CN108083272A - A kind of preparation method of graphite alkene carbon material - Google Patents
A kind of preparation method of graphite alkene carbon material Download PDFInfo
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- CN108083272A CN108083272A CN201711448442.2A CN201711448442A CN108083272A CN 108083272 A CN108083272 A CN 108083272A CN 201711448442 A CN201711448442 A CN 201711448442A CN 108083272 A CN108083272 A CN 108083272A
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- graphite alkene
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Abstract
The invention belongs to carbon material technical fields, are specially a kind of graphite alkene carbon materials preparation method for material.The method of the present invention includes:Phenyl-hexahalide, calcium carbide and ball milling pearl vacuum ball grinder ball sealer are ground;Then the unreacted calcium carbide of removal is washed with deionized;Drying, and pulverize;Washing removes unreacted phenyl-hexahalide;It is dried again to get to class graphite alkene powder.Present invention process flow and required equipment are simple, are suitable for industrialized production.Prepared graphite alkene material has good Photocatalytic activity, available for photocatalysis degradation organic contaminant.
Description
Technical field
The invention belongs to carbon material technical fields, and in particular to a kind of graphite alkene carbon materials preparation method for material.
Background technology
Graphite alkene material is after graphene, another is known as the new carbon of super material, because of its uniqueness
Electric property and electrochemical properties, and gather around and have wide practical use in fields such as the energy, electronics, catalysis.Preferable graphite alkene
It is to be connected phenyl ring by several acetylene bonds, is formed by sp2Hydbridized carbon atoms and sp3The two dimensional surface net that hybridized atom conjugation is formed
The carbon material of network structure, the prior art are obtained by the cross-coupling reaction of six alkynyl benzene.The present invention proposes one kind with phenyl-hexahalide
It is raw material with calcium carbide, passes through the new method of mechanochemical reaction synthetic graphite alkynes.By the mechanical ball mill of planetary ball mill,
The powder containing graphite alkene is directly obtained under room temperature, impurity is removed by washing, obtains pure graphite alkene, the phenyl ring of the graphite alkene
Between pass through 1 acetylene bond and connect.Compared to existing method, this method simplifies synthesis procedure, and device requirement is low.
The content of the invention
It is an object of the invention to provide a kind of process is simple, the low graphite alkene preparation method of device requirement, and will prepare
Obtained graphite alkene is applied to catalysis material, electrochemistry and lithium ion battery negative material.
The preparation method of graphite alkene carbon material provided by the invention, concretely comprises the following steps:
(1)By a certain amount of phenyl-hexahalide(C6X6), calcium carbide(CaC2)It is placed in vacuum ball grinder, adds in a certain amount of with ball milling pearl
Absolute ethyl alcohol;Ball grinder is sealed, inert gas is vacuumized or be passed through to ball grinder;
(2)By planetary ball mill it is small with 400 ~ 600 revs/min of rate ball milling 6 ~ 18 when;The sample that ball milling is completed is taken out,
The unreacted calcium carbide of removal is washed with deionized;
(3)By step(2)Obtained sample is pulverized with 40 ~ 90 DEG C of drying;Washing removes unreacted phenyl-hexahalide;
(4)By step(3)Obtained sample is with 40 ~ 90 DEG C of drying to get to class graphite alkene powder.
In the present invention, phenyl-hexahalide can be hexachloro-benzene, hexabromobenzene or hexaiodo benzene.
In the present invention, control ball material mass ratio is 20:1~100:1, preferably ball material mass ratio is 40:1~80:1,.
In the present invention, it is 1 to control the molar ratio of phenyl-hexahalide and calcium carbide:6~1:18, i.e., 1:(6~18), preferred molar ratio is
1:10~1:15。
In the present invention, the amount of absolute ethyl alcohol need to not there be ball milling pearl at least.
In the present invention, the inert atmosphere is nitrogen(N2)Or argon gas(Ar).
Experiment shows that class graphite alkene material is a kind of p-type semiconductor prepared by the present invention, can be applied to electrochemistry neck
Domain.
Experiment shows that graphite alkene material has good Photocatalytic activity prepared by the present invention, can be applied to light
Catalytic degradation organic pollution.
Experiment shows that graphite alkene material prepared by the present invention has certain storage lithium activity, can be applied to lithium ion battery and bears
Pole material.
Graphite alkene is a kind of new carbon newly proposed in recent years, is possessed widely in fields such as the energy, electronics, catalysis
Application prospect.At present, the preparation method of graphite alkene only prepares graphite diine one kind, forerunner's system by cross-coupling reaction
Standby difficulty is big, and sample yield is relatively low.Therefore, graphite alkene material is prepared in stone by the big preparation method of this amount of mechanochemical reaction
Two aspect of preparation and application of black alkynes has good prospect.
