CN107151010A - A kind of method that graphene is prepared by reducing agent of leaf extract solution - Google Patents
A kind of method that graphene is prepared by reducing agent of leaf extract solution Download PDFInfo
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- CN107151010A CN107151010A CN201710426747.7A CN201710426747A CN107151010A CN 107151010 A CN107151010 A CN 107151010A CN 201710426747 A CN201710426747 A CN 201710426747A CN 107151010 A CN107151010 A CN 107151010A
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- C—CHEMISTRY; METALLURGY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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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 discloses a kind of method that graphene is prepared by reducing agent of leaf extract solution.Graphene oxide is prepared using improvement Hummers methods first, i.e., graphite oxide is prepared as oxidant using graphite powder, the concentrated sulfuric acid, potassium permanganate, hydrogen peroxide etc., graphene oxide is obtained through ultrasonic disperse, freeze-drying；Then using leaf extract solution as reducing agent and stabilizer, graphene is prepared by redox graphene.This method has that cost is low, effect is good, easy to use, advantages of environment protection.
Description
Technical field
The invention belongs to the preparation field of graphene, and in particular to one kind prepares graphene using leaf extract solution as reducing agent
Method.
Background technology
Graphene is as one kind by carbon atom with sp2The two-dimension nano materials of hybrid form formation, become current nanometer
The popular research object of science and technology subject.It is extensive because it has the mechanical, electric of uniqueness, calorifics and optical property
Applied to fields such as nanoelectronic, sensor, ultracapacitor and composites.Therefore, finding one kind can be synthesized with large area
The method of high-quality single-layer graphene becomes to be even more important.The preparation method that presently, there are has：Mechanical stripping method, chemical gaseous phase
The precipitation method, epitaxial growth method and oxidation-reduction method.Wherein, oxidation-reduction method has the advantages that cost is low and easy to operate, is current
The most method of industrialized production graphene potential quality.The reducing agent often used has hydrazine and its derivative, sodium borohydride, aluminum hydride
Lithium and hydroquinones etc., but these reducing agents have very high toxicity and danger, especially hydrazine and its derivative, Jin Jinwei
Magnitude there is damaging effect.And reaction after these hazardous wastes are handled, will greatly increase commercial scale into
This.In addition, in the case of without cosolvent, the graphene synthesized by these reducing agents is easily reunited.In a word, this
A little defect problems will have a strong impact on its application in many fields.
Current research finds that graphene nano material is in drug delivery, microbiological fuel cell, biological detection and tissue work
The application in the fields such as journey biomedicine has tremendous potential, but the graphene synthesized by above oxide-reduction method has appearance
The shortcoming easily reunited with poor biocompatibility.Accordingly, it would be desirable to environment-friendly material is explored as reducing agent redox graphene,
Efficiently prepare the graphene with biocompatibility.
Contain substantial amounts of polyphenoils in plant extraction liquid, with very strong reducing property, reduction-oxidation can be used as
The reducing agent and stabilizer of graphene, can not only avoid chemical reducing agent from occurring the phenomenon reunited in reduction process, and
Environmental protection theory is also practiced.Abundant residues leaf by the use of agricultural generation is not only easy to as the raw material for preparing graphene
Obtain, it is with low cost, and solve and the processing such as arbitrarily stack and burn the problem of cause environmental pollution, finally realize solid waste
High-qualityization is utilized.
The content of the invention
It is an object of the invention to for the shortcomings of the prior art there is provided one kind using leaf extract solution as also
The method that former agent prepares graphene.Graphene prepared by this method can improve its biocompatibility, so as to promote it in micro- life
The fields such as thing fuel cell, biological medicine and electrochemica biological sensor have certain application potential.
In order to realize foregoing invention purpose, the present invention is adopted the following technical scheme that：
A kind of method that graphene is prepared by reducing agent of leaf extract solution, comprises the following steps：
1）Graphene oxide is prepared using improvement Hummers methods；
2）The preparation of leaf extract solution：By in the leaf immersion distilled water after drying process, the ratio of leaf and distilled water for 2 ~
15 g:1L, produces leaf extract solution at 60 ~ 80 DEG C after 1 ~ 2h of heating water bath, filtering；
3）The preparation of graphene：By step 1）The graphene oxide that obtained graphene oxide is configured to 0.2g/L ~ 2g/L is water-soluble
Liquid, then adds step 2 thereto）Obtained leaf extract solution, be well mixed, 80 DEG C heat 6-8h, then through suction filtration, wash
After washing, being freeze-dried, that is, obtain graphene.
