CN107311142A - A kind of method of the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping - Google Patents
A kind of method of the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping Download PDFInfo
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- CN107311142A CN107311142A CN201710639585.5A CN201710639585A CN107311142A CN 107311142 A CN107311142 A CN 107311142A CN 201710639585 A CN201710639585 A CN 201710639585A CN 107311142 A CN107311142 A CN 107311142A
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Abstract
The invention discloses a kind of method of the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping; this method be by organic sulfonate and/or organic phosphonate and oxygen-containing organic polymer by ground and mixed after; it is placed in protective atmosphere; it is carbonized at high temperature; carbonized product is by washing, drying; produce specific surface area high; it is provided simultaneously with the graphitized carbon of the Heteroatom doping of mesoporous and microcellular structure; this method is simple to operate, controllable without using solvent, yield height, content of heteroatoms; and production cost is greatly reduced, be conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of graphitized carbon, the high-specific surface area stone of more particularly to a kind of Heteroatom doping
The method of inkization carbon, and in particular to a kind of quick, convenient by organic molecule salt and organic polymer, under condition of no solvent
The method for preparing the high-specific surface area graphitized carbon material of rich Heteroatom doping；Belong to carbon material preparing technical field.
Background technology
Graphene is due to excellent conduction, heat conduction and mechanical property attention in recent years, in catalytic field, energy storage
Field and gas field of storage are extremely welcome.But preparation method complexity, the cost of graphene are high at present, significantly limit it
Application.Graphitized carbon has the design feature similar with graphene, and with excellent electric conductivity, thermal conductivity is most possible
Replace a kind of material of graphene.However, the preparation method of graphitized carbon is complicated at present, specific surface area is relatively low, and interlamellar spacing compared with
It is small, greatly limit its large-scale application in energy storage field.Heteroatom doping can significantly improve the electric conductivity of carbon material,
The specific surface area of carbon material is greatly improved, and expands its interlamellar spacing to a certain extent and enriches the species of its surface functional group,
So as to improve its chemical property and catalytic activity.
Preparing the method for graphitized carbon at present mainly has arc discharge method, laser ablation, chemical vapour deposition technique, electronics
The methods such as beam radiation method.According to the difference of used presoma, the shape such as nanotrees, nanobelt, nanometer sheet, Nano capsule
Graphitized carbon is successfully prepared.These methods mostly react complicated, react in a solvent, and need a point several steps to complete, than
Surface area it is low and can not Effective Regulation, interlamellar spacing is small.And due to the problem of containing carbon matrix precursor, the material of prepared carbon coating
Substantially can not adulterate hetero atom, and its electric conductivity needs further lifting.Due to prepared graphitized carbon specific surface area and
The uncontrollability of interlamellar spacing, this significantly limit its application in other various aspects.
The content of the invention
Big for there is energy consumption in the preparation process of graphitized carbon in the prior art, cost is high, and solvent usage amount is big, step
The defect such as cumbersome, the purpose of the present invention be to provide a kind of simple and convenient, cycle it is short, in the condition without using solvent
The method that next step prepares the high-specific surface area graphitized carbon of Heteroatom doping.
In order to realize above-mentioned technical purpose, the invention provides a kind of solvent-free quick Gao Bibiao for preparing Heteroatom doping
The method of area graphite carbon, this method is by grinding by organic sulfonate and/or organic phosphonate with oxygen-containing organic polymer
After mill mixing, it is placed in protective atmosphere, is carbonized at a temperature of 600~1400 DEG C, carbonized product is produced by washing, drying.
The preparation process of the graphitized carbon of the present invention is main to be come using organic molecule sulfonate and phosphonate as hetero atom
Source, template and graphitizer, under the high temperature conditions, organic molecule sulfonate and phosphonate are first rearranged, and are being had
The surface in situ of machine polymer generates uniform organic thin film, plays template action, oxygen-containing organic after high temperature cabonization
Polymer directly generates graphitized carbon, and the metal (such as sodium, potassium) that small molecule sulfonate and phosphonate are produced can effectively live
Graphitized carbon, increases its specific surface area and abundant surface functional group, and hetero atom in situ can expand its layer into graphite layers
Spacing, therefore, it is possible to obtain with high-specific surface area, and has the electric conductivity of the Heteroatom doping of abundant mesoporous and micropore simultaneously
Good graphitized carbon material.
