CN105255176A - Preparation method for carbon material-conducting polymer with controllable appearance - Google Patents
Preparation method for carbon material-conducting polymer with controllable appearance Download PDFInfo
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- CN105255176A CN105255176A CN201510650794.0A CN201510650794A CN105255176A CN 105255176 A CN105255176 A CN 105255176A CN 201510650794 A CN201510650794 A CN 201510650794A CN 105255176 A CN105255176 A CN 105255176A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
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- 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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- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/16—Cyclodextrin; Derivatives thereof
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Abstract
The invention provides a preparation method for a carbon material-conducting polymer with the controllable appearance, and belongs to the technical field of nanometer material production. Aniline monomers, aqueous hydrochloric acid solutions and ammonium persulfate are mixed for reacting, centrifugation is performed to take solid phases, and the solid phases are washed and dried to obtain polyaniline; poly-beta-cyclodextrin is dispersed into deionized water, concentrated hydrochloric acid and the aniline monomers are added for reacting, then the ammonium persulfate are added for continuous reacting, and after centrifuging, washing and drying are performed, poly-beta-cyclodextrin-polyaniline is obtained; carbon nanotubes and the poly-beta-cyclodextrin are mixed, ground and dispersed into the deionized water, the concentrated hydrochloric acid, the aniline monomers and the ammonium persulfate are added, centrifuging, washing and drying are performed after reacting is completed, and the carbon material-conducting polymer is obtained. According to the preparation method, the high-purity binary supercapacitor nanomaterial can be obtained.
Description
Technical field
The invention belongs to nano material production technical field, be specifically related to the method for producing polymer of carbon material and conduction.
Background technology
In ultracapacitor, maximum electrode materialss is used to be exactly the carbon material with vesicular structure and high-specific surface area.So far the carbon material reported has gac, carbon fiber, carbon black, charcoal-aero gel, carbon nanotube and Graphene etc.Carbon-based material utilizes electrostatic double layer energy storage, namely insert electrode surface in electrolytic solution and solution both sides and understand the equal and sheath that symbol is contrary of distributed charge quantity, define two charge layers in the solution with on electrode, the electrostatic double layer that Here it is often says, thus alternate generation potential difference, the specific surface area therefore by increasing carbon material increases the ratio capacitance of electrical condenser.
In recent years, metal oxide receives much concern with its good chemical property; Conductive polymers is then with advantage rapid temperature increases such as good electron conduction, little internal resistance and height ratio capacities.Can be found out by the research direction of electrode material for super capacitor in recent years, the development trend of electrode materials mainly contains both direction: the Composite of (1) material: utilize the synergy between differing materials, by modes such as the compound between differing materials, doping, to obtaining the electrode materials of excellent performance.(2) nanometer of material: nanometer materials not only have high specific surface area, and electronics, ion transport the evolving path can be improved, thus improve electrode performance.
Therefore, it is expected to the application of nanocomposite in ultracapacitor and there is better prospect.
Summary of the invention
The object of the invention is to the preparation method of the carbon material/conductive polymers proposing a kind of morphology controllable.
The present invention includes following steps:
1) prepare conductive polymer polyanaline (PANI): by aniline monomer and combined, then add ammonium persulphate and react, question response terminates rear centrifugal, gets solid phase washing, dries, obtain polyaniline;
2) the poly-beta-cyclodextrin/polyaniline of preparation: under ultrasound condition, poly-beta-cyclodextrin is scattered in deionized water, then concentrated hydrochloric acid and aniline monomer is added, add ammonium persulphate after question response terminates again and continue reaction, reaction terminates rear centrifugal, get solid phase washing, dry, obtain poly-beta-cyclodextrin/polyaniline;
3) carbon material/conductive polymers is prepared: after carbon nanotube and poly-beta-cyclodextrin mixed grinding, be scattered under ultrasound condition in deionized water, and then add concentrated hydrochloric acid and aniline monomer, ammonium persulphate, carry out stirring reaction, reaction terminates rear centrifugal, get solid phase washing, dry, obtain carbon material/conductive polymers.
Advantage of the present invention is: the plant and instrument of employing is simple, and preparation cost is low, and operating process is easy, reaction process material requested low toxicity, harmless, and effectively can control the pattern of matrix material, obtains highly purified binary ultracapacitor nano material.The binary ultracapacitor nano material made, diameter 50 ~ 200nm, length 100 ~ 300nm, pattern is homogeneous, has great specific surface area.
