CN108470629B - A kind of nickel ion doping polythiophene/graphene combination electrode material and preparation method thereof - Google Patents
A kind of nickel ion doping polythiophene/graphene combination electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of nickel ion doping polythiophene/graphene combination electrode materials and preparation method thereof, belong to the preparation technical field of functional polymer material.The preparation method is the following steps are included: (1) prepares the thienyl graphene (GO-Th) connected with ester bond using chloride graphene (GO-COCl) and the reaction of 3- ethyl alcohol thiophene；(2) GO-Th, the nickel chloride (NiCl for preparing step (1)2) and 3,4-rthylene dioxythiophene (EDOT) be added sequentially in chloroform, utilize chemical oxidising polymerisation reaction preparation Ni2+Poly- (3,4-rthylene dioxythiophene)/graphene composite material is adulterated, the as described nickel ion adulterates polythiophene/graphene combination electrode material.Combination electrode material prepared by the present invention not only specific capacitance with higher, but also there is excellent electrochemical cycle stability, it has broad application prospects in supercapacitor field.
Description
Technical field
The invention belongs to the preparation technical fields of functional polymer material, and in particular to and a kind of nickel ion doping polythiophene/
Graphene combination electrode material and preparation method thereof.
Background technique
Polythiophene is a kind of important structural conductive macromolecular material, due to high conductivity, good environment
The features such as stability and the molecular chain structure for being easy to regulate and control is also a kind of electrode material of important supercapacitor.But
When polythiophene is used as the electrode material of supercapacitor, itself have the shortcomings that specific capacitance is lower, theoretical research shows its specific volume
Amount only up to reach 210 F/g.For this disadvantage, researcher's discovery utilizes protonic acid doping polythiophene, can be effective
Improve its specific capacitance.Jiang Jieqing (Jiang Jieqing, Li Wei, Liu Dongzhi, Tian Jianhua, Guo Yafang, Zhou Xueqin;Poly- (3,4- ethylene
Dioxy thiophene)/camphorsulfonic acid composite material synthesis and chemical property, fine chemistry industry, 2012,29 (6): 541 ~
541.) it is oxidant by dopant, ferric trichloride of camphorsulfonic acid, poly- (3,4- enedioxies has been synthesized by chemical oxidization method
Thiophene)/camphorsulfonic acid composite material.Studies have shown that composite material has good when the ratio of the amount of the two substance is 2:1
Electric conductivity and chemical property, conductivity are 10.4 S/cm, and capacity remains at 140 F/g after 150 cycle charge-discharges
More than.Graphene has big specific surface area and excellent mechanical performance.The study found that conjugated polymer and graphene are carried out
Compound, graphene forms spatial network support construction in the composite, can dramatically increase conjugated polymer and electrolyte
Contact area, to increase the specific capacitance of conjugated polymer.But due to existing between layers between untreated graphene
Van der Waals force, be easy to happen reunion, it is difficult to evenly dispersed in conjugated polymer.Therefore, Yao Fahui graphene improves compound
The advance of material, it is necessary on the basis of interface and property are designed, effective functional modification processing is carried out to it.
Summary of the invention
It is an object of the invention to this lower disadvantage of specific capacitance for polythiophene in the prior art, provide a kind of nickel from
Son doping polythiophene/graphene combination electrode material and preparation method thereof.Combination electrode material prepared by the present invention not only has
Higher specific capacitance, and there is excellent electrochemical cycle stability, before there is wide application in supercapacitor field
Scape.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of nickel ion doping polythiophene/graphene combination electrode material preparation method, comprising the following steps:
(1) chloride graphene (GO-COCl) (He Yaping, Yang Xiaohui, Han Quan, Huo Yanyan is utilized;[ (5- is chloro- by 4-
Pyridine) azo -1,3- diaminobenzene functional graphene oxide preparation, Xi'an University's journal (natural science edition),
2017,20 (3): it 90 ~ 93.) is reacted with 3- ethyl alcohol thiophene, prepares the thienyl graphene (GO-Th) connected with ester bond；
(2) GO-Th, the nickel chloride (NiCl for preparing step (1)2) and 3,4- ethene dioxythiophene (EDOT) sequentially add
Into chloroform, preparation Ni is reacted using chemical oxidising polymerisation2+Poly- (3,4-rthylene dioxythiophene)/graphene composite material is adulterated,
The as described nickel ion adulterates polythiophene/graphene combination electrode material.
