CN109292760A - A method of preparing graphene - Google Patents
A method of preparing graphene Download PDFInfo
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- CN109292760A CN109292760A CN201811456420.5A CN201811456420A CN109292760A CN 109292760 A CN109292760 A CN 109292760A CN 201811456420 A CN201811456420 A CN 201811456420A CN 109292760 A CN109292760 A CN 109292760A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The invention discloses a kind of methods for preparing graphene, are raw material using recyclable organism material, graphene can be prepared by freeze-drying and high temperature cabonization processing, and opened up freeze-drying new method.Graphene prepared by the present invention in the form of sheets, can regulate and control the appearance structure of graphene by adjusting the concentration of biomass solution, can adjust graphene chemical component by high temperature cabonization temperature.All raw materials and reagent source easily obtain extensively, are low in cost, degradable, to human body and environmentally friendly；Preparation process does not need catalyst, and simple process is convenient, it is easy to accomplish large-scale industrial production prepares graphene for simplicity and provides new theoretical direction and technical support, while improving the value added applications of biological material, with good economic efficiency.
Description
Technical field
The present invention relates to carbon material preparation technical fields, in particular to a kind of method for preparing graphene.
Background technique
Graphene be it is a kind of by hexagonal peak nest lattice heap Lai two-dimentional monoatomic layer carbon material, it is this almost thoroughly
Bright, light, flexible material is not only to be currently known most thin, most hard nano material, and has many excellent performances,
For example the thermal coefficient of graphene is about 5300W/mK, is higher than the materials such as natural graphite, carbon nanotube and diamond；Graphene
Electron mobility under room temperature is greater than 15000cm2/ Vs is higher than carbon nanotubes and silicon crystal；The conductivity of graphene is up to
10-6 S/m, it is lower than copper or silver, it is the highest material of current conductivity.This be these unique physics based on graphene and
Chemical property makes it in lithium ion battery, supercapacitor, solar battery, light emitting diode, sensor, hydrogen storage, catalyst
The fields such as carrier, composite material, coating, biologic bracket material, drug controlled release have wide practical use, increasingly by
The attention of people.
It is used equally for preparing graphene currently, many kinds of methods can be used, such as micromechanics stripping method, solvent stripping method, oxygen
Change-reduction method, crystal epitaxy method, chemical vapour deposition technique, microwave method and electrochemical process etc..In these methods, microcomputer
Tool stripping method and crystal epitaxy method preparation efficiency are relatively low, are difficult to meet the needs of large-scale production at present；Chemical gaseous phase
Although sedimentation can obtain the continuous graphene film of large scale, it is suitable for electronic device and transparent conductive film, but
It is not able to satisfy the extensive demand in energy storage material and functional composite material field；Oxidation-reduction method prepare graphene powder at
This is cheap and easy to accomplish, but prepared graphene usually contains more defect, and can generate during the preparation process big
The waste water or exhaust gas of amount cause seriously to pollute to environment；Microwave method and electrochemical process have that reaction time is short, high efficiency, green
The advantages that pollution-free and prepared graphene pattern is more complete, defect is few, however the graphene yield thus prepared is few, still not
It is able to achieve large-scale industrial production.
The biomass carbons source material such as lignin, alkali lignin, cellulose, sodium alginate, tannic acid be a kind of rich reserves,
Reproducible valuable source, recyclable organism material is to store up carbon amounts resource the most abundant in the world, since its is from a wealth of sources
It easily obtains, low in cost, the features such as containing carbon rich can be used as a kind of excellent porous carbon material precursor；Currently, using can be again
Raw biological material is as precursor preparation carbon material, so that production is to human body and environmentally friendly, degradable, inexpensive biomass
Carbon aerogels are the research directions to receive much attention.But few document report application biological materials prepare biomass-based graphite
Alkene.
Summary of the invention
In view of the above shortcomings of the prior art, the object of the present invention is to provide a kind of new and effective graphenes for preparing
Method solves existing graphene preparation cost height, and complex process condition harshness is not easily controlled, and environmental pollution is big, and energy consumption is high, and
And can not achieve large-scale industrial production, prepared graphene is not easy the problems such as storing, while having expanded freeze-drying side
Method realizes freeze-drying in atmospheric conditions, and promotes the value added applications of recyclable organism material.
