CN109941983A - A kind of High-conductivity carbon material and preparation method thereof - Google Patents
A kind of High-conductivity carbon material and preparation method thereof Download PDFInfo
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- CN109941983A CN109941983A CN201711386613.3A CN201711386613A CN109941983A CN 109941983 A CN109941983 A CN 109941983A CN 201711386613 A CN201711386613 A CN 201711386613A CN 109941983 A CN109941983 A CN 109941983A
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Abstract
The invention discloses a kind of carbon materials and preparation method thereof, and the preparation method comprises the following steps: by least containing three alkynyls compound and catalyst be added in solvent, reacted at a certain temperature and obtain the carbon material.The present invention utilizes the high activity feature of alkynyl, compound at least containing three alkynyls is obtained into carbon material in very mild conditions, its preparation efficiency is significantly better than the preparation process of current pyrocarbon material, and the microscopic appearance control of the obtained carbon material of this method is easy, molecular structure can design, and can sufficiently be regulated and controled according to practical application request to carbon material structure, gained carbon material good conductivity, stability is good, and carbon material processing performance is more excellent.Meanwhile this method simple process and low cost, applied widely, more conducively industrialized production, be conducive to carbon material further genralrlization to the application field for much needing to operate in temperate condition.
Description
Technical field
The invention belongs to carbon material preparation fields, and in particular to a kind of High-conductivity carbon material and preparation method thereof.
Background technique
Carbon material plays increasingly important role in modern society, and the development of carbon material provides weight for every profession and trade
The development opportunity wanted.In recent years, the whole world is faced with weather and gradual warms up, and pollution is on the rise and non-renewable fossil energy
The challenge of reduction year by year, countries in the world are higher and higher for the cry of the more clean energy, including fuel cell, lithium from
Sub- battery, supercapacitor, solar battery, microbiological fuel cell etc. become science and industrialization in recent years and give priority to
Project.It is well known that the above clean energy resource all be unable to do without the carbon material haveing excellent performance without exception, especially want to more
High performance carbon material is prepared under mild system.
Current commercialized carbon material includes carbon black, active carbon, graphite, carbon nanotube, graphene etc., these material parts
It is succeeded (such as carbon black, active carbon, graphite etc.) in commercialized application, remarkable result is partially obtained in basic research
(such as carbon nanotube, graphene etc.).However, these materials are (to be higher than 800 DEG C) at very high temperatures to produce, in electrification
It is not well positioned to meet the characteristic that each energy system is badly in need of when learning energy source use.For example current carbon material also cannot achieve one
The cryogenic carbon coating technology that a little potential high energy density cells electrode materials need, to realize through the electrode material
Carbon coating promotes the circulation, safety and rapid charging performance of the electrode material；For another example current carbon material does not have fuel cell also
The high-ratio surface of cathode and anode needs high conductivity, has very high adhesive force to catalyst, while needing to gas and liquid
Body has the performances such as efficient transmission；For another example photochemical catalyst needs the carrier of certain semiconductor property, increases catalyst and carrier
Active force, and advanced optimize catalyst photocatalysis performance, and current carbon material can't make as such carrier
With.
Many applications as described above all propose sternness to the property of traditional carbon material production method and carbon material
Challenge.Thus need to develop the highly efficient method for preparing high performance carbon material, the microstructure of adjustable carbon material
And molecular morphosis, it will be that the above clean energy resource performance boost is significantly pushed to play an important role.
Summary of the invention
To solve the above problems, the present invention provides a kind of carbon materials preparation method for material, can be prepared with this method has
The High-conductivity carbon material of various microscopic appearances.
The invention provides the following technical scheme:
A kind of carbon materials preparation method for material, the described method comprises the following steps: by least containing three alkynyls compound and
Catalyst is added in solvent, is reacted at a certain temperature and obtains the carbon material.
