CN106564883A - High-quality graphene prepared from plant membrane layer and preparation method thereof - Google Patents
High-quality graphene prepared from plant membrane layer and preparation method thereof Download PDFInfo
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- 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
- C01B2204/04—Specific amount of layers or specific thickness
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention provides high-quality graphene prepared from a plant membrane layer and a preparation method thereof. The preparation method comprises the following steps: firstly, selecting a plant tissue containing the plant membrane layer, washing the plant tissue cleanly, and soaking the washed plant tissue in an ethanol and ultrapure water acidic mixed solution; then dipping the plant tissue in a glucose solution, followed by placing the plant tissue in an ultrasonic microwave synthesis instrument, and carrying out microwave ultrasonic treatment; then carrying out centrifugal separation, and washing and drying; and finally, placing the dried plant tissue in a tube furnace, calcining, naturally cooling to room temperature, and thus obtaining the high-quality graphene. The nanoscale self-assembly ability of biological macromolecules is utilized, the plant membrane layer is used as a carbon source and a template, glucose is used as a net supplementing agent, the relatively simple chemical process is used for preparing the graphene material, the required chemical raw materials have fewer types and no toxicity, the reaction has no need of complex equipment, the cost is relatively low, and the method has no pollution to the environment, has good experimental repeatability and has relatively great industrial promotion value.
Description
Technical field
The invention belongs to technical field of graphene, is related to a kind of with plant film layer preparation high-quality Graphene and its preparation side
Method, and in particular to a kind of polysaccharide biomacromolecule contained by plant film layer synthesizes the preparation method of large stretch of graphene layer, more
It is the preparation method with different types of plant film layer as templated synthesis high-quality Graphene body.
Background technology
In recent years, Graphene causes the very big concern of scientific circles, and it has excellent heat conduction, conduction, optics and mechanics
Performance makes it have broad application prospects in the field such as electronics, energy storage and conversion, biological detection and sensing.Preferable graphite
Alkene is by sp2The single layer structure that hydbridized carbon atoms are sprawled by the hexagoinal lattice of covalent bond formed in two dimension.It is actual most
Number graphene product is stacked into by mono-layer graphite, and every group of lamination often containing multiple superthin sections and can pass through seven yuan of octatomic rings
Folded etc. defect, so as to form tubulose or even spherical, and folding mode and the number of plies often can be produced to the performance of Graphene
Raw considerable influence.Single-layer graphene such as suspend in close absolute zero, electron mobility is up to 230000 cm2/ (V s), and
3 layers of Graphene electron mobility only about 1500 cm at room temperature2/ (V s), this is that the number of plies due to stacking makes band structure
There are significant changes with overlap zone.
At present, the preparation of Graphene and process are research fields that is extremely active and developing rapidly, and its main method is concentrated
In Graphene quality highest prepared by solid phase method, three kinds of approach of liquid phase method and vapor phase method, traditional solid phase mechanical stripping method, but because
The number of plies is excessively not readily separated causes yield extremely low.Liquid phase method is the effective way for realizing Graphene volume production, and main points are that graphite need to be
Graphene oxide is converted under strong acid condition, the reduction generation such as Jing compounds such as hydrazine is put into after organic solvent dispersion again flat
Whole Graphene, defect is to cause serious acid solution to pollute, dangerous higher, and final product still includes substantial amounts of C-O keys.And
Vapor phase method the most accurate, such as high temperature epitaxy growth method and chemical vapour deposition technique (CVD), although more complete list can be produced
Layer graphene piece, but loaded down with trivial details step and complicated technology controlling and process is needed, and high-quality substrate is depended in its growth, causes cost mistake
Height, therefore be not suitable for producing Graphene on a large scale.The backwardness of technology seriously hinders the industrialization of high-quality grapheme material
Production.
