washing 4 times,
Drying can be prepared by Ni (OH)2- GO, its TEM collection of illustrative plates such as Fig. 2 b;
(3)The preparation of Ni-rGO
Take a certain amount of Ni (OH)2- GO is placed in tube furnace, rises to 360 DEG C with the heating rate of 2 DEG C/min in air atmosphere
Lower insulation 2 h are sintered into NiO-GO, then in H2-N2Rising to 400 DEG C of insulation 2 h with the heating rate of 2 DEG C/min in gaseous mixture is
Ni-rGO can be obtained, its XRD spectrum such as Fig. 1, TEM collection of illustrative plates such as Fig. 2 c;
(4)MgH2The preparation of-Ni-rGO
Take 20 mg Ni-rGO, 35 mL hexamethylenes, 1.4 mL dibutylmagnesiums are placed in autoclave, add 3.0MPa H2,
Ultrasonic 40 min, stir 2 h, 200 DEG C of oil baths are reacted 24 h, after having reacted, vacuumize at 80 DEG C 12 h remove molten
Agent can be prepared by MgH2- Ni-rGO, its XRD spectrum such as Fig. 1, TEM collection of illustrative plates such as Fig. 2 d.
Embodiment 2:
(1)The preparation of graphene oxide GO
Weigh 2.5 g native graphites to pour in there-necked flask, add the HNO that 150 mL concentration are 65%3, then keep 0 in ice-water bath
It is slowly added to the H that 150 mL concentration are 98% at DEG C2SO4, after stirring 1 h, add 15 g KMnO4, it is warming up to 35 DEG C of reaction 2 h,
It is warming up to 75 DEG C of reaction 1 h again;500 mL distilled water diluting concentrated acids are added to obtain brown colloidal material after being cooled to room temperature, then
Add 35% H of 50 mL2O2And 150 mL 10% HCl cleaning, obtain brown yellow solution;Centrifugation is washed to neutrality;50-60 ℃
Lower air drying obtains graphene oxide;
(2)Ni(OH)2Prepared by-GO
By 0.1 g C4H5O6Ni·4H20th, 0.08 g cetyl trimethylammonium bromide, 0.14 g hexamethylenetetramine are dissolved in
In 40 mL deionized waters, separately weigh 180 mg GO ultrasonic 2 h in 40mL deionized water, then will both mix and blend 10 min
Afterwards as in ptfe autoclave, react 4 h at 120 DEG C, after having reacted, deionized water centrifuge washing 4 times, it is dried
Can be prepared by Ni (OH)2-GO;
(3)The preparation of Ni-rGO
Take a certain amount of Ni (OH)2- GO is placed in tube furnace, rises to 360 DEG C with the heating rate of 3 DEG C/min in air atmosphere
Lower insulation 3 h are sintered into NiO-GO, then in H2-N2Rising to 400 DEG C of insulation 3 h with the heating rate of 3 DEG C/min in gaseous mixture is
Ni-rGO can be obtained;
(4)MgH2The preparation of-Ni-rGO
Take 25 mg Ni-rGO, 40 mL hexamethylenes, 1.6 mL dibutylmagnesiums are placed in autoclave, add 3.5MPa H2,
Ultrasonic 40 min, stir 2 h, 200 DEG C of oil baths are reacted 24 h, after having reacted, vacuumize at 80 DEG C 12 h remove molten
Agent can be prepared by MgH2-Ni-rGO.
Embodiment 3:
First three step is identical with first three step of embodiment 1;
MgH2The preparation of-Ni-rGO
Take 30 mg Ni-rGO, 45 mL hexamethylenes, 1.8 mL dibutylmagnesiums are placed in autoclave, add 4 MPa H2, surpass
Sound 40 min, stirs 2 h, reacts 24 h, after having reacted, vacuumize 12 h and remove solvent at 80 DEG C in 200 DEG C of oil baths
Can be prepared by MgH2-Ni-rGO.
Claims (6)
1. a kind of composite for hydrogen storage MgH2The preparation method of-Ni-rGO is it is characterised in that comprise the following steps that:
(1)Graphene oxide(GO)Preparation;
(2)Ni(OH)2Prepared by-GO:Using hydro-thermal method, by graphene oxide(GO)、C4H5O6Ni·4H2O, cetyl trimethyl
Ammonium bromide, hexamethylenetetramine mix in aqueous, and then in water heating kettle, heating response generates Ni (OH)2-GO;
(3)The preparation of Ni-rGO:By Ni (OH)2- GO calcines generation NiO-GO in atmosphere;Finally in H2-N2Middle calcining reduction becomes
Ni-rGO;
(4)MgH2The preparation of-Ni-rGO:Ni-rGO is added in hexamethylene with di-t-butyl magnesium, in H2Protection is lower to pass through solvent heat
Reaction, that is, generate MgH2-Ni-rGO.
