CN105949459B - A kind of netted polyaniline nano piece and preparation method thereof - Google Patents
A kind of netted polyaniline nano piece and preparation method thereof Download PDFInfo
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- CN105949459B CN105949459B CN201610344759.0A CN201610344759A CN105949459B CN 105949459 B CN105949459 B CN 105949459B CN 201610344759 A CN201610344759 A CN 201610344759A CN 105949459 B CN105949459 B CN 105949459B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
Abstract
The invention discloses a kind of preparation methods of netted polyaniline nano piece, belong to electrode material for super capacitor technical field, the following steps are included: 1) disperse sodium acetate in deionized water, aniline monomer blending is added after being uniformly dispersed, reaction temperature is controlled at 20~40 DEG C, ammonium persulfate aqueous solution is added dropwise, after being added dropwise, the reaction was continued 5~20h, standing；2) after the product for obtaining step 1) filters, it is in colourless for being washed respectively with deionized water and dehydrated alcohol to filtrate, and netted polyaniline nano piece is obtained after vacuum drying；The invention also discloses polyanilines made from the preparation method.Method of the invention is environmentally protective and preparation process is simple；The polyaniline nano piece of this method preparation, average diameter are 5~6 microns, and average thickness is 180~220nm, can reach 473.6Fg as electrode material for super capacitor specific capacitance‑1, while can reach -27.2dB in 2~18GHz frequency range interior suction intensity of wave, it can be widely applied to supercapacitor and electromagnetic shielding field, have good practicability.
Description
Technical field
The invention belongs to electrode material for super capacitor technical fields, and in particular to a kind of netted polyaniline nano piece and its
Preparation method.
Background technique
Polyaniline is a kind of excellent super capacitor and electro-magnetic wave absorption shielding material, environmental stability is good, high conductivity,
Raw material is cheap, is readily synthesized, while having good mechanical strength and processing performance, thus in electrode of super capacitor preparation and
Electro-magnetic wave absorption field has broad application prospects.
Since the chemical property of polyaniline is largely dependent upon its specific surface area, the ratio table of polyaniline is promoted
Area is the most effective method for promoting its specific capacitance value and absorbing property.Such as disclosed in Chinese patent 201510387659.1
" a kind of electrode of super capacitor and preparation method thereof being made of the tree-shaped polyaniline of nanometer ".This method is under acidic environment with tree
Shape macromolecular is template, obtains diameter 1nm, the tree-shaped polyaniline of the nanometer of length 18nm by chemical oxidising polymerisation；The polyphenyl
Amine is blended with conductive agent, binder and dehydrated alcohol, is coated on stainless (steel) wire, by drying, super electricity is prepared into after tabletting
Container electrode material, specific capacitance value can reach 631.7~812.5Fg-1.But the preparation method is needed in acid condition
Under using dendrimer as template, and preparation process is complicated, is unfavorable for industrial application and environmental protection, to influence the material
The extensive use of material.
For another example " a kind of supercapacitor polyaniline nano fiber electrode material disclosed in Chinese patent 200910243308.8
Aniline monomer and initiator are dissolved in methylene chloride organic phase by the preparation method of material ", this method, and oxidant is dissolved in inorganic acid and is mixed
Miscellaneous dose of water phase, the interfacial polymerization at 0~30 DEG C prepare polyaniline nano fiber, and are applied to electrode of super capacitor material
Material, specific capacitance can reach 549Fg-1；This method is unfavorable for environmental protection and cost control using high toxicity methylene chloride as solvent
System, to influence the competitiveness of product in market and application range.
Summary of the invention
Goal of the invention: the purpose of the present invention is to provide a kind of preparation methods of netted polyaniline nano piece, not only prepare
Simple process, and cost is relatively low；It is a further object of the present invention to provide the polyaniline nano pieces of preparation method preparation.