In addition, react in step 1) of the present invention and carry out under the temperature of reaction system is 30 ~ 50 DEG C of conditions, prepared Polyaniline is homogeneous, in the process preparing carbon nano-tube/poly aniline further, well control pattern.
Described step 2) in, described ultrasonic frequency is 50 ~ 55KHz.Reaction is carried out under the temperature of reaction system is 30 ~ 50 DEG C of conditions.Can ensure that reactant can disperse in a solvent, fully to contact uniformly, react completely.
Described step 2) in, the feed ratio of described carbon nanotube, beta-cyclodextrin monomer and aniline monomer is 0.05 ~ 0.1g: 0.5 ~ 1.0g: 10 ~ 200uL.Mixture carbon nano-tube/poly aniline synthesized under this ratio, carbon nanotube enters the cavity of poly-beta-cyclodextrin, utilize the interior hydrophobic outer hydrophilic character of poly-beta-cyclodextrin, by the amino load on aniline monomer on its surface, thus prepare carbon nano-tube/poly aniline binary complex.
In step 3), react and carry out under the temperature of reaction system is 20 ~ 60 DEG C of conditions, the molar ratio of described aniline monomer and poly-beta-cyclodextrin is 0.3 ~ 2: 1.This design can ensure that aniline is dispersed at poly-beta-cyclodextrin skin, is conducive to synthesizing the higher polyaniline of dispersity.
In addition, above-mentioned steps 1), 2) and 3) in, dry temperature condition is respectively 50 ~ 80 DEG C, and under this temperature condition, moisture is removed preferably, and has no adverse effects to product.
Accompanying drawing explanation
Fig. 1, Fig. 2 are respectively the transmission electron microscope picture of carbon nanotube under different amplification.
Fig. 3 is the transmission electron microscope picture of the pure polyaniline of preparation.
Fig. 4 is the transmission electron microscope picture of the poly-beta-cyclodextrin/polyaniline of preparation.
Fig. 5, Fig. 6 are respectively the transmission electron microscope picture of Polymerization of Polyaniline/carbon Nanotube under different ratios.
Embodiment
One, in order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
1, polyaniline is prepared:
Under water bath condition, mechanical stirring, 4 ~ 6mL concentrated hydrochloric acid is added in certain aqueous solution, to be mixed evenly after, add 30uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product polyaniline after oven dry.
2, the poly-beta-cyclodextrin/polyaniline (β CDP/PANI) of preparation:
Take 0.5 ~ 1.0g and gather beta-cyclodextrin in deionized water, ultrasonic disperse is even, mechanical stirring under water bath condition, adds concentrated hydrochloric acid wherein, to be mixed evenly after, add 30uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product and gathers beta-cyclodextrin/polyaniline (β CDP/PANI) after oven dry.
3, carbon material conductive polymers (PANI/CNT) is prepared:
The poly-beta-cyclodextrin of the carbon nanotube and 0.5 ~ 1.0g that take 0.05 ~ 0.1g is in mortar, and evenly, in water, ultrasonic disperse is even in grinding, transfer mechanical stirring to, water-bath, adds a certain amount of concentrated hydrochloric acid, stirs for some time, add 30uL aniline monomer, stir 3 ~ 6h, add the ammonium persulphate of 0.3 ~ 0.5g, sustained reaction 10 ~ 16h, products therefrom centrifuge washing, dries and obtains the product carbon naotube-polyaniline mixture of different ratios.
Embodiment 2
1, polyaniline is prepared:
Under water bath condition, mechanical stirring, 4 ~ 6mL concentrated hydrochloric acid is added in certain aqueous solution, to be mixed evenly after, add 50uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product polyaniline after oven dry;
2, the poly-beta-cyclodextrin/polyaniline (β CDP/PANI) of preparation:
Take 0.5 ~ 1.0g and gather beta-cyclodextrin in deionized water, ultrasonic disperse is even, mechanical stirring under water bath condition, adds concentrated hydrochloric acid wherein, to be mixed evenly after, add 50uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product and gathers beta-cyclodextrin/polyaniline (β CDP/PANI) after oven dry.