2. composite for hydrogen storage MgH according to claim 12The preparation method of-Ni-rGO is it is characterised in that step(1)
Operating process be:Weigh 2-2.5 g native graphite to pour in there-necked flask, add the HNO that 100-150 mL concentration is 65%3,
It is slowly added to, at ice-water bath keeps 0 DEG C, the H that 100-150 mL concentration is 98% again2SO4, after stirring 1-2 h, add 8-15 g
KMnO4, it is warming up to 30-40 DEG C of reaction 2-3 h, then be warming up to 70-90 DEG C of reaction 1-2 h;300-500 is added after being cooled to room temperature
ML distilled water diluting concentrated acid obtains brown colloidal material, adds 35% H of 30-50 mL2O2And the 10% of 100-150 mL
HCl cleans, and obtains brown yellow solution;Centrifugation is washed to neutrality;At 50-60 DEG C, air drying obtains graphene oxide.
3. composite for hydrogen storage MgH according to claim 12The preparation method of-Ni-rGO is it is characterised in that step(2)
Operating process be:Weigh 0.09-0.10 g C4H5O6Ni·4H2O, 0.07-0.08 g cetyl trimethylammonium bromide,
0.10-0.14 g hexamethylenetetramine is added in 40 mL distilled water, stirs;Separately take 160-180 mg GO in 40 mL
In water, ultrasonic 2-4 h, then by two kinds of solution mix and blend 10-20 min, put in ptfe autoclave after mixing, then
It is placed in baking oven and react 4-6 h at 120 DEG C -130 DEG C;Use distilled water centrifuge washing 4-6 time after having reacted, be obtained after drying
Ni(OH)2-GO.
4. the composite for hydrogen storage MgH according to claim 1,2 or 32The preparation method of-Ni-rGO is it is characterised in that walk
Suddenly(3)Operating process be:Take a certain amount of Ni (OH)2- GO is placed in tube furnace, in air atmosphere with 2 DEG C/min-3 DEG C/
The heating rate of min rises to 350-360 DEG C, is incubated 2-4 h at this temperature, is sintered into NiO-GO;Again in H2-N2In gaseous mixture
Rise to 400-420 DEG C with the heating rate of 2 DEG C/min-3 DEG C/min, be incubated 2-4 h at this temperature, be reduced into Ni-rGO.
5. composite for hydrogen storage MgH according to claim 42The preparation method of-Ni-rGO is it is characterised in that step(4)
Operating process be:The Ni-rGO first claiming 20-30 mg adds in autoclave, adds 35-45 mL hexamethylene, 1.4-
1.8 mL dibutylmagnesiums, add 3-4 MPa H2, ultrasonic 30-40 min, stirs 1-2 h, reacts in 200-220 DEG C of oil bath
20-24 h, after having reacted, vacuumizes 10-12 h at 75-85 DEG C and removes solvent, that is, MgH is obtained2-Ni-rGO.
6. the composite for hydrogen storage MgH being obtained by the described preparation method of one of claim 1-52-Ni-rGO.
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Cited By (6)
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CN108220728A (en) * | 2017-12-26 | 2018-06-29 | 钢铁研究总院 | A kind of high power capacity light graphite alkene catalytic rare earth magnesium-aluminum-based hydrogen storage material and preparation method |
CN108264018A (en) * | 2018-02-06 | 2018-07-10 | 北京科技大学 | The method of the high power capacity storage hydrogen material of ferrum-based catalyst modification three-dimensional grapheme confinement |
CN109319732A (en) * | 2018-10-15 | 2019-02-12 | 浙江大学 | A kind of preparation method of two dimension loaded nano magnesium hydride hydrogen storage material |
CN112390224A (en) * | 2019-08-16 | 2021-02-23 | 中国科学院大连化学物理研究所 | Polymer-coated hydrogen storage material and preparation method and application thereof |
CN115231514A (en) * | 2022-07-15 | 2022-10-25 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Magnesium-based hydrogen storage material catalyzed by hexagonal boron nitride loaded nano nickel particles and preparation method thereof |
WO2023071963A1 (en) * | 2021-10-25 | 2023-05-04 | 上海交通大学 | Nano magnesium hydride-loaded composite material and preparation method therefor |
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Cited By (8)
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CN108264018A (en) * | 2018-02-06 | 2018-07-10 | 北京科技大学 | The method of the high power capacity storage hydrogen material of ferrum-based catalyst modification three-dimensional grapheme confinement |
CN108264018B (en) * | 2018-02-06 | 2019-10-22 | 北京科技大学 | The method that ferrum-based catalyst modifies the high power capacity storage hydrogen material of three-dimensional grapheme confinement |
CN109319732A (en) * | 2018-10-15 | 2019-02-12 | 浙江大学 | A kind of preparation method of two dimension loaded nano magnesium hydride hydrogen storage material |
CN112390224A (en) * | 2019-08-16 | 2021-02-23 | 中国科学院大连化学物理研究所 | Polymer-coated hydrogen storage material and preparation method and application thereof |
WO2023071963A1 (en) * | 2021-10-25 | 2023-05-04 | 上海交通大学 | Nano magnesium hydride-loaded composite material and preparation method therefor |
CN115231514A (en) * | 2022-07-15 | 2022-10-25 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Magnesium-based hydrogen storage material catalyzed by hexagonal boron nitride loaded nano nickel particles and preparation method thereof |
CN115231514B (en) * | 2022-07-15 | 2023-08-04 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Hexagonal boron nitride loaded nano nickel particle catalyzed magnesium-based hydrogen storage material and preparation method thereof |
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