According to the present invention, described at least containing there are three the compounds of alkynyl to be selected from the compound of alkynyl containing there are three, contains
The compound of four alkynyls, containing there are five the compound of alkynyl or containing there are six one of compound of alkynyl or a variety of groups
It closes.
According to the present invention, the alkynyl at least containing there are three in the compound of alkynyl is end alkynyl radical.
Preferably, the compound of the alkynyl at least containing there are three is selected from one of compound as described below or more
Kind combination:
According to the present invention, the solvent is water, methylene chloride, chloroform, ethyl acetate, pyridine, tetrahydrofuran, first
Benzene, methanol, ethyl alcohol, butanol, the tert-butyl alcohol, 1-Methyl-2-Pyrrolidone, benzene, dichloroethanes, carbon tetrachloride, tetrachloromethane, three second
Amine, ethylenediamine, hexamethylene, n-hexane, cyclohexanone, toluene cyclohexanone, acetone, espeleton, methylisobutylketone, petroleum ether, two
Toluene, pentane, hexane, octane, methyl acetate, ethyl acetate, propyl acetate, dimethyl acetamide, dimethylformamide, second two
Alcohol monomethyl ether, ethylene glycol monoethyl ether, propene carbonate, ethylene carbonate, methyl esters, 1,4-fourth propyl ester, dimethyl carbonate, ethylene glycol
Monobutyl ether, acetonitrile, propionitrile, chlorobenzene, carbon disulfide, N, N- diethyl -1,3- propane diamine, 1,3- propane diamine, N, dimethyl -1 N-,
3- propane diamine, hempa, triethylene tetramine, hexamethylenetetramine, melamine, dipropylenetriamine, tetramethylethylenediamine, dichloro
One or more of benzene, ether etc. mixed solvent.
For example, the solvent is the mixed solvent of following two classes solvents:
The first kind is selected from least one of following solvents: water, methylene chloride, chloroform, ethyl acetate, tetrahydro furan
It mutters, toluene, methanol, ethyl alcohol, butanol, the tert-butyl alcohol, 1-Methyl-2-Pyrrolidone, benzene, dichloroethanes, carbon tetrachloride, four chloromethanes
Alkane, hexamethylene, n-hexane, cyclohexanone, toluene cyclohexanone, acetone, espeleton, methylisobutylketone, petroleum ether, dimethylbenzene, penta
Alkane, hexane, octane, methyl acetate, ethyl acetate, propyl acetate, dimethyl acetamide, dimethylformamide, ethylene glycol list first
Ether, ethylene glycol monoethyl ether, propene carbonate, ethylene carbonate, methyl esters, 1,4-fourth propyl ester, dimethyl carbonate, ethylene glycol only son
Ether, acetonitrile, propionitrile, chlorobenzene, carbon disulfide, dichloro-benzenes, ether；
Second class is selected from least one of following solvents: pyridine, triethylamine, ethylenediamine, N, N- diethyl -1,3- the third two
Amine, 1,3- propane diamine, N, N- dimethyl -1,3- propane diamine, hempa, triethylene tetramine, hexamethylenetetramine, melamine,
Dipropylenetriamine, tetramethylethylenediamine.
Wherein, the dosage volume ratio of first kind solvent and the second class solvent is 10000:1 to 1:10000；It is preferred that 100:1 is arrived
1:10。
According to the present invention, the reaction carries out in gas shield atmosphere, and the gas is nitrogen, argon gas, helium, ammonia
One or more of gas, hydrogen, air, oxygen mixed gas.
According to the present invention, the pattern of the catalyst be one of nanometer rods, nano wire, nano particle, nanometer sheet or
Person is a variety of.
According to the present invention, the catalyst is one of copper, copper alloy, copper alloyed compound, copper compound or more
Kind.
According to the present invention, the copper alloy be copper and metallic aluminium, iron, zinc, manganese, cobalt, nickel, chromium, gold, platinum, silver, tin, titanium,
The alloy of one or more of germanium, zirconium, niobium, molybdenum, ruthenium, cadmium, indium, antimony, tantalum, lead.
