CN104464888B - Sulfonated macromolecule/graphene nanocomposite and manufacturing method and application thereof - Google Patents
Sulfonated macromolecule/graphene nanocomposite and manufacturing method and application thereof Download PDFInfo
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- CN104464888B CN104464888B CN201310443373.1A CN201310443373A CN104464888B CN 104464888 B CN104464888 B CN 104464888B CN 201310443373 A CN201310443373 A CN 201310443373A CN 104464888 B CN104464888 B CN 104464888B
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- graphene
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Abstract
The invention discloses a sulfonated macromolecule/graphene nanocomposite and a manufacturing method and application of the sulfonated macromolecule/graphene nanocomposite. The manufacturing method of the sulfonated macromolecule/graphene nanocomposite includes the following steps that oxidized graphene and sulfonated macromolecules are mixed in a solvent, so that a mixed solution is acquired; a reducing agent is added to the mixed solution for a reduction reaction, and the sulfonated macromolecule/graphene nanocomposite is acquired, wherein the sulfonated macromolecule/graphene nanocomposite comprises the graphene and the sulfonated macromolecules evenly dispersed between graphene layers. When the oxidized graphene is reduced to the graphene through hydrazine, due to the fact that the sulfonated macromolecules are evenly inserted into the portions between the oxidized graphene layers in a penetrating mode, when the reduction reaction is conducted, the sulfonated macromolecules cannot be extruded by the graphene, and the proportion of the graphene added to the sulfonated macromolecules can be greatly increased.
Description
Technical field
The present invention relates to graphene composite material, particularly relate to a kind of sulfonated polymer/graphene nanocomposite material
And its preparation method and application.
Background technology
Tin indium oxide (ITO) transparent conductive film is wide in the electronic devices such as solaode, touch screen, flat faced display
General application, but the raw material indium preparing tin indium oxide (ITO) transparency electrode is rare precious metals, and tin indium oxide (ITO) is nothing
Machine sull, in fragility, limits its application in flexible touch screen.
After 2004 Univ Manchester UK's research worker prepare monoatomic layer Graphene first, Graphene shows
Excellent electric property started research boom in the whole world.Graphene is that the hexagonal honeycomb lattice plane that carbon atom is formed is empty
In the monoatomic layer bidimensional material that rearranges, be also called monoatomic layer graphite, its existing height of the structures shape of its uniqueness
Toughness, has again high rigidity, and chemical stability is good, optically and electrically excellent performance.The visible-light absorptivity of monoatomic layer Graphene
It is only 2.3%, theoretical surface resistance 20 Ω-1.The optically and electrically performance that Graphene is excellent, high-flexibility and abundant raw material, make
It becomes the preferable substitution material of tin indium oxide (ITO).When using Graphene to prepare transparent conductive film, need Graphene
Mix with macromolecular material.But, often produce the phenomenon of gathering when graphene dispersion is in macromolecule, cause and added
Graphene ratio is the lowest.
Summary of the invention
Based on this, it is necessary to provide sulfonated polymer/graphene nanocomposite material that a kind of Graphene content is higher.
A kind of sulfonated polymer/graphene nanocomposite material, including Graphene be dispersed in described graphene layer
Between sulfonated polymer, described Graphene constitutes a conductive network.
Wherein in an embodiment, described sulfonated polymer is the macromolecule with sulfonate radical segment.
Wherein in an embodiment, described sulfonated polymer is selected from sulfonated polyimide (Sulfonated
Polyimide), sulfonation polydiacetylene (sulfonated poly-diacetylene) and sulfonation poly-(vinyl alcohol)
One in (sulfonated poly (vinyl alcohol)).
Wherein in an embodiment, described Graphene makes an addition to described sulfonated polymer/graphene nanocomposite material
Percentage by weight be 0.1%～1%.
