CN102583343B - A kind of method preparing Graphene in enormous quantities - Google Patents
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- CN102583343B CN102583343B CN201210028332.1A CN201210028332A CN102583343B CN 102583343 B CN102583343 B CN 102583343B CN 201210028332 A CN201210028332 A CN 201210028332A CN 102583343 B CN102583343 B CN 102583343B
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Abstract
The present invention relates to a kind of method preparing Graphene in enormous quantities.The method comprises the oxidation of graphite, and oxygenant and reductive agent, at the common intercalation of oxidized graphite flake interlayer, expand while the vigorous reaction initiated oxidation graphite under specified temp and reduction three steps.The present invention has that expansion temperature is low, technique is simple, low raw-material cost, productive rate are higher, high repeatability and other advantages, be easy to realize producing in enormous quantities, and high performance composite, ultracapacitor, lithium ion battery can be widely used in, the field such as fuel cell and microelectronics, is with a wide range of applications.
Description
Technical field
The present invention relates to a kind of method preparing Graphene in enormous quantities, belong to chemical technology field.
Background technology
Grapheme material, due to the two dimensional crystal structure of its uniqueness, has excellent machinery, optics, electricity and chemical property, is with a wide range of applications in fields such as microtronics, matrix material, transparent conductive film and stored energies.From 2004 by since AndreGeim and the KonstantinNovoselov Late Cambrian of University of Manchester (see NovoselovKS, GeimAK, MorozovSV, JiangD, ZhangY, etal.Science, 2004,306,666), more and more be subject to the attention of scientific circles, and cause the climax of research Graphene in the world; Find that therefore two scientists of Graphene also win the Nobel Prize in physics in 2010 years the earliest.
But the prerequisite that Graphene excellent properties is achieved is extensive, the low cost preparation of grapheme material, therefore, the technology of preparing of Graphene is ready-made is the study hotspot of academia and engineering circles.Up to now, many physics and chemical process are used to prepare high-quality grapheme material, mainly comprise graphite oxide reduction method, micromechanics stripping method, chemical Vapor deposition process and epitaxial growth method etc. (see BergerC, SongZ, LiX.Science, 2006,312,1191.; TungVC, AllenMJ.NatureNanotechnology, 2009,4,25.; HernandezY, NicolosiV.NatureNanotechnology, 2008,3,563.; KimKS, ZhaoY.Nature, 2009,457,706.; LiX, CaiW.Science, 2009,324,1312.; ChoucairM, ThordarsonP.NatureNanotechnology, 2009,4,30.; CaiJ, RuffieuxP.Nature, 2010,466,470).Wherein, micromechanics stripping method refers to and is directly stripped down from larger crystal by graphene platelet; Epitaxial growth method refers to the Graphene becoming to have large conjugated system by chemical reaction by the molecule construction with benzene ring structure; Chemical Vapor deposition process is then remove Si by heating monocrystalline 6H-SiC, thus decomposites graphene sheet layer on monocrystalline (001) face; But all there is the high and poor controllability of cost in these three kinds of methods, is not suitable for preparing Graphene on a large scale.Graphite oxide reduction method refers to and is oxidized (strong acid strong oxidizer condition) Graphite Powder 99, obtains graphene oxide after supersound process; Again graphene oxide is prepared Graphene by the method for chemical reduction; Compared with first three methods, the major advantage of graphene oxide reduction method is that cost and energy consumption are low, and Graphene productive rate is high, and being one of graphene preparation method paid close attention to the most at present, is also one of approach most possibly realizing Graphene mass production.But the industrialized prerequisite of this method is the preparation in enormous quantities of graphene oxide; But graphene oxide is a kind of two-dimensional slice shape structure, its good film-forming property, good dispersity in water; And adopt the methods such as common suction filtration, centrifugal settling or evaporation to be all difficult to it to separate from the aqueous solution.Therefore, for the large-scale industry preparation of Graphene, this method cost is high, efficiency is low, is thus unfavorable for applying.