Compared with prior art, the present invention has following outstanding feature:
(1)The present invention is prepared for a kind of new class graphite alkene material(One alkynes of graphite);
(2)The present invention relates to preparation method compared with existing cross-coupling reaction, technological process is simplified;
(3)The present invention relates to preparation method compared with existing cross-coupling reaction, simplify needed for equipment it is simple, be suitable for work
Industry metaplasia is produced.
The prominent substantive distinguishing features of the present invention and marked improvement can be emerged from from following embodiment, but are not limited to
This.
Description of the drawings
Fig. 1 is the graphite alkene powder preparing processes schematic diagram in embodiment 1.
Fig. 2 is the full spectrogram of the x-ray photoelectron spectroscopy of the graphite alkene powder in embodiment 1.
Fig. 3 is the carbon spectrogram of the x-ray photoelectron spectroscopy of the graphite alkene powder in embodiment 1.
Fig. 4 is the Raman figure of the graphite alkene powder in embodiment 1.
Fig. 5 is the photo-catalytic degradation of methyl-orange graph of the graphite alkene sample in embodiment 1.
Fig. 6 is the diffusing reflection abosrption spectrogram of the graphite alkene powder in embodiment 2.
Fig. 7 is the linear sweep voltammetry spectrogram of the graphite alkene electrode in embodiment 2.
Fig. 8 is the not special Schottky curve of the graphite alkene electrode in embodiment 2.
Fig. 9 is the energy band diagram of the graphite alkene sample in embodiment 2.
Figure 10 is applied to cycle performance curve during negative electrode of lithium ion battery, charge and discharge for the graphite alkene sample in embodiment 3
Electric current density is 100 milliamperes/gram, and charging/discharging voltage scope is 0.01 ~ 3.0 volt.
Specific embodiment
The specific implementation of the present invention is described further below in conjunction with example and attached drawing, but the implementation and protection of the present invention
It is without being limited thereto.
Embodiment 1
With 1:20 ball material mass ratio, according to 1:6 molar ratio weighs hexachloro-benzene(C6Cl6)And calcium carbide(CaC2), it is placed in vacuum
In spheroidal graphite tank, absolute ethyl alcohol is added in no mistake abrasive material.Ball grinder is sealed, ball grinder is vacuumized.With 400 revs/min of rate
By planetary ball mill ball milling 18 it is small when.The sample that ball milling is completed is taken out, makes the unreacted carbon of removal is washed with deionized
Change calcium.Hot benzene washing is reused after drying and removes unreacted phenyl-hexahalide, directly obtains graphite alkene powder.
Measure 50 milliliters of methyl orange solutions(10 mg/litres), add in 50 milligrams of samples, stand 3 it is small when after, with it is ultraviolet-can
See that illumination injects the reaction of row photocatalytic degradation.Every 20 minutes, the absorbance of UV-vis absorption spectrum measurement solution is used
Variation.
The full spectrum of the x-ray photoelectron spectroscopy of sample(Fig. 2)Illustrate, the oxygen element that sample is brought into except surface contamination
Outside, only it is made of carbon.The carbon spectrum of the x-ray photoelectron spectroscopy of sample(Fig. 3)With Raman pattern(Fig. 4)Illustrate in sample
Carbon only exists sp2Hydridization and sp3Hydridization two states, with reference to Fig. 2, it is thus identified that sample is graphite alkene.Sample UV, visible light again
Photo-catalytic degradation of methyl-orange curve under light(Fig. 5)Illustrate that graphite alkene sample has photocatalysis degradation organic contaminant performance.
Embodiment 2
With 1:50 ball material mass ratio, according to 1:12 molar ratio weighs hexabromobenzene(C6Br6)And calcium carbide(CaC2), it is placed in true
In empty spheroidal graphite tank, absolute ethyl alcohol is added in no mistake abrasive material.Ball grinder is sealed, nitrogen is passed through after being vacuumized to ball grinder(N2).With
500 revs/min of rate by planetary ball mill ball milling 12 it is small when.
After the sample completed according to 1 the method for example to ball milling is washed and dried, by sample and polyethylene glycol, ethyl
Cellulose, ethyl alcohol are according to mass ratio:9:9:1:1 mixing, when magnetic agitation 2 ~ 10 is small at 40 ~ 90 DEG C.Obtained slurry is revolved
It is applied on electro-conductive glass, polyethylene glycol, ethyl cellulose is removed in Muffle furnace to anneal under conditions of 260 ~ 300 DEG C after drying
The surfactants such as element.Using conducting wire, conducting resinl, insulating cement etc. by the electrode package after annealing to get electric to the work of sample
Pole.
