CN104876216B - The method that Graphene is prepared using high molecular polymer conbustion synthesis - Google Patents
The method that Graphene is prepared using high molecular polymer conbustion synthesis Download PDFInfo
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Abstract
The invention provides a kind of method that utilization high molecular polymer conbustion synthesis prepare Graphene, methods described step is as follows：First, 10～65% magnesium powders are weighed according to mass percent and 35～90% high molecular polymer uniformly mixes；2nd, the mixture in step one is placed in protective atmosphere, is lighted with detonator or Resistant heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing；3rd, purified impurity of the removing containing magnesium of crude product powder for obtaining step 2, obtains pure Graphene.The Graphene that the present invention is obtained has special pattern, such as petal-shaped, accordion, hollow ball-shape, flakey etc., resulting Graphene or N doping or Fluorin doped or boron doping or boron are nitrogen co-doped, and the number of plies is below 10 layers, it is easy to industrialized production, can be applicable to the fields such as composite, energy-storage battery, ultracapacitor, electronic device, catalyst carrier, Sensitive Apparatus.
Description
Technical field
The invention belongs to material with carbon element technical field, is related to one kind and passes through SHS process by various high molecular polymers
The method that method prepares grapheme material.
Background technology
Graphene is referred to by sp2Only an atomic layer level thickness and the mono-layer graphite with cellular crystal structure of hydridization
Synusia.In single-layer graphene, each carbon atom passes through sp with the carbon atom of surrounding2Hydridization is into bond formed regular hexagon.Individual layer
The thickness of Graphene is only 0.335nm, is current most thin, most hard nano material known in the world.Graphene has excellent
Different mechanics, calorifics, optics and electric property.It is intensity and hardness highest material in known material, its tensile strength
125GPa and 1.1TPa is respectively with elastic modelling quantity；Room temperature thermal conductivity is 5 × 103W/m·K；The light transmittance of single-layer graphene is
97.7%, with the increase of the number of plies, it is seen that the light transmittance of light reduces 2.3% successively, its translucency can be matched in excellence or beauty with ITO；Electronics is moved
Shifting rate is up to 2 × 105cm2/ (Vs), electrical conductivity is up to 106S/m；Meanwhile, Graphene also have significant room temperature Hall effect,
Stable diracelectron structure.Therefore, Graphene is in ultracapacitor, electronic information, nano electron device, composite etc.
Field has a wide range of applications.The preparation method of Graphene has much at present, and main has：Mechanical stripping method, oxidation are also
Former method, epitaxial growth method and chemical meteorology deposition method (CVD) etc., but these methods have the pluses and minuses of oneself, for example：Machinery
The process is simple of the Graphene that stripping method is obtained, cost are relatively low, quality is good, thickness is little, but yield is too small, is not suitable for industrial metaplasia
Produce；The graphene oxide good dispersion that oxidation-reduction method is obtained, can be prepared on a large scale, but surface is contained oxygen-containing functional group etc. and lacked
Fall into so as to which excellent performance such as electric conductivity declines even to be lost；The Graphene quality that epitaxial growth method is obtained is good, can large area system
It is standby, but it is difficult to control to pattern, high cost；Graphene quality prepared by CVD is high, the number of plies is controllable, band gap is adjustable, but high cost,
Product needs transfer.In sum, develop a kind of simple to operate, Graphene quality for preparing preferably, be easy to industrial mass
The preparation technology of amount production is of great value.
The content of the invention
In order to develop, operating procedure is simple, save energy, raw material sources are wide, efficiency high, the stone for being easy to industrialized production
Black alkene preparation method, the invention provides a kind of method that utilization high molecular polymer conbustion synthesis prepare Graphene, using many
It is carbon source to plant high molecular polymer, prepares Graphene using burning synthesis method.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method that utilization high molecular polymer conbustion synthesis prepare Graphene, the preparation method are entered according to the following steps
OK：
First, 10～65% magnesium powders are weighed according to mass percent and 35～90% high molecular polymer uniformly mixes；
2nd, the mixture in step one is placed in protective atmosphere, is lighted with detonator or Resistant heating, burnt
Synthetic reaction, obtains the crude product powder of graphene-containing；
3rd, the crude product powder for obtaining step 2 pickling in the HCl/water solution that mass fraction is 10～37%, removes
Impurity containing magnesium, obtains pure Graphene.
