CN105732980A - Method for preparing polyaniline nano-tube/graphene composite with tartaric acid as template - Google Patents
Method for preparing polyaniline nano-tube/graphene composite with tartaric acid as template Download PDFInfo
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- CN105732980A CN105732980A CN201610245419.2A CN201610245419A CN105732980A CN 105732980 A CN105732980 A CN 105732980A CN 201610245419 A CN201610245419 A CN 201610245419A CN 105732980 A CN105732980 A CN 105732980A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a method for preparing a polyaniline nano-tube/graphene composite with tartaric acid as a template. The method comprises the steps of dispersing aniline into an aqueous solution containing tartaric acid, then adding self-made graphene oxide, after the materials are dispersed uniformly, adding ammonium persulfate for triggered polymerization, conducting a reaction for 12 hours at the room temperature, and adding tartaric acid again for sufficiently reducing graphene oxide, so that the polyaniline /graphene composite of a nanometer tubular structure is obtained. According to the method, tartaric acid plays two roles in the reaction process, on one hand, aniline is subjected to hydrogen bond self-assembly with tartaric acid as the template, and subsequently, the composite of the tubular structure is formed by aniline and graphite oxide through oxidation polymerization; on the other hand, the green reducing agent, namely tartaric acid, can reduce graphene oxide. The prepared polyaniline /graphene composite not only is of the nanometer tubular structure but also has good electrochemical performance. The method is simple in preparation process and environmentally friendly.
Description
Technical field
The invention belongs to technical field of composite preparation, particularly to a kind of method preparing polyaniline nanotube/graphene composite material for template with tartaric acid.
Background technology
Graphene (graphene) is the new material of a kind of monolayer laminated structure being made up of carbon atom, the flat film of to be a kind of by carbon atom with the hexangle type that sp2 hybrid orbital forms be honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness.It has very big specific surface area, excellent electric conductivity and the peculiar property such as heat conductivity, significantly high mechanical strength, it is possible to is widely used in the electrode material of battery and ultracapacitor, causes huge interest and the concern of scientist.But, Graphene, as electrode material, has low ratio electric capacity, simultaneously, Graphene and graphene oxide thereof are susceptible to stacking in the process of preparation, have impact on its dispersibility in the electrolyte and surface wettability, reduce reference area and the electrical conductivity of material.Therefore the interlamellar spacing controlling Graphene is the major subjects being currently needed for solving.
Polyaniline is a kind of common conducting polymer, has synthesis simple, and specific surface area with low cost, big, good environmental stability and significantly high theory, than electric capacity, have great application prospect as electrode material for super capacitor.But the doping of the energy storage mechnism of uniqueness and dedoping process so that it is change in volume can occur in charge and discharge process thus causing special capacity fade very fast and degradation shortcoming under cyclical stability.
Therefore, by Graphene and polyaniline are carried out compound, polyaniline is polymerized at the interlayer of Graphene, effectively hinder the stacking of Graphene, Graphene is that polyaniline provides skeleton simultaneously, enhance the mechanical performance of self, so the composite of preparation both can take into account the high electrical conductivity of Graphene, high-specific surface area and good mechanical performance, the high ratio electric capacity of polyaniline can be taken into account again.
With the Graphene of chemical preparation, main use hydrazine hydrate and sodium borohydride are as reducing agent (M.M.Sk, etal, Synthesisofgraphene/vitaminCtemplate-controlledpolyanili nenanotubescompositeforhighperformancesupercapacitorelec trode.Polymer2014,55,798-805;K.Zhang,etal,Graphene/PolyanilineNanofiberCompositesasSupercapacitorElectrodes.Chem.Mater.2010,22,1392-1401;H.J.Shin, etal, Efficientreductionofgraphiteoxidebysodiumborohydrideandi tseffectonelectricalconductance, Adv.Funct.Mater.2009,19,1987-1992.), but these reducing agents are not only poisonous, harmful, and need (about 90 DEG C) at a relatively high temperature just can give full play to reduction, preparation technology is loaded down with trivial details simultaneously.Therefore, adopt a kind of environmental protection and the reducing agent of reaction condition gentleness, graphene oxide is carried out reduction and seems very necessary.The present invention is using tartaric acid as template, aniline passes through H-bonding self-assembly, after in-situ polymerization, using tartaric acid as reducing agent (utilizing the reproducibility that tartaric acid is stronger) redox graphene, one-step method preparation has the polyaniline/graphene composite material of nano tubular structure.
