CN108010729A - The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material - Google Patents

The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material Download PDF

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CN108010729A
CN108010729A CN201711159748.6A CN201711159748A CN108010729A CN 108010729 A CN108010729 A CN 108010729A CN 201711159748 A CN201711159748 A CN 201711159748A CN 108010729 A CN108010729 A CN 108010729A
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graphene oxide
composite material
nano line
graphene
polypyrrole nano
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樊新
庞树花
陈韦良
黄烈可
方东
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Guilin University of Technology
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Guilin University of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/48Conductive polymers
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a kind of preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material.Using graphene oxide three-dimensional structure as skeleton, polypyrrole nano line array is grown in surface of graphene oxide using the electrostatic tension between the epoxy bond on the nitrogen and surface of graphene oxide of positively charged on pyrroles's segment;At the same time, Sn (II) ion of positively charged is entered between electronegative graphene oxide layer, and redox reaction occurs with graphene oxide and generates Sn (IV) ion, graphene oxide is reduced to graphene at the same time, then add sodium hydroxide solution and reaction generation nano-stannic oxide particle is deposited between the graphene layer after reduction at 180 DEG C, polypyrrole nano line array/graphene film/tin dioxide composite material is made.The method of the present invention preparation process is simple, reliable, environmentally protective, and obtained composite material has regular space structure, high-energy-density and power density, and outstanding cycle performance.