Step 1）Specially：2.00 g 800 mesh graphite powders are added in the 35 mL concentrated sulfuric acid, the h of uniform stirring 2,
Obtain mixed liquor；6 g KMnO are slowly added into mixed liquor4, the temperature of adition process holding mixed liquor is below 20 DEG C；Then
4 h are kept at 35 DEG C, the dilution of 90 mL deionized waters is slowly added to, is sufficiently stirred for 1 h, obtains dark brown suspension；Add dropwise again
Enter 30 wt%H2O2Solution, until color is changed into glassy yellow, suction filtration while hot；Washed, removed wherein with 5 wt %HCl solution
Manganese ion, and cause solution to be changed into neutral, then ultrasonic disperse, is freeze-dried 48 h, you can obtain the graphite oxide of solid-state
Alkene.
Step 2）Described leaf is the one or more of grape leaf, mulberry leaves and tea free.
Step 3）Middle graphene oxide water solution and the volume ratio of leaf extract solution are 5:1.
Graphene made from a kind of method as described above：Lamellar spacing is 1.1 ~ 1.3nm.
The leaf be in the one or more of grape leaf, mulberry leaves and tea free, such leaves of plants rich in polyphenol etc. also
Immunogenic substance.Compared with common graphite alkene, green syt reduction reduces the use of poisonous reducing agent, improves electric conductivity, biology
Compatibility and dispersibility.
Compared with prior art, the present invention has advantages below：
The graphenic surface aufwuch organic molecule that the present invention is prepared, can make it have good dispersiveness in water,
Overcome in preparation process and occur easily reuniting, the shortcomings of toxicity is greatly and cost is high；Graphenic surface pattern is smooth, and lamellar spacing is about
For 1.129 nm, the weightlessness of thermogravimetric analysis graphene prepared when being shown in 1000 °C is only 33%, and the mistake of graphene oxide
The 60%, electrochemical property test that weighs finds the oxygen of the very poor and prepared graphene modified electrode of the electric conductivity of graphene oxide
Change reduction potential and reach 209mV, illustrate that graphene prepared by the present invention has good stability and electric conductivity, so as to promote it
There is certain application potential in fields such as microbiological fuel cell, biological medicine and electrochemica biological sensors.
Brief description of the drawings
Fig. 1 is prepared graphene oxide（GO）, leaf extract solution（EL）With graphene (EL-RGO) sample drawing；
The transmission electron microscope figure of graphene oxide (a, b) and graphene (c, d) prepared by Fig. 2；
The atomic force microscopy diagram of graphene oxide (a) and graphene (b) prepared by Fig. 3.
The thermogravimetric analysis figure of graphene oxide and graphene prepared by Fig. 4；
The cyclic voltammogram of graphene oxide and graphene modified electrode prepared by Fig. 5.
Embodiment
Technical scheme is further described below by way of specific embodiment.Following embodiment is to this
That invents further illustrates, and does not limit the scope of the invention.
Embodiment 1
A kind of method that graphene is prepared by reducing agent of leaf extract solution, is concretely comprised the following steps：
1）The graphite powder for taking 2.00 g sizes to be 800 mesh is added in the 35 mL concentrated sulfuric acids, and the h of uniform stirring 2 obtains mixed liquor；It is slow
It is slow to add 6 g KMnO4, the temperature of mixed liquor is kept in adition process below 20 DEG C；It is subsequently placed in 35 DEG C of water-baths and keeps
After 4 h, the dilution of 90 mL deionized waters is slowly added to, 1 h is sufficiently stirred for, just can obtain dark brown suspension；It is gradually added into again
30wt% H2O2, until color is changed into glassy yellow, suction filtration while hot；Washed again with 5wt% HCl solution, remove manganese therein
Ion, and cause solution to be changed into neutral, then it is allowed to scattered with ultrasonic wave, is freeze-dried 48 h, you can obtain the oxidation of solid-state
Graphene；
2）The grape leaf of 1.00 g dryings is weighed, and shreds and is added in the beaker for filling 200 mL distilled water, is then put
Enter to be heated in 80 DEG C of thermostat water bath to heat 1 h, with 0.45 μm of filter membrane suction filtration, the filtrate of acquirement is that grape leaf is extracted
Liquid, it is standby；
3）Graphene oxide (GO) solid after 10 mg freeze-dryings is weighed to be added in the conical flask for filling 20 mL distilled water,
And ultrasonic 30 min is allowed to scattered, 5 mL leaf extract solution is then added to it, 80 DEG C of thermostat water bath heating 8 is put into
H, with 0.45 μm of filter membrane suction filtration, and is washed 3 times with absolute ethyl alcohol, removes the unnecessary organic matter on its surface, then remove filter membrane
On sample, then be freeze-dried 48 hours, that is, obtain dry graphene.