The preparation method of a kind of sulfonated polymer/graphene nanocomposite material, comprises the steps:
Graphene oxide and sulfonated polymer are mixed to get mixed solution in a solvent；And
In described mixed solution, addition reducing agent carries out reduction reaction and obtains sulfonated polymer/graphene nano composite wood
Material, described sulfonated polymer/graphene nanocomposite material includes Graphene and is dispersed between described stone graphene layer
Sulfonated polymer.
Wherein in an embodiment, described sulfonated polymer is the macromolecule having sulfonate radical segment.
Wherein in an embodiment, described sulfonated polymer is selected from sulfonated polyimide (Sulfonated
Polyimide), sulfonation polydiacetylene (sulfonated poly-diacetylene), sulfonation poly-(vinyl alcohol)
One in (sulfonated poly (vinyl alcohol)).
Wherein in an embodiment, described Graphene is at the weight of described sulfonated polymer/graphene nanocomposite material
Amount percentage ratio is 0.1%～1%.
Wherein in an embodiment, described solvent is selected from deionized water, dimethyl sulfoxide, dimethylformamide, N-first
One in base ketopyrrolidine and ethanol.
Wherein in an embodiment, it is 1mg/ml that described graphene oxide makes an addition to the concentration in described mixed solution.
Wherein in an embodiment, described reducing agent is diamine.
Wherein in an embodiment, in described mixed solution, addition reducing agent carries out reduction reaction and obtains sulfonation high score
The step of son/graphene nanocomposite material is, according to the ratio of graphene oxide Yu diamine be 200mg/mL (50% concentration
Diamine) in described mixed solution, add diamine, add stirring 1 minute the temperature of 25 DEG C, be heated at 100 DEG C backflow afterwards
React 2 hours, isolated and purified, and then obtain sulfonated polymer/graphene nanocomposite material.
The application on contact panel of the described sulfonated polymer/graphene nanocomposite material.
When graphene oxide is reduced into Graphene by reducing agent, uniformly it is interspersed in graphite oxide due to sulfonated polymer
The interlayer of alkene, therefore when carrying out reduction reaction, sulfonated polymer will not be squeezed by Graphene, and graphite therefore can be significantly increased
Alkene makes an addition to the ratio in macromolecule.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart of the sulfonated polymer/graphene nanocomposite material of an embodiment；
Fig. 2 is the preparation method simulation drawing of the sulfonated polymer/graphene nanocomposite material of an embodiment；
Fig. 3 is the sulfonated polymer/graphene nanocomposite material dispersion situation contrast with pure Graphene of an embodiment
Photo；
Fig. 4 is the sulfonated polymer/graphene nanocomposite material fourier infrared light with pure Graphene of an embodiment
Spectrogram；And
Fig. 5 is the TEM photo of the sulfonated polymer/graphene nanocomposite material of embodiment 1.
Wherein, description of reference numerals is as follows:
S101, S102 step
Detailed description of the invention
Sulfonated polymer/the graphene nanocomposite material of one embodiment, including Graphene be dispersed in described
Sulfonated polymer between graphene layer, described Graphene constitutes a conductive network.
Preferably, sulfonated polymer is the macromolecule with sulfonate radical segment.
Preferably, sulfonated polymer is selected from sulfonated polyimide
Sulfonation polydiacetylene
Sulfonated polyethylene alcohol (One in).
The ratio of its sulfonation, will have a certain impact for dilute being scattered in solution of graphite oxide.Wherein, the ratio of n/m
Example is preferably 4/1；It is more highly preferred to, n=80；m=20.
Preferably, Graphene is 0.1～1wt% at the percentage by weight of sulfonated polymer/graphene nanocomposite material.
Please refer to Fig. 1 and Fig. 2, the preparation method of above-mentioned sulfonated polymer/graphene nanocomposite material, including such as
Lower step:
Step S101, graphene oxide and sulfonated polymer are mixed to get mixed solution in a solvent.