3, carbon material conductive polymers (PANI/CNT) is prepared:
The poly-beta-cyclodextrin of the carbon nanotube and 0.5 ~ 1.0g that take 0.05 ~ 0.1g is in mortar, and evenly, in water, ultrasonic disperse is even in grinding, transfer mechanical stirring to, water-bath, adds a certain amount of concentrated hydrochloric acid, stirs for some time, add 50uL aniline monomer, stir 3 ~ 6h, add the ammonium persulphate of 0.3 ~ 0.5g, sustained reaction 10 ~ 16h, products therefrom centrifuge washing, dries and obtains the product carbon naotube-polyaniline mixture of different ratios.
Embodiment 3
1, polyaniline is prepared
Under water bath condition, mechanical stirring, 4 ~ 6mL concentrated hydrochloric acid is added in certain aqueous solution, to be mixed evenly after, add 100uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product polyaniline after oven dry.
2, the poly-beta-cyclodextrin/polyaniline (β CDP/PANI) of preparation
Take 0.5 ~ 1.0g and gather beta-cyclodextrin in deionized water, ultrasonic disperse is even, mechanical stirring under water bath condition, adds concentrated hydrochloric acid wherein, to be mixed evenly after, add 100uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product and gathers beta-cyclodextrin/polyaniline (β CDP/PANI) after oven dry.
3, carbon material conductive polymers (PANI/CNT) is prepared
The poly-beta-cyclodextrin of the carbon nanotube and 0.5 ~ 1.0g that take 0.05 ~ 0.1g is in mortar, and evenly, in water, ultrasonic disperse is even in grinding, transfer mechanical stirring to, water-bath, adds a certain amount of concentrated hydrochloric acid, stirs for some time, add 100uL aniline monomer, stir 3 ~ 6h, add the ammonium persulphate of 0.3 ~ 0.5g, sustained reaction 10 ~ 16h, products therefrom centrifuge washing, dries and obtains the product carbon naotube-polyaniline mixture of different ratios.
Embodiment 4
1, polyaniline is prepared:
Under water bath condition, mechanical stirring, 4 ~ 6mL concentrated hydrochloric acid is added in certain aqueous solution, to be mixed evenly after, add 200uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product polyaniline after oven dry.
2, the poly-beta-cyclodextrin/polyaniline (β CDP/PANI) of preparation:
Take 0.5 ~ 1.0g and gather beta-cyclodextrin in deionized water, ultrasonic disperse is even, mechanical stirring under water bath condition, adds concentrated hydrochloric acid wherein, to be mixed evenly after, add 200uL aniline monomer, after treating 3 ~ 6 hours, add the ammonium persulphate of 0.3 ~ 0.5g, continue reaction 10 ~ 16h, products therefrom centrifuge washing, namely obtains product and gathers beta-cyclodextrin/polyaniline (β CDP/PANI) after oven dry.
3, carbon material conductive polymers (PANI/CNT) is prepared:
The poly-beta-cyclodextrin of the carbon nanotube and 0.5 ~ 1.0g that take 0.05 ~ 0.1g is in mortar, and evenly, in water, ultrasonic disperse is even in grinding, transfer mechanical stirring to, water-bath, adds a certain amount of concentrated hydrochloric acid, stirs for some time, add 200uL aniline monomer, stir 3 ~ 6h, add the ammonium persulphate of 0.3 ~ 0.5g, sustained reaction 10 ~ 16h, products therefrom centrifuge washing, dries and obtains the product carbon naotube-polyaniline mixture of different ratios.
Two, product checking:
As shown in Figure 1, 2, be the transmission electron microscope picture under the carbon nanotube different amplification that the present invention relates to, from figure: the diameter of carbon nanotube itself is about 30nm, the enlarged view (magnification is 50nm) of length to be 1 ~ 2um, Fig. 2 be single carbon pipe.
Fig. 3 is the transmission electron microscope picture of pure polyaniline prepared by the inventive method, and Fig. 4 is the transmission electron microscope picture of poly-beta-cyclodextrin/polyaniline prepared by the inventive method, and mean diameter is at about 50nm.