Embodiment 2
A kind of method that graphene is prepared by reducing agent of leaf extract solution, is concretely comprised the following steps：
1）2.00 g sizes are taken to be added to for 800 mesh graphite powders in the 35 mL concentrated sulfuric acids, the h of uniform stirring 2 obtains mixed liquor；Slowly
Add 6 g KMnO4, the temperature of mixed liquor is kept in adition process below 20 DEG C；It is subsequently placed in 35 DEG C of water-bath and keeps
After 4 h, the dilution of 90 mL deionized waters is slowly added to, 1 h is sufficiently stirred for, just can obtain dark brown suspension；It is gradually added into again
30wt% H2O2, until color is changed into glassy yellow, suction filtration while hot；Washed again with 5wt% HCl solution, remove manganese therein
Ion, and cause solution to be changed into neutral, then it is allowed to scattered with ultrasonic wave, is freeze-dried 48 h, you can obtain the oxidation of solid-state
Graphene；
2）The mulberry leaves of 2.00 g dryings are weighed, and shreds and is added in the beaker for filling 200 mL distilled water, are then put
Enter to be heated in 80 DEG C of thermostat water bath to heat 1 h, with 0.45 μm of filter membrane suction filtration, the filtrate of acquirement is tree extract solution, standby
With；
3）Graphene oxide (GO) solid after 20 mg freeze-dryings is weighed to be added in the conical flask for filling 20 mL distilled water,
And ultrasonic 30 min is allowed to scattered, 5 mL leaf extract solution is then added to it, 80 DEG C of thermostat water bath heating 8 is put into
H, with 0.45 μm of filter membrane suction filtration, and is washed 2 times with absolute ethyl alcohol, removes the unnecessary organic matter on its surface, then remove filter membrane
On sample, then be freeze-dried 48 hours, that is, obtain dry graphene.
Embodiment 3
A kind of method that graphene is prepared by reducing agent of leaf extract solution, is concretely comprised the following steps：
1）2.00 g sizes are taken to be added to for 800 mesh graphite powders in the 35 mL concentrated sulfuric acids, the h of uniform stirring 2 obtains mixed liquor；Slowly
Add 6 g KMnO4, the temperature of mixed liquor is kept in adition process below 20 DEG C；It is subsequently placed in 35 DEG C of water-bath and keeps
After 4 h, the dilution of 90 mL deionized waters is slowly added to, 1 h is sufficiently stirred for, just can obtain dark brown suspension；It is gradually added into again
30wt% H2O2, until color is changed into glassy yellow, suction filtration while hot；Washed again with 5wt% HCl solution, remove manganese therein
Ion, and cause solution to be changed into neutral, then it is allowed to scattered with ultrasonic wave, is freeze-dried 48 h, you can obtain the oxidation of solid-state
Graphene；
2）The tea free of 3.00 g dryings is weighed, and shreds and is added in the beaker for filling 200 mL distilled water, is then put
Enter to be heated in 80 DEG C of thermostat water bath to heat 1 h, with 0.45 μm of filter membrane suction filtration, the filtrate of acquirement is tree extract solution, standby
With；
3）Graphene oxide (GO) solid after 30 mg freeze-dryings is weighed to be added in the conical flask for filling 20 mL distilled water,
And ultrasonic 30 min is allowed to scattered, 5 mL leaf extract solution is then added to it, 80 DEG C of thermostat water bath heating 8 is put into
H, with 0.45 μm of filter membrane suction filtration, and is washed 3 times with absolute ethyl alcohol, removes the unnecessary organic matter on its surface, then remove filter membrane
On sample, then be freeze-dried 48 hours, that is, obtain dry graphene.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (5)
1. a kind of method that graphene is prepared by reducing agent of leaf extract solution, it is characterised in that：Comprise the following steps：
1）Graphene oxide is prepared using improvement Hummers methods；
2）The preparation of leaf extract solution：By in the leaf immersion distilled water after drying process, the ratio of leaf and distilled water for 2 ~
15 g:1L, produces leaf extract solution at 60 ~ 80 DEG C after 1 ~ 2h of heating water bath, filtering；
3）The preparation of graphene：By step 1）The graphene oxide that obtained graphene oxide is configured to 0.2g/L ~ 2g/L is water-soluble
Liquid, then adds step 2 thereto）Obtained leaf extract solution, be well mixed, 80 DEG C heat 6-8h, then through suction filtration, wash
After washing, being freeze-dried, that is, obtain graphene.