In order to solve the above-mentioned technical problem, present invention employs the following technical solutions: a method of graphene is prepared,
The following steps are included:
1) biomass carbon source material is dissolved in solvent, is sufficiently mixed, the mixed solution that concentration is 5 ~ 50mg/mL is obtained, by institute
Mixed solution freeze-drying is stated, the laminated structure porous aerogel of nano thickness is obtained；
2) high temperature cabonization is handled the laminated structure porous aerogel for obtaining step 1) in a vacuum or inert atmosphere, can be obtained
Graphene.
In this way, directly using Freeze Drying Technique, the piece of the single-layer or multi-layer of the biomass molecules such as lignin may be implemented
Shape distribution, and precursor construction and distribution can be regulated and controled by controlled concentration, the graphene presoma being prepared has nanometer function
The biogas gel of energy can greatly increase its specific surface area and pore structure, physical pattern structure and graphene or oxygen
Graphite alkene is extremely similar；Further, the carbonization and graphitization of organic carbon source material are realized by way of high-temperature heat treatment, it is complete
At the conversion of chemical structure, by organic transformation it is the carbon component of graphite, and finally realizes the preparation of graphene, and pass through adjusting
Carburizing temperature can control degree of graphitization.
Preferably, the biomass carbon source material is lignin, alkali lignin, hydroxyethyl cellulose, tannic acid and seaweed
One of sour sodium is a variety of.
Preferably, the solvent is deionized water, organic solvent, alkaline aqueous solution or organic solvent and deionized water
Mixed solution.
In this way, the dissolution to heterogeneity carbon source material may be implemented by using different solvents；And alkali is also certain
The graphitization efficiency of carbon material can be improved in degree.
Preferably, the concentration of the alkaline solution is 1 ~ 20%, and the alkali in the alkaline solution is sodium hydroxide or hydroxide
Potassium；The organic solvent is the tert-butyl alcohol.
Preferably, it is described freeze-drying the following steps are included: first mixed solution is freezed in -196 ~ -0 DEG C it is solid, then
It is transferred in freeze-drying machine dry complete；The processing time is 24 ~ 72h；It further include first freezing mixed solution in -196 ~ -0 DEG C
After solid, the mixed solution is placed on water-absorbent material at -10 ~ 10 DEG C, is dried 48 ~ 120h.
In this way, the porous pattern of material can be kept by carrying out freeze-drying in atmospheric conditions, and do not need in vacuum condition
Lower realization, it is simple to operate.
Preferably, the aeroge with a thickness of 10 ~ 500nm.
Preferably, the inert atmosphere is argon gas or nitrogen, helium or neon.
Preferably, the extreme temperatures of the carbonization treatment are 1000 ~ 2500 DEG C, and the time is 0.5 ~ 6h.
Under the high temperature conditions, the graphitization of carbon material is realized, and degree of graphitization is directly related with temperature.In certain temperature
In range, properly increasing heat treatment temperature can be improved the degree of graphitization of material.
The graphene obtained according to above-mentioned preparation method.
Compared with prior art, the invention has the following beneficial effects:
1, graphene prepared by the present invention, by the way of first carrying out structural stratification to presoma, process is extremely simple, greatly
The preparation efficiency of single-layer or multi-layer persursor material is improved, and graphite can be regulated and controled by adjusting the concentration of biomass solution
The appearance structure and characteristic distributions of alkene.
2, the method for the present invention prepares graphene, using first layering or separates, then the mode of graphitization processing, tradition side of forgoing
The extremely complex and difficult problem of the direct or indirect strip step to graphite, significantly simplifies preparation work during method preparation
Skill, hence it is evident that improve preparation efficiency, and prepared target graphene is easy dispersion and stores for a long time.
