CN106449181B - A kind of preparation method of polypyrrole/graphene/tin dioxide composite material - Google Patents

A kind of preparation method of polypyrrole/graphene/tin dioxide composite material Download PDF

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CN106449181B
CN106449181B CN201611068284.3A CN201611068284A CN106449181B CN 106449181 B CN106449181 B CN 106449181B CN 201611068284 A CN201611068284 A CN 201611068284A CN 106449181 B CN106449181 B CN 106449181B
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polypyrrole
graphene
graphene oxide
solution
dimensional porous
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CN106449181A (en
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樊新
陈韦良
庞树花
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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    • 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 methods of polypyrrole/graphene/tin dioxide composite material.Polypyrrole/graphene oxide composite colloids are prepared with hydro-thermal method, i.e. using the electrostatic tension between the epoxy bond of nitrogen and surface of graphene oxide positively charged on polypyrrole segment in a large amount of graphene oxide of polypyrrole adsorption, the reunion of graphene oxide is effectively prevented, then uses SnCl2Graphene oxide in colloid is reduced to graphene by solution, it adds sodium hydroxide solution containing the graphene surface absorption generation Sn (IV) on a small quantity containing oxygen key using hydro-thermal method simultaneously and is reacted at 180 DEG C and prepare three-dimensional porous netted polypyrrole/graphene/tin dioxide composite material.The method of the present invention preparation process is simple, environmentally protective, reliable, and gained composite material has regular space structure, good dispersibility, high-energy density and power density, outstanding cycle performance, it is a kind of ideal electrode material for super capacitor, is suitble to industrialized production.