2. the method according to claim 1 that graphene is prepared by reducing agent of leaf extract solution, it is characterised in that：Step
1）Specially：2.00 g 800 mesh graphite powders are added in the 35 mL concentrated sulfuric acid, the h of uniform stirring 2 obtains mixed liquor；It is past mixed
Close in liquid and be slowly added to 6 g KMnO4, the temperature of adition process holding mixed liquor is below 20 DEG C；Then 4 h are kept at 35 DEG C,
The dilution of 90 mL deionized waters is slowly added to, 1 h is sufficiently stirred for, obtains dark brown suspension；30 wt%H are added dropwise again2O2It is molten
Liquid, until color is changed into glassy yellow, suction filtration while hot；Washed with 5 wt %HCl solution, remove manganese ion therein, and make
Obtain solution and be changed into neutral, then ultrasonic disperse, is freeze-dried 48 h, you can obtain the graphene oxide of solid-state.
3. the method according to claim 1 that graphene is prepared by reducing agent of leaf extract solution, it is characterised in that：Step
2）Described leaf is the one or more of grape leaf, mulberry leaves and tea free.
4. the method according to claim 1 that graphene is prepared by reducing agent of leaf extract solution, it is characterised in that：Step
3）Middle graphene oxide water solution and the volume ratio of leaf extract solution are 5:1.
5. graphene made from a kind of method as described in claim any one of 1-4, it is characterised in that：Lamellar spacing be 1.1 ~
1.3nm。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108906131A (en) * | 2018-06-29 | 2018-11-30 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of composite photocatalyst material |
| CN109331775A (en) * | 2018-10-09 | 2019-02-15 | 福建师范大学 | A kind of graphene-supported Nanoscale Iron/nickel composite material of green syt and preparation method |
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| CN103910355A (en) * | 2014-04-28 | 2014-07-09 | 南京新月材料科技有限公司 | Preparation method of porous three-dimensional graphene |
| CN105036123A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Preparation method of hemicellulose-based graphene |
| CN105236391A (en) * | 2015-08-28 | 2016-01-13 | 华南理工大学 | Method of preparing graphene with lignin solution |
| CN105253873A (en) * | 2015-08-26 | 2016-01-20 | 苏州卓伟企业管理咨询有限公司 | Green reduction method for graphene oxide |
| CN106744824A (en) * | 2015-11-19 | 2017-05-31 | 青岛智信生物科技有限公司 | The green restoring method of graphene oxide |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103910355A (en) * | 2014-04-28 | 2014-07-09 | 南京新月材料科技有限公司 | Preparation method of porous three-dimensional graphene |
| CN105036123A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Preparation method of hemicellulose-based graphene |
| CN105253873A (en) * | 2015-08-26 | 2016-01-20 | 苏州卓伟企业管理咨询有限公司 | Green reduction method for graphene oxide |
| CN105236391A (en) * | 2015-08-28 | 2016-01-13 | 华南理工大学 | Method of preparing graphene with lignin solution |
| CN106744824A (en) * | 2015-11-19 | 2017-05-31 | 青岛智信生物科技有限公司 | The green restoring method of graphene oxide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108906131A (en) * | 2018-06-29 | 2018-11-30 | 佛山腾鲤新能源科技有限公司 | A kind of preparation method of composite photocatalyst material |
| CN109331775A (en) * | 2018-10-09 | 2019-02-15 | 福建师范大学 | A kind of graphene-supported Nanoscale Iron/nickel composite material of green syt and preparation method |
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Application publication date: 20170912 |