Description

The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material
Technical field
The invention belongs to novel energy field of material technology, more particularly to a kind of prepared with interfacial polymerization and hydro-thermal method surpasses The method of level capacitor polypyrrole nano line array/graphene film/tin dioxide composite material.
Background technology
Ultracapacitor is quick due to being used as with high-energy-density and power density and outstanding cycle performance etc. With the primary selection in high-power energy stocking system field.Electrode material in ultracapacitor plays the performance of ultracapacitor To vital effect, therefore, it is to prepare and develop high performance electricity to realize the widely applied most important thing of ultracapacitor Pole material.
Conducting polymer, transition metal oxide and carbon material are the common three kinds of materials of electrode material for super capacitor. It is current super electricity to overcome deficiency existing for homogenous material to prepare combination electrode material using the advantageous characteristic of these three materials One of hot spot of container electrode investigation of materials.Yuan etc. using liquid phase deposition and in-situ chemical polymerization synthesis stannic oxide/ Polypyrrole hollow microsphere compound, the material have good cycle performance(J. Yuan, et al. SnO2/ polypyrrole hollow spheres with improved cycle stability as lithium-ion battery anodes[J]. Journal of Alloys and Compounds,2017, 691: 34-39.).Liu et al. with Stannic oxide and pyrroles are raw material using hollow SnO of the hydro-thermal method synthesis with core shell structure2@PPy nanocomposites, can Effectively suppress the reunion of stannic oxide microballoon and relax the volumetric expansion of polypyrrole in charge and discharge process;In addition, cladding polypyrrole The compound of hollow structure afterwards can be more conducive to the diffusion of lithium ion with respect to stannic oxide microballoon, so as to improve composite wood The chemical property of material(R. Liu, et al. Core-shell structured hollow SnO2-polypyrrole nanocomposite anodes with enhanced cyclic performance for lithium-ion batteries[J]. Nano Energy, 2014, 6: 73-81.)The SWNTs@SnO of the preparations such as Zhao2@PPy composite materials By realizing SnO2Change with Sn completely reversibilities and obtain outstanding chemical property(Good capacity retention ratio and outstanding times Rate performance)(Y. Zhao, et al. Fully reversible conversion between SnO2 and Sn in SWNTs@SnO2@PPy coaxial nanocable as high performance anode material for lithium ion batteries[J]. J. Phys. Chem. C, 2012, 116 (35): 18612-18617.).
Therefore high-performance super capacitor electrode material is prepared for it in electrochemical energy storage using simple synthetic technology The application in field is of great significance.The present invention is with three-dimensional graphene oxide, SnCl2It is raw material with pyrroles, is gathered using interface Legal and hydro-thermal method prepares polypyrrole nano line array/graphene film/tin dioxide composite material.Gained composite material has rule Whole space arrangement, good dispersiveness, high-energy-density and power density, outstanding cycle performance, are a kind of preferably super Level capacitor electrode material, is especially suitable for industrialized production.
The content of the invention
The object of the present invention is to provide a kind of system of polypyrrole nano line array/graphene film/tin dioxide composite material Preparation Method.
Thinking of the present invention:Using graphene oxide three-dimensional structure as skeleton, nitrogen and oxidation using positively charged on pyrroles's segment The electrostatic tension between epoxy bond on graphene surface grows polypyrrole nano line array in surface of graphene oxide, effectively Prevent the reunion of graphene oxide;Meanwhile Sn (II) ion of positively charged is entered between electronegative graphene oxide layer, And redox reaction occurs with graphene oxide and generates Sn (IV) ion, while graphene oxide is reduced to graphene, Then add sodium hydroxide solution and reaction generation nano-stannic oxide particle is deposited on the graphene after reduction at 180 DEG C Between layer(The effective reunion for preventing graphene), finally obtained polypyrrole nano line array/graphene film/stannic oxide is multiple Condensation material.
Concretely comprise the following steps:
(1)Three-dimensional graphene oxide is dissolved in deionized water, three-dimensional graphene oxide solution is made in 10 min of ultrasound, is Water phase.
(2)Pyrroles after purification is dissolved in chloroform oil phase is made, with step(1)Obtained water mixes, using boundary Face polymerization, reacts 24 h at 0 ~ 5 DEG C, and oil-water interfaces blackish green product occur, after filtered, washing, done at 60 DEG C Dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution and HI solution, are transferred in autoclave after being ultrasonically treated 5 min, react 4 at 180 DEG C H, is subsequently cooled to room temperature and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution, after being ultrasonically treated 5 min, is reacted at 180 DEG C 2 h, after cooled to room temperature, products therefrom is dried after being washed with deionized to neutrality, that is, polypyrrole nanometer is made Linear array/graphene film/tin dioxide composite material.
The mass ratio of pyrroles and three-dimensional graphene oxide after the purification are 0.1 ~ 4:1;The SnCl2With the thing of NaOH The ratio between amount of matter is 1:4;The mass ratio of the three-dimensional graphene oxide and HI is 1:2.56;The stannic oxide is aoxidized with three-dimensional The mass ratio of graphene is 0.1 ~ 2:1.
The method of the present invention preparation process is simple, reliable, environmentally protective, and there is obtained composite material regular space to tie Structure, high-energy-density and power density, and outstanding cycle performance, are a kind of preferable electrode material for super capacitor, especially It is adapted to industrialized production.
Brief description of the drawings
Fig. 1 is obtained polypyrrole nano line array/graphene film/tin dioxide composite material in the embodiment of the present invention 11 Scanning electron microscope (SEM) photograph.