Using biomolecule self assembly and special construction construct with specific physics, chemical property new material
Become the focus of current material technology development, the method often eliminates the prefabricated chelating polymer template of costliness, and operation is simple, easily
Extension production.The development of more than ten years is have passed through, multiple Research Teams have prepared number by the use of natural plant material as template
Plant high performance carbon material.If professor Xu Anwu of Chinese University of Science and Technology is by the use of flesh of Pulp Citrulli as template, 180 DEG C of hydrothermal conditions of Jing
It is prepared for carbon gel within lower 12 hours.In 6 A g-1Discharge current density under energy storage density can also be maintained at 222.3 F g-1, far
It is better than the materials such as nitrogen-doped carbon pipe and reduced graphene.Dong Shaojun of Electroanalytical Chemistry National Key Laboratory of the Chinese Academy of Sciences etc. is with bean
Milk is template, has synthesized the fluorescence nano point of doping nitrogen, and this new material has embodied good electricity in oxygen reduction reaction and urged
Change performance.It can thus be seen that in terms of material with carbon element is prepared, biological template is both using the polysaccharide contained by itself, protein, core
Acid etc. can form advantageous advantage, so as to synthesize the material with carbon element of high-quality using its unique texture again as natural carbon source.
Plant cell wall film is one kind of cell membrane, is made up of intercellular layer, primary wall and secondary wall, and its chemical composition is mainly
Pectin and cellulose, play a part of to separate cell.Plant cell wall film layer（Plant film layer）Thickness is about 1 ~ 10 micron, containing receiving
Metre hole, it is overall that there is preferable mechanical strength, relatively it is suitable as preparing the template of carbons new material.At present with regard to plant membrane lamination
Into the Patents of grapheme material, there is not been reported.
The content of the invention
The technical problem of solution：In view of the shortcomings of the prior art, the invention provides preparing Gao Pin with plant film layer
Matter Graphene and preparation method thereof, the present invention provides a kind of brand-new plant film layer as template, choose cell it is larger and
Intracellular aqueous abundant plant tissue, by pretreatment, then the high-temperature calcination under being protected by nitrogen removes the impurity in template, from
And obtain the material of molding；From different plant film layers, the grapheme material of the different numbers of plies can be obtained.The preparation method into
This cheap, process is simple, it is to avoid conventional various chemistry higher to equipment requirements and physics prepare Graphene tube method and brought
Tedious steps and complicated technology.
Technical scheme：The preparation method that high-quality Graphene is prepared with plant film layer that the present invention is provided, including following step
Suddenly：
The first step：Pre-treatment
Choose the plant tissue containing plant film layer to clean, it is standby；Ethanol and ultra-pure water are made into into mixed liquor, and adjust pH of mixed
It is standby for 2 ~ 4；Clean plant tissue is completely soaked carries out activation processing in the mixed liquor；
Second step：Post processing
Plant tissue after immersion is taken out, then be impregnated in and carry out in glucose solution net mending process；
3rd step：Separate
Plant tissue after process is centrifuged, is washed and is dried；
4th step：Heat treatment
Under nitrogen protection, calcining heat treatment is carried out to dried plant tissue；
5th step：Cooling
After calcining terminates, product is taken out, naturally cool to room temperature, obtain final product high-quality Graphene.
Wherein, in second step, after plant tissue Jing glucose solutions dipping net mending is processed, also including following post processing
Step：In being placed in ultrasonic microwave synthesizer again, microwave ultrasound process is carried out.Wherein, the condition of the microwave ultrasound process is：
With 2450 MHz microwave frequencies, with 15 ~ 25 KHz supersonic frequencies, 20 ~ 60 min are reacted.
Wherein, in the 4th step, the calcination condition is：700 ~ 900 DEG C, it is incubated 2 ~ 4 hours.
Wherein, in second step, the mass fraction of glucose is 5 % ~ 10 % in the glucose solution.
Wherein, in the second step, the impregnation process time is 12 ~ 24 h, and the volume of the glucose solution is not
Less than 20 mL/g plant membranes.
Wherein, in the third step, the rotating speed of the centrifugation is 8000 r/min, and the centrifugation time is 5 ~ 10min；
In the 4th step, the heating rate is 2 DEG C/min.
Wherein, in the first step, the volume ratio of ethanol and ultra-pure water is 1 in the mixed liquor:3；During the immersion treatment
Between be 36 h ~ 72 h；In the third step, baking temperature is 40 DEG C, and drying time is 8 ~ 24 hours.
