CN109216037A - Ternary composite electrode material based on bacteria cellulose and preparation method thereof - Google Patents
Ternary composite electrode material based on bacteria cellulose and preparation method thereof Download PDFInfo
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- CN109216037A CN109216037A CN201810922707.6A CN201810922707A CN109216037A CN 109216037 A CN109216037 A CN 109216037A CN 201810922707 A CN201810922707 A CN 201810922707A CN 109216037 A CN109216037 A CN 109216037A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/24—Electrodes 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of ternary composite electrode material and preparation method thereof based on bacteria cellulose.Pyrrole monomer and oxidant is first added in the method in bacterial cellulose suspension, at a lower reaction temperature, polypyrrole/bacteria cellulose binary complex of nucleocapsid structure is prepared through in-situ oxidizing-polymerizing, then, polypyrrole/bacteria cellulose binary complex is dispersed in water, source metal presoma is added, is co-deposited in aqueous slkali, room temperature ageing prepares core-shell structure copolymer-shell structure nickel manganese double-metal hydroxide/polypyrrole/bacteria cellulose ternary composite electrode material.Raw material of the present invention is easy to get, is cheap, reaction is mild, preparation is simple, and the ternary electrode material of preparation has be cross-linked with each other space structure and high specific capacitance, has broad application prospects in electrochemical energy storage field.
Description
Technical field
The invention belongs to electrode material technical field, be related to a kind of ternary composite electrode material based on bacteria cellulose and
Preparation method.
Background technique
Supercapacitor is as a kind of novel energy storage and energy conversion device, because its production cost is low, production method is simple
The features such as single efficient, production process is environmentally protective, chemical property is superior, service life is longer, has received widespread attention.Simultaneously
Supercapacitor compensates for the deficiency of battery and traditional capacitor, high energy density and power density is provided, in electronic vapour
Vehicle, portable electronic device, backup power source etc. have a wide range of applications.Core of the electrode material as supercapacitor
Part has vital influence (1. Wang, F. to the performance of supercapacitor；et al.,Latest advances in
supercapacitors:from new electrode materials to novel device designs.Chemical
Society reviews 2017,46(22),6816-6854)。
Bacteria cellulose has excellent biological degradability and bio-compatible as environmental-friendly biological macromolecule material
Property.Meanwhile bacteria cellulose has porous hyperfine network structure, porosity is high；A large amount of hydroxy functional group is contained on surface,
Hydrophily is strong, can be embedded in the size and size of nano particle in its network structure (2. by the control of different synthetic methods
Wang,X.；et al.,All-biomaterial supercapacitor derived from bacterial
cellulose.Nanoscale 2016,8(17),9146-50.③Wang,Z.；et al.,Cellulose based
supercapacitors:materials and performance considerations.Advanced Energy
Materials 2017,1700130)。
Traditional carbon material has very high load capacity and stability, but the contribution margin of capacitor is not high.Conducting polymer
It, can be in electrode material surface and internal generation Rapid reversible when with transistion metal compound as electrode material for super capacitor
Redox reaction, make electrode store charge density improve, to generate bigger quasi- faraday's capacitor.Except this it
Outside, the nanosizing of electrode material and porous structure are constructed, can be effectively reduced metallic compound in electrode reaction from
Son diffusion and charge transporting resistance, have synergistic effect.
In recent years, researcher has studied bacteria cellulose carbonization and prepares the carbon nano-fiber of Heteroatom doping and its super
The application of capacitor area.Ning et al. first passes through polypyrrole/bacterial fibers that oxidation polymerization method has prepared nucleocapsid structure
Plain active material, after in N2Lower calcining obtains the carbonized celulose of N doping, obtains nickel cobalt sulfide/N doping through hydro-thermal method
Carbonized celulose compound.The compound is in 1A g-1Under, specific capacitance reaches 1078F g-1, when current density increases to 5A g-1
When, specific capacitance retention rate reaches 94.6% (4. Ning, X.；et al.,Confined growth of uniformly
dispersed NiCo2S4 nanoparticles on nitrogen-doped carbon nanofibers for high-
performance asymmetric supercapacitors.Chemical Engineering Journal 2017,328,
599-608.).At the same time, bacteria cellulose is directly obtained with conducting polymer, the compound electrode material for preparing of metallic compound
Certain achievement.Lv et al. first passes through hydro-thermal method and has prepared ferroso-ferric oxide/bacteria cellulose binary composite, after
N-butanol/water in the mixed solvent has been prepared polypyrrole/ferroso-ferric oxide/bacteria cellulose ternary by oxidation polymerization method and has been answered
Close object.The ternary complex has fabulous mechanical performance and high area specific capacitance, reaches 8.4mg in active material load capacity
cm-2When, area specific capacitance is 5.4F cm-2(⑤Lv,X.；et al.,Fabricate BC/Fe3O4@PPy 3D nanofiber
film as flexible electrode for supercapacitor application.Journal of Physics
and Chemistry of Solids 2018,116,153-160)。
Summary of the invention
The purpose of the present invention is to provide a kind of ternary composite electrode material and preparation method thereof based on bacteria cellulose.
