CN108470629A - 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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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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Abstract
The invention discloses a kind of nickel ions to adulterate polythiophene/graphene combination electrode material and preparation method thereof, belongs to the preparing technical field of functional high molecule material.The preparation method includes the following steps：（1）Utilize chloride graphene（GO‑COCl）It is reacted with 3 ethyl alcohol thiophene, prepares the thienyl graphene connected with ester bond（GO‑Th）；（2）By step（1）GO Th, the nickel chloride of preparation（NiCl2）With 3,4 ethene dioxythiophenes（EDOT）It is added sequentially in chloroform, is reacted using chemical oxidising polymerisation and prepare Ni2+Doping is poly-（3,4 ethene dioxythiophenes）/ graphene composite material, the as described nickel ion adulterate polythiophene/graphene combination electrode material.Combination electrode material prepared by the present invention not only has higher specific capacitance, but also has excellent electrochemical cycle stability, has broad application prospects in ultracapacitor field.
Description
Technical field
The invention belongs to the preparing technical fields of functional high molecule material, and in particular to and a kind of nickel ion doping polythiophene/
Graphene combination electrode material and preparation method thereof.
Background technology
Polythiophene is a kind of important structural conductive macromolecular material, due to high conductivity, good environment
The features such as stability and molecular chain structure for being easy to regulation and control, be also a kind of electrode material of important ultracapacitor.But
When polythiophene is used as the electrode material of ultracapacitor, itself have the shortcomings that specific capacitance is relatively low, theoretical research shows its specific volume
Amount only up to reach 210 F/g.For this disadvantage, researcher has found to utilize protonic acid doping polythiophene, can be effective
Improve its specific capacitance.Jiang Jieqing（Jiang Jieqing, Li Wei, Liu Dongzhi, field Jian Hua, Guo Yafang, Zhou Xueqin;Poly- (3,4- ethylenes
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, has been synthesized by chemical oxidization method poly-（3,4- enedioxies
Thiophene）/ camphorsulfonic acid composite material.Studies have shown that when the ratio of the amount of the two substance is 2:When 1, composite material has good
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, it is compound to play graphene improvement
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.
Invention content
It is an object of the invention to this relatively low disadvantage of the 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 ultracapacitor field has wide application
Scape.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of nickel ion doping polythiophene/graphene combination electrode material, includes the following steps：
（1）Utilize chloride graphene（GO-COCl）（He Yaping, Yang Xiaohui, Han Quan, Huo Yanyan;4- ［ (the chloro- pyridines of 5-)
Azo ］ -1,3- diaminobenzene functional graphene oxides preparation, Xi'an University's journal (natural science edition), 2017,
20(3): 90~93.）It is reacted with 3- ethyl alcohol thiophene, prepares the thienyl graphene connected with ester bond（GO-Th）；
（2）By step（1）GO-Th, the nickel chloride of preparation（NiCl2）With 3,4- ethene dioxythiophenes（EDOT）It is added sequentially to chlorine
In imitative, reacted using chemical oxidising polymerisation and prepare Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphene composite material, as
The nickel ion adulterates polythiophene/graphene combination electrode material.
More specifically steps are as follows：
（1）0.4 ~ 1 g GO-COCl are added to 100 ~ 500 mL chloroforms（CHCl3）In, at room temperature ultrasound 30 ~ 60
Min prepares 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, in nitrogen
Gas（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
It is fully washed with 200 ~ 500 mL absolute ethyl alcohols, 24 h is freeze-dried at -50 DEG C, prepare GO-Th；
（2）0.1 ~ 0.2 g GO-Th are added to 200 ~ 500 mL CHCl3In, 30 ~ 90 min of ultrasound, prepare at room temperature
The dispersion liquid of GO-Th；1 ~ 6 g NiCl are added into above-mentioned dispersion liquid2, 5 ~ 30 min of ultrasound, add 1 ~ 8 g at room temperature
EDOT continues 5 ~ 20 min of ultrasound at room temperature；In N2Under protection, by 1.5 ~ 12 g ferric trichlorides（FeCl3）It is added to above-mentioned
In mixed liquor, 30 ~ 50 DEG C are warming up to, magnetic is stirred to react 4 ~ 8 h；After reaction, mixed liquor is poured into methanol and is settled, sunk
The black powder obtained after drop washs with deionized water and methanol repeatedly, it is colourless to filtrate to filter；It is dried in vacuo 24 at 60 DEG C
H prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphene composite material, the as described nickel ion adulterate polythiophene/graphite
Alkene 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
The thienyl graphene connect（Sun Chenglong, Dong Yanmao, Li Jiaxuan, Zhu Guangai, Dai Xu;Poly- 3- hexyl thiophenes/graphite oxide
The preparation of alkene composite material and optical property research, 2016,44 (2): 95-97, 101.）.Thienyl group in the present invention
With graphene connected by ester bond.
