CN104876216A - Method for preparing graphene through combustion synthesis by virtue of macromolecular polymers - Google Patents
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Abstract
The invention provides a method for preparing graphene through combustion synthesis by virtue of macromolecular polymers. The method for preparing graphene through combustion synthesis by virtue of the macromolecular polymers comprises the following steps: firstly, weighing 10-65wt% of magnesium powder and 35-90% of macromolecular polymers, and uniformly mixing; secondly, putting the mixture obtained in the step 1 in protective atmosphere, igniting the mixture by adopting an igniting agent or through resistance wire heating, and carrying out combustion synthesis reaction, so that crude product powder containing graphene is obtained; and thirdly, purifying the crude product powder obtained in the step 2 for removing impurities containing magnesium, so that pure graphene is obtained. The obtained graphene has special morphologies such as a petal shape, a fold shape, a hollow spherical shape and a scaly shape, the obtained graphene is doped with nitrogen, or fluorine, or boron, or boron and nitrogen, and number of layers is less then 10, so that the obtained graphene is convenient for industrial production and can be applied to the fields of composite materials, energy storage batteries, super capacitors, electronic devices, catalyst carriers, sensitive devices and the like.
Description
Technical field
The invention belongs to carbon material technical field, relate to a kind of method being prepared grapheme material by multiple high molecular polymer by self-propagating high-temperature synthesis.
Background technology
Graphene refers to by sp
2only the having an atomic layer level thickness and there is the mono-layer graphite synusia of cellular crystalline structure of hydridization.In single-layer graphene, the carbon atom of each carbon atom and surrounding passes through sp
2hydridization becomes key to form regular hexagon.The thickness of single-layer graphene is only 0.335nm, is thin, the hardest known in the world at present nano material.Graphene has excellent mechanics, calorifics, optics and electric property.It is intensity and the highest material of hardness in known material, and its tensile strength and Young's modulus are respectively 125GPa and 1.1TPa; Room temperature thermal conductivity is 5 × 10
3w/mK; The transmittance of single-layer graphene is 97.7%, and along with the increase of the number of plies, the transmittance of visible ray reduces 2.3% successively, and its light transmission can match in excellence or beauty with ITO; Electronic mobility can reach 2 × 10
5cm
2/ (Vs), specific conductivity can reach 10
6s/m; Meanwhile, Graphene also has significant room temperature Hall effect, stable dirac electron structure.Therefore, Graphene has a wide range of applications in fields such as ultracapacitor, electronic information, nano electron device, matrix materials.The preparation method of current Graphene has a lot, main has: mechanically peel method, oxidation reduction process, epitaxial growth method and chemical meteorology deposition method (CVD) etc., but these methods have the relative merits of oneself, such as: the technique of the Graphene that mechanically peel method obtains is simple, cost compared with low, quality good, thickness is little, but output is too small, be not suitable for suitability for industrialized production; The graphene oxide good dispersity that oxidation reduction process obtains, can prepare on a large scale, but surface is containing defects such as oxygen-containing functional groups, and the performance making it excellent is even lost as electroconductibility declines; The Graphene quality that epitaxial growth method obtains is good, can big area preparation, but it is high to be difficult to control pattern, cost; Graphene quality prepared by CVD is high, the number of plies is controlled, band gap is adjustable, but cost is high, product needs transfer.In sum, it is of great value for developing a kind of Graphene quality simple to operate, preparation preparation technology that is better, that be convenient to industrialized mass.
Summary of the invention
In order to development and operation technique is simple, save the energy, raw material sources is wide, efficiency is high, be convenient to the graphene preparation method of suitability for industrialized production, the invention provides a kind of method utilizing high molecular polymer conbustion synthesis to prepare Graphene, adopt multiple high molecular polymer to be carbon source, utilize burning synthesis method to prepare Graphene.
The object of the invention is to be achieved through the following technical solutions:
Utilize high molecular polymer conbustion synthesis to prepare a method for Graphene, this preparation method carries out according to the following steps:
One, the high molecular polymer Homogeneous phase mixing of 10 ~ 65% magnesium powder and 35 ~ 90% is taken according to mass percent;
Two, the mixture in step one is placed in protective atmosphere, lights with detonator or Resistant heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing;
Three, the HCl aqueous acid medium that crude product powder step 2 obtained is 10 ~ 37% at massfraction is washed, and removing, containing the impurity of magnesium, obtains pure Graphene.