In said method, the purity of the magnesium powder is 92～99.999%, and average particulate diameter is 0.02～5mm.
In said method, the purity of the high molecular polymer is 92～99.999%.
In said method, the high molecular polymer be high molecular polymer powder, high molecular polymer chopped strand or
High molecular polymer film, wherein：Powder average particulate diameter is 0.005～1mm；Chopped strand length is less than 10mm, diameter
0.0001～0.01mm；0.001～0.05mm of film thickness.
In said method, described protective atmosphere is Ar, He, CO2, one or more in CO gases.
In said method, the high molecular polymer is polyvinyl chloride, haloflex, Kynoar, poly- super chloroethene
It is alkene, polychlorobutadiene, hexachloro-benzene, phenolic resin, boron modified phenolic resin, borate, polyvinyl alcohol, polyvinyl acetate, poly-
Methyl methacrylate, Merlon, epoxy resin, PEO, polyformaldehyde, polyphenylene oxide, polyvinyl formal, poly- third
Olefin(e) acid, polyvinyl fluoride, polytrifluorochloroethylene, polytetrafluoroethylene (PTFE), polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, ureaformaldehyde tree
One or more in fat.It is when high molecular polymer is polyvinyl fluoride, polytrifluorochloroethylene, polytetrafluoroethylene (PTFE), resulting
Graphene of the product for Fluorin doped；When high molecular polymer is polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, gained
Graphene of the product for arriving for N doping；When high molecular polymer is boron modified phenolic resin, borate, resulting product
For boron doped Graphene；When high molecular polymer be polyacrylamide, polyacrylonitrile, the one kind or several in nylon 6, nylon66 fiber
Kind, with boron modified phenolic resin, borate in one or two mixtures when, resulting product is the nitrogen co-doped stone of boron
Black alkene.
The present invention has the advantages that：
(1) high molecular polymer low price, it is numerous in variety, be easy to storage transport；And some of them resin is providing carbon
The elements such as N, B, F can also be provided to be doped while source, a step obtains the Graphene for adulterating.
(2) Graphene that the present invention is obtained has special pattern, such as petal-shaped, accordion, hollow ball-shape, flakey
Deng, resulting Graphene or N doping or Fluorin doped or boron doping, and the number of plies is below 10 layers, is easy to industrialized production, can
It is applied to the fields such as composite, energy-storage battery, ultracapacitor, electronic device, catalyst carrier, Sensitive Apparatus.
Description of the drawings
Fig. 1 is the SEM figures of the Graphene that specific embodiment one is obtained；
Fig. 2 is the SEM figures of the Graphene that specific embodiment two is obtained；
Fig. 3 is the SEM figures of the Graphene that specific embodiment three is obtained；
Fig. 4 is the TEM figures of the Graphene that specific embodiment three is obtained.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, also including between each specific embodiment
Any combination, in order to help understand the present invention, with example, the invention will be further described below, protection scope of the present invention
It is defined by the claims.
Specific embodiment one：According to mass fraction weigh a diameter of 1mm, 16.1% magnesium powder, 83.9% polychlorostyrene second
Alkene powder, is sufficiently mixed, in CO2Under atmosphere, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain graphene-containing
Crude product powder, weighs the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 15%, then spend from
Sub- water is rinsed, and obtains pure graphene powder, and its SEM figure is as shown in Figure 1.
Specific embodiment two：According to mass fraction weigh a diameter of 0.5mm, 18.3% magnesium powder, 81.7% phenolic aldehyde
Toner, is sufficiently mixed, in CO2In atmosphere, lighted with detonator, carry out combustion synthesis reaction, obtain the thick of graphene-containing
Product powder, weighs the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 30%, is used after filtration again
Deionized water rinsing, obtains pure graphene powder, and its SEM figure is as shown in Figure 2.