Description

A kind of preparation method of polypyrrole/graphene/tin dioxide composite material
Technical field
The invention belongs to novel energy field of material technology, more particularly to one kind prepares ultracapacitor with three with hydro-thermal method The method for tieing up holey polypyrrole/graphene/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, realize that the widely applied most important thing of ultracapacitor is to prepare and develop high performance electricity 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 that deficiency existing for homogenous material is overcome 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. It is that raw material synthesizes the hollow SnO with nucleocapsid using hydro-thermal method using stannic oxide and pyrroles2@PPy nanocomposites, energy Enough reunions for effectively inhibiting stannic oxide microballoon and the volume expansion for mitigating polypyrrole in charge and discharge process;In addition, coat poly- pyrrole The compound of hollow structure after coughing up can be more conducive to the diffusion of lithium ion with respect to stannic oxide microballoon, compound so as to improve 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 three-dimensional porous polypyrrole, Three-dimensional porous netted polypyrrole/graphene/tin dioxide composite material is prepared using hydro-thermal method.
Invention content
The object of the present invention is to provide a kind of preparation methods of polypyrrole/graphene/tin dioxide composite material.
Thinking of the present invention:Polypyrrole/graphene oxide composite colloids are prepared with hydro-thermal method, i.e., using on polypyrrole segment Electrostatic tension between positively charged nitrogen and the epoxy bond of surface of graphene oxide largely aoxidizes stone in polypyrrole adsorption Black alkene effectively prevents the reunion of graphene oxide, then uses SnCl2Graphene oxide in colloid is reduced to graphite by solution Alkene, while it is molten to be added containing the graphene surface absorption generation Sn (IV) on a small quantity containing oxygen key using hydro-thermal method for sodium hydroxide Liquid reacts at 180 DEG C prepares three-dimensional porous netted polypyrrole/graphene/tin dioxide composite material.
The specific steps are:
(1) graphene oxide is dissolved in deionized water, graphene oxide solution is made in 10 min of ultrasound.
(2) three-dimensional porous polypyrrole is added in into graphene oxide solution made from step (1), is sufficiently stirred lower addition SnCl2Solution and HI solution are transferred in autoclave after being ultrasonically treated 5 min, 4 h are reacted at 180 DEG C, then natural It is cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2), 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, obtains polypyrrole/graphite Alkene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1 ~ 4:1;The graphene oxide and HI's Mass ratio is 1:2.56;The SnCl2It is 1 with the ratio between the amount of substance of NaOH:4;The stannic oxide and graphene oxide Mass ratio is 0.1 ~ 2:1.
The method of the present invention preparation process is simple, environmentally protective, reliable, and gained polypyrrole/graphene/stannic oxide is compound Material has regular space structure, good dispersibility, high-energy density and power density, outstanding cycle performance, is one The ideal electrode material for super capacitor of kind, is suitble to industrialized production.
Description of the drawings
Fig. 1 is the scanning electron microscope of polypyrrole/graphene/tin dioxide composite material obtained in the embodiment of the present invention 20 Figure.
Specific embodiment
Embodiment 1:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 0.0629 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 0.1:1.
Embodiment 2:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 0.1258 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 0.2:1.
Embodiment 3:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 0.1573 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 0.25:1.
Embodiment 4:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 0.3145 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 0.5:1.
Embodiment 5:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 0.6290 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 1:1.
Embodiment 6:
(1) 0.5 g three-dimensional graphene oxides are dissolved in 100 mL deionized waters, graphite oxide is made in 10 min of ultrasound Alkene solution.
(2) the three-dimensional porous polypyrroles of 0.05 g are added in into graphene oxide solution made from step (1), are sufficiently stirred down Add in SnCl2Solution(Containing 1.2580 g SnCl2)With the HI solution of 10 mL, 1 M, it is ultrasonically treated after 5 min that be transferred to high pressure anti- It answers in kettle, 4 h is reacted at 180 DEG C, then cooled to room temperature, mixed solution is made.
(3) NaOH solution is added in into mixed solution made from step (2)(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, obtain polypyrrole/graphene/tin dioxide composite material.
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1:1;The SnCl2With the substance of NaOH The ratio between amount is 1:4;The mass ratio of the stannic oxide and graphene oxide is 2:1.
Embodiment 7:
The step of repeating embodiment 1, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 8:
The step of repeating embodiment 1, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 9:
The step of repeating embodiment 1, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 10:
The step of repeating embodiment 1, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 11:
The step of repeating embodiment 1, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.
Embodiment 12:
The step of repeating embodiment 2, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 13:
The step of repeating embodiment 2, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 14:
The step of repeating embodiment 2, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 15:
The step of repeating embodiment 2, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 16:
The step of repeating embodiment 2, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.
Embodiment 17:
The step of repeating embodiment 3, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 18:
The step of repeating embodiment 3, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 19:
The step of repeating embodiment 3, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 20:
The step of repeating embodiment 3, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 21:
The step of repeating embodiment 3, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.
Embodiment 22:
The step of repeating embodiment 4, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 23:
The step of repeating embodiment 4, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 24:
The step of repeating embodiment 4, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 25:
The step of repeating embodiment 4, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 26:
The step of repeating embodiment 4, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.
Embodiment 27:
The step of repeating embodiment 5, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 28:
The step of repeating embodiment 5, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 29:
The step of repeating embodiment 5, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 30:
The step of repeating embodiment 5, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 31:
The step of repeating embodiment 5, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.
Embodiment 32:
The step of repeating embodiment 6, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.125 g.
Embodiment 33:
The step of repeating embodiment 6, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.25 g.
Embodiment 34:
The step of repeating embodiment 6, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 0.5 g.
Embodiment 35:
The step of repeating embodiment 6, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 1 g.
Embodiment 36:
The step of repeating embodiment 6, the addition for only changing the step three-dimensional porous polypyrrole in (2) are 2 g.

Claims (1)

1. a kind of preparation method of polypyrrole/graphene/tin dioxide composite material, it is characterised in that the specific steps are:
(1) graphene oxide is dissolved in deionized water, graphene oxide solution is made in 10 min of ultrasound;
(2) three-dimensional porous polypyrrole is added in into graphene oxide solution made from step (1), is sufficiently stirred lower addition SnCl2It is molten Liquid and HI solution are transferred in autoclave after being ultrasonically treated 5 min, 4 h are reacted at 180 DEG C, then naturally cool to room Mixed solution is made in temperature;
(3) NaOH solution is added in into mixed solution made from step (2), 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, obtain polypyrrole/graphene/ Tin dioxide composite material;
The mass ratio of the three-dimensional porous polypyrrole and graphene oxide is 0.1 ~ 4:1;The quality of the graphene oxide and HI Than being 1:2.56;The SnCl2It is 1 with the ratio between the amount of substance of NaOH:4;The quality of the stannic oxide and graphene oxide Than being 0.1 ~ 2:1.
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CN108010752A (en) * 2017-11-20 2018-05-08 桂林理工大学 The preparation method of polypyrrole nano line array/graphene film/manganese oxide composite material
CN108010729A (en) * 2017-11-20 2018-05-08 桂林理工大学 The preparation method of polypyrrole nano line array/graphene film/tin dioxide composite material

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