At present, the production in enormous quantities of graphite oxide causes researcher and pays close attention to widely.Wang Shimin etc. (see Wang Shimin, Wan Li, etc.A method for realizing large-scale preparation of monolayer oxidized graphene, CN101591014B) propose ultrasonic for graphite oxide stripping, then the graphite oxide flocculating settling after peeling off is carried out the method that mass obtains single-layer graphene oxide.But products obtained therefrom is graphene oxide, the further reduction of need just can be transformed into Graphene truly; In addition, in the method, the stripping of graphite oxide is still based upon on the basis of ultrasonic technique, because of the process of a ultrasonic stripping inherently length consuming time, does not thus inherently solve the problem of the production in enormous quantities of grapheme material.Chen Guohua etc. (see Chen Guohua, Fang Ming, Zhao Liping.Prepare a method for Graphene in enormous quantities, CN102167311A) propose employing graphite oxidation-flocculating settling-pyroprocessing three step and prepare Graphene in enormous quantities.But there is length consuming time in this method, graphene oxide needs through problems such as high temperature reductions equally, and the requirement of the method to equipment is high, is difficult to realize preparation in enormous quantities.
Prepare Graphene Problems existing in enormous quantities for existing, a kind of method preparing Graphene in a large number of simple and practical, economical and efficient is provided, thus solve the production in enormous quantities of Graphene, there is very important using value and academic significance.
Summary of the invention
In order to overcome the deficiency that prior art exists, the object of the present invention is to provide a kind of method preparing Graphene in a large number of simple and practical, economical and efficient, thus solve the production in enormous quantities of Graphene.
To achieve the above object of the invention, the technical solution used in the present invention is:
A kind of method preparing Graphene is in enormous quantities provided, it is characterized in that: the described step preparing Graphene in enormous quantities comprises: the 1) oxidation of graphite; 2) oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer; 3) expand while the vigorous reaction initiated oxidation graphite under specified temp and reduction.
Graphite Powder 99 is placed in the mixed solution of strong acid and strong oxidizer by the oxidation system of described graphite, be oxidized 0.1-120 hour at 25-100 DEG C after, and dilute with water, add a certain amount of hydrogen peroxide, filtered while hot, then use dilute hydrochloric acid and deionized water wash to neutral, obtain graphite oxide after drying.
Described strong acid is the one in the vitriol oil, concentrated nitric acid and perchloric acid, or their combination; Described strong oxidizer is the one in potassium permanganate, Potcrate, sodium chlorate, Potassium Persulphate, SODIUMNITRATE and potassium bichromate, or their combination.
Described oxygenant and reductive agent comprise in the step of the common intercalation of oxidized graphite flake interlayer: 1) 10 parts of graphite oxides being added 10-1000 part oxygenant mass percent concentration is the aqueous solution of 0.5-98%, room temperature is cooled to soak 0.01-120h at 0-100 DEG C after, after filtration, after vacuum-drying, obtain the graphite oxide containing oxygenant; 2) graphite oxide containing oxygenant is added in reductive agent, at 0-35 DEG C, soak 0.001-120h, after filtering, obtain the graphite oxide of oxygenant and reductive agent intercalation.
Described oxygenant is the one in nitric acid, sulfuric acid and perchloric acid, or their combination; Described reductive agent is the one in acetone, ethanol and methyl alcohol, or their combination.
Expanding while vigorous reaction initiated oxidation graphite under described specified temp with reduction is the graphite oxide of oxygenant and reductive agent intercalation is placed in temperature to process 0.001-120h higher than the atmosphere furnace of 50 DEG C, obtains the graphene powder of high loft.
Described atmosphere is the one in oxygen, air, nitrogen, argon gas, helium and hydrogen, or their combination.