For example, it is possible to graphene oxide and sulfonated polymer are separately added in different vessels, and it are separately added into solvent and enter
Row dispersion and dissolving.The dilute solvent of dissolved oxygen graphite can be selected from deionized water, dimethyl sulfoxide (DMSO), dimethyl formyl
One in amine (DMF), N-Methyl pyrrolidone (NMP) and ethanol.The solvent dissolving sulfonated polymer can select dimethyl
Sulfoxide (DMSO) or N-Methyl pyrrolidone (NMP) one of which.Preferably graphite oxide is dilute is to use ultrasonic wave concussion dispersion,
Fully mix in dilute for homodisperse graphite oxide progressively instillation sulfonated polymer again.Graphene oxide is in a solvent
Preferred concentration is 1mg/mL, and the preferred concentration of sulfonated polymer is 200mg/mL.Graphite oxide is dilute makes an addition to sulfonated polymer
Ratio can be from 0.1wt% to 1wt%.On material, graphene oxide through being commercially available, or can use improvement
Hummers method prepares peeling off after graphite oxidation.
The dilute greatest problem faced with macromolecule of graphite is compatibility.Composite described in existing document, its
The dilute ratio of graphite of institute's blending is the lowest, and the graphite under at high proportion is dilute, and the phenomenon of gathering can be caused again to produce, therefore
How will graphite is dilute at high proportion is dispersed in macromolecule, will be a great problem.
Referring to Fig. 3, pure graphite is dilute is dispersed in water and stands 1 hour, i.e. can be seen that the generation of the rare sedimentation of graphite.
And be scattered in sulfonation pi solution when graphite is dilute, under the identical time, not finding the rare sedimentation phenomenon of graphite, this is
Because the surface of Graphene also exists relatively multiple polar group (such as-COOH ,-OH etc.), these polar groups can be with sulfonic acid
Root (-SO3H) Hyarogen-bonding is produced.As shown in Figure 4, when the graphite of 1wt% dilute importing sulfonation pi, its-OH group
Can be toward high wave number direction displacement, the existence of its hydrogen the most provable mirror active force.And by this active force, the Graphene after reduction
It can be uniformly dispersed in polymer system.
Step S102, carry out reduction reaction and obtain sulfonated polymer/graphene nano toward mixed solution adds reducing agent
Composite, described sulfonated polymer/graphene nanocomposite material includes single-layer graphene and dilute with Multi-layer graphite uniform point
It is dispersed in sulfonated polymer.
Preferably, reducing agent is diamine (Hydrazine).
For example, it is possible at a temperature of 25 DEG C, be that the ratio of 1g:5mL is toward mixed solution according to graphene oxide and diamine
Middle addition mass concentration is the diamine of 50%, stirs 1 minute, is heated to back flow reaction 2 hours at 100 DEG C afterwards, isolated and purified,
And then obtain sulfonated polymer/graphene nanocomposite material.
In said method, when graphene oxide is reduced into Graphene by diamine, owing to sulfonated polymer uniformly interts
In the interlayer of graphene oxide, therefore when carrying out reduction reaction, sulfonated polymer will not be squeezed by Graphene, therefore can be big
Width increases Graphene and makes an addition to the ratio in macromolecule.It addition, the feature of said method is single step reaction generates nano combined material
Material, and the Graphene of first making in non-existing document makes an addition in macromolecule again, this not only eliminates a step, additionally also
Graphene can be substantially improved and make an addition to high molecular ratio.
Sulfonated polymer/the graphene nanocomposite material of present embodiment has excellent light transmission and electric conductivity, because of
This can apply to contact panel to replace tin indium oxide (ITO).
Further illustrate below by way of specific embodiment.
Embodiment 1
By 0.1wt% graphite dilute/sulfonation pi composite as a example by, first 10mg graphene oxide is scattered in
In the deionized water of 10ml, carry out ultrasonic vibration 30 minutes, it addition, sulfonation pi 90mg to be added the dimethyl of 0.45ml
Sulfoxide (DMSO), and stir 30 minutes.Afterwards by graphite oxide weak solution, slowly instill in sulfonation pi solution, and hold
Continuous stirring i.e. can get mixed solution in 15 minutes.Then the diamine of about 0.05ml mass concentration 50% is joined in mixed solution,
Back flow reaction 2 hours at a temperature of 100 DEG C, make graphene oxide be reduced into Graphene, are then peeled off purification, dry, obtain
Sulfonation pi/graphene nanocomposite material.
