CN106564883B - High-quality graphene and preparation method thereof is prepared with plant film layer - Google Patents
High-quality graphene and preparation method thereof is prepared with plant film layer Download PDFInfo
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Abstract
The present invention provides high-quality graphene and preparation method thereof is prepared with plant film layer, the preparation method comprises the following steps：The plant tissue for first choosing the film layer containing plant is cleaned, and is soaked in ethyl alcohol and ultra-pure water acid mixed solution；Then be impregnated in glucose solution, be placed in ultrasonic microwave synthesizer, carry out microwave ultrasound processing；It then centrifuges, washs and dry；It is finally placed in tube furnace and calcines, cooled to room temperature is to get high-quality graphene.The present invention utilizes the nanoscale self assembly ability of large biological molecule, using plant film layer as carbon source and template, using glucose as net mending agent, it uses relatively simple chemical technology and has prepared grapheme material, required chemical raw material type is less and non-toxic, and reaction is without complicated equipment, cost is relatively low, environmentally safe, assay reproducibility is good, there is larger commercial introduction value.
Description
Technical field
The invention belongs to technical field of graphene, are 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 large biological molecule by contained by plant film layer synthesizes the preparation method of large stretch of graphene layer, more
It is body using different types of plant film layer as the preparation method of templated synthesis high-quality graphene.
Background technology
In recent years, graphene causes the very big concern of scientific circles, it has excellent heat conduction, conduction, optics and mechanics
Performance makes it be had broad application prospects in the fields such as electronics, energy storage and conversion, biological detection and sensing.Ideal graphite
Alkene is by sp2Single layer structure made of the hexagoinal lattice that hydbridized carbon atoms are formed by covalent bond is sprawled in two dimension.It is practical most
Number graphene product is stacked by mono-layer graphite, and every group of lamination often contains multiple superthin sections and can pass through seven yuan of octatomic rings
The defects of folded, to form tubulose or even spherical, and folding mode and the number of plies can often produce the performance of graphene
Raw larger impact.Single-layer graphene such as suspend when close to 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 because the number of plies stacked makes band structure
Significant changes occur with overlap zone.
Currently, the preparation and processing of graphene are research fields that is extremely active and rapidly developing, main method is concentrated
In graphene quality highest prepared by three kinds of solid phase method, liquid phase method and vapor phase method approach, traditional solid phase mechanical stripping method, but because
The number of plies, which 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
It is converted into graphene oxide under strong acid condition, is put into generate through reduction such as compound such as hydrazines again after organic solvent dispersion and put down
Whole graphene, defect are that serious acid solution is caused to pollute, dangerous higher, and final product still includes a large amount 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 can generate more complete single
Layer graphene piece, but cumbersome step and complicated technology controlling and process are needed, and growth depends on high-quality substrate, leads to 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 the self assembly and special construction of biomolecule construct with specific physics, chemical property new material
As the hot spot of current material technology development, this method often eliminates expensive prefabricated chelating polymer template, and process is simple, easily
Extension production.The development of more than ten years is have passed through, multiple Research Teams have prepared number using natural plant material as template
Kind high performance carbon material.If professor Xu Anwu of Chinese University of Science and Technology is using flesh of Pulp Citrulli as template, through 180 DEG C of hydrothermal conditions
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 beans
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 preparing carbon material, biological template is both using polysaccharide, protein, the core contained by itself
Acid etc. is used as natural carbon source, and can form advantageous advantage using its unique texture, to synthesize good carbon material.
Plant cell wall film is one kind of cell membrane, is made of intercellular layer, primary wall and secondary wall, and chemical composition is mainly
Pectin and cellulose play a part of separating cell.Plant cell wall film layer（Plant film layer）Thickness is about 1 ~ 10 micron, containing receiving
Metre hole, it is whole that there is preferable mechanical strength, it is relatively suitable as preparing the template of carbons new material.It is laminated about plant membrane at present
At the related patents of grapheme material, there is not been reported.
Invention content
The technical issues of solution：In view of the deficiencies of the prior art, the present invention provides prepare Gao Pin with plant film layer
Matter graphene and preparation method thereof, the present invention provide a kind of completely new plant film layer as template, choose cell it is larger and
Intracellular aqueous abundant plant tissue removes the impurity in template by pretreatment, then by the high-temperature calcination under nitrogen protection, from
And obtain molding material；Different plant film layers is selected, different layers of grapheme materials can be obtained.The preparation method at
This is cheap, simple for process, avoids previous various chemistry higher to equipment requirement and physics prepares graphene tube method and brought
Tedious steps and complicated technology.
