CN109128219A - A kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material - Google Patents
A kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material Download PDFInfo
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- CN109128219A CN109128219A CN201811154087.2A CN201811154087A CN109128219A CN 109128219 A CN109128219 A CN 109128219A CN 201811154087 A CN201811154087 A CN 201811154087A CN 109128219 A CN109128219 A CN 109128219A
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Abstract
The present invention provides a kind of methods that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material, belong to nano material synthesis technical field.It is uniformly placed in Gaseous Detonation reaction kettle according to the mixed uniformly acetylacetone cobalt of cobalt copper molar ratio (III) and acetylacetone copper, is vacuumized after closed.Imflammable gas and oxygen-containing gas are injected, Gaseous Detonation reaction kettle is heated to 160~180 DEG C, keeps the temperature several minutes.Stop heating, ignites mixed gas in reaction kettle with electric spark；Detonation after completion of the reaction, opens control valve and gas is discharged, collect solid powder in Gaseous Detonation reaction kettle, as carbon-based cobalt copper nano material.Beneficial effects of the present invention: 1) the Gaseous Detonation method provided synthesizes the method for carbon-based cobalt-copper alloy nano material simply, quickly.2) detonation provides high temperature and high pressure environment, can synthesize a large amount of carbon-based cobalt-copper alloy nano materials in a very short period of time.3) product purity prepared by is higher, structure with it is functional, cost is relatively low.
Description
Technical field
It is using acetylacetone cobalt (III) and acetylacetone copper as carbon source the invention belongs to nano material synthesis technical field
With source metal, the technology of carbon-based cobalt-copper alloy nano material is synthesized with the mode of Gaseous Detonation.
Background technique
Nanometer cobalt-copper alloy is a kind of highly active catalyst, is widely used in Industrial Catalysis field.With carbon packet cobalt copper
Nano particle or carbon nanotube be representative etc. carbon-based cobalt copper nano material can not only prevent the oxidation of cobalt-copper alloy, can be with
Effectively weaken metal core to react with sour, and then protects the activity of cobalt-copper alloy nanocatalyst.In addition, carbon-based cobalt copper nanometer
Particle has certain ferromagnetism, applies also for rubber-ferrite, drug loading, heavy metal adsorption, electronic field etc..
The common method of carbon-based cobalt copper nano material has chemical vapor infiltration (Ekaterina
A.PonomarevaIrina V.KrasnikovaEkaterina V.EgorovaIlya V.MishakovAleksey
A.Vedyagin.Dehydrogenation of ethanol over carbon-supported Cu–Co catalysts
modified by catalytic chemical vapor deposition.《Reaction Kinetics,Mechanisms
And Catalysis " .2017,122 (1): 399-408), thermal annealing method (Zeng Jun, Fan Huiqing, Wang
Yangli,Zhang Shiquan,Xue Jun,Cheng Xinying.Ferromagnetic and microwave
absorption properties of copperoxide/cobalt/carbon fiber multilayer film
Composites. " Thin Solid Films " .2012,520 (15): 5053-5059), liquid phase method (Bulut, A.Yurderi,
M.Ertas,I.E.Celebi,M.Kaya,M.Zahmakiran,M.Carbon dispersed copper-cobalt alloy
nanoparticles:A cost-effective heterogeneous catalyst with exceptional
performance in the hydrolytic dehydrogenation of ammonia-borane.《Applied
Catalysis B-Environmental " .2016,180:121-129) etc..Wherein chemical vapor infiltration is preparing carbon-based cobalt
It needs to consume higher energy when copper nano material, and relatively high to equipment requirement.Thermal annealing method although required temperature
It is not very high, but whole preparation process takes a long time.The sample that liquid phase method obtains is purer, but consumption of chemical reaction
Longer time, later period still need to further be dried.Therefore, study it is a kind of efficiently, quickly synthesize carbon-based cobalt-copper alloy
The method of nano material is particularly significant.For this purpose, the present invention is using acetylacetone cobalt (III) and acetylacetone copper as carbon source and metal
Source synthesizes carbon-based cobalt-copper alloy nano material by the Gaseous Detonation of imflammable gas, can in a very short period of time efficiently
Synthesize pure carbon-based cobalt-copper alloy nano material.