3, the present invention is raw material using recyclable organism material, can be made by freeze-drying and high temperature cabonization processing
Standby to obtain graphene, preparation process does not need catalyst, and simple process is convenient, raw material and solvent source easily acquisition, cost extensively
It is cheap, degradable, to human body and environmentally friendly, it is easy to accomplish large-scale industrial production prepares graphene for simplicity and provides
New theoretical direction and technical support, while the value added applications of biological material are improved, it is with good economic efficiency.
4, the method that the method for the present invention has also expanded freeze-drying, it is directly dry with water-absorbent material, material can be kept more
Hole pattern, and do not need to realize under vacuum conditions, simple to operate, material is simple and easy to get, and low energy consumption, at low cost, can be with
Large area uses.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the graphene prepared in embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the graphene prepared in embodiment 3.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
1) by water-soluble alkali lignin dissolution in deionized water, it is configured to the lignin aqueous solution of 50 mg/mL concentration, then will
Lignin aqueous solution is rapidly frozen in liquid nitrogen, is then dried in freeze dryer and is obtained the piece that thickness is about 300nm for 24 hours
Shape lignin aeroge；
2) the lignin aeroge that step 1) obtains is placed in tube furnace as graphene presoma, in argon atmosphere and 2500
It is carbonized 0.5 hour under the conditions of DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component stone of Raman spectrum analysis
Black alkene ingredient is 90%, yield 8.8%.
Embodiment 2
1) by water-soluble alkali lignin dissolution in ionized water, the lignin aqueous solution of 20 mg/mL concentration is prepared, then will be wooden
Plain aqueous solution is rapidly frozen in liquid nitrogen, and 48 h are then dried in freeze dryer, obtains the lignin that thickness is about 100nm
Aeroge；
2) be placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in argon atmosphere and
It is carbonized 1 hour under the conditions of 2000 DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component of Raman spectrum analysis
Graphene ingredient is 95%, yield 13%.
Embodiment 3
1) by water-soluble alkali lignin dissolution in deionized water, the lignin aqueous solution of 10 mg/mL concentration is prepared, then will be wooden
After quality aqueous solution is rapidly frozen in -20 DEG C of refrigerator, 72h then is handled in freeze dryer is dry, obtaining thickness is about 60nm
Lignin aeroge；
2) be placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in nitrogen atmosphere and
It is carbonized 2 hours under the conditions of 1500 DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component of Raman spectrum analysis
Graphene ingredient is 88%, yield 19%.
Embodiment 4
1) alkali lignin is dissolved in the tert-butyl alcohol, prepares the lignin liquor of 5 mg/mL concentration, then lignin liquor is existed
After being freezed in -20 DEG C of refrigerator, then the mixed solution is placed on hygienic blotting paper at 0 DEG C and is dried 120h, is obtained
The lignin aeroge for being about 20nm to thickness；
2) be placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in nitrogen atmosphere and
It is carbonized 6 hours under the conditions of 1000 DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component of Raman spectrum analysis
Graphene ingredient is 71%, yield 18%.
Embodiment 5
1) alkali lignin is dissolved in the in the mixed solvent of deionized water Yu the tert-butyl alcohol (volume ratio 1:1), being configured to concentration is
The lignin liquor of 10 mg/mL, then after lignin aqueous solution is rapidly frozen in liquid nitrogen, then by institute under the conditions of 10 DEG C
It states mixed solution and is placed on hygienic blotting paper and be dried 96h, obtain the lignin aeroge that thickness is about 50nm；
2) it is placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in vacuum and 1500 DEG C
Under the conditions of be carbonized 2 hours, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component graphene of Raman spectrum analysis
Ingredient is 90%, yield 16%.
Embodiment 6
1) by lignin dissolution in 5% KOH aqueous solution, the lignin liquor of 10 mg/mL concentration is prepared, then lignin is molten
After liquid freezes in -20 DEG C of refrigerator, in then handling 72h in freeze dryer is dry, the lignin gas that thickness is about 50nm is obtained
Gel；
2) be placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in nitrogen atmosphere and
It is carbonized 1 hour under the conditions of 1500 DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component of Raman spectrum analysis
Graphene ingredient is 93%, yield 17%.