Technical solution：The preparation method provided by the invention that high-quality graphene is prepared with plant film layer, including following step
Suddenly：
The first step：Pre-treatment
The plant tissue for choosing the film layer containing plant is cleaned, spare；Ethyl alcohol and ultra-pure water are made into mixed liquor, and adjust mixing
Liquid pH is 2 ~ 4, spare；Clean plant tissue is completely soaked in the mixed liquor and carries out activation process；
Second step：Post-processing
Plant tissue after immersion is taken out, progress net mending processing in glucose solution is then impregnated in；
Third walks：Separation
By treated, plant tissue is centrifuged, and washs and dries；
4th step：Heat treatment
Under nitrogen protection, calcining heat treatment is carried out to the plant tissue after drying；
5th step：It is cooling
After calcining, product is taken out, cooled to room temperature is to get high-quality graphene.
Wherein, further include following post-processing after plant tissue is handled through glucose solution dipping net mending in second step
Step：It is placed in again in ultrasonic microwave synthesizer, carries out microwave ultrasound processing.Wherein, the condition of the microwave ultrasound processing is：
With 2450 MHz microwave frequencies 20 ~ 60 min are reacted with 15 ~ 25 KHz supersonic frequencies.
Wherein, in the 4th step, the calcination condition is：700 ~ 900 DEG C, keep the temperature 2 ~ 4 hours.
Wherein, in second step, the mass fraction of glucose is the % of 5 % ~ 10 in the glucose solution.
Wherein, in the second step, the impregnation 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 ethyl alcohol and ultra-pure water is 1 in the mixed liquor:3；When the immersion treatment
Between be the h of 36 h ~ 72；In the third step, drying temperature is 40 DEG C, and drying time is 8 ~ 24 hours.
Wherein, the plant film layer is derived 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, stalk, blade or marc；More preferably, the plant
Object film is Flos micheliae Albae petal, oriental cherry petal, maize straw, bagasse, apple pomace or maple leaf.
Wherein, in the first step, the dosage of the mixed liquor is that can at least be completely soaked plant membrane to be advisable, and is implemented one
In example, the dosage of the mixed liquor is 20mL/g plant membranes, but its specific dosage is without being limited thereto.
It is provided by the invention that high-quality graphene is prepared with plant film layer, prepared by above-described preparation method and
At.
Grapheme material has excellent electron mobility, thermal conductivity and mechanical property, is taken after being expected to 2025
For the Nano electric material of new generation of silicon.But it is always industrial difficulty with low cost production high quality and regulatable graphene
Point.
Beneficial effects of the present invention：
1. the present invention utilizes the nanoscale self assembly ability of large biological molecule, using plant film layer as carbon source and template, with
Glucose uses relatively simple chemical technology and has prepared grapheme material, required chemical raw material type as net mending agent
Less and non-toxic, without complicated equipment, cost is relatively low, environmentally safe, and assay reproducibility is good, has larger for reaction
Commercial introduction is worth.
2. the present invention can prepare high-quality graphene film layer material, by selecting different plant film layers, can flexibly adjust
Control the number of plies of grapheme material.
3. in the present invention using ultrasonic microwave handle, by ultrasonic microwave synthesizer to the microwave ultrasound of sample at
Reason, can remove the fold of fibrous layer, improve the flatness of subsequent product.
4. the product prepared by the present invention is characterized by items, result shows that products therefrom is the graphene of high-quality
Lamellar structure, large stretch of grapheme material with single layer six-membered ring structure, 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, have
Larger commercial introduction value.
Description of the drawings
Fig. 1 is the high-resolution-ration transmission electric-lens figure of the graphene prepared by embodiment 1 in the present invention；
Fig. 2 is the Raman spectrogram of the graphene prepared by embodiment 1 in the present invention；
Fig. 3 is the atomic force microscopy diagram of the graphene prepared by embodiment 1 in the present invention.
Specific implementation mode
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are only the feature and advantage further illustrated the present invention, rather than to the claims in the present invention
Limitation.