As shown in Figure 5,6, the transmission electron microscope picture of the Polymerization of Polyaniline/carbon Nanotube of the different ratios prepared for the inventive method.From figure: each routine step 3, the product that the mol ratio of different aniline monomers and beta-cyclodextrin monomer is prepared respectively presents coarse tubular structure shape:
Ratio is that the PANI/CNT diameter of 0.3:1 is approximately 60 ~ 80nm;
Ratio is that 0.5:1PANI/CNT diameter is approximately 90 ~ 100nm;
Ratio is that the PANI/CNT diameter of 1:1 is approximately 150 ~ 160nm;
Ratio is that the PANI/CNT diameter of 2:1 is approximately 180 ~ 190nm;
The present invention can find out the PANI/CNT binary complex successfully synthesizing different ratios by the size of diameter.
Claims (10)
1. a preparation method for the carbon material/conductive polymers of morphology controllable, is characterized in that comprising the following steps:
1) prepare conductive polymer polyanaline: by aniline monomer and combined, then add ammonium persulphate and react, question response terminates rear centrifugal, gets solid phase washing, dries, obtain polyaniline;
2) the poly-beta-cyclodextrin/polyaniline of preparation: under ultrasound condition, poly-beta-cyclodextrin is scattered in deionized water, then concentrated hydrochloric acid and aniline monomer is added, add ammonium persulphate after question response terminates again and continue reaction, reaction terminates rear centrifugal, get solid phase washing, dry, obtain poly-beta-cyclodextrin/polyaniline;
3) carbon material/conductive polymers is prepared: after carbon nanotube and poly-beta-cyclodextrin mixed grinding, be scattered under ultrasound condition in deionized water, and then add concentrated hydrochloric acid and aniline monomer, ammonium persulphate, carry out stirring reaction, reaction terminates rear centrifugal, get solid phase washing, dry, obtain carbon material/conductive polymers.
2. preparation method according to claim 1, is characterized in that reacting in described step 1) and carries out under the temperature of reaction system is 30 ~ 50 DEG C of conditions.
3. preparation method according to claim 1 or 2, is characterized in that in described step 1), and dry temperature condition is 50 ~ 80 DEG C.
4. preparation method according to claim 1, is characterized in that described step 2) in, described ultrasonic frequency is 50 ~ 55KHz.
5. preparation method according to claim 1, is characterized in that described step 2) in, the feed ratio of described carbon nanotube, cyclodextrin polymer and aniline monomer is 0.05 ~ 0.1g: 0.5 ~ 1.0g: 10 ~ 200uL.
6. preparation method according to claim 1, is characterized in that described step 2) in, react and carry out under the temperature of reaction system is 30 ~ 50 DEG C of conditions.
7. preparation method according to claim 1 or 4 or 5 or 6, is characterized in that described step 2) in, dry temperature condition is 50 ~ 80 DEG C.
8. preparation method according to claim 1, is characterized in that in described step 3), reacts and carry out under the temperature of reaction system is 20 ~ 60 DEG C of conditions.
9. preparation method according to claim 1, it is characterized in that in described step 3), the molar ratio of aniline monomer and cyclodextrin polymer is 0.3 ~ 2: 1.
10. preparation method according to claim 1 or 8 or 9, is characterized in that in described step 3), and dry temperature condition is 50 ~ 80 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336083A (en) * | 2018-10-15 | 2019-02-15 | 福州大学 | A kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material |
| CN111533904A (en) * | 2020-05-07 | 2020-08-14 | 安徽大学 | Preparation method of hydroxyl modified polyaniline used as supercapacitor electrode material |
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| CN103242524A (en) * | 2013-05-16 | 2013-08-14 | 东华大学 | Method of preparing polyaniline nanotube by utilizing cyclodextrin as template |
| CN103409840A (en) * | 2013-07-15 | 2013-11-27 | 东华大学 | Method for preparing polyaniline nanofiber by using cyclodextrin as template |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109336083A (en) * | 2018-10-15 | 2019-02-15 | 福州大学 | A kind of method of High Internal Phase Emulsion template controllable preparation foamy carbon/carbon nano tube compound material |
| CN109336083B (en) * | 2018-10-15 | 2021-11-26 | 福州大学 | Method for controllably preparing foam carbon/carbon nanotube composite material by high internal phase emulsion template method |
| CN111533904A (en) * | 2020-05-07 | 2020-08-14 | 安徽大学 | Preparation method of hydroxyl modified polyaniline used as supercapacitor electrode material |
| CN111533904B (en) * | 2020-05-07 | 2022-06-07 | 安徽大学 | Preparation method of hydroxyl modified polyaniline used as supercapacitor electrode material |
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