Compared with prior art, the beneficial effect that the present invention obtains is: the small molecules that 1) violent oxidation-reduction reaction generates can make graphite oxide undergoes rapid expansion and peel off into graphene oxide, because its level of response is controlled, thus the extent of exfoliation of graphite oxide is controlled equally; 2) oxidation-reduction reaction can produce a large amount of heats simultaneously, makes the temperature of graphite oxide increase sharp; And under the synergy of heat and reductive agent, realize stripping and the reduction of graphite oxide simultaneously; 3) expansion temperature required for the present invention is low, technique simple, low raw-material cost, productive rate are higher, favorable reproducibility, is easy to realize producing in enormous quantities.Based on above-mentioned advantage, the grapheme material that the present invention prepares can be used for high performance composite, ultracapacitor, lithium ion battery, and the field such as fuel cell and microelectronics, is with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the FTIR spectrogram of the Graphene prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD spectra of the Graphene prepared by the embodiment of the present invention 1;
Fig. 3 is the Raman spectrogram of the Graphene prepared by the embodiment of the present invention 1;
Fig. 4 is the TEM spectrogram of the Graphene prepared by the embodiment of the present invention 1;
Fig. 5 is the TG spectrogram of the Graphene prepared by the embodiment of the present invention 1;
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The first step (oxidation of graphite): be that 98% vitriol oil mixing is placed in ice bath by 10g graphite, 230mL mass percent concentration, stir and make it mix, then, take 40g potassium permanganate and add above-mentioned mixed solution, react 2h under 35 DEG C of conditions; Adding the hydrogen peroxide of 100mL after 500mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains is added the nitric acid that 100g mass percent concentration is 90%, be cooled to room temperature soak 2h at 35 DEG C after, after filtration, obtain containing nitric acid graphite oxide after vacuum-drying; 2) graphite oxide containing nitric acid is added in acetone, at 25 DEG C, soak 1h, after filtering, obtain the graphite oxide of nitric acid and acetone intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the air atmosphere stove that the nitric acid obtain 10g step 2 and the graphite oxide of acetone intercalation are placed in 100 DEG C processes 0.01h, obtain the graphene powder of black, high loft.
The specific surface area of the graphene powder of gained is 421m2/g; Its FT-IR, XRD, Raman, TEM and TG spectrogram as Fig. 1,2,3, shown in 4 and 5.
Embodiment 2
The first step (oxidation of graphite): be that 90% vitriol oil mixing is placed in ice bath by 10g graphite, 100mL mass percent concentration, stirring makes it mix, then, take 10g potassium bichromate and add above-mentioned mixed solution, under 25 DEG C of conditions, react 0.1h; After 100mL water is added above-mentioned reaction system, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains is added the nitric acid that 10g mass percent concentration is 0.5%, be cooled to room temperature soak 0.01h at 0 DEG C after, after filtration, obtain containing nitric acid graphite oxide after vacuum-drying; 2) graphite oxide containing nitric acid is added in acetone, at 0 DEG C, soak 0.001h, after filtering, obtain the graphite oxide of nitric acid and acetone intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the oxygen atmosphere stove that the nitric acid obtain 10g step 2 and the graphite oxide of acetone intercalation are placed in 50 DEG C processes 1h, obtain the graphene powder of black, high loft.
Embodiment 3
The first step (oxidation of graphite): be that 60% concentrated nitric acid mixing is placed in ice bath by 10g graphite, 1000mL mass percent concentration, stirring makes it mix, then, take 100g Potcrate and add above-mentioned mixed solution, under 100 DEG C of conditions, react 120h; Adding the hydrogen peroxide of 1000mL after 10000mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains is added the sulfuric acid that 1000g mass percent concentration is 98%, be cooled to room temperature soak 120h at 100 DEG C after, after filtration, obtain vitriolated graphite oxide after vacuum-drying; 2) vitriolated graphite oxide is added in ethanol, at 35 DEG C, soak 120h, after filtering, obtain the graphite oxide of sulfuric acid and ethanol intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the argon gas atmosphere stove that the sulfuric acid obtain 10g step 2 and the graphite oxide of ethanol intercalation are placed in 110 DEG C processes 120h, obtain the graphene powder of black, high loft.
Embodiment 4
The first step (oxidation of graphite): be that 65% nitric acid mixing is placed in ice bath by 10g graphite, 300mL mass percent concentration, stir and make it mix, then, take 50g sodium chlorate and add above-mentioned mixed solution, react 3h under 55 DEG C of conditions; Adding the hydrogen peroxide of 200mL after 1000mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains is added the perchloric acid that 200g mass percent concentration is 60%, be cooled to room temperature soak 1h at 45 DEG C after, after filtration, obtain containing perchloric acid graphite oxide after vacuum-drying; 2) graphite oxide containing perchloric acid is added in methyl alcohol, at 35 DEG C, soak 2h, after filtering, obtain the graphite oxide of perchloric acid and methyl alcohol intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the nitrogen atmosphere stove that the perchloric acid obtain 10g step 2 and the graphite oxide of methyl alcohol intercalation are placed in 400 DEG C processes 0.001h, obtain the graphene powder of black, high loft.