According to the present invention, the copper compound is copper oxide, cuprous oxide, copper dioxide, copper sulfide, cuprous sulfide, hydrogen
One or more of copper oxide, cupric oxalate, copper chloride, stannous chloride, cupric phosphate.
According to the present invention, oxide of the copper alloyed compound for copper alloy, sulfide, halide, sulphate,
One or more of phosphate cpd or hydroxide.
According to the present invention, the copper alloy in the copper alloyed compound be copper and metallic aluminium, iron, zinc, manganese, cobalt, nickel, chromium,
The alloy of one or more of gold, platinum, silver, tin, titanium, germanium, zirconium, niobium, molybdenum, ruthenium, cadmium, indium, antimony, tantalum, lead.
According to the present invention, the mass ratio of the compound of alkynyl and solvent at least containing there are three is 1:10000 to 1:1,
Preferably 1:1000 to 1:100.
According to the present invention, described at least containing there are three the mass ratioes of the compound of alkynyl and catalyst to arrive for 1:1000
1000:1；Preferably 1:100 to 100:1.
According to the present invention, the condition of the reaction can be one of pressurization, microwave, infrared, ultrasonic, illumination, heating
Or it is a variety of.
According to the present invention, the reaction temperature is -50 DEG C to 300 DEG C.
According to the present invention, the reaction time is 0.5 hour to 200 hours.
The present invention also provides a kind of carbon materials prepared by the above method.
According to the present invention, the carbon material has high conductivity.
According to the present invention, the carbon material has various microscopic appearances, for example, the microscopic appearance is nano particle, receives
Rice noodles, nanometer sheet, hollow nano-sphere, nm wall array, nano-wire array, solid nanospheres etc..
Beneficial effect
The present invention provides a kind of method by synthesizing carbon material under cryogenic, and this method utilizes the high activity of alkynyl
Feature reacts the presoma of at least containing there are three alkynyl (preferably end-group alkyne) in very mild conditions and obtains carbon material,
Its preparation efficiency is significantly better than the preparation process of current pyrocarbon material, and the microscopic appearance control of carbon material that this method obtains
System is easy, and molecular structure can design, and can sufficiently be regulated and controled according to practical application request to carbon material structure, gained carbon material is led
Electrically good, stability is good, and carbon material processing performance is more excellent.Meanwhile this method simple process and low cost, it is applied widely,
More conducively industrialized production is conducive to carbon material further genralrlization to many application necks for needing to operate in temperate condition
Domain.
Detailed description of the invention
The SEM figure for the carbon nanocoils that the preparation of Fig. 1 embodiment 1 (compound 1 is raw material) obtains；
The SEM figure for the carbon nanosheet that the preparation of Fig. 2 embodiment 2 (compound 2 is raw material) obtains；
The stability for the supercapacitor that the carbon nanosheet that the preparation of Fig. 3 embodiment 2 (compound 2 is raw material) obtains is assembled into
Test curve；
The SEM figure for the big sheet multilevel structure carbon material of two dimension that the preparation of Fig. 4 embodiment 3 (compound 4 is raw material) obtains；
The SEM figure for the hollow Nano bead that the preparation of Fig. 5 embodiment 4 (compound 6 is raw material) obtains；
The SEM figure for the carbon nanowalls array that the preparation of Fig. 6 embodiment 5 (compound 8 is raw material) obtains；
The SEM figure for the carbon nanocoils array that the preparation of Fig. 7 embodiment 6 (compound 11 is raw material) obtains；
The SEM figure for the Nano carbon balls that the preparation of Fig. 8 embodiment 7 (compound 6 and compound 13 be raw material) obtains.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.Furthermore, it is to be understood that after having read documented content of the invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within limited range of the present invention.