The method of the high-specific surface area graphitized carbon for preparing Heteroatom doping of the present invention also includes following preferred scheme：
It is preferred that scheme, the organic sulfonate include benzene sulfonic acid sodium salt, sodium sulfanilate, DBSA
At least one in sodium, p-methyl benzenesulfonic acid potassium, Potassium dodecylbenzenesulfonate, neopelex, 2,4- diamino benzene sulfonic acid sodium
Kind.
It is preferred that scheme, the organic phosphonate includes at least one of sodium benzene phosphinate, phenyl-phosphonic acid potassium.
The organic sulfonate and organic phosphonate that the present invention is selected played in oxygen-containing organic polymer carbonisation three
Recast is with being that other organic salts and inorganic salts are difficult to replaces realization.Sulfur-bearing or phosphorous inorganic salts as etc. are difficult to play
Template action.
It is preferred that organic sulfonate and the constituent such as phosphate it is stable, can be effective and rich in elements such as nitrogen, sulphur, phosphorus
Adjust nitrogen content in graphitized carbon material and in the range of 0.1% to 10.8%, adjust the content of sulphur in 0.2% to 20% scope
Interior, phosphorus content is in the range of 0.1% to 6.5%.
It is preferred that scheme, the oxygen-containing organic polymer includes polydextrose (glucose monomer), poly- acetone, and (acetone is made single
Body), metacetaldehyde (acetaldehyde does monomer), poly- phenolic resin (phenol formaldehyde (PF) is monomer), PET (terephthaldehyde
At least one of sour ethylene glycol is monomer).These polymer are mainly comprising carbonyl, carboxyl, hydroxyl etc., the easy shape in carbonisation
Into porous carbon structure.
The gross mass of more preferably scheme, organic sulfonate and organic phosphonate is 1 with the mass ratio containing organic polymer:
0.5~1:20；More preferably it is 1:1~1:15；More preferably the gross mass of organic sulfonate and organic phosphonate with it is oxygen-containing organic
The mass ratio of polymer is 1:1.5~1:12.In the range of preferred mass ratio, the control of the amount of Heteroatom doping can be effectively controlled
System, so as to realize the regulation and control of interlamellar spacing and specific surface area.
It is preferred that scheme, the temperature of the carbonization is 650~1300 DEG C.
Heating rate is 1~20 DEG C/min in more preferably scheme, the carbonisation.
The time of the carbonization is 0.2~20h；More preferably 0.5~15h.
In the solution of the present invention, in carbonisation, 600~1400 DEG C are warming up to 1~20 DEG C/min heating rate
It is carbonized, carbonization time is 0.2~20h.
In the solution of the present invention, carbonized product is handled using deionized water or acid elution, and vacuum drying obtains graphitization
Carbon.
In the solution of the present invention, the graphitized carbon of preparation mainly includes micropore and mesoporous.
Compared with the prior art, the advantageous effects that technical scheme is brought：
1) method of the high-specific surface area graphitized carbon for preparing Heteroatom doping of the invention is made under condition of no solvent
It is standby, overcome hydro-thermal of the prior art and solvent-thermal method solvent consumption is big, the defect of environmental pollution.
2) method of the high-specific surface area graphitized carbon for preparing Heteroatom doping of the invention passes through step carbonization generation stone
Inkization carbon, short, simple to operate with flow, fast and efficiently feature, is conducive to industrialized production.
3) present invention is prepared for the high-specific surface area graphitized carbon material of Heteroatom doping first, by organic molecule sulfonic acid
Salt and phosphonate etc. are used as self-template, it is possible to achieve the Heteroatom doping of graphitized carbon, and heteroatomic content can be controlled, system
Specific surface area, the interlamellar spacing of standby graphitized carbon can regulate and control, and with abundant mesoporous and micropore, be effectively increased graphitization
Carbon conductive, enriches its surface texture, and it can be made to be widely used in the fields such as catalysis, energy storage and absorption.
Brief description of the drawings
【Fig. 1】It is the high-specific surface area graphitized carbon XRD obtained in embodiment 1；
【Fig. 2】It is the scanning electron microscope (SEM) photograph of the high-specific surface area graphitized carbon obtained in embodiment 1；
【Fig. 3】It is the transmission electron microscope picture of the high-specific surface area graphitized carbon obtained in embodiment 1；
【Fig. 4】It is the Raman figures of the high-specific surface area graphitized carbon obtained in embodiment 1；
【Fig. 5】It is the nitrogen adsorption desorption curve map of the high-specific surface area graphitized carbon obtained in embodiment 1；
【Fig. 6】It is the XPS survey figures of the high-specific surface area graphitized carbon obtained in embodiment 1.