Summary of the invention
It is an object of the invention to utilize tartaric template action and reduction, it is provided that a kind of method preparing polyaniline nanotube/graphene composite material for template with tartaric acid.
Concretely comprise the following steps:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance ratio of described tartaric acid and aniline is 0.1 ~ 5:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
The inventive method has the advantage that
The inventive method preparation technology is simple, environmental protection, by changing the tartaric acid amount of substance with aniline than the pattern of polyaniline nanotube, pore size and draw ratio in regulation and control polyaniline/graphene composite material.By optimizing the proportioning of tartaric acid and aniline, preparation has that pattern is homogeneous, the polyaniline/graphene nanocomposite material of certain pore size size and draw ratio, and obtained polyaniline/graphene composite material has good electrical chemical property.
Detailed description of the invention
Embodiment 1:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 0.1:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Embodiment 2:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 0.25:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Embodiment 3:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 0.5:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Embodiment 4:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 1:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Embodiment 5:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 2.5:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Embodiment 6:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain graphene oxide (GO) dispersion liquid of brown color.
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance of described tartaric acid and aniline is than for 5:1.
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor.
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
Claims (1)
1. the method preparing polyaniline nanotube/graphene composite material for template with tartaric acid, it is characterised in that concretely comprise the following steps:
(1) take the homemade graphene oxide of 0.02g and join in the beaker filled in 50mL deionized water, ultrasonic disperse 30min, obtain the graphene oxide dispersion of brown color；
(2) measure tartaric acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add 0.5mL aniline and 2mL concentration is the hydrochloric acid solution of 1mol/L, stir 0.5h when ice-water bath, prepare mixed liquor；The amount of substance ratio of described tartaric acid and aniline is 0.1 ~ 5:1；
(3) graphene oxide dispersion that step (1) prepares is joined in the mixed liquor that step (2) prepares, ice-water bath stirs 30min, obtains uniform brown color mixed liquor；
(4) ammonium persulfate solution is added dropwise in the brown color mixed liquor that step (3) prepares, 12h is at the uniform velocity stirred when ice-water bath, again add 0.6g tartaric acid and fully reduce the graphene oxide in mixed liquor, then with deionized water, mixed liquor is carried out sucking filtration, washing, until filtrate is in neutrality, again adding 2mL concentration is the hydrochloric acid solution of 1mol/L, stir when ice-water bath, finally with deionized water, product is carried out sucking filtration, washing, until filtrate is in neutrality, filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely polyaniline nanotube/graphene composite material is prepared；In described Ammonium persulfate. consumption and step (2), the amount of substance of aniline consumption ratio is for 1:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655859A (en) * | 2019-11-01 | 2020-01-07 | 陈志威 | Preparation method of anti-corrosion uniform polyaniline conductive film material |
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| CN102329976A (en) * | 2011-09-06 | 2012-01-25 | 上海交通大学 | Preparation method of graphene reinforced metal-matrix composite |
| CN104119529A (en) * | 2014-08-02 | 2014-10-29 | 桂林理工大学 | Preparation method of polyaniline/graphene composite material with nano tubular structure |
| CN104910378A (en) * | 2015-05-26 | 2015-09-16 | 浙江理工大学 | Preparation method for polyaniline/graphene oxide nanocomposite |
| WO2015148635A1 (en) * | 2014-03-25 | 2015-10-01 | Indiana University Research And Technology Corporation | Novel carbonized polyaniline-grafted silicon nanoparticles encapsulated in graphene sheets for li-ion battery anodes |
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- 2016-04-20 CN CN201610245419.2A patent/CN105732980A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329976A (en) * | 2011-09-06 | 2012-01-25 | 上海交通大学 | Preparation method of graphene reinforced metal-matrix composite |
| WO2015148635A1 (en) * | 2014-03-25 | 2015-10-01 | Indiana University Research And Technology Corporation | Novel carbonized polyaniline-grafted silicon nanoparticles encapsulated in graphene sheets for li-ion battery anodes |
| CN104119529A (en) * | 2014-08-02 | 2014-10-29 | 桂林理工大学 | Preparation method of polyaniline/graphene composite material with nano tubular structure |
| CN104910378A (en) * | 2015-05-26 | 2015-09-16 | 浙江理工大学 | Preparation method for polyaniline/graphene oxide nanocomposite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110655859A (en) * | 2019-11-01 | 2020-01-07 | 陈志威 | Preparation method of anti-corrosion uniform polyaniline conductive film material |
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Application publication date: 20160706 |