The electrode material has core-shell structure copolymer-shell microstructure, using bacteria cellulose as substrate, has stepped through in-situ chemical pyrrole polymerization, changes
It learns deposition nickel manganese double-hydroxide and prepares ternary composite electrode material.
Realize that the technical solution of the object of the invention is as follows:
The preparation method of ternary composite electrode material based on bacteria cellulose, the specific steps are as follows:
Step 1, pyrrole monomer is added in bacterial cellulose suspension, the hydrochloric acid that ferric trichloride is added dropwise under ice bath is molten
The mass ratio of liquid, pyrrole monomer and bacteria cellulose is 10:1~20:1, the chemical polymerization at 0~10 DEG C, after reacting 12~36h
Filtering, is washed with water and dehydrated alcohol respectively, polypyrrole/bacteria cellulose binary composite is obtained after freeze-drying；
Step 2, polypyrrole/bacteria cellulose is dispersed in water, six water nickel nitrates, four water manganese nitrates and fluorination is added
Ammonium, ultrasonic treatment obtain uniform dispersion liquid, wherein the mass ratio of polypyrrole/bacteria cellulose and nickel nitrate is 1:33~1:
11, the molar ratio of nickel nitrate and manganese nitrate is 3:1, and the mixed solution of sodium hydroxide and sodium carbonate, after being added dropwise, room temperature is added dropwise
Lower ageing, centrifugation, is washed with water and dehydrated alcohol, and it is fine that nickel manganese double-metal hydroxide/polypyrrole/bacterium is obtained after freeze-drying
Tie up plain ternary composite electrode material.
Preferably, in step 1, the concentration of the bacterial cellulose suspension is 2.5mg mL-1。
Preferably, in step 2, the mass ratio of the polypyrrole/bacteria cellulose and nickel nitrate is 2:33.
Preferably, in step 2, the molar concentration of the nickel nitrate is 11.3mM.
Compared with prior art, the present invention having the advantage that
(1) porous network structure of bacteria cellulose itself, Effective Regulation conducting polymer and metallic compound are utilized
Pattern, construct three-dimensional conductive network, meanwhile, this method greatly increases the specific surface area of combination electrode material, favorably
In electrolyte electrode interior transmission and diffusion；
(2) nickel manganese double-metal hydroxide/polypyrrole/bacteria cellulose electroactive material is in 1A g-1Current density
Under, specific capacity reaches 653.1C g-1；
(3) raw material is cheap and easy to get, reaction is mild, easy to operate, suitable for the compound of conducting polymer and metallic compound,
Suitable for large-scale production.
Detailed description of the invention
Fig. 1 is that nickel manganese double-metal hydroxide/polypyrrole/bacteria cellulose ternary composite electrode material preparation process is shown
It is intended to.
Fig. 2 is bacteria cellulose (a), polypyrrole/bacteria cellulose binary composite (b) made from embodiment 1, implements
The double-metal hydroxide of nickel manganese made from example 4/polypyrrole/bacteria cellulose ternary composite electrode material (c) scanning electron microscope (SEM) photograph.
Fig. 3 is polypyrrole/bacteria cellulose binary composite (a) made from embodiment 1, nickel manganese made from embodiment 4
Double-metal hydroxide/polypyrrole/bacteria cellulose ternary composite electrode material (b) transmission electron microscope picture.
Fig. 4 is polypyrrole made from embodiment 1-2 and comparative example 1/bacteria cellulose binary composite in 1A g-1Electric current
Discharge curve under density.
Fig. 5 is that nickel manganese double-hydroxide/polypyrrole/bacterial cellulose three-dimensional made from embodiment 3-5 and comparative example 2 is compound
Electrode material is in 1A g-1Discharge curve under current density.
Specific embodiment
The present invention is further elaborated with attached drawing combined with specific embodiments below, but the invention is not limited to implementations
Example.
Embodiment 1
Pyrrole monomer (2g, 2.1mL) is added to bacterial cellulose suspension (2.5mg mL-1, 80mL) in, it is dripped under ice bath
Add the hydrochloric acid solution (0.1M, 60mL) of ferric trichloride (0.98g), the mass ratio of pyrrole monomer and bacteria cellulose is 10:1,0
Chemical polymerization at DEG C, reaction are filtered afterwards for 24 hours, are washed respectively with water and dehydrated alcohol, and it is fine that polypyrrole/bacterium is obtained after freeze-drying
Tie up plain binary composite.