Embodiment 5
The first step (oxidation of graphite): be that 70% perchloric acid mixing is placed in ice bath by 10g graphite, 350mL mass percent concentration, stirring makes it mix, then, take 50g Potassium Persulphate and add above-mentioned mixed solution, under 65 DEG C of conditions, react 2.5h; Adding the hydrogen peroxide of 250mL after 1500mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains being added 300g mass percent concentration is the nitric acid of 50% and the mixed solution (mass ratio of nitric acid and sulfuric acid is 2:1) of sulfuric acid, be cooled to room temperature soak 2h at 55 DEG C after, after filtration, obtain containing nitric acid and sulfuric acid graphite oxide after vacuum-drying; 2) graphite oxide containing nitric acid and sulfuric acid is added in acetone, at 25 DEG C, soak 1h, after filtering, obtain the graphite oxide of nitric acid, sulfuric acid and acetone intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the helium atmosphere stove that the graphite oxide of nitric acid 10g step 2 obtained, sulfuric acid and acetone intercalation is placed in 85 DEG C processes 0.02h, obtain the graphene powder of black, high loft.
Embodiment 6
The first step (oxidation of graphite): be that 60% perchloric acid mixing is placed in ice bath by 10g graphite, 350mL mass percent concentration, stirring makes it mix, then, take 20g SODIUMNITRATE and 30g potassium bichromate adds above-mentioned mixed solution, under 65 DEG C of conditions, react 2.5h; Adding the hydrogen peroxide of 250mL after 1500mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains being added 100g mass percent concentration is in the nitric acid of 40%, be cooled to room temperature soak 2h at 65 DEG C after, after filtration, obtain containing nitric acid graphite oxide after vacuum-drying; 2) graphite oxide containing nitric acid is added in the mixed solution (volume ratio of acetone and methyl alcohol is 2:1) of acetone and methyl alcohol, at 25 DEG C, soak 1h, after filtering, obtain the graphite oxide of nitric acid and acetone intercalation.
3rd step (expanding while the vigorous reaction initiated oxidation graphite under specified temp and reduction): after the atmosphere furnace (volume ratio of nitrogen and oxygen is 9:1) that the oxygen that nitric acid 10g step 2 obtained, acetone and the graphite oxide of methyl alcohol intercalation are placed in 95 DEG C mixes with nitrogen processes 0.02h, obtain the graphene powder of black, high loft.
Embodiment 7
The first step (oxidation of graphite): by 10g graphite, 150mL mass percent concentration be 60% perchloric acid and 200mL mass percent concentration be 70% sulfuric acid mixing be placed in ice bath, stirring makes it mix, then, take 70g SODIUMNITRATE and add above-mentioned mixed solution, under 75 DEG C of conditions, react 1.5h; Adding the hydrogen peroxide of 1500mL after 2000mL water is added above-mentioned reaction system, is after glassy yellow until solution, filtered while hot; Finally, by dilute hydrochloric acid and water washing extremely neutrality, after vacuum-drying, graphite oxide is obtained.
Second step (oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer): 1) graphite oxide that 10g step 1 obtains being added 300g mass percent concentration is in the nitric acid of 30%, be cooled to room temperature soak 1h at 85 DEG C after, after filtration, obtain containing nitric acid graphite oxide after vacuum-drying; 2) graphite oxide containing nitric acid is added in methyl alcohol, at 15 DEG C, soak 1h, after filtering, obtain the graphite oxide of nitric acid and methyl alcohol intercalation.
3rd step (while the vigorous reaction initiated oxidation graphite under specified temp expand with reduction): after the hydrogen atmosphere stove that the nitric acid obtain 10g step 2 and the graphite oxide of methyl alcohol intercalation are placed in 75 DEG C processes 0.01h, obtain the graphene powder of black, high loft.
See Fig. 1, it is the FTIR spectrogram of grapheme material prepared by the embodiment of the present invention 1; See Fig. 2, it is the XRD spectra of the Graphene prepared by the embodiment of the present invention 1; See Fig. 3, it is the Raman spectrogram of the Graphene prepared by the embodiment of the present invention 1; See Fig. 4, it is the TEM spectrogram of the Graphene prepared by the embodiment of the present invention 1.As can be seen from Fig. 1, Fig. 2, Fig. 3 and Fig. 4, the grapheme material prepared by the present invention is peeled off fully becomes grapheme material with reduction;
See Fig. 5, it is the TG spectrogram of the Graphene prepared by the embodiment of the present invention 1.As can be seen from Figure 5, compared with graphite oxide, the grapheme material prepared by the present invention has more excellent thermostability.