More specifically steps are as follows:
(1) 0.4 ~ 1 g GO-COCl is added to 100 ~ 500 mL chloroform (CHCl3) in, at room temperature ultrasound 30 ~
60 min prepare the dispersion liquid of GO-COCl；2 ~ 10 g 3- ethyl alcohol thiophene and 3 ~ 15 g pyridines are added into above-mentioned dispersion liquid,
Nitrogen (N2) under protection, 70 ~ 90 DEG C of magnetic are stirred to react 20 ~ 30 h.After reaction, black powder is isolated using centrifuge,
And sufficiently washed with 200 ~ 500 mL dehydrated alcohols, it is freeze-dried 24 h at -50 DEG C, prepares GO-Th；
(2) 0.1 ~ 0.2 g GO-Th is added to 200 ~ 500 mL CHCl3In, 30 ~ 90 min of ultrasound, make at room temperature
The dispersion liquid of standby GO-Th；1 ~ 6 g NiCl is added into above-mentioned dispersion liquid2, 5 ~ 30 min of ultrasound, add 1 ~ 8 at room temperature
G EDOT continues 5 ~ 20 min of ultrasound at room temperature；In N2Under protection, by 1.5 ~ 12 g ferric trichloride (FeCl3) be added to
It states in mixed liquor, is warming up to 30 ~ 50 DEG C, magnetic is stirred to react 4 ~ 8 h；After reaction, mixed liquor is poured into methanol and is settled,
The black powder obtained after sedimentation washs with deionized water and methanol repeatedly, it is colourless to filtrate to filter；It is dried in vacuo at 60 DEG C
24 h prepare Ni2+Poly- (3,4-rthylene dioxythiophene)/graphene composite material is adulterated, the as described nickel ion doping polythiophene/
Graphene combination electrode material.
Nickel ion made from a kind of preparation method as described above adulterates polythiophene/graphene combination electrode material.
In the prior art, acid anhydrides reaction is carried out using chloride graphene and thenoic acid, preparation is connected with anhydride bond
Thienyl graphene (Sun Chenglong, Dong Yanmao, Li Jiaxuan, Zhu Guangai, the Dai Xu connect;Poly- 3- hexyl thiophene/graphite oxide
The preparation and optical property research of alkene composite material, 2016,44 (2): 95-97,101.).Thienyl group in the present invention
It with graphene is connected by ester bond.
Compared with the prior art, the present invention has the following advantages:
(1) present invention connects thienyl group with graphene by ester bond, and ester bond has stronger chemistry steady than anhydride bond
It is qualitative, so thienyl graphene prepared by the present invention has more excellent stability during chemical oxidising polymerisation；Together
When in composite material prepared by the present invention, there is bigger bonding strength, this is advantageous between graphene and polythiophene strand
In the specific capacitance and electrochemical cycle stability that improve composite material；
(2) GO-Th and Ni2+After ultrasonic disperse, Ni2+Pass through sulphur (S) atom network of coordinate bond and the thienyl group of graphene
It closes；After EDOT monomer is added, above-mentioned Ni2+It is complexed again with the S atom of EDOT monomer, EDOT monomer is adsorbed on graphene week
It encloses.As addition FeCl3Afterwards, the thienyl group caused on EDOT monomer and graphene carries out chemical oxidation reaction jointly, occur with
Thienyl group on graphene is the polymerization reaction of the EDOT monomer of starting point；The polythiophene that this feeding sequence is conducive to generate covers
It covers the bigger serface on the surface of graphene, by graphene and excellent mechanical performance, improves polythiophene and electrolyte
Contact area and help to form the support construction using graphene as skeleton in the composite, so as to improve composite wood
The specific capacitance and electrochemical cycle stability of material；
(3) in the composite, it is connected between graphene and polythiophene strand by ester bond；This not only can significantly change
Kind dispersion effect of the graphene in polythiophene matrix, and the bond strength between polythiophene and graphene can be improved；This
Outside, Ni2+With the coordination of S atom in polythiophene strand, polythiophene strand can be induced to align, form structure rule
Whole polythiophene strand helps to improve the specific capacitance and electrochemical cycle stability of composite material；
(4) nickel ion doping polythiophene/graphene composite material prepared by the present invention is distinguished in charging and discharging currents density
When for 0.2 g/A, 0.5 g/A, 1 g/A and 2 g/A, specific capacitance is respectively 207 F/g, 196 F/g, 182 F/g and 161 F/
234 %, 270 %, 344 % and 632 % are respectively increased than polythiophene in g, and after recycling 1000 times, the conservation rate of specific capacitance is
93%, than 24 % of raising of polythiophene；Because of this kind of material specific capacitance with higher and more excellent electrochemical cycle stability,
Mainly for the preparation of electrode for super capacitor.
Specific embodiment
With reference to embodiments, the present invention will be described in further detail.It should be appreciated that specific reality described herein
Example is applied only to explain the present invention, is not intended to limit the present invention.