Compared with the prior art, the present invention has the following advantages：
（1）The present invention connects thienyl group with graphene by ester bond, and ester bond has stronger chemical stability than anhydride bond,
So thienyl graphene prepared by the present invention has more excellent stability during chemical oxidising polymerisation；Simultaneously at this
It invents in the composite material prepared, the bonding strength with bigger between graphene and polythiophene strand, this is conducive to improve
The specific capacitance of composite material and electrochemical cycle stability；
（2）GO-Th and Ni2+After ultrasonic disperse, Ni2+Pass through the sulphur of coordinate bond and the thienyl group of graphene（S）Atom is complexed；
After EDOT monomers are added, above-mentioned Ni2+It is complexed again with the S atom of EDOT monomers, EDOT monomers is adsorbed on around graphene.When
FeCl is added3Afterwards, cause EDOT monomers and carry out chemical oxidation reaction jointly with the thienyl group on graphene, occur with graphene
On thienyl group be starting point EDOT monomers polymerisation；The polythiophene that this feeding sequence is conducive to generate is covered in stone
The surface of black alkene, the bigger serface by graphene and excellent mechanical performance improve the contact surface of polythiophene and electrolyte
It accumulates and helps to form the support construction using graphene as skeleton in the composite, so as to improve the ratio of composite material
Capacitance and electrochemical cycle stability；
（3）In the composite, it is connected by ester bond between graphene and polythiophene strand；This can not only significantly improve stone
Dispersion effect of the black alkene in polythiophene matrix, and the bond strength between polythiophene and graphene can be improved；In addition,
Ni2+With the coordination of S atom in polythiophene strand, polythiophene strand can be induced to align, form compound with regular structure
Polythiophene strand, help to improve the specific capacitance of composite material and electrochemical cycle stability；
（4）It is respectively 0.2 that nickel ion prepared by the present invention, which adulterates polythiophene/graphene composite material in charging and discharging currents density,
When 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/g, than poly-
234 %, 270 %, 344 % and 632 % are respectively increased in thiophene, and after recycling 1000 times, the conservation rate of specific capacitance is 93%, than poly-
24 % of raising of thiophene；Because this kind of material has higher specific capacitance and more excellent electrochemical cycle stability, it is mainly used for
Prepare electrode for super capacitor.
Specific implementation mode
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 preparation method of nickel ion doping polythiophene/graphene combination electrode material, the specific steps are：
（1）0.4 g GO-COCl are added to 100 mL CHCl3In, 30 min of ultrasound, prepare point of 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, 200 mL absolute ethyl alcohols is used in combination fully to wash, it is cold at -50 DEG C
Dry 24 h is lyophilized, prepares GO-Th；
（2）0.1 g GO-Th are added to 200 mL CHCl3In, 30 min of ultrasound, prepare the dispersion of GO-Th at room temperature
Liquid；1 g NiCl are added into above-mentioned dispersion liquid2, 5 min of ultrasound, add 1 g EDOT, continue at room temperature at room temperature
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；It is dried in vacuo 24 h at 60 DEG C and prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphite
Alkene composite material.
Embodiment 2
A kind of preparation method of nickel ion doping polythiophene/graphene combination electrode material, includes the following steps：
（1）0.7 g GO-COCl are added to 300 mL CHCl3In, 45 min of ultrasound, prepare point of 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, 400 mL absolute ethyl alcohols is used in combination fully to wash, it is cold at -50 DEG C
Dry 24 h is lyophilized, prepares GO-Th；
（2）0.15 g GO-Th are added to 400 mL CHCl3In, 60 min of ultrasound, prepare the dispersion of GO-Th at room temperature
Liquid；4 g NiCl are added into above-mentioned dispersion liquid2, 20 min of ultrasound, add 5 g EDOT, continue at room temperature at room temperature
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 is washed with deionized water and methanol repeatedly
Wash, filter it is colourless to filtrate；It is dried in vacuo 24 h at 60 DEG C and prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphene
Composite material.
Embodiment 3
A kind of preparation method of nickel ion doping polythiophene/graphene combination electrode material, includes the following steps：
（1）1 g GO-COCl are added to 500 mL CHCl3In, 60 min of ultrasound, prepare the dispersion of GO-COCl at room temperature
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, 500 mL absolute ethyl alcohols is used in combination fully to wash, it is cold at -50 DEG C
Dry 24 h is lyophilized, prepares GO-Th；
（2）0.2 g GO-Th are added to 500 mL CHCl3In, 90 min of ultrasound, prepare the dispersion of GO-Th at room temperature
Liquid；6 g NiCl are added into above-mentioned dispersion liquid2, 30 min of ultrasound, add 8 g EDOT, continue at room temperature at room temperature
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；It is dried in vacuo 24 h at 60 DEG C and prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphite
Alkene composite material.