The diffusing reflection absorption spectrum of sample(Fig. 6)It is middle to there is absorption band edge, illustrate sample for semiconductor, 2.2 electronics of band gap
Volt.The linear sweep voltammetry spectrum of sample electrode is as shown in fig. 7, compared with -0.5 volt to -1.2 volts of saturated calomel electrode
There is an electric current platform in place, which is since minority carrier by electric field is influenced can be neglected, and only is influenced to make by diffusion
Into;The electric current is that negative current illustrates that the sample is p-type semiconductor.Compared with -0.7 volt of saturated calomel electrode to -0.4
Volt place occur a zero current platform, illustrate sample the potential region for ideal polarizable electrode.The not spy of sample electrode
Schottky curve(Fig. 8)Confirm sample as p-type semiconductor, and measure the flat-band potential of sample(Fermi level).Due to p-type
The fermi level of semiconductor is approximately equal to valence band, and with reference to the band gap that Fig. 5 is obtained, Fig. 9 is the energy band of the graphite alkene sample in embodiment 2
Figure.
Embodiment 3
With 1:100 ball material mass ratio, according to 1:18 molar ratio weighs hexaiodo benzene(C6I6)And calcium carbide(CaC2), it is placed in true
In empty spheroidal graphite tank, absolute ethyl alcohol is added in full of ball grinder.Ball grinder is sealed, planetary ball is passed through with 500 revs/min of rate
When grinding machine ball milling 12 is small, and washed according to the sample that 1 the method for example completes ball milling with being dried.
With 8:1:1 mass ratio weighs active material(Graphite alkene powder), conductive agent(Super P fine powders)And binding agent
(Kynoar), add in solvent(1-Methyl-2-Pyrrolidone)In, it is stirred into slurry under dry atmosphere.By slurry
It is uniformly applied on copper foil, when being placed on small with 60 DEG C of temperature drying 24 in vacuum drying chamber, is cut into a diameter of 14 millimeters of circle
Piece is assembled into the button cell of CR2016 types in the glove box full of argon gas after weighing.Wherein, lithium metal is used as to electrode, and 1
M LiPF6EC/DMC(Volume ratio is 1:1)Solution is as electrolyte, using Celgard-2300 membranes.Constant current charge-discharge
Test carries out in LAND test systems, and charging and discharging currents density is 100 milliamperes/gram, charging/discharging voltage scope for 0.01 ~
3.0 volt.
Cycle performance of the graphite alkene material in 0.1 ~ 3.0 volt of voltage range is as shown in Figure 10.As can be seen that
Under the current density of 100 milliamperes/gram, sample possesses certain storage lithium performance.
Claims (6)
1. a kind of preparation method of graphite alkene carbon material, which is characterized in that concretely comprise the following steps:
(1)Phenyl-hexahalide, calcium carbide and ball milling pearl are placed in vacuum ball grinder, add in absolute ethyl alcohol;Ball grinder is sealed, to ball milling
Tank vacuumizes or is passed through inert gas;
(2)By planetary ball mill it is small with 400 ~ 600 revs/min of rate ball milling 6 ~ 18 when;The sample that ball milling is completed is taken out,
The unreacted calcium carbide of removal is washed with deionized;
(3)By step(2)Obtained sample is pulverized with 40 ~ 90 DEG C of drying;Washing removes unreacted phenyl-hexahalide;
(4)By step(3)Obtained sample is with 40 ~ 90 DEG C of drying to get to class graphite alkene powder.
2. preparation method according to claim 1, which is characterized in that step(1)Described in phenyl-hexahalide for hexachloro-benzene, hexabromo
Benzene or hexaiodo benzene.
3. preparation method according to claim 1, which is characterized in that step(1)Middle ball material mass ratio control is 20:1~
100:1。
4. preparation method according to claim 1, which is characterized in that step(1)Described in phenyl-hexahalide and calcium carbide rub
You are than being 1:6~1:18.
5. preparation method according to claim 1, which is characterized in that step(1)Described in the amount of absolute ethyl alcohol do not have at least
Cross ball milling pearl.
6. preparation method according to claim 1, which is characterized in that step(1)Described in inert atmosphere for nitrogen or
Argon gas.