Referring to Fig. 5, the TEM(of the sulfonation sulfonation pi/graphene nanocomposite material showing embodiment 1 is saturating
Penetrate ultramicroscope) photo.As shown in Figure 5, nano level graphene uniform is scattered in sulfonation sulfonation pi interlayer.
The PGSTAT30 type electric conductivity instrument using Autolab is measured, and the sulfonated polymer/graphene nano of the present embodiment is multiple
The electrical conductivity of condensation material is 0.145S/cm.
Table one
| Sample | Electrical conductivity (S/cm) |
| SPI | 0.137 |
| SPI/0.1wt% Graphene | 0.145 |
| SPI/0.3wt% Graphene | 0.155 |
| SPI/0.5wt% Graphene | 0.218 |
| SPI/1wt% Graphene | 0.361 |
In table 1, the electric conductivity being not added with the dilute sulfonation pi (SPI) of graphite is 0.137S/cm, along with graphite is dilute
Increasing, its conductivity also can and then promote.When graphite is dilute add 1wt% to time, electric conductivity is up to 0.361S/cm.Compared to not adding
Adding the sulfonation pi that graphite is dilute, the electric conductivity of SPI/1wt% Graphene improves the amplitude close to three times, it is accordingly obvious that
Explanation graphite dilute can effectively promote entirety electric conductivity.
It addition, sulfonation polydiacetylene/graphite is dilute, dilute with sulfonated polyethylene alcohol/graphite, all it is referred to the step of embodiment 1
Suddenly nano composite material is obtained.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (13)
1. the preparation method of sulfonated polymer/graphene nanocomposite material, it is characterised in that comprise the steps:
Directly graphene oxide and sulfonated polymer are mixed to get mixed solution in a solvent；And
In described mixed solution, addition reducing agent carries out reduction reaction and obtains sulfonated polymer/graphene nanocomposite material,
Described sulfonated polymer/graphene nanocomposite material includes that Graphene and the sulfonation being dispersed between described graphene layer are high
Molecule.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 1, it is characterised in that
Described sulfonated polymer is the macromolecule with sulfonate radical segment.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 2, it is characterised in that
Described sulfonated polymer one in sulfonated polyimide, sulfonation polydiacetylene and sulfonated polyethylene alcohol.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 1, it is characterised in that
Described Graphene is 0.1%～1% at the percentage by weight of described sulfonated polymer/graphene nanocomposite material.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 1, it is characterised in that
Described solvent one in deionized water, dimethyl sulfoxide, dimethylformamide, N monomethyl ketopyrrolidine and ethanol.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 1, it is characterised in that
Described graphene oxide concentration in described mixed solution is 1mg/mL.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 1, it is characterised in that
Described reducing agent is diamine.
The preparation method of sulfonated polymer/graphene nanocomposite material the most according to claim 7, it is characterised in that
In described mixed solution, addition reducing agent carries out reduction reaction and obtains the step of sulfonated polymer/graphene nanocomposite material
For: at a temperature of 25 DEG C, according to the ratio that described graphene oxide and described diamine are lg:5mL toward in described mixed solution
Adding mass concentration is the diamine of 50%, stirs 1 minute, is heated to back flow reaction 2 hours at 100 DEG C afterwards, isolated and purified, enters
And obtain sulfonated polymer/graphene nanocomposite material.
9. sulfonated polymer/the graphene nanocomposite material prepared by the method for a claim 1, it is characterised in that bag
Including Graphene and the sulfonated polymer being dispersed between described graphene layer, described Graphene constitutes a conductive network.
Sulfonated polymer/graphene nanocomposite material the most according to claim 9, it is characterised in that described sulfonation is high
Molecule is the macromolecule with sulfonate radical segment.