In aforesaid method, the purity of described magnesium powder is 92 ~ 99.999%, and average particulate diameter is 0.02 ~ 5mm.
In aforesaid method, the purity of described high molecular polymer is 92 ~ 99.999%.
In aforesaid method, described high molecular polymer is 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; Film thickness 0.001 ~ 0.05mm.
In aforesaid method, described protective atmosphere is Ar, He, CO
2, one or more in CO gas.
In aforesaid method, described high molecular polymer is one or more in polyvinyl chloride, chlorinatedpolyethylene, polyvinylidene difluoride (PVDF), poly-super vinylchlorid, sovprene, Perchlorobenzene, resol, boron modified phenolic resin, boric acid ester, polyvinyl alcohol, polyvinyl acetate (PVA), polymethylmethacrylate, polycarbonate, epoxy resin, polyethylene oxide, polyoxymethylene, polyphenylene oxide, polyvinyl formal, polyacrylic acid, fluorinated ethylene propylene, voltalef, tetrafluoroethylene, polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, urea-formaldehyde resin.When high molecular polymer is fluorinated ethylene propylene, voltalef, tetrafluoroethylene, the product obtained is the Graphene of Fluorin doped; When high molecular polymer is polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, the product obtained is the Graphene of N doping; When high molecular polymer is boron modified phenolic resin, boric acid ester, the product obtained is boron doped Graphene; When high molecular polymer is one or more in polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, during with one or both mixtures in boron modified phenolic resin, boric acid ester, the product obtained is the nitrogen co-doped Graphene of boron.
The present invention has following beneficial effect:
(1) high molecular polymer low price, numerous in variety, be convenient to store transport; And some of them resin also can provide the elements such as N, B, F to adulterate while providing carbon source, a step obtains the Graphene adulterated.
(2) Graphene that the present invention obtains has special pattern, as petal-shaped, accordion, hollow ball-shape, flakey etc., the Graphene obtained or N doping or Fluorin doped or boron doping, and the number of plies is below 10 layers, be convenient to suitability for industrialized production, can be applicable to the fields such as matrix material, energy-storage battery, ultracapacitor, electron device, support of the catalyst, susceptible device susceptor.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the Graphene that embodiment one obtains;
Fig. 2 is the SEM figure of the Graphene that embodiment two obtains;
Fig. 3 is the SEM figure of the Graphene that embodiment three obtains;
Fig. 4 is the TEM figure of the Graphene that embodiment three obtains.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment; also comprise the arbitrary combination between each embodiment; in order to help to understand the present invention, the invention will be further described below to use example, and protection scope of the present invention is limited by claims.
Embodiment one: taking diameter according to massfraction is 1mm, the magnesium powder of 16.1%, the polyvinyl chloride powder of 83.9%, fully mixes, at CO
2under atmosphere, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, take the crude product powder of graphene-containing, is the HCl solution acid pickling of 15% with massfraction, use deionized water rinsing again, obtain pure graphene powder, its SEM schemes as shown in Figure 1.
Embodiment two: taking diameter according to massfraction is 0.5mm, the magnesium powder of 18.3%, the Phenolic resin powder of 81.7%, fully mixes, at CO
2in atmosphere, light with detonator, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, take the crude product powder of graphene-containing, be the HCl solution acid pickling of 30% with massfraction, after filtration, use deionized water rinsing again, obtain pure graphene powder, its SEM schemes as shown in Figure 2.
Embodiment three: taking diameter according to massfraction is 2mm, the magnesium powder of 22.4%, the poly-super vinylchlorid powder of 77.6%, fully mixes, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, with the HCl solution acid pickling that massfraction is 20%, then use deionized water rinsing, obtain pure graphene powder, its SEM schemes as shown in Figure 3, and TEM figure as shown in Figure 4.
Embodiment four: taking diameter according to massfraction is 2mm, the magnesium powder of 55%, the pva powder of 22% and 23% polyvinyl acetate (PVA) powder, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 30% with massfraction, use deionized water rinsing again, obtain pure graphene powder.