Wherein, the plant film layer takes from aqueous abundant plant tissue cell, the plant tissue be cell it is larger and
It is intracellular aqueous abundant；Preferably, the plant tissue is petal, straw, blade or marc；It is more highly preferred to, the plant
Thing film is Flos micheliae Albae petal, oriental cherry petal, corn straw, bagasse, pomace or Folium Alangii.
Wherein, in the first step, the consumption of the mixed liquor is can be at least completely soaked plant membrane to be advisable, and is implemented one
In example, the consumption of the mixed liquor is 20mL/g plant membranes, but its concrete consumption not limited to this.
What the present invention was provided prepares high-quality Graphene with plant film layer, its prepared by above-described preparation method and
Into.
Grapheme material has excellent electron mobility, thermal conductivity and mechanical property, is to be expected to 2025 take afterwards
For the Nano electric material of new generation of silicon.But high-quality is produced with low cost and regulatable Graphene is always industrial difficulty
Point.
Beneficial effects of the present invention：
1. the present invention utilizes the nanoscale self assembly ability of biomacromolecule, using plant film layer as carbon source and template, with Fructus Vitis viniferae
Sugar employs relatively simple chemical technology and has prepared grapheme material as net mending agent, and required chemical raw material species is less
And avirulence, without the need for complicated equipment, cost is relatively low, and environmentally safe, assay reproducibility is good, there is larger industry for reaction
Promotional value.
2. the present invention can prepare high-quality graphene film layer material, by from different plant film layers, can flexibly adjust
The number of plies of control grapheme material.
3. using ultrasonic microwave process in the present invention, at microwave ultrasound of the ultrasonic microwave synthesizer to sample
Reason, can remove the fold of fibrous layer, improve the flatness of follow-up product.
4. by every sign, its result shows Graphene of the products therefrom for high-quality to the product prepared by the present invention
Lamellar structure, the large stretch of grapheme material with monolayer six-membered ring structure, its thickness is about 1.38 nm.
5. the graphene sheet layer that the present invention is prepared has excellent electron mobility, thermal conductivity and mechanical property, has
Larger commercial introduction value.
Description of the drawings
Fig. 1 is the high-resolution-ration transmission electric-lens figure of the Graphene in the present invention prepared by embodiment 1；
Fig. 2 is the Raman spectrogram of the Graphene in the present invention prepared by embodiment 1；
Fig. 3 is the atomic force microscopy diagram of the Graphene in the present invention prepared by embodiment 1.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limit.
Embodiment 1
The first step：5 g Flos micheliae Albaes petals are washed away into floating dust with the min of 100 mL distilled water immersions 10, ethanol and ultra-pure water are pressed into body
Product compares 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 4, using the h of this mixed liquor 100 mL immersion Flos micheliae Albaes petal 48；
Second step：Flos micheliae Albae petal after immersion is taken out, in being then put in glucose solutions of 100 mL containing 10 %, dipping
24 h, during ultrasonic microwave synthesizer is positioned over afterwards, with 2450 MHz microwave frequencies, with 18 KHz supersonic frequencies 20 are reacted
min；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, by the Flos micheliae Albae petal after process from glucose solution from
The heart is separated and taken out, and carries out multiple centrifuge washing with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, is dried 10 little
When；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 700 DEG C, be incubated 2 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Sample structure is observed using transmission electron microscope, and it is prepared by Raman spectrum and atomic force microscope test
The graphene-structured for obtaining and lamella.
The transmission electron microscope figure of grapheme tube as obtained in the technological parameter of embodiment 1, as shown in figure 1, wherein inserting
Figure is the hexagonal lattice image by Graphene after FFT amendments, and the Raman spectrum of sample is as shown in Fig. 2 its 2D peak is in height
To property, it was demonstrated that material is single-layer graphene lamella, and the atomic force microscopy diagram of material is as shown in Figure 3.It can be seen that
Prepared graphene sheet layer is larger, and its thickness is about 1.38 nm.