Embodiment 1
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 1 of 10mg is added in the two-mouth bottle of 250ml, and is dissolved in 100ml methylene chloride, fills
That divides stirs evenly, and nitrogen protection gas is passed through in the solution, stirs 30 minutes；
(2) 1ml pyridine is added in the above solution and is sufficiently stirred 30 minutes；
(3) copper nano-wire of 50mg is added in the above solution, reaction temperature is controlled at 25 DEG C, reacts 10 with this condition
Hour, obtain the carbon material of microstructure as shown in Figure 1, reaction yield 90%.
Embodiment 2
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 2 of 100mg is added in the two-mouth bottle of 250ml, and is dissolved in 100ml ether and acetic acid second
It in ester (the two volume ratio 5:5), adequately stirs evenly, argon gas protection gas is passed through in the solution, is stirred 60 minutes；
(2) triethylamine 2ml is added in the above solution and is sufficiently stirred 30 minutes；
(3) the copper cobalt nanowire of 20mg is added in the above solution, reaction temperature is controlled at 30 DEG C, reacted with this condition
20 hours, obtain the carbon material of microstructure as shown in Figure 2, reaction yield 95%.
The supercapacitor that the above-mentioned carbon nanosheet being prepared is assembled into has excellent stability, and test result is as schemed
Shown in 3.
Embodiment 3
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 4 of 200mg is added in the two-mouth bottle of 500ml, and is dissolved in 300ml benzene, adequately stirs
It mixes uniformly, argon gas protection gas is passed through in the solution, is stirred 60 minutes；
(2) triethylene tetramine 5ml is added in the above solution and is sufficiently stirred 30 minutes；
(3) the cupric oxide nano piece of 100mg is added in the above solution, reaction temperature is controlled at 50 DEG C, with this condition
Reaction 15 hours, obtains the carbon material of microstructure as shown in Figure 4, reaction yield 85%.
Embodiment 4
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 6 of 50mg is added in the two-mouth bottle of 250ml, and is dissolved in 100ml acetone, adequately
It stirs evenly, ammonia is passed through in the solution, stir 60 minutes；
(2) N is added in the above solution, N- diethyl -1,3- propane diamine 1ml is simultaneously sufficiently stirred 30 minutes；
(3) the chlorination copper nano particles of 100mg are added in the above solution, reaction temperature is controlled at 50 DEG C, in this condition
Lower reaction 30 hours, obtains the carbon material of microstructure as shown in Figure 5, reaction yield 85%.
Embodiment 5
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 8 of 50mg is added in the two-mouth bottle of 250ml, and is dissolved in 200ml ethyl alcohol and tetrahydrofuran
In solution (the two volume ratio is 5:5), it is sufficiently stirred 10 minutes；
(2) ethylenediamine 1ml is added in the above solution and is sufficiently stirred 30 minutes；
(3) 100mg ambrose alloy oxidate nano chip arrays are added in the above solution, reaction temperature is controlled at -30 DEG C, herein
Under the conditions of react 100 hours, obtain the carbon material of microstructure as shown in Figure 6.
Embodiment 6
A kind of carbon materials preparation method for material, comprising the following steps:
(1) in the solvent thermal reaction kettle of 100ml be added 30mg compound 11, and be dissolved in 50ml n-hexane and
In tetrachloromethane solution (the two volume ratio is 5:5), it is sufficiently stirred 10 minutes；
(2) hexamethylenetetramine 1ml is added in the above solution and is sufficiently stirred 10 minutes；
(3) in the above solution be added 100mg copper manganese nano wire hydroxide array, reaction temperature control at 60 DEG C,
It reacts 12 hours under this condition, obtains the carbon material of microstructure as shown in Figure 7.
Embodiment 7
A kind of carbon materials preparation method for material, comprising the following steps:
(1) compound 6 (15mg) and compound 13 (15mg) are added in the vial of 100ml, and is dissolved in
In 80ml dimethyl carbonate, it is sufficiently stirred 10 minutes；
(2) melamine 2ml is added in the above solution and is sufficiently stirred 10 minutes；
(3) in the above solution be added 100mg copper and tin nano particle, reacted 2 hours under the conditions of microwave irradiation, obtain as
The carbon material of microstructure shown in Fig. 8.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to above embodiment.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in guarantor of the invention
Within the scope of shield.