Specific embodiment three：According to mass fraction weigh a diameter of 2mm, 22.4% magnesium powder, 77.6% gather super chlorine
Ethylene powder, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, lighted with resistance wire heating, carry out conbustion synthesis
Reaction, obtains the crude product powder of graphene-containing, is rushed with the HCl/water solution pickling that mass fraction is 20%, then deionized water
Wash, obtain pure graphene powder, its SEM schemes as shown in figure 3, TEM figures are as shown in Figure 4.
Specific embodiment four：According to mass fraction weigh a diameter of 2mm, 55% magnesium powder, 22% polyvinyl alcohol powder
End and 23% polyvinyl acetate powder, are sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out conbustion synthesis anti-
Should, the crude product powder of graphene-containing is obtained, the crude product powder of graphene-containing is taken, it is molten with the HCl/water that mass fraction is 30%
Liquid pickling, then deionized water flushing, obtain pure graphene powder.
Specific embodiment five：According to mass fraction weigh a diameter of 5mm, 58% magnesium powder, 18% polyvinyl alcohol contracting
Formaldehyde powder, 10% Phenolic resin powder and 14% polyvinyl butyral powder end, are sufficiently mixed, in Ar and CO2Respectively account for
In 50% mixed gas, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing,
The crude product powder of graphene-containing is taken, is rinsed with the HCl/water solution pickling that mass fraction is 30%, then deionized water, is obtained
Pure graphene powder.
Specific embodiment six：According to mass fraction weigh a diameter of 0.05mm, 31.2% magnesium powder, 68.8% poly- third
Alkene nitrile chopped strand, is sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain containing stone
The crude product powder of black alkene, takes the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 30%, then uses
Deionized water rinsing, obtains the graphene powder of N doping.
Specific embodiment seven：According to mass fraction weigh a diameter of 0.02mm, 34.7% magnesium powder, 65.3% nylon
6 chopped strands, are sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain graphene-containing
Crude product powder, take the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 36%, then spend from
Sub- water is rinsed, and obtains the graphene powder of N doping.
Specific embodiment eight：According to mass fraction weigh a diameter of 0.05mm, 40.3% magnesium powder, 59.7% poly- third
Acrylamide film, is sufficiently mixed, in CO2In gas, ignited with detonator, carry out combustion synthesis reaction, obtain graphene-containing
Crude product powder, takes the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 30%, then uses deionization
Water is rinsed, and obtains the graphene powder of N doping.
Specific embodiment nine：According to mass fraction weigh a diameter of 0.02mm, 40% magnesium powder, 33% nylon 6 it is short
Fiber, 27% polyacrylamide film are cut, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, with resistance wire plus
Focus fires, and carries out combustion synthesis reaction, obtains the crude product powder of graphene-containing, takes the crude product powder of graphene-containing, use matter
The HCl/water solution pickling that fraction is 37% is measured, then deionized water is rinsed, and obtains the graphene powder of N doping.
Specific embodiment ten：A diameter of 0.05mm, 15.2% magnesium powder, 84.8% boron are weighed according to mass fraction to change
Property Phenolic resin powder, is sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction, contained
The crude product powder of Graphene, takes the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 30%, then
Deionized water is rinsed, and obtains boron doped graphene powder.
Specific embodiment 11：According to mass fraction weigh a diameter of 0.02mm, 25.7% magnesium powder, 40.1% it is poly-
Acrylonitrile chopped strand, 34.2% boron modified phenolic resin powder, are sufficiently mixed, in Ar and CO250% gaseous mixture is accounted for respectively
In body, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, take graphene-containing
Crude product powder, is rinsed with the HCl/water solution pickling that mass fraction is 37%, then deionized water, obtains boron nitrogen co-doped
Graphene powder.