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Cited By (13)
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CN108373147A (en) * | 2018-01-18 | 2018-08-07 | 复旦大学 | A kind of preparation method and applications of alkynyl carbon material |
CN108946698A (en) * | 2018-08-18 | 2018-12-07 | 复旦大学 | A method of based on benzene precursor preparation γ type graphite list alkynes nano-carbon material |
CN109136970A (en) * | 2018-09-11 | 2019-01-04 | 太原师范学院 | A kind of Bipolar Membrane and preparation method thereof of area load graphite alkene |
CN109985602A (en) * | 2019-03-13 | 2019-07-09 | 北京化工大学 | CaC2And CO2Or the method and its absorption demercuration application of carbonate ball milling preparation carbon material containing oxycetylene |
CN111217417A (en) * | 2019-11-29 | 2020-06-02 | 广东石油化工学院 | Method for treating 2-naphthol wastewater by utilizing graphdiyne modified silver phosphate composite photocatalyst |
CN111490258A (en) * | 2020-05-12 | 2020-08-04 | 超威电源集团有限公司 | Preparation method of graphite alkyne-loaded monatomic catalyst |
CN112408381A (en) * | 2020-12-09 | 2021-02-26 | 西北大学 | Two-dimensional gamma-graphite mono-alkyne powder and preparation method thereof |
CN113083234A (en) * | 2021-03-08 | 2021-07-09 | 西北大学 | Adsorbent for adsorbing dye-containing wastewater, preparation method and application |
CN113104838A (en) * | 2021-04-30 | 2021-07-13 | 天津工业大学 | Preparation method of plasma fluorine-doped modified gamma-type graphite single alkyne carbon material |
CN114789995A (en) * | 2022-04-16 | 2022-07-26 | 复旦大学 | Specific site sulfur/nitrogen co-doped graphite monoalkyne and preparation method and application thereof |
CN115557492A (en) * | 2022-10-20 | 2023-01-03 | 长江大学 | Method for synthesizing graphite from calcium carbide and amorphous carbon at low temperature |
CN115832314A (en) * | 2023-02-22 | 2023-03-21 | 江苏正力新能电池技术有限公司 | Composite graphdiyne modified layered oxide material, preparation method thereof, positive plate and sodium-ion battery |
CN117023561A (en) * | 2023-09-07 | 2023-11-10 | 河南农业大学 | Synthesis method of electrochemical active oxazine-alkyne carbon material |
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CN108946698B (en) * | 2018-08-18 | 2021-08-20 | 复旦大学 | Method for preparing gamma-type graphite single alkyne nano carbon material based on benzene precursor |
CN108946698A (en) * | 2018-08-18 | 2018-12-07 | 复旦大学 | A method of based on benzene precursor preparation γ type graphite list alkynes nano-carbon material |
CN109136970A (en) * | 2018-09-11 | 2019-01-04 | 太原师范学院 | A kind of Bipolar Membrane and preparation method thereof of area load graphite alkene |
CN109136970B (en) * | 2018-09-11 | 2019-11-15 | 太原师范学院 | A kind of Bipolar Membrane and preparation method thereof of area load graphite alkene |
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CN112408381A (en) * | 2020-12-09 | 2021-02-26 | 西北大学 | Two-dimensional gamma-graphite mono-alkyne powder and preparation method thereof |
CN113083234A (en) * | 2021-03-08 | 2021-07-09 | 西北大学 | Adsorbent for adsorbing dye-containing wastewater, preparation method and application |
CN113083234B (en) * | 2021-03-08 | 2022-08-09 | 西北大学 | Adsorbent for adsorbing dye-containing wastewater, preparation method and application |
CN113104838A (en) * | 2021-04-30 | 2021-07-13 | 天津工业大学 | Preparation method of plasma fluorine-doped modified gamma-type graphite single alkyne carbon material |
CN114789995A (en) * | 2022-04-16 | 2022-07-26 | 复旦大学 | Specific site sulfur/nitrogen co-doped graphite monoalkyne and preparation method and application thereof |
CN114789995B (en) * | 2022-04-16 | 2023-11-07 | 复旦大学 | Specific site sulfur/nitrogen co-doped graphite monoacetylene and preparation method and application thereof |
CN115557492A (en) * | 2022-10-20 | 2023-01-03 | 长江大学 | Method for synthesizing graphite from calcium carbide and amorphous carbon at low temperature |
CN115557492B (en) * | 2022-10-20 | 2023-10-03 | 长江大学 | Method for synthesizing graphite from calcium carbide and amorphous carbon at low temperature |
CN115832314A (en) * | 2023-02-22 | 2023-03-21 | 江苏正力新能电池技术有限公司 | Composite graphdiyne modified layered oxide material, preparation method thereof, positive plate and sodium-ion battery |
CN117023561A (en) * | 2023-09-07 | 2023-11-10 | 河南农业大学 | Synthesis method of electrochemical active oxazine-alkyne carbon material |
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