Shown in the scanning electron microscope (SEM) photograph of products therefrom such as Fig. 2 (b) and transmission electron microscope Fig. 3 (a), compared to the scanning of bacteria cellulose
The nanofiber surface of electron microscope 2 (a), product it is more coarse and have nucleocapsid structure, the nanofiber being cross-linked with each other it is straight
Diameter about 150nm.Product is in 1A g-1For discharge curve under current density as shown in curve c in Fig. 4, specific capacity reaches 234.2C
g-1。
Embodiment 2
Pyrrole monomer (4g, 4.2mL) is added to bacterial cellulose suspension (2.5mg mL-1, 80mL) in, it is dripped under ice bath
Add the hydrochloric acid solution (0.1M, 60mL) of ferric trichloride (1.96g), the mass ratio of pyrrole monomer and bacteria cellulose is 20:1,0
Chemical polymerization at DEG C, reaction are filtered afterwards for 24 hours, are washed respectively with water and dehydrated alcohol, and it is fine that polypyrrole/bacterium is obtained after freeze-drying
Tie up plain binary composite.
Products therefrom is in 1A g-1As shown in curve b in Fig. 4, specific capacity reaches discharge curve under current density
185.1C g-1。
Embodiment 3
Pyrrole monomer (2g, 2.1mL) is added to bacterial cellulose suspension (2.5mg mL by step 1-1, 80mL) in, ice
Bath is descended the hydrochloric acid solution (0.1M, 60mL) of ferric trichloride (0.98g) is added dropwise, and the mass ratio of pyrrole monomer and bacteria cellulose is
10:1, the chemical polymerization at 0 DEG C, reaction filter afterwards for 24 hours, are washed respectively with water and dehydrated alcohol, poly- pyrrole is obtained after freeze-drying
Cough up/bacteria cellulose binary composite.
Polypyrrole/bacteria cellulose (10mg) is dispersed in 100mL water by step 2, six water nickel nitrates (330mg) of addition,
Four water manganese nitrates (94mg) and ammonium fluoride (167mg), ultrasonic treatment obtain uniform dispersion liquid, wherein polypyrrole/bacterial fibers
The mass ratio of element and nickel nitrate is 1:33, and the mixed solution (60mL) of sodium hydroxide (12mM) and sodium carbonate (30mM), drop is added dropwise
It after adding, is aged at room temperature, is centrifuged, is washed with water and dehydrated alcohol, nickel manganese bimetal hydroxide is obtained after freeze-drying
Object/polypyrrole/bacteria cellulose trielement composite material.
Products therefrom is in 1A g-1As shown in curve b in Fig. 5, specific capacity reaches discharge curve under current density
400.3C g-1, compared to for the resulting polypyrrole of embodiment 1/bacteria cellulose binary complex, specific capacity is greatly improved, electricity
Chemical property is preferable.
Embodiment 4
Pyrrole monomer (2g, 2.1mL) is added to bacterial cellulose suspension (2.5mg mL by step 1-1, 80mL) in, ice
Bath is descended the hydrochloric acid solution (0.1M, 60mL) of ferric trichloride (0.98g) is added dropwise, and the mass ratio of pyrrole monomer and bacteria cellulose is
10:1, the chemical polymerization at 0 DEG C, reaction filter afterwards for 24 hours, are washed respectively with water and dehydrated alcohol, poly- pyrrole is obtained after freeze-drying
Cough up/bacteria cellulose binary composite.
Polypyrrole/bacteria cellulose (20mg) is dispersed in 100mL water by step 2, six water nickel nitrates (330mg) of addition,
Four water manganese nitrates (94mg) and ammonium fluoride (167mg), ultrasonic treatment obtain uniform dispersion liquid, wherein polypyrrole/bacterial fibers
The mass ratio of element and nickel nitrate is 2:33, and the mixed solution (60mL) of sodium hydroxide (12mM) and sodium carbonate (30mM), drop is added dropwise
It after adding, is aged at room temperature, is centrifuged, is washed with water and dehydrated alcohol, nickel manganese bimetal hydroxide is obtained after freeze-drying
Object/polypyrrole/bacteria cellulose trielement composite material.
Shown in scanning electron microscope Fig. 2 (c) and transmission electron microscope Fig. 3 (b) of products therefrom, product has flower-like structure.Compared to poly-
Pyrroles/bacteria cellulose binary complex scanning electron microscope Fig. 2 (b) and transmission electron microscope Fig. 3 (a), nanofiber have core-shell structure copolymer-
Shell structure, the nanofiber diameter being cross-linked with each other is bigger, about 250nm.Product is in 1A g-1Discharge curve under current density is such as
In Fig. 5 shown in curve d, specific capacity reaches 653.1C g-1。
Embodiment 5
Pyrrole monomer (2g, 2.1mL) is added to bacterial cellulose suspension (2.5mg mL by step 1-1, 80mL) in, ice
Bath is descended the hydrochloric acid solution (0.1M, 60mL) of ferric trichloride (0.98g) is added dropwise, and the mass ratio of pyrrole monomer and bacteria cellulose is
10:1, the chemical polymerization at 0 DEG C, reaction filter afterwards for 24 hours, are washed respectively with water and dehydrated alcohol, poly- pyrrole is obtained after freeze-drying
Cough up/bacteria cellulose binary composite.