Embodiment 1
The first step：5 g Flos micheliae Albaes petals are washed away into floating dust with 100 mL distilled water immersions, 10 min, by ethyl alcohol and ultra-pure water
By volume 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 4, impregnate Flos micheliae Albae petal using 100 mL of this mixed liquor
48 h；
Second step：Flos micheliae Albae petal after immersion is taken out, is then put in glucose solutions of 100 mL containing 10 %,
24 h are impregnated, are positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, are reacted with 18 KHz supersonic frequencies
20 min；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, will treated Flos micheliae Albae petal from glucose solution
Middle centrifugation is taken out, and is used in combination ultra-pure water to carry out multiple centrifuge washing, is laid in culture dish, dry in 40 DEG C of baking oven
10 hours；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 700 DEG C, keeps the temperature 2 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
Sample structure is observed using transmission electron microscope, and by prepared by Raman spectrum and atomic force microscope test
The graphene-structured and lamella obtained.
The transmission electron microscope figure of grapheme tube made from technological parameter by embodiment 1, as shown in Figure 1, wherein inserting
Figure is the hexagonal lattice image of graphene after being corrected by FFT, and the Raman spectrum of sample is as shown in Fig. 2, its peak 2D 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 thickness is about 1.38 nm.
Embodiment 2
The first step：5 g oriental cherries petals are washed away into floating dust with 100 mL distilled water immersions, 10 min, ethyl alcohol and ultra-pure water are pressed
Volume ratio 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 4, impregnate 36 h of oriental cherry petal using 100 mL of this mixed liquor；
Second step：Oriental cherry petal after immersion is taken out, is then put in glucose solutions of 120 mL containing 10 %, leaching
24 h of stain, is positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, reacts 20 with 15 KHz supersonic frequencies
min；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, will treated oriental cherry petal from glucose solution
It centrifuges and takes out, be used in combination ultra-pure water to carry out multiple centrifuge washing, be laid in culture dish, in 40 DEG C of baking oven, dry 8
Hour；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 700 DEG C, keeps the temperature 2 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
Embodiment 3
The first step：8 g maize straws are washed away into floating dust with 100 mL distilled water immersions, 10 min, ethyl alcohol and ultra-pure water are pressed
Volume ratio 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 2, impregnate 48 h of stalk using 180 mL of this mixed liquor；
Second step：Stalk after immersion is taken out, is then put in glucose solutions of 160 mL containing 3 %, dipping 12
H is positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, reacts 60 min with 25 KHz supersonic frequencies；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, by treated, stalk is centrifuged from glucose solution
Separation is taken out, and is used in combination ultra-pure water to carry out multiple centrifuge washing, is laid in culture dish, and in 40 DEG C of baking oven, dry 24 is small
When；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 900 DEG C, keeps the temperature 4 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
Embodiment 4
The first step：5 g bagasse are washed away into floating dust with 100 mL distilled water immersions, 10 min, ethyl alcohol and ultra-pure water are pressed into body
Product ratio 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 2, impregnate 48 h of bagasse using 120 mL of this mixed liquor；
Second step：Bagasse after immersion is taken out, is then put in glucose solutions of 150 mL containing 8 %, dipping
12 h are positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, react 60 with 20 KHz supersonic frequencies
min；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, will treated bagasse from glucose solution from
Heart separation is taken out, and is used in combination ultra-pure water to carry out multiple centrifuge washing, is laid in culture dish, and in 40 DEG C of baking oven, dry 10 is small
When；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 900 DEG C, keeps the temperature 4 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
Embodiment 5
The first step：7 g apple pomaces are washed away into floating dust with 100 mL distilled water immersions, 10 min, ethyl alcohol and ultra-pure water are pressed into body
Product ratio 1:3 are made into mixed liquor, and the use of salt acid for adjusting pH are 3, impregnate 48 h of the leaf of bamboo using 140 mL of this mixed liquor；
Second step：Apple pomace after immersion is taken out, is then put in glucose solutions of 180 mL containing 7 %, dipping
12 h are positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, react 50 with 18 KHz supersonic frequencies
min；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, will treated apple pomace from glucose solution from
Heart separation is taken out, and is used in combination ultra-pure water to carry out multiple centrifuge washing, is laid in culture dish, and in 40 DEG C of baking oven, dry 10 is small
When；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 800 DEG C, keeps the temperature 3 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
Embodiment 6
The first step：5 g maple leaves are washed away into floating dust with 100 mL distilled water immersions, 10 min, ethyl alcohol 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 3, impregnate 48 h of maple leaf using 150 mL of this mixed liquor；
Second step：Maple leaf after immersion is taken out, is then put in glucose solutions of 100 mL containing 2 %, dipping 12
H is positioned over later in ultrasonic microwave synthesizer, with 2450 MHz microwave frequencies, reacts 60 min with 20 KHz supersonic frequencies；
Third walks：Using 50 mL centrifuge tubes at 8000 r/min, by treated, maple leaf is centrifuged from glucose solution
Separation is taken out, and is used in combination ultra-pure water to carry out multiple centrifuge washing, is laid in culture dish, and in 40 DEG C of baking oven, dry 10 is small
When；
4th step：Plant membrane after drying is put into corundum porcelain boat, is placed in tube furnace, passes to nitrogen protection, by 2 DEG C/
The rate of min is warming up to 800 DEG C, keeps the temperature 3 hours；
5th step：After calcining, by the graphene being prepared take out, cooled to room temperature to get.