Embodiment 1
A kind of nickel ion doping polythiophene/graphene combination electrode material preparation method, specific steps are as follows:
(1) 0.4 g GO-COCl is added to 100 mL CHCl3In, 30 min of ultrasound, prepare GO-COCl at room temperature
Dispersion liquid；2 g 3- ethyl alcohol thiophene and 3 g pyridines are added into above-mentioned dispersion liquid, in N2Under protection, 70 DEG C of magnetic are stirred to react
30 h；After reaction, black powder is isolated using centrifuge, and is sufficiently washed with 200 mL dehydrated alcohols, at -50 DEG C
24 h of lower freeze-drying prepare GO-Th；
(2) 0.1 g GO-Th is added to 200 mL CHCl3In, 30 min of ultrasound, prepare point of GO-Th at room temperature
Dispersion liquid；1 g NiCl is added into above-mentioned dispersion liquid2, 5 min of ultrasound, add 1 g EDOT at room temperature, at room temperature after
Continuous 5 min of ultrasound；In N2Under protection, by 1.5 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 30 DEG C, magnetic is stirred to react 8
h；After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation uses deionized water and methanol repeatedly
Washing, filtering are colourless to filtrate；24 h preparation Ni is dried in vacuo at 60 DEG C2+Adulterate poly- (3,4- ethene dioxythiophene)/graphite
Alkene composite material.
Embodiment 2
A kind of nickel ion doping polythiophene/graphene combination electrode material preparation method, comprising the following steps:
(1) 0.7 g GO-COCl is added to 300 mL CHCl3In, 45 min of ultrasound, prepare GO-COCl at room temperature
Dispersion liquid；6 g 3- ethyl alcohol thiophene and 9 g pyridines are added into above-mentioned dispersion liquid, in N2Under protection, 80 DEG C of magnetic are stirred to react
25 h；After reaction, black powder is isolated using centrifuge, and is sufficiently washed with 400 mL dehydrated alcohols, at -50 DEG C
24 h of lower freeze-drying prepare GO-Th；
(2) 0.15 g GO-Th is added to 400 mL CHCl3In, 60 min of ultrasound, prepare GO-Th's at room temperature
Dispersion liquid；4 g NiCl are added into above-mentioned dispersion liquid2, 20 min of ultrasound, add 5 g EDOT, at room temperature at room temperature
Continue 10 min of ultrasound；In N2Under protection, by 8 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 40 DEG C, magnetic is stirred to react
6 h；After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation uses deionized water and first repeatedly
Alcohol washing, filtering are colourless to filtrate；24 h preparation Ni is dried in vacuo at 60 DEG C2+Adulterate poly- (3,4- ethene dioxythiophene)/stone
Black alkene composite material.
Embodiment 3
A kind of nickel ion doping polythiophene/graphene combination electrode material preparation method, comprising the following steps:
(1) 1 g GO-COCl is added to 500 mL CHCl3In, 60 min of ultrasound, prepare GO-COCl's at room temperature
Dispersion liquid；10 g 3- ethyl alcohol thiophene and 15 g pyridines are added into above-mentioned dispersion liquid, in N2Under protection, 90 DEG C of magnetic are stirred to react
20 h；After reaction, black powder is isolated using centrifuge, and is sufficiently washed with 500 mL dehydrated alcohols, at -50 DEG C
24 h of lower freeze-drying prepare GO-Th；
(2) 0.2 g GO-Th is added to 500 mL CHCl3In, 90 min of ultrasound, prepare point of GO-Th at room temperature
Dispersion liquid；6 g NiCl are added into above-mentioned dispersion liquid2, 30 min of ultrasound, add 8 g EDOT at room temperature, at room temperature after
Continuous 20 min of ultrasound.In N2Under protection, by 12 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 50 DEG C, magnetic is stirred to react 4
h；After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation uses deionized water and methanol repeatedly
Washing, filtering are colourless to filtrate；24 h preparation Ni is dried in vacuo at 60 DEG C2+Adulterate poly- (3,4- ethene dioxythiophene)/graphite
Alkene composite material.
Comparative example 1
1 g EDOT is added to 200 mL CHCl3In, 5 min of ultrasound at room temperature.In N2Under protection, by 1.5 g
FeCl3It is added in above-mentioned solution, is warming up to 30 DEG C, magnetic is stirred to react 8 h.After reaction, mixed liquor is poured into methanol
Sedimentation, the black powder obtained after sedimentation washs with deionized water and methanol repeatedly, it is colourless to filtrate to filter.It is true at 60 DEG C
Dry 24 h of sky prepare poly- (3,4- ethene dioxythiophene).