Specific embodiment 12：According to mass fraction weigh a diameter of 0.1mm, 32.4% magnesium powder, 67.6% it is poly-
Tetrafluoroethene film, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, lighted with resistance wire heating, burnt
Synthetic reaction, obtains the crude product powder of graphene-containing, takes the crude product powder of graphene-containing, is 36% with mass fraction
HCl/water solution pickling, then deionized water flushing, obtain the graphene powder of Fluorin doped.
Specific embodiment 13：According to mass fraction weigh a diameter of 1.5mm, 20.7% magnesium powder, 79.3% it is poly-
Fluoroethylene film, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, with detonator, carry out combustion synthesis reaction,
The crude product powder of graphene-containing is obtained, the crude product powder of graphene-containing is taken, with the HCl/water solution acid that mass fraction is 20%
Wash, then deionized water is rinsed, and obtains the graphene powder of Fluorin doped.
Specific embodiment 14：According to mass fraction weigh a diameter of 1.0mm, 35% magnesium powder, 40% poly- fluorine second
Alkene film, 25% polytetrafluoroethylene film, are sufficiently mixed, in CO2In gas, with detonator, combustion synthesis reaction is carried out, is obtained
To the crude product powder of graphene-containing, the crude product powder of graphene-containing is taken, with the HCl/water solution acid that mass fraction is 25%
Wash, then deionized water is rinsed, and obtains the graphene powder of Fluorin doped.
Specific embodiment 15：According to mass fraction weigh a diameter of 0.5mm, 57.1% magnesium powder, 42.9% urea
Urea formaldehyde powder, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, lighted with resistance wire heating, carry out burning conjunction
Into reaction, the crude product powder of graphene-containing is obtained, take the crude product powder of graphene-containing, with the HCl that mass fraction is 37%
Aqueous solution pickling, then deionized water flushing, obtain the graphene powder of N doping.
Specific embodiment 16：According to mass fraction weigh a diameter of 2mm, 34.7% magnesium powder, 65.3% nylon
66 chopped strands, are sufficiently mixed, in He and CO2Respectively account in 50% mixed gas, with detonator, carry out combustion synthesis reaction,
The crude product powder of graphene-containing is obtained, the crude product powder of graphene-containing is taken, with the HCl/water solution acid that mass fraction is 25%
Wash, then deionized water is rinsed, and obtains the graphene powder of N doping.
Specific embodiment 17：According to mass fraction weigh a diameter of 0.02mm, 29.2% magnesium powder, 70.8% it is poly-
CTFE powder, is sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction, contained
The crude product powder of Graphene, takes the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 15%, then
Deionized water is rinsed, and obtains the graphene powder of Fluorin doped.
Specific embodiment 18：According to mass fraction weigh a diameter of 0.3mm, 16.7% magnesium powder, 83.3% it is poly-
Phenylate powder, is sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction, obtain graphene-containing
Crude product powder, take the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 10%, then spend from
Sub- water is rinsed, and obtains graphene powder.
Specific embodiment 19：According to mass fraction weigh a diameter of 0.1mm, 21.4% magnesium powder, 78.6% it is poly-
Polycarbonate powder, is sufficiently mixed, in Ar and CO2Respectively account in 50% mixed gas, lighted with resistance wire heating, carry out burning conjunction
Into reaction, the crude product powder of graphene-containing is obtained, take the crude product powder of graphene-containing, with the HCl that mass fraction is 20%
Aqueous solution pickling, then deionized water flushing, obtain graphene powder.
Specific embodiment 20：According to mass fraction weigh a diameter of 0.05mm, 63.2% magnesium powder, 36.8% it is poly-
Vinyl alcohol powder, is sufficiently mixed, in CO2In gas, lighted with detonator, carry out combustion synthesis reaction, obtain graphene-containing
Crude product powder, takes the crude product powder of graphene-containing, with the HCl/water solution pickling that mass fraction is 20%, then uses deionization
Water is rinsed, and obtains graphene powder.