Embodiment 2
The first step：5 g oriental cherries petals are washed away into floating dust with the min of 100 mL distilled water immersions 10, ethanol and ultra-pure water are pressed into volume
Than 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 4, using the h of this mixed liquor 100 mL immersion oriental cherries petal 36；
Second step：Oriental cherry petal after immersion is taken out, in being then put in glucose solutions of 120 mL containing 10 %, dipping 24
H, during ultrasonic microwave synthesizer is positioned over afterwards, with 2450 MHz microwave frequencies, with 15 KHz supersonic frequencies 20 min is reacted；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, the oriental cherry petal after process is centrifuged from glucose solution
Separate and take out, and multiple centrifuge washing is carried out with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, be dried 8 hours；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 700 DEG C, be incubated 2 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Embodiment 3
The first step：8 g corn straw are washed away into floating dust with the min of 100 mL distilled water immersions 10, ethanol and ultra-pure water are pressed into volume
Than 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 2, and using this mixed liquor 180 mL the h of straw 48 is soaked；
Second step：Straw after immersion is taken out, in being then put in glucose solutions of 160 mL containing 3 %, 12 h is impregnated, it
After be positioned in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, with 25 KHz supersonic frequencies 60 min are reacted；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, the centrifugation from glucose solution by the straw after process
Take out, and multiple centrifuge washing is carried out with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, be dried 24 hours；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 900 DEG C, be incubated 4 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Embodiment 4
The first step：5 g bagasse are washed away into floating dust with the min of 100 mL distilled water immersions 10, by ethanol and ultra-pure water by volume
1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 2, and using this mixed liquor 120 mL the h of bagasse 48 is soaked；
Second step：Bagasse after immersion is taken out, in being then put in glucose solutions of 150 mL containing 8 %, 12 h is impregnated,
In being positioned over ultrasonic microwave synthesizer afterwards, with 2450 MHz microwave frequencies, with 20 KHz supersonic frequencies 60 min are reacted；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, the bagasse after process is centrifuged from glucose solution and is divided
From taking-up, and multiple centrifuge washing is carried out with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, be dried 10 hours；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 900 DEG C, be incubated 4 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Embodiment 5
The first step：7 g pomaces are washed away into floating dust with the min of 100 mL distilled water immersions 10, by ethanol and ultra-pure water by volume
1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 3, and using this mixed liquor 140 mL the h of Folium Bambusae 48 is soaked；
Second step：Pomace after immersion is taken out, in being then put in glucose solutions of 180 mL containing 7 %, 12 h is impregnated,
In being positioned over ultrasonic microwave synthesizer afterwards, with 2450 MHz microwave frequencies, with 18 KHz supersonic frequencies 50 min are reacted；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, the pomace after process is centrifuged from glucose solution and is divided
From taking-up, and multiple centrifuge washing is carried out with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, be dried 10 hours；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 800 DEG C, be incubated 3 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Embodiment 6
The first step：5 g Folium Alangives are washed away into floating dust with the min of 100 mL distilled water immersions 10, by ethanol and ultra-pure water by volume 1:
3 are made into mixed liquor, and the use of salt acid for adjusting pH are 3, and using this mixed liquor 150 mL the h of Folium Alangii 48 is soaked；
Second step：Folium Alangii after immersion is taken out, in being then put in glucose solutions of 100 mL containing 2 %, 12 h is impregnated, it
After be positioned in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, with 20 KHz supersonic frequencies 60 min are reacted；
3rd step：Using 50 mL centrifuge tubes under 8000 r/min, the centrifugation from glucose solution by the Folium Alangii after process
Take out, and multiple centrifuge washing is carried out with ultra-pure water, in being laid in culture dish, in 40 DEG C of baking oven, be dried 10 hours；
4th step：Dried plant membrane is put into into corundum porcelain boat, in being placed in tube furnace, nitrogen protection is passed to, by 2 DEG C/min
Ramp to 800 DEG C, be incubated 3 hours；
5th step：After calcining terminates, the Graphene for preparing is taken out, naturally cool to room temperature, obtained final product.