Currently, Gaseous Detonation method be commonly used to prepare carbon- coated iron nanoparticles (H.Yan, T.Zhao, X.Li,
Ch.Hun.Hydrogen and air detonation(deflagration)synthesis of carbon-
encapsulated iron nanoparticles.《Combustion,Explosion,and Shock Waves》.2015,
51 (4): 495-501), (Yan Honghao, Zhang Xiaofei, Zhao Bibo, Zhao Tiejun, Li Xiaojie gas phase/cohesion are fried for carbon copper-clad nano particle
Carbon copper-clad nanoparticle features " light laser and the particle beams " .2017,29:74-78 of medicine Explosive detonation), carbon packet cobalt nano-particle
(Tiejun Zhao,Xiaojie Li,Honghao Yan.Metal catalyzed preparation of carbon
nanomaterials by hydrogen–oxygen detonation method.《Combustion and Flame》
.2018,196:108-115) this kind of carbon packet monometallic nano material, and rarely have report for the research of C-base alloy nano material
Road.The boiling point of acetylacetone cobalt (III) is 150 DEG C, and the boiling point of acetylacetone copper is 160 DEG C, and the two is not much different, when gas phase is quick-fried
When initial temperature is more than 160 DEG C in Hong reaction kettle, the two can be mixed equably, this synthesizes carbon-based cobalt-copper alloy for Gaseous Detonation and receives
Rice material provides advantage.
Summary of the invention
The object of the present invention is to provide a kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material, this method
Have the characteristics that easy to operate, quick, efficient, yield is considerable and pure.
Technical solution of the present invention:
A kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material, steps are as follows:
(1) acetylacetone cobalt (III) and acetylacetone copper presoma are uniformly mixed according to certain cobalt copper molar ratio, be placed in
In Gaseous Detonation reaction kettle, after closed and vacuumize；
(2) it is filled with the imflammable gas and oxygen-containing gas for meeting explosion limit ratio into Gaseous Detonation reaction kettle, and adds
Heat is to 160~180 DEG C；
(3) heating system is closed, ignites the mixed gas in Gaseous Detonation reaction kettle with electric spark；
(4) detonation reaction terminates, and after product precipitating, opens gas after control valve discharge reaction, collects solid powder in kettle,
As carbon-based cobalt-copper alloy nano material.
Wherein cobalt, copper molar ratio be 3:1~1:3.
The imflammable gas is hydrogen, methane, acetylene, propane, natural gas, liquefied petroleum gas, carbon monoxide, benzene steaming
The mixing of one or more of gas.
The oxygen-containing gas is the mixed gas of oxygen, air and they and nitrogen, argon gas, carbon dioxide.
Beneficial effects of the present invention:
1) the Gaseous Detonation method provided synthesizes the method for carbon-based cobalt-copper alloy nano material simply, quickly.
2) detonation provides high temperature and high pressure environment, can synthesize a large amount of carbon-based cobalt-copper alloy nano materials in a very short period of time.
3) product purity prepared by is higher, structure with it is functional, cost is relatively low.
Detailed description of the invention
Fig. 1 is the detonation reaction kettle device schematic diagram that Gaseous Detonation experiment is used used in the present invention.
Fig. 2 is X-ray diffraction (XRD) map of embodiment 1 and embodiment 2.
Fig. 3 is transmission electron microscope (TEM) picture of carbon-based cobalt-copper alloy nano material in embodiment 1.
Fig. 4 is the TEM picture of carbon-based cobalt-copper alloy nano material in embodiment 2.
In figure: 1 ring flange；2 control valves；3 vacuum meters；4 aeration apertures vacuumize hole；5 spark plugs；6 detonation reaction chambers；7
Temperature control system；The XRD spectrum of carbon-based cobalt-copper alloy nano material in 8 embodiments 1；Carbon-based cobalt-copper alloy nanometer material in 9 embodiments 2
The XRD spectrum of material；● it is the diffraction maximum of copper；▼ is Co0.52Cu0.48Diffraction maximum；■ is the diffraction maximum of cobalt.
Specific embodiment
A specific embodiment of the invention is further illustrated below in conjunction with attached drawing and technical solution.
Embodiment 1
Acetylacetone cobalt (III) and acetylacetone copper are weighed respectively according to n (Co): n (Co)=2:1, in the agate mortar
Uniformly mixing takes in 3g merging Gaseous Detonation reaction kettle.Detonation reaction kettle is sealed, 1kPa is evacuated to by control valve 2.According to rubbing
You are successively filled with hydrogen and oxygen to atmospheric pressure by control valve 2 than being 2:1.Temperature control system 7 is opened, setting temperature is 165 DEG C,
Detonation reaction chamber 6 is kept for several minutes at 165 DEG C, uniformly stops heating to gas mixing.Control valve 2 is closed, by high-energy igniter
The mixed gas ignited in detonation reaction chamber 6 is connect with spark plug 5.Detonation after reaction, opens control valve 2 and gas is discharged,
It opens ring flange 1 and collects solid powder product.Product is characterized, as carbon-based cobalt-copper alloy nano material.Curve in Fig. 2
8 be the XRD spectrum of the carbon-based cobalt-copper alloy nano material of hydrogen or oxygen gas detonation preparation, main peak Co0.52Cu0.48, containing a small amount of
Copper, cobalt.TEM chart levies (see Fig. 3), and discovery product is carbon nanotube and carbon covered metal particle.Length of carbon nanotube be 200~
300nm, outer diameter about 15nm, internal diameter is about 9nm.Carbon packet cobalt-copper alloy nanoparticle size about 20nm, slightly reunites.