Comparative example 2
By 4 g NiCl2It is added to 400 mL CHCl3In, 20 min of ultrasound, add 5 g EDOT, in room at room temperature
Temperature is lower to continue 10 min of ultrasound.In N2Under protection, by 8 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 40 DEG C, magnetic stirring
React 6 h.After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation uses deionized water repeatedly
It is colourless to filtrate with methanol washing, filtering.24 h preparation Ni is dried in vacuo at 60 DEG C2+Adulterate poly- (3,4- ethylene dioxy thiophene
Pheno).
Comparative example 3
0.2 g graphene oxide (GO) is added to 500 mL CHCl3In, 90 min of ultrasound, prepare GO at room temperature
Dispersion liquid.6 g NiCl are added into above-mentioned dispersion liquid2, 30 min of ultrasound, add 8 g EDOT, in room temperature at room temperature
20 min of lower continuation ultrasound.In N2Under protection, by 12 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 50 DEG C, magnetic stirring
React 4 h.After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation uses deionized water repeatedly
It is colourless to filtrate with methanol washing, filtering.24 h preparation Ni is dried in vacuo at 60 DEG C2+Adulterate poly- (3,4- ethylene dioxy thiophene
Pheno)/graphene composite material.
80 % products, 15 % acetylene carbon blacks and 5 % Kynoar are uniformly mixed and are coated on stainless (steel) wire as work
Electrode, using platinum filament as to electrode, using saturated calomel electrode as reference electrode, using 1 mol/L aqueous sulfuric acid as electrolysis
Liquid is tested using the specific capacitance of product prepared by constant current charge-discharge method testing example and comparative example using cyclic voltammetry
The electrochemical cycle stability of product prepared by embodiment and comparative example, wherein voltage range is -0.2 ~ 0.8 V, charge and discharge electricity
Current density is respectively 0.2 g/A, 0.5 g/A, 1 g/A and 2 g/A, and sweep speed is 100 mV/s.Test result is as follows 1 institute of table
Show.
1 the performance test results of table
It can be seen that composite material prepared by three groups of embodiments from the test result of three groups of embodiments and three groups of comparative examples
Specific capacitance and electrochemical cycle stability be improved significantly.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of nickel ion adulterates polythiophene/graphene combination electrode material preparation method, it is characterised in that: including following step
It is rapid:
(1) it is reacted using chloride graphene oxide-GO-COCl and 3- ethyl alcohol thiophene, prepares the thienyl oxygen connected with ester bond
Graphite alkene-GO-Th；
(2) GO-Th, nickel chloride and 3,4-rthylene dioxythiophene prepared by step (1) are added sequentially in chloroform, utilize chemistry
Oxidative polymerization prepares nickel ion doping polythiophene/graphene combination electrode material；
Above-mentioned steps (2) specifically: 0.1 ~ 0.2 g GO-Th is added to 200 ~ 500 mL CHCl3In, at room temperature ultrasound 30
~ 90 min prepare the dispersion liquid of GO-Th；1 ~ 6 g NiCl is added into the dispersion liquid of GO-Th2, at room temperature ultrasound 5 ~ 30
Min adds 1 ~ 8 g 3,4-rthylene dioxythiophene, continues 5 ~ 20 min of ultrasound at room temperature, obtains mixed liquor；In N2Protection
Under, 1.5 ~ 12 g ferric trichlorides are added in above-mentioned mixed liquor, are warming up to 30 ~ 50 DEG C, magnetic is stirred to react 4 ~ 8 h；Reaction
After, reaction solution is poured into methanol and is settled, the black powder obtained after sedimentation washs with deionized water and methanol repeatedly, mistake
It filters colourless to filtrate；It is dried in vacuo 24 h at 60 DEG C and prepares nickel ion doping polythiophene/graphene combination electrode material.
2. nickel ion according to claim 1 adulterates polythiophene/graphene combination electrode material preparation method, feature
It is: step (1) specifically: 0.4 ~ 1 g GO-COCl is added in 100 ~ 500 mL chloroforms, at room temperature ultrasound 30
~ 60 min prepare the dispersion liquid of GO-COCl；Then be added into the dispersion liquid of GO-COCl 2 ~ 10 g 3- ethyl alcohol thiophene and 3 ~
15 g pyridines are stirred to react 20 ~ 30 h in 70 ~ 90 DEG C of magnetic under nitrogen protection；After reaction, it is isolated using centrifuge
Black powder, and sufficiently washed with 200 ~ 500 mL dehydrated alcohols, it is freeze-dried 24 h at -50 DEG C, prepares GO-Th.
3. a kind of doping of the nickel ion as made from claim 1-2 described in any item preparation methods polythiophene/graphene is compound
Electrode material.
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| CN110203916A (en) * | 2019-05-15 | 2019-09-06 | 华东理工大学 | A method of flexible extensible device is prepared based on graphene composite material |
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