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, maize straw, bagasse, apple pomace and maple leaf, but it is not limited to this, plant tissue raw material can be any cell it is larger and
Intracellular aqueous abundant plant tissue, may be, for example, petal, stalk, blade and marc etc..
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be apparent to 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, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest range caused.
Claims (8)
1. preparing the preparation method of high-quality graphene with plant film layer, which is characterized in that include the following steps：
The first step：Pre-treatment
The plant tissue for choosing the film layer containing plant is cleaned, spare；Ethyl alcohol and ultra-pure water are made into mixed liquor, and adjust pH of mixed
It is 2 ~ 4, it is spare；Clean plant tissue is completely soaked in the mixed liquor and carries out activation process；
Second step：Post-processing
Plant tissue after immersion is taken out, is then impregnated in progress net mending processing in glucose solution, then be placed in ultrasonic wave
In microwave synthesizer, microwave ultrasound processing is carried out；
Third walks：Separation
By treated, plant tissue is centrifuged, and washs and dries；
4th step：Heat treatment
Under nitrogen protection, calcining heat treatment is carried out to the plant tissue after drying；
5th step：It is cooling
After calcining, product is taken out, cooled to room temperature is to get high-quality graphene.
2. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that the
In four steps, the condition of the calcining heat treatment is：700 ~ 900 DEG C, keep the temperature 2 ~ 4 hours.
3. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that described
Microwave ultrasound processing condition be：With 2450 MHz microwave frequencies 20 ~ 60 min are reacted with 15 ~ 25 KHz supersonic frequencies.
4. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that the
In two steps, the mass fraction of glucose is the % of 5 % ~ 10 in the glucose solution.
5. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that the
In two steps, the impregnation time is 12 ~ 24 h, and the volume of the glucose solution is not less than 20 mL/g plant membranes.
6. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that the
In three steps, the rotating speed of the centrifugation is 8000 r/min, and the centrifugation time is 5 ~ 10 min；In the 4th step, calcining
The heating rate of heat treatment process is 2 DEG C/min.
7. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that the
In one step, the volume ratio of ethyl alcohol and ultra-pure water is 1 in the mixed liquor:3；The immersion treatment time is the h of 36 h ~ 72；
In three steps, the drying temperature is 40 DEG C, and drying time is 8 ~ 24 hours.
8. the preparation method according to claim 1 for preparing high-quality graphene with plant film layer, which is characterized in that described
The plant tissue of the film layer containing plant is Flos micheliae Albae petal, oriental cherry petal, maize straw, bagasse, apple pomace or maple leaf.
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| CN104724696A (en) * | 2013-12-24 | 2015-06-24 | 中国科学院宁波材料技术与工程研究所 | Method for preparing graphene by taking biomass as raw material |
| CN105060289A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing fewer-layer graphene on basis of biomass waste |
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| US20160060123A1 (en) * | 2014-11-03 | 2016-03-03 | Alimorad Rashidi | Producing graphene and nanoporous graphene |
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| US20160060123A1 (en) * | 2014-11-03 | 2016-03-03 | Alimorad Rashidi | Producing graphene and nanoporous graphene |
| CN105060289A (en) * | 2015-09-21 | 2015-11-18 | 中南大学 | Method for preparing fewer-layer graphene on basis of biomass waste |
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