Claims (10)
1. a kind of carbon materials preparation method for material, which is characterized in that the described method comprises the following steps: will be at least containing three alkynyls
Compound and catalyst are added in solvent, are reacted at a certain temperature and obtain the carbon material.
2. the method according to claim 1, wherein the compound of the alkynyl at least containing there are three is selected from and contains
The compound of three alkynyls, containing there are four the compound of alkynyl, containing there are five the compound of alkynyl or containing there are six the changes of alkynyl
Close one of object or multiple combinations.
Preferably, the alkynyl at least containing there are three in the compound of alkynyl is end alkynyl radical.
Preferably, described at least containing there are three the compounds of alkynyl to be selected from one or more of compound as described below group
It closes:
3. method according to claim 1 or 2, which is characterized in that the solvent is water, methylene chloride, chloroform, second
Acetoacetic ester, pyridine, tetrahydrofuran, toluene, methanol, ethyl alcohol, butanol, the tert-butyl alcohol, 1-Methyl-2-Pyrrolidone, benzene, two chloroethenes
Alkane, carbon tetrachloride, tetrachloromethane, triethylamine, ethylenediamine, hexamethylene, n-hexane, cyclohexanone, toluene cyclohexanone, acetone, methyl
Butanone, methylisobutylketone, petroleum ether, dimethylbenzene, pentane, hexane, octane, methyl acetate, ethyl acetate, propyl acetate, diformazan
Yl acetamide, dimethylformamide, glycol monoethyl ether, ethylene glycol monoethyl ether, propene carbonate, ethylene carbonate, methyl esters, 1,
4-fourth propyl ester, dimethyl carbonate, ethylene glycol monobutyl ether, acetonitrile, propionitrile, chlorobenzene, carbon disulfide, N, N- diethyl-1,3- the third two
Amine, 1,3- propane diamine, N, N- dimethyl -1,3- propane diamine, hempa, triethylene tetramine, hexamethylenetetramine, melamine,
One or more of dipropylenetriamine, tetramethylethylenediamine, dichloro-benzenes, ether etc. mixed solvent.
Preferably, the solvent is the mixed solvent of following two classes solvents:
The first kind is selected from least one of following solvents: water, methylene chloride, chloroform, ethyl acetate, tetrahydrofuran, first
Benzene, methanol, ethyl alcohol, butanol, the tert-butyl alcohol, 1-Methyl-2-Pyrrolidone, benzene, dichloroethanes, carbon tetrachloride, tetrachloromethane, hexamethylene
Alkane, n-hexane, cyclohexanone, toluene cyclohexanone, acetone, espeleton, methylisobutylketone, petroleum ether, dimethylbenzene, pentane, hexane,
Octane, methyl acetate, ethyl acetate, propyl acetate, dimethyl acetamide, dimethylformamide, glycol monoethyl ether, ethylene glycol
Single ether, propene carbonate, ethylene carbonate, methyl esters, 1,4-fourth propyl ester, dimethyl carbonate, ethylene glycol monobutyl ether, acetonitrile, third
Nitrile, chlorobenzene, carbon disulfide, dichloro-benzenes, ether；
Second class is selected from least one of following solvents: pyridine, triethylamine, ethylenediamine, N, N- diethyl -1,3- propane diamine,
1,3- propane diamine, N, N- dimethyl -1,3- propane diamine, hempa, triethylene tetramine, hexamethylenetetramine, melamine, dipropyl
Alkene triamine, tetramethylethylenediamine.