Claims (1)
1. prepare a method for Graphene in enormous quantities, it is characterized in that: the described step preparing Graphene in enormous quantities comprises: the 1) oxidation of graphite; 2) oxygenant and reductive agent are at the common intercalation of oxidized graphite flake interlayer; 3) expand while the vigorous reaction initiated oxidation graphite under specified temp and reduction; Graphite Powder 99 is placed in the mixed solution of strong acid and strong oxidizer by the oxidation system of described graphite, be oxidized 0.1-120 hour at 25-100 DEG C after, and dilute with water, add a certain amount of hydrogen peroxide, filtered while hot, then use dilute hydrochloric acid and deionized water wash to neutral, obtain graphite oxide after drying; Described strong acid is the one in the vitriol oil, concentrated nitric acid and perchloric acid, or their combination; Described strong oxidizer is the one in potassium permanganate, Potcrate, sodium chlorate, Potassium Persulphate, SODIUMNITRATE and potassium bichromate, or their combination; Described oxygenant and reductive agent comprise in the step of the common intercalation of oxidized graphite flake interlayer: 1) 10 parts of graphite oxides being added 10-1000 part oxygenant mass percent concentration is the aqueous solution of 0.5-98%, room temperature is cooled to soak 0.01-120h at 0-100 DEG C after, after filtration, after vacuum-drying, obtain the graphite oxide containing oxygenant; 2) graphite oxide containing oxygenant is added in reductive agent, at 0-35 DEG C, soak 0.001-120h, after filtering, obtain the graphite oxide of oxygenant and reductive agent intercalation; Described oxygenant is the one in nitric acid, sulfuric acid and perchloric acid, or their combination; Described reductive agent is the one in acetone, ethanol and methyl alcohol, or their combination; Expanding while vigorous reaction initiated oxidation graphite under described specified temp with reduction is the graphite oxide of oxygenant and reductive agent intercalation is placed in temperature to process 0.001-120h higher than the atmosphere furnace of 50 DEG C, obtains the graphene powder of high loft; Described atmosphere is the one in oxygen, air, nitrogen, argon gas, helium and hydrogen, or their combination.
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| CN102807212A (en) * | 2012-08-28 | 2012-12-05 | 武汉大学 | Method for preparing graphene at low temperature |
| CN103833008A (en) * | 2012-11-20 | 2014-06-04 | 中国科学院兰州化学物理研究所 | Method for preparing graphene at normal temperature |
| CN103407995A (en) * | 2013-07-17 | 2013-11-27 | 苏州艾特斯环保材料有限公司 | Graphite oxide preparation method |
| CN103553033B (en) * | 2013-11-11 | 2015-08-19 | 河北大学 | The preparation method of grapheme material |
| CN103613093B (en) * | 2013-11-25 | 2015-09-02 | 黄德欢 | A kind of hydrogen reducing prepares the method for Graphene |
| CN106802295B (en) * | 2017-03-16 | 2020-01-10 | 合肥学院 | Chemical preparation method of graphene quantum dot fluorescent probe for trace TNT detection |
| CN109666350B (en) * | 2017-10-16 | 2021-06-29 | 山东欧铂新材料有限公司 | Water-based conductive coating containing high-conductivity graphene and preparation method thereof |
| CN110902671B (en) * | 2019-10-18 | 2021-11-16 | 东北大学 | Preparation method of low-layer graphene |
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| CN102167311A (en) * | 2011-03-09 | 2011-08-31 | 华侨大学 | Method for preparing graphene on large scale |
| CN102173414A (en) * | 2011-03-18 | 2011-09-07 | 中国地质大学（武汉） | Method for preparing graphene oxide by chemical peeling |
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| CN102167311A (en) * | 2011-03-09 | 2011-08-31 | 华侨大学 | Method for preparing graphene on large scale |
| CN102173414A (en) * | 2011-03-18 | 2011-09-07 | 中国地质大学（武汉） | Method for preparing graphene oxide by chemical peeling |
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