Polypyrrole/bacteria cellulose (30mg) is dispersed in 100mL water by step 2, six water nickel nitrates (330mg) of addition,
Four water manganese nitrates (94mg) and ammonium fluoride (167mg), ultrasonic treatment obtain uniform dispersion liquid, wherein polypyrrole/bacterial fibers
The mass ratio of element and nickel nitrate is 1:11, and the mixed solution (60mL) of sodium hydroxide (12mM) and sodium carbonate (30mM), drop is added dropwise
It after adding, is aged at room temperature, is centrifuged, is washed with water and dehydrated alcohol, nickel manganese bimetal hydroxide is obtained after freeze-drying
Object/polypyrrole/bacteria cellulose trielement composite material.
Products therefrom is in 1A g-1As shown in curve c in Fig. 5, specific capacity reaches discharge curve under current density
500.9C g-1, compared with the resulting nickel manganese double-hydroxide/polypyrrole/bacteria cellulose ternary complex of embodiment 4, than
Capacity is smaller, and chemical property is poor.
Comparative example 1
This comparative example is substantially the same manner as Example 1, the difference is that the mass ratio of pyrrole monomer and bacteria cellulose is 5:1.
Pyrrole monomer (1g, 1.05mL) is added to bacterial cellulose suspension (2.5mg mL-1, 80mL) in, trichlorine is added dropwise under ice bath
Change the hydrochloric acid solution (0.1M, 60mL) of iron (0.49g), other steps are all the same.
Products therefrom is in 1A g-1For discharge curve under current density as shown in curve a in Fig. 4, specific capacity reaches 164C
g-1, compared with 1 products therefrom of embodiment, specific capacity is smaller, and chemical property is poor.
Comparative example 2
This comparative example is substantially the same manner as Example 3, uniquely the difference is that the quality of polypyrrole/bacteria cellulose and nickel nitrate
Than for 5:33.Polypyrrole/bacteria cellulose (50mg) is dispersed in 100mL water, six water nickel nitrates (330mg) are added, it is other
Operating procedure is all the same.
Products therefrom is in 1A g-1As shown in curve a in Fig. 5, specific capacity reaches discharge curve under current density
275.4C g-1, compared with 4 products therefrom of embodiment, specific capacity very little, chemical property is poor.
Claims (5)
1. the preparation method of the ternary composite electrode material based on bacteria cellulose, which is characterized in that specific step is as follows:
Step 1, pyrrole monomer is added in bacterial cellulose suspension, the hydrochloric acid solution of ferric trichloride, pyrrole is added dropwise under ice bath
The mass ratio for coughing up monomer and bacteria cellulose is 10:1~20:1, and the chemical polymerization at 0~10 DEG C filters after reacting 12~36h,
It is washed respectively with water and dehydrated alcohol, polypyrrole/bacteria cellulose binary composite is obtained after freeze-drying；
Step 2, polypyrrole/bacteria cellulose is dispersed in water, six water nickel nitrates, four water manganese nitrates and ammonium fluoride is added, surpassed
Sonication obtains uniform dispersion liquid, wherein the mass ratio of polypyrrole/bacteria cellulose and nickel nitrate is 1:33~1:11, nitre
The molar ratio of sour nickel and manganese nitrate is 3:1, and the mixed solution of sodium hydroxide and sodium carbonate is added dropwise, old at room temperature after being added dropwise
Change, centrifugation is washed with water and dehydrated alcohol, nickel manganese double-metal hydroxide/polypyrrole/bacteria cellulose is obtained after freeze-drying
Ternary composite electrode material.
2. preparation method according to claim 1, which is characterized in that in step 1, the bacterial cellulose suspension
Concentration is 2.5mg mL-1。
3. preparation method according to claim 1, which is characterized in that in step 2, the polypyrrole/bacteria cellulose
Mass ratio with nickel nitrate is 2:33.
4. preparation method according to claim 1, which is characterized in that in step 2, the molar concentration of the nickel nitrate is
11.3mM。
5. ternary composite electrode material made from preparation method according to any one of claims 1 to 4.
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Cited By (1)
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| CN110581027A (en) * | 2019-09-30 | 2019-12-17 | 长江勘测规划设计研究有限责任公司 | Preparation method of composite pseudo capacitor electrode material |
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Application publication date: 20190115 |