Embodiment 7
1) water-soluble cellulose is dissolved in deionized water, prepares the cellulose solution of 10 mg/mL concentration, then by cellulose
After solution freezes in -20 DEG C of refrigerator, it is then dried 72 h in freeze dryer, obtains the cellulose that thickness is about 100nm
Aeroge；
2) it is placed in aeroge as graphene presoma what step 1) obtained in tube furnace, in nitrogen atmosphere and 1500 DEG C of items
Be carbonized 1 hour under part, be prepared into the microcosmic graphene for sheet after cooling, with its chemical component graphene of Raman spectrum analysis at
It is divided into 79%, yield 15%.
Embodiment 8
1) tannic acid is dissolved in deionized water, prepares the tannin aqueous acid of 50 mg/mL concentration, then tannic acid is water-soluble
Then liquid is dried 48 h in freeze dryer, obtains the tannic acid airsetting that thickness is about 250nm after -20 DEG C of refrigerator freezings
Glue；
2) be placed in lignin aeroge as graphene presoma what step 1) obtained in tube furnace, in argon atmosphere and
It is carbonized 1 hour under the conditions of 1500 DEG C, the microcosmic graphene for sheet is prepared into after cooling, with its chemical component of Raman spectrum analysis
Graphene ingredient is 74%, yield 20%.
Embodiment 9
1) sodium alginate is dissolved in deionized water, prepares the sodium alginate aqueous solution of 10 mg/mL concentration, then by alginic acid
Sodium water solution and then -50 DEG C of 72 h of drying process in freeze dryer, obtain the sodium alginate aeroge that thickness is about 100nm；
2) it is placed in aeroge as graphene presoma what step 1) obtained in tube furnace, in argon atmosphere and 1500 DEG C of items
Be carbonized 1 hour under part, be prepared into the microcosmic graphene for sheet after cooling, with its chemical component graphene of Raman spectrum analysis at
It is divided into 65%, yield 16%.
Embodiment 10
1) water-soluble alkali lignin and sodium alginate are dissolved in deionized water, prepare lignin and the sea of 50 mg/mL concentration
The aqueous solution of mosanom after being rapidly frozen it in liquid nitrogen, is placed on smooth hygienic blotting paper under the conditions of 0 DEG C,
72 h are dried, the aeroge that thickness is about 400nm is obtained；
2) it is placed in aeroge as graphene presoma what step 1) obtained in tube furnace, under the conditions of vacuum and 1500 DEG C
Carbonization 1 hour is prepared into the microcosmic graphene for sheet after cooling, and with Raman spectrum analysis, its chemical component graphene ingredient is
89%, yield 26%.
Fig. 1 and Fig. 2 is respectively the scanning electron microscope (SEM) photograph of graphene prepared by embodiment 1 and 3, as seen from Figure 1, dense
In the case where spending higher (50mg/mL), more continuous laminated structure graphene can be kept after carbonization.With biomass solution
The thickness of the reduction of concentration, prepared sheet presoma and graphene is more and more thinner, and hole is easy to appear among graphene layer
Hole, such as when solution concentration is 10mg/mL (Fig. 2), when hole configurations ratio 50mg/mL more than it is very much；Especially concentration is 5mg/
When mL is even lower, hole is more obvious, much smaller when leading to gained graphene film than high concentration.
To sum up, the present invention can regulate and control appearance structure and the distribution spy of graphene by adjusting the concentration of biomass solution
Point；The chemical component of graphene can also be regulated and controled by adjusting carburizing temperature.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not limitation with the present invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of method for preparing graphene, which comprises the following steps:
1) biomass carbon source material is dissolved in solvent, is sufficiently mixed, obtain the mixed solution that concentration is 5 ~ 50mg/mL, then will
The mixed solution freeze-drying, obtains the laminated structure porous aerogel of nano thickness；
2) high temperature cabonization is handled to get stone is arrived the laminated structure porous aerogel for obtaining step 1) in a vacuum or inert atmosphere
Black alkene.
2. preparing the method for graphene according to claim 1, which is characterized in that the biomass carbon source material is wooden
One of element, alkali lignin, hydroxyethyl cellulose, tannic acid and sodium alginate are a variety of.
