CN104211959A - Preparation method of network polyaniline conducting active material - Google Patents
Preparation method of network polyaniline conducting active material Download PDFInfo
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- CN104211959A CN104211959A CN201410481671.4A CN201410481671A CN104211959A CN 104211959 A CN104211959 A CN 104211959A CN 201410481671 A CN201410481671 A CN 201410481671A CN 104211959 A CN104211959 A CN 104211959A
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- aniline
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Abstract
The invention discloses a preparation method of a network polyaniline conducting active material. The method comprises the following steps: dispersing 0.5mL of aniline in a beaker containing 50mL of deionized water by ultrasonic for 1 hour to obtain an aniline ultrasonic dispersion solution; weighing a certain amount of phytic acid, adding into the aniline ultrasonic dispersion solution, carrying out ultrasonic dispersion for 1 hour to obtain an aniline-phytic acid mixed solution, putting in an ice water bath, and cooling the aniline-phytic acid mixed solution to 0-5 DEG C; weighing ammonium persulfate and 5mL of 1mol/L hydrochloric acid solution, adding into a beaker containing 50mL of deionized water, and uniformly mixing to obtain a mixed solution; and dropwisely adding the mixed solution into the aniline-phytic acid mixed solution, carrying out polymerization reaction for 6 hours, carrying out vacuum filtration and washing with deionized water until the filtrate is neutral, putting the filter cake in a 50-DEG C vacuum drying oven, drying for 24 hours, grinding, and collecting to obtain the network polyaniline conducting active material.
Description
Technical field
The invention belongs to technical field of material, particularly a kind of preparation method of network-like layer/polyaniline conductive active material.The method utilizes the self-assembly property of phytic acid, and using phytic acid as polymerization activity site, preparation has the network-like layer/polyaniline conductive active material of good electrical chemical property.
Background technology
Electrical conductive activities polymkeric substance, owing to synthesizing simple, with low cost and high fake capacitance, effectively can improve the chemical property of energy storage device, obtains the concern energetically of countries in the world researcher.As the one of electrical conductive activities polymkeric substance, the chemical environment stability that polyaniline has had, the acid doping/dedoping mechanism of the redox rate be exceedingly fast and uniqueness, receives the concern energetically of Scientific Research Workers.
There is the polyaniline of network-like structure, there is very large specific surface area, the pore passage structure of shorter transport passage can be provided for electrolyte ion, and mechanical property preferably, be a kind of desirable energy storage material.The method preparing network-like polyaniline is generally divided into hard template method and soft template method.Hard template method is a kind of method that effectively can control Polyaniline, but this method needs to remove template by aftertreatment, and the complex steps of removing template, even likely destroy the structure that polyaniline has been formed.Kings etc. take bacteria cellulose as Template preparation bacteria cellulose/polyaniline composite material (Wang H, Zhu E, Yang J, et al. Bacterial cellulose nanofiber-supported polyaniline nanocomposites with flake-shaped morphology as supercapacitor electrodes [J]. The Journal of Physical Chemistry C, 2012, 116 (24): 13013-13019.), the matrix material of preparation is used as electrode material for super capacitor, pass through electro-chemical test, when to record current density be 0.2A/g, material ratio capacitance is 273 F/g.
Soft template method a kind ofly obtains the molecule of certain space structure by molecular self-assembling process and with this molecule for template carries out a kind of method of being polymerized, the method is with low cost, simple to operate, causes the interest of people.Although compared with hard template, the pattern of the netted polyaniline using soft template to be formed is not easy to control, and we can control the pattern of polyaniline by the change proportioning of reactant and the condition of polymerization, thus prepare network-like layer/polyaniline conductive active material.
The present invention makes soft template with phytic acid, utilizes the self-assembly behavior of phytic acid and carries out the oxypolymerization of polyaniline using phytic acid as polymerization activity site; Meanwhile, by optimizing the ratio of aniline and phytic acid, preparation has that pattern is homogeneous, the network-like layer/polyaniline conductive active material of good electrical chemical property.This thinking has no bibliographical information.
Summary of the invention
The object of this invention is to provide a kind of preparation method of network-like layer/polyaniline conductive active material.
Thinking of the present invention: the structural performance utilizing phytic acid, phytate molecule becomes network-like structure by H-bonding self-assembly, then aniline monomer carries out oxypolymerization with the hydroxyl in phytate molecule for polymerization activity site, prepares the layer/polyaniline conductive active material with network structure.
Concrete steps are:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 0-5 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is the one in 1:9,1:7,1:5,1:3,1:2,1:1 and 2:1.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
The inventive method preparation technology is simple, environmental protection, and prepared netted polyaniline material pattern homogeneous, there is higher specific surface area and good chemical property.
Accompanying drawing explanation
Fig. 1 is the SEM figure of network-like layer/polyaniline conductive active material prepared by the embodiment of the present invention 3.
Fig. 2 is the SEM figure of network-like layer/polyaniline conductive active material prepared by the embodiment of the present invention 4.
Fig. 3 is the constant current charge-discharge curve that the network-like layer/polyaniline conductive active material of the embodiment of the present invention 3 preparation is tested when different current density.