Embodiment
Embodiment 1:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 0.0629 g SnCl2)With the HI solution of 10 mL, 1 M, shifted after being ultrasonically treated 5 min Into autoclave, 4 h are reacted at 180 DEG C, room temperature is subsequently cooled to and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 0.0531 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 2:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 0.1258 g SnCl2)With the HI solution of 10 mL, 1 M, shifted after being ultrasonically treated 5 min Into autoclave, 4 h are reacted at 180 DEG C, room temperature is subsequently cooled to and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 0.1062 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 3:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 0.1573 g SnCl2)With the HI solution of 10 mL, 1 M, shifted after being ultrasonically treated 5 min Into autoclave, 4 h are reacted at 180 DEG C, room temperature is subsequently cooled to and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 0.1327 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 4:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 0.3145 g SnCl2)With the HI solution of 10 mL, 1 M, shifted after being ultrasonically treated 5 min Into autoclave, 4 h are reacted at 180 DEG C, room temperature is subsequently cooled to and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 0.2654 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 5:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 0. 6290 g SnCl2)With the HI solution of 10 mL, 1 M, turn after being ultrasonically treated 5 min Move in autoclave, 4 h are reacted at 180 DEG C, be subsequently cooled to room temperature and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 0.5308 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 6:
(1)0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, three-dimensional graphite oxide is made in 10 min of ultrasound Alkene solution, is water phase.
(2)Pyrroles after 0.05 g is purified, which is dissolved in 50 mL chloroforms, is made oil phase, with step(1)Obtained water phase Mixing, using interfacial polymerization, reacts 24 h at 3 DEG C, and substantial amounts of blackish green product occur in oil-water interfaces, filtered, wash After washing, dry 12 h, that is, be made polypyrrole nano line/graphene oxide composite material at 60 DEG C.
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is filled Divide stirring is lower to add SnCl2Solution(Containing 1.2580 g SnCl2)With the HI solution of 10 mL, 1 M, shifted after being ultrasonically treated 5 min Into autoclave, 4 h are reacted at 180 DEG C, room temperature is subsequently cooled to and mixed solution is made.
(4)To step(3)NaOH solution is added in obtained mixed solution(Containing 1.0616 g NaOH), it is ultrasonically treated 5 After min, 2 h are reacted at 180 DEG C, after cooled to room temperature, products therefrom is done after being washed with deionized to neutrality It is dry, that is, polypyrrole nano line array/graphene film/tin dioxide composite material is made.
Embodiment 7:
The step of repeating embodiment 1, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 8:
The step of repeating embodiment 1, only changes the step(2)The addition of pyrroles after middle purification is 0.25 g.
Embodiment 9:
The step of repeating embodiment 1, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 10:
The step of repeating embodiment 1, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 11:
The step of repeating embodiment 1, only changes the step(2)The addition of pyrroles after middle purification is 2 g.
Embodiment 12:
The step of repeating embodiment 2, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 13:
The step of repeating embodiment 2, only changes the step(2)The addition of pyrroles after middle purification is 0.25 g.
Embodiment 14:
The step of repeating embodiment 2, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 15:
The step of repeating embodiment 2, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 16:
The step of repeating embodiment 2, only changes the step(2)The addition of pyrroles after middle purification is 2 g.
Embodiment 17:
The step of repeating embodiment 3, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 18:
The step of repeating embodiment 3, the mass ratio for changing pyrroles and graphene oxide is 0.5(0.25 g pyrroles).
Embodiment 19:
The step of repeating embodiment 3, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 20:
The step of repeating embodiment 3, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 21:
The step of repeating embodiment 3, only changes the step(2)The addition of pyrroles after middle purification is 2 g.
Embodiment 22:
The step of repeating embodiment 4, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 23:
The step of repeating embodiment 4, only changes the step(2)The addition of pyrroles after middle purification is 0.25 g.
Embodiment 24:
The step of repeating embodiment 4, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 25:
The step of repeating embodiment 4, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 26:
The step of repeating embodiment 4, only changes the step(2)The addition of pyrroles after middle purification is 2 g.
Embodiment 27:
The step of repeating embodiment 5, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 28:
The step of repeating embodiment 5, only changes the step(2)The addition of pyrroles after middle purification is 0.25 g.
Embodiment 29:
The step of repeating embodiment 5, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 30:
The step of repeating embodiment 5, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 31:
The step of repeating embodiment 5, only changes the step(2)The addition of pyrroles after middle purification is 2 g.
Embodiment 32:
The step of repeating embodiment 6, only changes the step(2)The addition of pyrroles after middle purification is 0.125 g.
Embodiment 33:
The step of repeating embodiment 6, only changes the step(2)The addition of pyrroles after middle purification is 0.25 g.
Embodiment 34:
The step of repeating embodiment 6, only changes the step(2)The addition of pyrroles after middle purification is 0.5 g.
Embodiment 35:
The step of repeating embodiment 6, only changes the step(2)The addition of pyrroles after middle purification is 1 g.
Embodiment 36:
The step of repeating embodiment 6, only changes the step(2)The addition of pyrroles after middle purification is 2 g.