3. preparing the method for graphene according to claim 1, which is characterized in that the solvent is deionized water, You Jirong
The mixed solution of agent, alkaline aqueous solution or organic solvent and deionized water.
4. preparing the method for graphene according to claim 3, which is characterized in that the concentration of the alkaline aqueous solution be 1 ~
20%, the alkali in the alkaline aqueous solution is sodium hydroxide or potassium hydroxide；The organic solvent is the tert-butyl alcohol.
5. preparing the method for graphene according to claim 1, which is characterized in that it is described freeze-drying the following steps are included:
First mixed solution is freezed in -196 ~ -0 DEG C it is solid after, then be transferred in freeze-drying machine it is dry completely, the processing time is 24 ~
72h。
6. preparing the method for graphene according to claim 1, which is characterized in that it is described freeze-drying the following steps are included:
First mixed solution is freezed in -196 ~ -0 DEG C it is solid after, the mixed solution is placed on water-absorbent material at -10 ~ 10 DEG C
48 ~ 120h of upper drying process.
7. preparing the method for graphene according to claim 1, which is characterized in that the aeroge with a thickness of 10 ~
500nm。
8. preparing the method for graphene according to claim 1, which is characterized in that the inert protective atmosphere is argon gas, nitrogen
Gas, helium or neon.
9. preparing the method for graphene according to claim 1, which is characterized in that the temperature of the carbonization treatment be 1000 ~
2500 DEG C, the time is 0.5 ~ 6h.
10. a kind of graphene obtained such as any one of claim 1 ~ 9 preparation method.
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Cited By (7)
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| CN109867270A (en) * | 2019-03-01 | 2019-06-11 | 北京化工大学 | A kind of preparation method and applications of carbon nano-material spherical shape assembly |
| CN110106008A (en) * | 2019-05-29 | 2019-08-09 | 连云港华明泰材料科技有限公司 | A kind of preparation method and application of lithium base thickening agent |
| CN110562964A (en) * | 2019-07-02 | 2019-12-13 | 中国科学院城市环境研究所 | All-carbon graphene aerogel and preparation method thereof |
| CN110803695A (en) * | 2019-10-29 | 2020-02-18 | 浙江工业大学 | Method for preparing graphene by using large-sized seaweed as raw material |
| CN111470495A (en) * | 2020-04-24 | 2020-07-31 | 山东龙力生物科技股份有限公司 | Raw material for preparing graphene and method for preparing graphene by using raw material |
| CN113247887A (en) * | 2021-04-13 | 2021-08-13 | 齐鲁工业大学 | Preparation method of hierarchical porous graphene and application of hierarchical porous graphene |
| CN115678102A (en) * | 2022-11-08 | 2023-02-03 | 福州大学 | Tannin-based single-component intumescent flame retardant and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109867270A (en) * | 2019-03-01 | 2019-06-11 | 北京化工大学 | A kind of preparation method and applications of carbon nano-material spherical shape assembly |
| CN110106008A (en) * | 2019-05-29 | 2019-08-09 | 连云港华明泰材料科技有限公司 | A kind of preparation method and application of lithium base thickening agent |
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| CN110562964A (en) * | 2019-07-02 | 2019-12-13 | 中国科学院城市环境研究所 | All-carbon graphene aerogel and preparation method thereof |
| CN110562964B (en) * | 2019-07-02 | 2021-08-20 | 中国科学院城市环境研究所 | All-carbon graphene aerogel and preparation method thereof |
| CN110803695A (en) * | 2019-10-29 | 2020-02-18 | 浙江工业大学 | Method for preparing graphene by using large-sized seaweed as raw material |
| CN111470495A (en) * | 2020-04-24 | 2020-07-31 | 山东龙力生物科技股份有限公司 | Raw material for preparing graphene and method for preparing graphene by using raw material |
| CN113247887A (en) * | 2021-04-13 | 2021-08-13 | 齐鲁工业大学 | Preparation method of hierarchical porous graphene and application of hierarchical porous graphene |
| CN115678102A (en) * | 2022-11-08 | 2023-02-03 | 福州大学 | Tannin-based single-component intumescent flame retardant and preparation method and application thereof |
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