Specific embodiment 21：According to mass fraction weigh a diameter of 0.05mm, 32.4% magnesium powder, 67.6%
Polymethylmethacrylate powder, is sufficiently mixed, in CO2In gas, lighted with resistance wire heating, carry out combustion synthesis reaction,
The crude product powder of graphene-containing is obtained, the crude product powder of graphene-containing is taken, with the HCl/water solution acid that mass fraction is 30%
Wash, then deionized water is rinsed, and obtains graphene powder.
Claims (8)
1. a kind of method that utilization high molecular polymer conbustion synthesis prepare Graphene, it is characterised in that methods described step is such as
Under：
First, 10～65% magnesium powders are weighed according to mass percent and 35～90% high molecular polymer uniformly mixes；
2nd, the mixture in step one is placed in protective atmosphere, is lighted with detonator or Resistant heating, carry out conbustion synthesis
Reaction, obtains the crude product powder of graphene-containing；
3rd, the crude product powder for obtaining step 2 pickling in the HCl/water solution that mass fraction is 10～37%, removes containing magnesium
Impurity, obtain pure Graphene；
Wherein, the high molecular polymer is boron modified phenolic resin, borate, polyvinyl fluoride, polytrifluorochloroethylene, polytetrafluoro
One or more in ethene, polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, Lauxite.
2. the method that utilization high molecular polymer conbustion synthesis according to claim 1 prepare Graphene, it is characterised in that
The purity of the magnesium powder is 92～99.999%, and average particulate diameter is 0.02～5mm.
3. the method that utilization high molecular polymer conbustion synthesis according to claim 1 prepare Graphene, it is characterised in that
The purity of the high molecular polymer is 92～99.999%.
4. the method that the utilization high molecular polymer conbustion synthesis according to claim 1 or 3 prepare Graphene, its feature exist
In the high molecular polymer be high molecular polymer powder, high molecular polymer chopped strand or high molecular polymer film.
5. the method that utilization high molecular polymer conbustion synthesis according to claim 4 prepare Graphene, it is characterised in that
The high molecular polymer powder average particulate diameter is 0.005～1mm.
6. the method that utilization high molecular polymer conbustion synthesis according to claim 4 prepare Graphene, it is characterised in that
The high molecular polymer chopped strand length is less than 10mm, 0.0001～0.01mm of diameter.
7. the method that utilization high molecular polymer conbustion synthesis according to claim 4 prepare Graphene, it is characterised in that
0.001～0.05mm of the high molecular polymer film thickness.
8. the method that utilization high molecular polymer conbustion synthesis according to claim 1 prepare Graphene, it is characterised in that
The protective atmosphere is Ar, He, CO2, one or more in CO gases.
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| CN105600780B (en) * | 2016-02-29 | 2017-12-19 | 昆明物理研究所 | The cofiring preparation method of chlorine doped graphene quantum dot |
| CN106115675B (en) | 2016-06-24 | 2018-04-17 | 中国科学院电工研究所 | A kind of method for preparing mesoporous graphene |
| CN107628599B (en) * | 2016-07-14 | 2020-04-28 | 南京理工大学 | Preparation method of graphene |
| CN107324310A (en) * | 2017-07-07 | 2017-11-07 | 西安建筑科技大学 | A kind of preparation method of nano-sized carbon |
| CN109319765B (en) * | 2017-07-31 | 2022-06-07 | 哈尔滨工业大学 | Preparation method and application of graphene synthesized by biomass combustion |
| CN109319764B (en) * | 2017-07-31 | 2022-05-06 | 哈尔滨工业大学 | Preparation method and application of lignin combustion synthesis graphene |
| CN108788135B (en) * | 2018-06-26 | 2021-02-26 | 中国科学院兰州化学物理研究所 | Method for in-situ self-generation of graphene/titanium shell-core structure material |
| CN111892041A (en) * | 2020-08-27 | 2020-11-06 | 北京理工大学 | Preparation method of graphene powder |
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| WO2012145605A1 (en) * | 2011-04-22 | 2012-10-26 | The Regents Of The University Of California | Graphene based optical modulator |
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