Embodiment five: according to massfraction take diameter be 5mm, 58% magnesium powder, the polyvinyl formal powder of 18%, the Phenolic resin powder of 10% and 14% polyvinyl butyral powder end, fully mix, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 30% with massfraction, use deionized water rinsing again, obtain pure graphene powder.
Embodiment six: taking diameter according to massfraction is 0.05mm, the magnesium powder of 31.2%, the polyacrylonitrile chopped strand of 68.8%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 30% with massfraction, use deionized water rinsing again, obtain the graphene powder of N doping.
Embodiment seven: taking diameter according to massfraction is 0.02mm, the magnesium powder of 34.7%, nylon 6 chopped strand of 65.3%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 36% with massfraction, use deionized water rinsing again, obtain the graphene powder of N doping.
Embodiment eight: taking diameter according to massfraction is 0.05mm, the magnesium powder of 40.3%, the polyacrylamide film of 59.7%, fully mixes, at CO
2in gas, ignite with detonator, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, be the HCl solution acid pickling of 30% with massfraction, then use deionized water rinsing, obtain the graphene powder of N doping.
Embodiment nine: according to massfraction take diameter be 0.02mm, 40% magnesium powder, nylon 6 chopped strand of 33%, the polyacrylamide film of 27%, fully mix, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 37% with massfraction, use deionized water rinsing again, obtain the graphene powder of N doping.
Embodiment ten: taking diameter according to massfraction is 0.05mm, the magnesium powder of 15.2%, the boron modified phenolic resin powder of 84.8%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 30% with massfraction, use deionized water rinsing again, obtain boron doped graphene powder.
Embodiment 11: according to massfraction take diameter be 0.02mm, 25.7% magnesium powder, the polyacrylonitrile chopped strand of 40.1%, the boron modified phenolic resin powder of 34.2%, fully mix, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, with the HCl solution acid pickling that massfraction is 37%, then use deionized water rinsing, obtain the graphene powder that boron is nitrogen co-doped.
Embodiment 12: taking diameter according to massfraction is 0.1mm, the magnesium powder of 32.4%, the polytetrafluoroethylene film of 67.6%, fully mixes, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 36% with massfraction, use deionized water rinsing again, obtain the graphene powder of Fluorin doped.
Embodiment 13: taking diameter according to massfraction is 1.5mm, the magnesium powder of 20.7%, the polyvinyl fluoride thin film of 79.3%, fully mixes, at Ar and CO
2respectively account in the mixed gas of 50%, with detonator, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 20% with massfraction, use deionized water rinsing again, obtain the graphene powder of Fluorin doped.
Embodiment 14: according to massfraction take diameter be 1.0mm, 35% magnesium powder, the polyvinyl fluoride thin film of 40%, the polytetrafluoroethylene film of 25%, fully mix, at CO
2in gas, with detonator, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, be the HCl solution acid pickling of 25% with massfraction, then use deionized water rinsing, obtain the graphene powder of Fluorin doped.
Embodiment 15: taking diameter according to massfraction is 0.5mm, the magnesium powder of 57.1%, the urea-formaldehyde resin powder of 42.9%, fully mixes, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 37% with massfraction, use deionized water rinsing again, obtain the graphene powder of N doping.
Embodiment 16: taking diameter according to massfraction is 2mm, the magnesium powder of 34.7%, the nylon66 fiber chopped strand of 65.3%, fully mixes, at He and CO
2respectively account in the mixed gas of 50%, with detonator, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 25% with massfraction, use deionized water rinsing again, obtain the graphene powder of N doping.
Embodiment 17: taking diameter according to massfraction is 0.02mm, the magnesium powder of 29.2%, the voltalef powder of 70.8%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 15% with massfraction, use deionized water rinsing again, obtain the graphene powder of Fluorin doped.
Embodiment 18: taking diameter according to massfraction is 0.3mm, the magnesium powder of 16.7%, the polyphenylene ether powder of 83.3%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, be the HCl solution acid pickling of 10% with massfraction, then use deionized water rinsing, obtain graphene powder.
Embodiment 19: taking diameter according to massfraction is 0.1mm, the magnesium powder of 21.4%, the polycarbonate powder of 78.6%, fully mixes, at Ar and CO
2respectively account in the mixed gas of 50%, light with resistance wire heating, carry out combustion synthesis reaction, obtaining the crude product powder of graphene-containing, get the crude product powder of graphene-containing, is the HCl solution acid pickling of 20% with massfraction, use deionized water rinsing again, obtain graphene powder.