Embodiment
Following examples are that, in order to which the present invention is explained in greater detail, these embodiments do not constitute any limitation to the present invention,
The present invention can be as described in the content of the invention either type implement.
Embodiment 1
1g metacetaldehyde yellow solid and 10g benzene sulfonic acid sodium salts are ground, are placed in porcelain boat, is sealed, argon gas is protected at 1000 DEG C
Lower calcining 2h, programming rate is 5 DEG C per minute, after having reacted, and is cooled down, and is washed, and dries, obtains 200mg or so sulphur atoms and mix
Miscellaneous high-specific surface area graphitized carbon.Fig. 1 is its XRD piece, it is observed that the height of the sulphur atom doping prepared by this method
Specific surface area graphitized carbon has the diffraction maximum of an obvious carbon in (001) crystal face.Fig. 2 is its stereoscan photograph, can be seen
The high-specific surface area graphitized carbon for going out obtained sulphur atom doping is made up of many Nano ultrathin thin slices.Fig. 3, which is shown, to be obtained
Sulphur atom doping high-specific surface area graphitized carbon high-resolution projection electron microscopic picture, its surface can also be observed that one layer
Obvious lattice fringe, illustrates that its degree of graphitization is high.Fig. 4 is the high-specific surface area graphitized carbon of obtained sulphur atom doping
Raman spectrum, wherein D peaks and G peaks can be significantly observed by curve, peak intensity ratio is 0.542, it was demonstrated that its height stone
The structure of inkization.Fig. 5 (left side) is the nitrogen adsorption desorption curve of obtained product, bent which show the adsorption desorption of type in VI
Line, indicates obtained material while having mesoporous and micropore characteristic.Specific surface area is 868.9m2g-1, embody and carry significantly
The specific surface area risen.Fig. 5 (right side) shows its pore size distribution curve, and its aperture is mainly distributed at 1.1nm and 3.9nm.Fig. 6 is
The XPS survey spectrograms of obtained material, can significantly be obtained in this material containing 2.64% element sulphur, sulphur therefrom
Atom doped structure.
Comparative example 1
1g benzene sulfonic acid sodium salts and 5g benzene sulfonic acid mixed grindings, are placed in tube furnace, argon at 800 DEG C are risen to 10 DEG C/min
2h is calcined in gas atmosphere, does not have material remaining in porcelain boat after having reacted.Illustrate that the inventive method is unsuitable for using organic molecule
Salt prepares graphitized carbon with organic molecule.
Comparative example 2
1g Na2SO4With 5g polydextrose mixed grindings, it is placed in tube furnace, is risen under 10 DEG C/min programming rates
2h is calcined in argon gas atmosphere to 800 DEG C, black solid is obtained after having reacted, through its degree of graphitization of Raman spectras
It is very low, produced without graphitized carbon.Illustrate that the inventive method is unsuitable for preparing graphitized carbon material containing na oxide.
With 1g Na3PO4Replace Na2SO4Use, produced also without graphitized carbon.
Embodiment 2
By 500mg neopelexes and the poly- acetone mixed grindings of 2000mg, 1100 DEG C are placed in tube furnace
Lower reaction 2h is calcined in argon gas atmosphere, heating rate is 2 DEG C/min, obtains about 50mg products, the graphitization of obtained sulfur doping
The specific surface area of carbon is 968.5m2g-1, its sulfur content is 3.2%.
Comparative example 3
1g neopelexes and 2g PET mixed grindings are placed in tube furnace
2h is calcined at 400 DEG C in nitrogen atmosphere, heating rate is 2 DEG C/min, and what is obtained after reaction is agraphitic carbon.Illustrate reaction temperature
Spend low, it is impossible to obtain graphitized carbon.