Comparative example 1
1 g EDOT are added to 200 mL CHCl3In, 5 min of ultrasound at room temperature.In N2Under protection, by 1.5 g FeCl3
It 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 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 poly-（3,4- ethene dioxythiophenes）.
Comparative example 2
By 4 g NiCl2It is added to 400 mL CHCl3In, 20 min of ultrasound, add 5 g EDOT, in room temperature at room temperature
10 min of lower continuation ultrasound.In N2Under protection, by 8 g FeCl3It is added in above-mentioned mixed liquor, is warming up to 40 DEG C, magnetic stirring is anti-
Answer 6 h.After reaction, mixed liquor is poured into methanol and is settled, the black powder obtained after sedimentation repeatedly use deionized water and
Methanol washing, filtering are colourless to filtrate.It is dried in vacuo 24 h at 60 DEG C and prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）.
Comparative example 3
By 0.2 g graphene oxides（GO）It is added to 500 mL CHCl3In, 90 min of ultrasound, prepare point of GO 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
20 min of continuous 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.It is dried in vacuo 24 h at 60 DEG C and prepares Ni2+Doping is poly-（3,4- ethene dioxythiophenes）/ graphite
Alkene composite material.
80 % products, 15 % acetylene carbon blacks and 5 % Kynoar are uniformly mixed to be coated on stainless (steel) wire and are used as work
Electrode, using platinum filament as to electrode, using saturated calomel electrode as reference electrode, using 1 mol/L aqueous sulfuric acids 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 the ratio of the composite material prepared by three groups of embodiments from the test result of three groups of embodiments and three groups of comparative examples
Capacitance and electrochemical cycle stability are 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 should all belong to the covering scope of the present invention.
Claims (4)
1. a kind of preparation method of nickel ion doping polythiophene/graphene combination electrode material, it is characterised in that：Including following step
Suddenly：
（1）It is reacted using chloride graphene-GO-COCl and 3- ethyl alcohol thiophene, prepares the thienyl graphite connected with ester bond
Alkene-GO-Th；
（2）By step（1）GO-Th, nickel chloride and the 3,4-rthylene dioxythiophene of preparation are added sequentially in chloroform, utilize chemistry
Oxidative polymerization prepares nickel ion doping polythiophene/graphene combination electrode material.
2. the preparation method of nickel ion doping polythiophene/graphene combination electrode material according to claim 1, feature
It is：Step（1）Specially：0.4 ~ 1 g GO-COCl are 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 is used in combination 200 ~ 500 mL absolute ethyl alcohols fully to wash, and 24 h are freeze-dried at -50 DEG C, prepares GO-Th.
3. the preparation method of nickel ion doping polythiophene/graphene combination electrode material according to claim 1, feature
It is：Step（2）Specially：0.1 ~ 0.2 g GO-Th are added to 200 ~ 500 mL CHCl3In, at room temperature ultrasound 30 ~
90 min prepare the dispersion liquid of GO-Th；1 ~ 6 g NiCl are added into the dispersion liquid of GO-Th2, at room temperature ultrasound 5 ~ 30
Min adds 1 ~ 8 g 3,4-rthylene dioxythiophenes, 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
Filter is colourless to filtrate；It is dried in vacuo 24 h at 60 DEG C and prepares nickel ion doping polythiophene/graphene combination electrode material.
4. nickel ion doping polythiophene/graphene made from a kind of preparation method as described in any one of claims 1-3 is compound
Electrode material.
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| CN109326455A (en) * | 2018-10-31 | 2019-02-12 | 南京林业大学 | A kind of hydrophily polythiophene grafted graphene oxide electrode material for super capacitor and preparation method thereof |
| 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 |
| CN110534353A (en) * | 2019-09-19 | 2019-12-03 | 福州大学 | A kind of preparation method and applications of the poly- 3,4- ethylenedioxy thiophene bonding graphene nanobelt of Congo red doping |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109326455A (en) * | 2018-10-31 | 2019-02-12 | 南京林业大学 | A kind of hydrophily polythiophene grafted graphene oxide electrode material for super capacitor and preparation method thereof |
| 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 |
| CN110534353A (en) * | 2019-09-19 | 2019-12-03 | 福州大学 | A kind of preparation method and applications of the poly- 3,4- ethylenedioxy thiophene bonding graphene nanobelt of Congo red doping |
| CN110534353B (en) * | 2019-09-19 | 2020-11-03 | 福州大学 | Preparation method and application of poly (3, 4-ethylenedioxythiophene) composite material |
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