Fig. 4 is the cyclic voltammetry curve that the network-like layer/polyaniline conductive active material of the embodiment of the present invention 3 preparation is tested when scanning speed is 5mV/s.
Embodiment
embodiment 1:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 2:1.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 2:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:1.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 3:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:2.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 4:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:3.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 5:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:5.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 6:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:7.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
embodiment 7:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid.
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 3 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is 1:9.
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1.
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
Claims (1)
1. a preparation method for network-like layer/polyaniline conductive active material, is characterized in that concrete steps are:
(1) by the aniline ultrasonic disperse of 0.5ml in the beaker filling 50mL deionized water, ultrasonic disperse 1 hour, makes it be uniformly dispersed, obtained aniline ultrasonic disperse liquid;
(2) taking phytic acid joins in aniline ultrasonic disperse liquid prepared by step (1), ultrasonic disperse is after 1 hour, obtained aniline-phytic acid mixed solution, then obtained aniline-phytic acid mixed solution is moved in flask, and flask is positioned in ice-water bath, make the temperature of aniline-phytic acid mixed solution be down to 0-5 DEG C; The mol ratio of the phytic acid taken and the middle aniline consumption of step (1) is the one in 1:9,1:7,1:5,1:3,1:2,1:1 and 2:1;
(3) take the hydrochloric acid soln that ammonium persulphate and 5mL concentration are 1 mol/L, join in the beaker filling 50mL deionized water, mix, obtained mixing solutions; The mol ratio of the ammonium persulphate taken and the middle aniline consumption of step (1) is 1;
(4) mixing solutions that step (3) is obtained is dropwise joined in the obtained aniline-phytic acid mixed solution of step (2), polyreaction is after 6 hours, filtering and washing is carried out with deionized water, until filtrate is in neutral, gained filter cake is positioned in the vacuum drying oven of 50 DEG C, dry 24 hours, finally grind collection, i.e. obtained network-like layer/polyaniline conductive active material.
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| CN104892936A (en) * | 2015-06-18 | 2015-09-09 | 武汉大学 | Cellulose/polyaniline nano-porous composite microspheres as well as preparation method and application thereof |
| CN105720272A (en) * | 2016-02-24 | 2016-06-29 | 哈尔滨工业大学（威海） | Preparation method of nitrogen and phosphorus doubly-doping porous carbon nanofiber material for air electrode |
| CN105906805A (en) * | 2016-04-28 | 2016-08-31 | 桂林理工大学 | Method for preparing conductive polyaniline nanotubes by taking niacin as template and dopant |
| CN108659358A (en) * | 2018-05-30 | 2018-10-16 | 安徽渡江电缆集团有限公司 | A kind of safety and environmental protection electric vehicle cable |
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| CN112002946A (en) * | 2020-08-06 | 2020-11-27 | 山东科技大学 | Preparation method and application of polyaniline zinc ion battery of high-voltage platform |
| CN113308113A (en) * | 2021-05-17 | 2021-08-27 | 上海交通大学 | Porous alumina/polyaniline photo-thermal material and preparation method and application thereof |
| CN115602454A (en) * | 2022-12-12 | 2023-01-13 | 深圳市今朝时代股份有限公司（Cn） | Super capacitor pole piece and preparation method thereof |
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| CN104892936B (en) * | 2015-06-18 | 2017-03-01 | 武汉大学 | A kind of cellulose/polyaniline nano porous complex microsphere and preparation method thereof and purposes |
| CN105720272A (en) * | 2016-02-24 | 2016-06-29 | 哈尔滨工业大学（威海） | Preparation method of nitrogen and phosphorus doubly-doping porous carbon nanofiber material for air electrode |
| CN105720272B (en) * | 2016-02-24 | 2018-08-24 | 哈尔滨工业大学（威海） | A kind of air electrode nitrogen phosphorus codope porous carbon nanofiber material preparation method |
| CN105906805A (en) * | 2016-04-28 | 2016-08-31 | 桂林理工大学 | Method for preparing conductive polyaniline nanotubes by taking niacin as template and dopant |
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| CN108690288A (en) * | 2018-05-30 | 2018-10-23 | 安徽渡江电缆集团有限公司 | A kind of flame-proof cable sheath material that thermostabilization is high |
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| CN110707288A (en) * | 2018-07-10 | 2020-01-17 | 北京理工大学 | Silicon-based negative electrode active material and preparation method and application thereof |
| CN110707288B (en) * | 2018-07-10 | 2021-07-02 | 北京理工大学 | Silicon-based negative electrode active material and preparation method and application thereof |
| CN111004400A (en) * | 2019-11-01 | 2020-04-14 | 浙江大学 | Alkali-soluble chitosan-polyacrylamide-polyaniline conductive hydrogel material with adjustable conductive polymer network structure |
| CN111004400B (en) * | 2019-11-01 | 2021-04-06 | 浙江大学 | Alkali-soluble chitosan-polyacrylamide-polyaniline conductive hydrogel material with adjustable conductive polymer network structure |
| CN112002946A (en) * | 2020-08-06 | 2020-11-27 | 山东科技大学 | Preparation method and application of polyaniline zinc ion battery of high-voltage platform |
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