Preferably, the dosage volume ratio of first kind solvent and the second class solvent is 10000:1 to 1:10000；It is preferred that 100:1 to 1:
10。
4. method according to claim 1-3, which is characterized in that it is described reaction in gas shield atmosphere into
Row, the gas are one or more of nitrogen, argon gas, helium, ammonia, hydrogen, air, oxygen mixed gas.
5. method according to claim 1-4, which is characterized in that the pattern of the catalyst is nanometer rods, receives
One or more of rice noodles, nano particle, nanometer sheet.
6. method according to claim 1-5, which is characterized in that the catalyst is copper, copper alloy, copper alloy
One or more of compound, copper compound.
Preferably, the copper alloy be copper and metallic aluminium, iron, zinc, manganese, cobalt, nickel, chromium, gold, platinum, silver, tin, titanium, germanium, zirconium, niobium,
The alloy of one or more of molybdenum, ruthenium, cadmium, indium, antimony, tantalum, lead.
Preferably, the copper compound is copper oxide, cuprous oxide, copper dioxide, copper sulfide, cuprous sulfide, Kocide SD, grass
One or more of sour copper, copper chloride, stannous chloride, cupric phosphate.
Preferably, the copper alloyed compound is the oxide of copper alloy, sulfide, halide, sulphate, phosphoric acid chemical combination
One or more of object or hydroxide.
Preferably, the copper alloy in the copper alloyed compound be copper and metallic aluminium, iron, zinc, manganese, cobalt, nickel, chromium, gold, platinum, silver,
The alloy of one or more of tin, titanium, germanium, zirconium, niobium, molybdenum, ruthenium, cadmium, indium, antimony, tantalum, lead.
7. method according to claim 1-6, which is characterized in that described at least containing there are three the compounds of alkynyl
Mass ratio with solvent is 1:10000 to 1:1, preferably 1:1000 to 1:100.
Preferably, the mass ratio of the compound of alkynyl and catalyst at least containing there are three is 1:1000 to 1000:1；It is preferred that
For 1:100 to 100:1.
8. method according to claim 1-7, which is characterized in that the condition of the reaction can be pressurization, micro-
One or more of wave, infrared, ultrasonic, illumination, heating.
9. method according to claim 1-8, which is characterized in that the reaction temperature is -50 DEG C to 300 DEG C.
Preferably, the reaction time is 0.5 hour to 200 hours.
10. a kind of carbon material being prepared by the described in any item methods of claim 1-9.
Preferably, the carbon material has high conductivity.
Preferably, the carbon material has various microscopic appearances, for example, the microscopic appearance is nano particle, nano wire, nanometer
Piece, hollow nano-sphere, nm wall array, nano-wire array, solid nanospheres.
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| CN101125649A (en) * | 2007-09-22 | 2008-02-20 | 兰州大学 | Method for separating metallic single-wall carbon nano-tube |
| CN101774570A (en) * | 2010-01-27 | 2010-07-14 | 中国科学院化学研究所 | Method for preparing graphite alkyne film |
| CN102205959A (en) * | 2011-03-28 | 2011-10-05 | 中国科学院化学研究所 | Graphite alkene nanotube and preparation method thereof |
| CN102515146A (en) * | 2011-10-25 | 2012-06-27 | 合肥工业大学 | Catalytic graphitization method of polyvinyl tri(phenylethynyl)silane |
-
2017
- 2017-12-20 CN CN201711386613.3A patent/CN109941983B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125649A (en) * | 2007-09-22 | 2008-02-20 | 兰州大学 | Method for separating metallic single-wall carbon nano-tube |
| CN101774570A (en) * | 2010-01-27 | 2010-07-14 | 中国科学院化学研究所 | Method for preparing graphite alkyne film |
| CN102205959A (en) * | 2011-03-28 | 2011-10-05 | 中国科学院化学研究所 | Graphite alkene nanotube and preparation method thereof |
| CN102515146A (en) * | 2011-10-25 | 2012-06-27 | 合肥工业大学 | Catalytic graphitization method of polyvinyl tri(phenylethynyl)silane |
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