11. sulfonated polymer/graphene nanocomposite materials according to claim 10, described sulfonated polymer is selected from sulphur
Change the one in polyimides, sulfonation polydiacetylene, sulfonated polyethylene alcohol.
12. sulfonated polymer/graphene nanocomposite materials according to claim 9, it is characterised in that described Graphene
Percentage by weight at described sulfonated polymer/graphene nanocomposite material is 0.1%～1%.
13. 1 kinds of sulfonated polymer/graphene nanocomposite material according to claim 9 answering on contact panel
With.
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| TW103129163A TWI568781B (en) | 2013-09-25 | 2014-08-25 | Sulfonated polymer/graphene nano-composite material and its preparation method and application |
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| CN105001581A (en) * | 2015-07-14 | 2015-10-28 | 安徽雄亚塑胶科技有限公司 | TPE composition and high-performance sealing material obtained from same |
| CN105273403B (en) * | 2015-10-13 | 2017-11-24 | 中国科学院宁波材料技术与工程研究所 | A kind of high conductivity polyimides graphene composite material and preparation method thereof |
| CN113201246A (en) * | 2021-04-24 | 2021-08-03 | 深圳市撒比斯科技有限公司 | High-conductivity photosensitive electronic ink |
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| CN102544542A (en) * | 2010-12-30 | 2012-07-04 | 财团法人工业技术研究院 | Organic-inorganic hybrid composite proton exchange membrane with low penetration rate |
| CN102723209A (en) * | 2012-05-25 | 2012-10-10 | 上海第二工业大学 | Preparation method for graphene nanosheet/conducting polymer nanowire composite material |
| CN102989420A (en) * | 2012-12-11 | 2013-03-27 | 湖南大学 | Sulfonylation graphene oxide magnetic adsorbent, and preparation method and application thereof |
| TW201326329A (en) * | 2011-12-28 | 2013-07-01 | Taiwan Textile Res Inst | Transparent conductive coating solution/thin film and preparation methods thereof |
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| US20110186789A1 (en) * | 2008-05-22 | 2011-08-04 | The University Of North Carolina At Chapel Hill | Synthesis of graphene sheets and nanoparticle composites comprising same |
| TWI577078B (en) * | 2012-06-29 | 2017-04-01 | 財團法人工業技術研究院 | Bilayer complex proton exchange membrane and membrane electrode assembly |
| CN103849008B (en) * | 2012-11-29 | 2018-04-13 | 深圳先进技术研究院 | Hybrid particulates, polymer matrix composite and preparation method and application |
| CN103091318B (en) * | 2013-02-07 | 2015-01-21 | 哈尔滨工业大学 | Preparation method of grapheme/polydiacetylene composite film and method for quantitatively detecting gas organic by applying composite film |
| CN103219533B (en) * | 2013-04-12 | 2015-09-30 | 清华大学深圳研究生院 | A kind of composite graphene ion exchange membrane for flow battery and preparation method thereof |
| CN103435828B (en) * | 2013-07-31 | 2018-02-27 | 复旦大学 | Graphene oxide silicon dioxide compound/polymer hybridization proton exchange membrane of sulfonation and preparation method thereof |
| CN103746130B (en) * | 2014-01-15 | 2015-11-18 | 天津工业大学 | A kind of preparation method of fuel cell hollow fiber conduit |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102544542A (en) * | 2010-12-30 | 2012-07-04 | 财团法人工业技术研究院 | Organic-inorganic hybrid composite proton exchange membrane with low penetration rate |
| TW201326329A (en) * | 2011-12-28 | 2013-07-01 | Taiwan Textile Res Inst | Transparent conductive coating solution/thin film and preparation methods thereof |
| CN102723209A (en) * | 2012-05-25 | 2012-10-10 | 上海第二工业大学 | Preparation method for graphene nanosheet/conducting polymer nanowire composite material |
| CN102989420A (en) * | 2012-12-11 | 2013-03-27 | 湖南大学 | Sulfonylation graphene oxide magnetic adsorbent, and preparation method and application thereof |
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