Embodiment 20: taking diameter according to massfraction is 0.05mm, the magnesium powder of 63.2%, the pva powder of 36.8%, fully mixes, at CO
2in gas, light with detonator, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, be the HCl solution acid pickling of 20% with massfraction, then use deionized water rinsing, obtain graphene powder.
Embodiment 21: taking diameter according to massfraction is 0.05mm, the magnesium powder of 32.4%, the polymethylmethacrylate powder of 67.6%, fully mixes, at CO
2in gas, light with resistance wire heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing, get the crude product powder of graphene-containing, be the HCl solution acid pickling of 30% with massfraction, then use deionized water rinsing, obtain graphene powder.
Claims (9)
1. utilize high molecular polymer conbustion synthesis to prepare a method for Graphene, it is characterized in that described method steps is as follows:
One, the high molecular polymer Homogeneous phase mixing of 10 ~ 65% magnesium powder and 35 ~ 90% is taken according to mass percent;
Two, the mixture in step one is placed in protective atmosphere, lights with detonator or Resistant heating, carry out combustion synthesis reaction, obtain the crude product powder of graphene-containing;
Three, the HCl aqueous acid medium that crude product powder step 2 obtained is 10 ~ 37% at massfraction is washed, and removing, containing the impurity of magnesium, obtains pure Graphene.
2. the method utilizing high molecular polymer conbustion synthesis to prepare Graphene according to claim 1, it is characterized in that the purity of described magnesium powder is 92 ~ 99.999%, average particulate diameter is 0.02 ~ 5mm.
3. the method utilizing high molecular polymer conbustion synthesis to prepare Graphene according to claim 1, is characterized in that the purity of described high molecular polymer is 92 ~ 99.999%.
4. the high molecular polymer conbustion synthesis that utilizes according to claim 1 or 3 prepares the method for Graphene, it is characterized in that described high molecular polymer is high molecular polymer powder, high molecular polymer chopped strand or high molecular polymer film.
5. the method utilizing high molecular polymer conbustion synthesis to prepare Graphene according to claim 4, is characterized in that described high molecular polymer powder average particulate diameter is 0.005 ~ 1mm.
6. the method utilizing high molecular polymer burning conjunction ~ one-tenth to prepare Graphene according to claim 4, is characterized in that described high molecular polymer chopped strand length is less than 10mm, diameter 0.0001 ~ 0.01mm.
7. the method utilizing high molecular polymer conbustion synthesis to prepare Graphene according to claim 4, is characterized in that described high molecular polymer film thickness 0.001 ~ 0.05mm.
8. the high molecular polymer conbustion synthesis that utilizes according to claim 1 or 3 prepares the method for Graphene, it is characterized in that described high molecular polymer is polyvinyl chloride, chlorinatedpolyethylene, polyvinylidene difluoride (PVDF), poly-super vinylchlorid, sovprene, Perchlorobenzene, resol, boron modified phenolic resin, boric acid ester, polyvinyl alcohol, polyvinyl acetate (PVA), polymethylmethacrylate, polycarbonate, epoxy resin, polyethylene oxide, polyoxymethylene, polyphenylene oxide, polyvinyl formal, polyacrylic acid, fluorinated ethylene propylene, voltalef, tetrafluoroethylene, polyacrylamide, polyacrylonitrile, nylon 6, nylon66 fiber, one or more in urea-formaldehyde resin.
9. the method utilizing high molecular polymer conbustion synthesis to prepare Graphene according to claim 1, is characterized in that described protective atmosphere is Ar, He, CO
2, one or more in CO gas.
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| CN109319764A (en) * | 2017-07-31 | 2019-02-12 | 哈尔滨工业大学 | Lignin conbustion synthesis graphene preparation method and its application |
| CN111892041A (en) * | 2020-08-27 | 2020-11-06 | 北京理工大学 | Preparation method of graphene powder |
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| CN109319764A (en) * | 2017-07-31 | 2019-02-12 | 哈尔滨工业大学 | Lignin conbustion synthesis graphene preparation method and its application |
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| CN111892041A (en) * | 2020-08-27 | 2020-11-06 | 北京理工大学 | Preparation method of graphene powder |
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