Embodiment 2
According to the experimental method of embodiment 1, after Gaseous Detonation reaction kettle is vacuumized by control valve 2, temperature control system is opened
7, setting temperature is 165 DEG C.3ml benzole soln is injected through control valve 4, after 3 registration of vacuum meter is stablized, is filled with 5 times through control valve 2
In the oxygen of benzene vapor, keep the temperature several minutes.After mixing, tube wall control valve 2 connects spark plug 5 with high-energy igniter to steam
Ignite the mixed gas in detonation reaction chamber 6.Detonation after reaction, opens control valve 2 and gas is discharged, and opens ring flange 1 and receives
Collect solid powder product.Product is characterized, as carbon-based cobalt-copper alloy nano material.Curve 9 is hydrogen or oxygen gas in Fig. 2
The XRD spectrum of the carbon-based cobalt-copper alloy nano material of detonation preparation, main peak Co0.52Cu0.48, contain a small amount of copper, cobalt.TEM chart
It levies (see Fig. 4), discovery product is carbon nanotube and carbon covered metal particle.Length of carbon nanotube is 150~250nm, and outer diameter is about
18nm, internal diameter are about 9nm.Carbon packet cobalt-copper alloy nanoparticle size about 50nm, slightly reunites.
Embodiment 3
According to the experimental method of embodiment 1, the molar ratio of cobalt, copper is changed into 1:1, remaining step and embodiment 1 are complete
It is identical, obtain carbon-based cobalt-copper alloy nano material.
Embodiment 4
According to the experimental method of embodiment 1, imflammable gas changes methane into, and methane and oxygen molar ratio are 1:1, remaining step
Suddenly identical with embodiment 1, it is similarly obtained carbon-based cobalt-copper alloy nano material.
In conclusion the present invention prepares carbon-based cobalt-copper alloy nano material by the method for Gaseous Detonation, utilization is flammable
Property gas detonation generate high temperature and pressure pyrolysis acetylacetone cobalt (III) and acetylacetone copper mixed vapour, provide synthesis
The method of carbon-based cobalt-copper alloy nano material.This synthetic method efficiently, simply, there is the potentiality of industrialized production.
The parameter and scheme that the present invention is not limited to the above embodiment, be not limited to compared with low boiling point, sublimation point containing cobalt, copper
Substance, all any modification, improvement and equivalent replacements made within spirit of the invention and principle should be included in this hair
Within bright protection scope.
Claims (5)
1. a kind of method that Gaseous Detonation method synthesizes carbon-based cobalt-copper alloy nano material, which is characterized in that steps are as follows:
(1) acetylacetone cobalt (III) and acetylacetone copper presoma are uniformly mixed according to certain cobalt copper molar ratio, is placed in gas phase
In detonation reaction kettle, after closed and vacuumize；
(2) it is filled with the imflammable gas and oxygen-containing gas for meeting explosion limit ratio into Gaseous Detonation reaction kettle, and is heated to
160~180 DEG C；
(3) heating system is closed, ignites the mixed gas in Gaseous Detonation reaction kettle with electric spark；
(4) detonation reaction terminates, and after product precipitating, opens gas after control valve discharge reaction, collects solid powder in kettle, as
Carbon-based cobalt-copper alloy nano material.
2. the method according to claim 1, wherein the molar ratio of the cobalt, copper is 3:1~1:3.
3. method according to claim 1 or 2, which is characterized in that the imflammable gas be hydrogen, methane, acetylene,
The mixing of one or more of propane, natural gas, liquefied petroleum gas, carbon monoxide, benzene vapor.
4. method according to claim 1 or 2, which is characterized in that the oxygen-containing gas be oxygen, air and it
Mixed gas with nitrogen, argon gas, carbon dioxide.
5. according to the method described in claim 3, it is characterized in that, the oxygen-containing gas be oxygen, air and they with
The mixed gas of nitrogen, argon gas, carbon dioxide.
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| CN114112407A (en) * | 2021-12-02 | 2022-03-01 | 内蒙动力机械研究所 | Powder detonation engine conveying system and method |
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Application publication date: 20190104 |