Embodiment 3
2g sodium benzene phosphinates and 8g poly- acetone mixed grindings are placed in tube furnace, with 10 DEG C/min programming rate liters
The high-specific surface area graphitized carbon that about 100mg phosphorus dopings are obtained after 1h, reaction, XPS knots are calcined into 1200 DEG C of argon gas atmospheres
Fruit shows that its phosphorus content is 8.6%, and specific surface area is 687.6m2g-1。
Embodiment 4
2g neopelexes and 10g poly- phenolic resin mixed grindings are placed in tube furnace, with 12 DEG C/
To 900 DEG C under min programming rates, calcined in argon gas atmosphere and obtain about 400mg graphitized carbon materials, wherein sulphur after 8h, reaction
Content is 1.5%, and its specific surface area is 498.6m2g-1。
Comparative example 4
100mg dodecyl sodium sulfates and 10g metacetaldehyde mixed grindings are placed in tube furnace, in 5 DEG C/min liters
1200 DEG C are risen under warm speed, 4h is calcined in argon gas atmosphere, graphitized carbon is not obtained.Illustrate organic molecule salt content too
It is low, it is unfavorable for the formation of graphitized carbon.
Embodiment 5
2g sodium sulfanilates and 6g metacetaldehyde mixed grindings are placed in tube furnace, are risen to 5 DEG C/min
800 DEG C, calcined in argon gas atmosphere and obtain the sulfur and nitrogen co-doped graphitized carbons of about 400mg after 1h, reaction, wherein sulfur content is
5%, nitrogen content is 4%, and its specific surface area is 888.6m2g-1。
Claims (10)
1. a kind of method of the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping, it is characterised in that：It is organic
After sulfonate and/or organic phosphonate and oxygen-containing organic polymer are by ground and mixed, it is placed in protective atmosphere, 600~
It is carbonized at a temperature of 1400 DEG C, carbonized product is produced by washing, drying.
2. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 1,
It is characterized in that：The organic sulfonate include benzene sulfonic acid sodium salt, sodium sulfanilate, neopelex, to toluene
At least one of potassium sulfonate, Potassium dodecylbenzenesulfonate, neopelex, 2,4- diamino benzene sulfonic acid sodium；It is described to have
Organic phosphonates include at least one of sodium benzene phosphinate, phenyl-phosphonic acid potassium.
3. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 1,
It is characterized in that：The oxygen-containing organic polymer includes polydextrose, poly- acetone, metacetaldehyde, poly- phenolic resin, poly- terephthaldehyde
At least one of sour second diester.
4. the solvent-free quick high-specific surface area graphitization for preparing Heteroatom doping according to any one of claims 1 to 3
The method of carbon, it is characterised in that：The gross mass of organic sulfonate and organic phosphonate is 1 with the mass ratio containing organic polymer:
0.5~1:20.
5. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 4,
It is characterized in that：The mass ratio of the gross mass of organic sulfonate and organic phosphonate and oxygen-containing organic polymer is 1:1~1:15.
6. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 5,
It is characterized in that：The mass ratio of the gross mass of organic sulfonate and organic phosphonate and oxygen-containing organic polymer is 1:1.5~1:
12。
7. the solvent-free quick high-specific surface area stone for preparing Heteroatom doping according to claims 1 to 3,5,6 any one
The method of inkization carbon, it is characterised in that：The temperature of the carbonization is 650~1300 DEG C.
8. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 7,
It is characterized in that：Heating rate is 1~20 DEG C/min in the carbonisation.
9. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 7,
It is characterized in that：The time of the carbonization is 0.2~20h.
10. the method for the solvent-free quick high-specific surface area graphitized carbon for preparing Heteroatom doping according to claim 9,
It is characterized in that：The time of the carbonization is 0.5~15h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108636393A (en) * | 2018-05-14 | 2018-10-12 | 北京化工大学 | Method for preparing covalent organic polymer by utilizing reactive grinding and application |
| CN111943166A (en) * | 2020-07-17 | 2020-11-17 | 中国科学院兰州化学物理研究所 | Preparation of solvent-free hydrothermal carbon material |
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| CN106115633A (en) * | 2016-06-28 | 2016-11-16 | 湖北博凯医药科技有限公司 | A kind of method utilizing thionyl chloride tail gas of acyl chlorination synthesis sodium thiosulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636393A (en) * | 2018-05-14 | 2018-10-12 | 北京化工大学 | Method for preparing covalent organic polymer by utilizing reactive grinding and application |
| CN108636393B (en) * | 2018-05-14 | 2020-08-25 | 北京化工大学 | Method for preparing covalent organic polymer by utilizing reactive grinding and application |
| CN111943166A (en) * | 2020-07-17 | 2020-11-17 | 中国科学院兰州化学物理研究所 | Preparation of solvent-free hydrothermal carbon material |
| CN111943166B (en) * | 2020-07-17 | 2023-01-20 | 中国科学院兰州化学物理研究所 | Preparation of solvent-free hydrothermal carbon material |
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