Ultrasonic microwave synthesizer used in the various embodiments described above is that the ultrasonic microwave collaboration of Nanjing Xian Ou companies is anti-
Answer system.It should be noted that the plant tissue raw material used in above-described embodiment 1-6 is respectively Flos micheliae Albae petal, oriental cherry
Petal, corn straw, bagasse, pomace and Folium Alangii, but be not limited to this, plant tissue raw material can for any cell it is larger and
Intracellular aqueous abundant plant tissue, for example, can be petal, straw, blade and marc etc..
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope for causing.
Claims (10)
1. the preparation method of high-quality Graphene is prepared with plant film layer, it is characterised in that comprised the following steps：
The first step：Pre-treatment
Choose the plant tissue containing plant film layer to clean, it is standby；Ethanol and ultra-pure water are made into into mixed liquor, and adjust pH of mixed
It is standby for 2 ~ 4；Clean plant tissue is completely soaked carries out activation processing in the mixed liquor；
Second step：Post processing
Plant tissue after immersion is taken out, then be impregnated in and carry out in glucose solution net mending process；
3rd step：Separate
Plant tissue after process is centrifuged, is washed and is dried；
4th step：Heat treatment
Under nitrogen protection, calcining heat treatment is carried out to dried plant tissue；
5th step：Cooling
After calcining terminates, product is taken out, naturally cool to room temperature, obtain final product high-quality Graphene.
2. the preparation method that high-quality Graphene is prepared with plant film layer according to claim 1, it is characterised in that the
In two steps, after plant tissue Jing glucose solutions dipping net mending is processed, also including following post-processing step：Ultrasound wave is placed in again
In microwave synthesizer, microwave ultrasound process is carried out.
3. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
In the 4th step, the condition of the calcining heat treatment is：700 ~ 900 DEG C, it is incubated 2 ~ 4 hours.
4. it is according to claim 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that institute
State microwave ultrasound process condition be：With 2450 MHz microwave frequencies, with 15 ~ 25 KHz supersonic frequencies, 20 ~ 60 min are reacted.
5. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
In second step, the mass fraction of glucose is 5 % ~ 10 % in the glucose solution.
6. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
In second step, the impregnation process time is 12 ~ 24 h, and the volume of the glucose solution is not less than 20 mL/g plants
Film.
7. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
In the third step, the rotating speed of the centrifugation is 8000 r/min, and the centrifugation time is 5 ~ 10 min；In the 4th step,
The heating rate is 2 DEG C/min.
8. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
In the first step, the volume ratio of ethanol and ultra-pure water is 1 in the mixed liquor:3；The immersion treatment time is 36 h ~ 72 h；
In the third step, the baking temperature is 40 DEG C, and drying time is 8 ~ 24 hours.
9. it is according to claim 1 and 2 with plant film layer prepare high-quality Graphene preparation method, it is characterised in that
The plant tissue containing plant film layer is Flos micheliae Albae petal, oriental cherry petal, corn straw, bagasse, pomace or Folium Alangii.
10. high-quality Graphene is prepared with plant film layer, it is characterised in that the Graphene is by any one of claim 1-9 institute
The preparation method stated is prepared from.
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| CN107973282A (en) * | 2017-10-31 | 2018-05-01 | 华南理工大学 | A kind of carbon material and preparation method and application produces hydrogen peroxide in electro-catalysis |
| CN109364951A (en) * | 2018-12-21 | 2019-02-22 | 苏州科技大学 | A kind of visible light catalytic composite material and preparation method and application |
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| CN107973282A (en) * | 2017-10-31 | 2018-05-01 | 华南理工大学 | A kind of carbon material and preparation method and application produces hydrogen peroxide in electro-catalysis |
| CN109364951A (en) * | 2018-12-21 | 2019-02-22 | 苏州科技大学 | A kind of visible light catalytic composite material and preparation method and application |
| CN109364951B (en) * | 2018-12-21 | 2022-09-30 | 苏州科技大学 | Visible light catalytic composite material and preparation method and application thereof |
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| CN106564883B (en) | 2018-08-28 |
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