Claims (1)

1. a kind of preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material, it is characterised in that specific Step is:
(1)Three-dimensional graphene oxide is dissolved in deionized water, three-dimensional graphene oxide solution is made in 10 min of ultrasound, is Water phase;
(2)Pyrroles after purification is dissolved in chloroform oil phase is made, with step(1)Obtained water mixes, and is gathered using interface It is legal, 24 h are reacted at 0 ~ 5 DEG C, blackish green product occur in oil-water interfaces, after filtered, washing, dry 12 at 60 DEG C H, that is, be made polypyrrole nano line/graphene oxide composite material;
(3)Take step(2)Obtained polypyrrole nano line/graphene oxide composite material dissolving in deionized water, is fully stirred Mix lower addition SnCl2Solution and HI solution, are transferred in autoclave after being ultrasonically treated 5 min, 4 h are reacted at 180 DEG C, It is subsequently cooled to room temperature and mixed solution is made;
(4)To step(3)NaOH solution is added in obtained mixed solution, after being ultrasonically treated 5 min, 2 h are reacted at 180 DEG C, After cooled to room temperature, products therefrom is dried after being washed with deionized to neutrality, that is, polypyrrole nano line battle array is made Row/graphene film/tin dioxide composite material;
The mass ratio of pyrroles and three-dimensional graphene oxide after the purification are 0.1 ~ 4:1;The SnCl2With the material of NaOH The ratio between amount is 1:4;The mass ratio of the three-dimensional graphene oxide and HI is 1:2.56;The stannic oxide and three-dimensional graphite oxide The mass ratio of alkene is 0.1 ~ 2:1.
CN201711159748.6A 2017-11-20 2017-11-20 The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material Pending CN108010729A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052375A (en) * 2018-10-08 2018-12-21 江苏安纳泰环保科技有限公司 A kind of preparation method for the high stability nitrogen-doped graphene quantum dot that glass putty is modified
CN109585053A (en) * 2018-11-08 2019-04-05 上海萃励电子科技有限公司 A kind of one-step method for synthesizing of tri compound conductive powder body
CN109742381A (en) * 2019-02-28 2019-05-10 南京邮电大学 A kind of SnO2/ graphene/PPy trielement composite material preparation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106409526A (en) * 2016-11-24 2017-02-15 桂林理工大学 Preparation method of sulfonated graphene oxide/manganese dioxide/polyaniline composite material
CN106449182A (en) * 2016-11-29 2017-02-22 桂林理工大学 Preparation method of polyaniline/graphene/tin dioxide composite material
CN106449181A (en) * 2016-11-29 2017-02-22 桂林理工大学 Preparation method of polypyrrole/graphene/tin dioxide composite material
CN106531468A (en) * 2016-11-24 2017-03-22 桂林理工大学 Preparation method for sulfonated graphene oxide/stannic dioxide/polypyrrole composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106409526A (en) * 2016-11-24 2017-02-15 桂林理工大学 Preparation method of sulfonated graphene oxide/manganese dioxide/polyaniline composite material
CN106531468A (en) * 2016-11-24 2017-03-22 桂林理工大学 Preparation method for sulfonated graphene oxide/stannic dioxide/polypyrrole composite material
CN106449182A (en) * 2016-11-29 2017-02-22 桂林理工大学 Preparation method of polyaniline/graphene/tin dioxide composite material
CN106449181A (en) * 2016-11-29 2017-02-22 桂林理工大学 Preparation method of polypyrrole/graphene/tin dioxide composite material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109052375A (en) * 2018-10-08 2018-12-21 江苏安纳泰环保科技有限公司 A kind of preparation method for the high stability nitrogen-doped graphene quantum dot that glass putty is modified
CN109585053A (en) * 2018-11-08 2019-04-05 上海萃励电子科技有限公司 A kind of one-step method for synthesizing of tri compound conductive powder body
CN109742381A (en) * 2019-02-28 2019-05-10 南京邮电大学 A kind of SnO2/ graphene/PPy trielement composite material preparation method

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Application publication date: 20180508