Technical solution: for achieving the above object, the present invention adopts the following technical scheme:
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it disperses sodium acetate in deionized water, aniline monomer blending, reaction temperature control is added after being uniformly dispersed
At 20~40 DEG C, ammonium persulfate aqueous solution is added dropwise, after being added dropwise, the reaction was continued 5~20h, standing；
2) after the product for obtaining step 1) filters, it is in colourless for being washed respectively with deionized water and dehydrated alcohol to filtrate,
Netted polyaniline nano piece nano material is obtained after vacuum drying.
In step 1), the mass ratio of the sodium acetate, aniline and ammonium persulfate is 1:1~5.1:2.8~13.2.
In step 1), the mass ratio of the sodium acetate, aniline and ammonium persulfate is 1:2.75:7.4.
The product that step 2) is obtained is scattered in chloride solution, and magnetic stirs for 24 hours, is then filtered, is washed, vacuum drying
Up to the netted polyaniline nano piece nano material after doping.
The chloride is hydrochloric acid, and molar concentration is 0.01~0.05mol/L.
The chloride is sodium chloride or potassium chloride, and molar concentration is 0.01~0.05mol/L.
The vacuum drying oven temperature is 50~70 DEG C, and the time is 10~30h.
The polyaniline nano piece prepared by the preparation method of netted polyaniline nano piece, the polyaniline nano piece average diameter
It is 5~6 microns, average thickness is 180~220nm.
Inventive principle: using nontoxic sodium acetate for dopant, in the work of suitable temperature and appropriate initiator ammonium persulfate
Under, aniline monomer polymerize in deionized water obtains high-specific surface area tabular polyaniline nano material, by doping chlorine from
It is sub effectively to promote polyaniline conductivity, while the nanostructure specific capacitance with higher and electromagnetic consumable of high-specific surface area are special
Property, electric storage performance can be effectively improved, the electromaganic wave absorbing property of material is increased.
The utility model has the advantages that compared with prior art, the preparation method of netted polyaniline nano piece of the invention not only green ring
It protects, and preparation process is simple, cost is easily-controllable, meets current social economic development green low-carbon requirement；By side provided by the invention
The netted polyaniline nano piece of method preparation, average diameter are 5~6 microns, and average thickness is 180~220nm, as super electricity
Container electrode material specific capacitance can reach 473.6Fg-1, while can reach -27.2dB in 2~18GHz frequency range interior suction intensity of wave,
It can be widely applied to supercapacitor and electromagnetic shielding field, have good practicability.
Detailed description of the invention
Fig. 1 is netted polyaniline nano piece scanning electron microscope (SEM) figure prepared by the present invention；
Fig. 2 is common polyaniline scanning electron microscope (SEM) figure of in-situ polymerization；
Fig. 3 is netted polyaniline nano piece cycle charge-discharge curve graph prepared by the present invention；
Fig. 4 is the common polyaniline cycle charge-discharge curve graph of in-situ polymerization；
Fig. 5 is netted polyaniline nano electromagnetic wave reflection loss (R-F) curve graph prepared by the present invention；
Fig. 6 is that (R-F) curve graph is lost in the reflection of electromagnetic wave of the common polyaniline of in-situ polymerization.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
Embodiment 1
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it at room temperature disperses 0.17g sodium acetate in 500ml deionized water, magnetic is dispersed with stirring uniformly；Add 0.86g
Mixed solution is continued magnetic stirring 60min by aniline monomer；It disperses the ammonium persulfate of 2.34g in 500ml deionized water；Instead
It answers temperature control at 20 DEG C, ammonium persulfate solution is added dropwise to the mixed solution of sodium acetate and aniline；After being added dropwise, continue anti-
5h is answered, is stood；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 50 DEG C of vacuum drying 30h to get to netted polyaniline nano piece nano material,
Scanning electron microscope (SEM) figure is as shown in Figure 1, it is known that its average diameter is 5~6 μm, and average thickness is 180~220nm；
3) product for obtaining step 2) is scattered in 0.1mol/L hydrochloric acid solution, and magnetic stirs for 24 hours, is then filtered, and is washed,
30h is dried in vacuo under the conditions of 50 DEG C to get the netted polyaniline nano piece nano material of acidification is arrived.
Embodiment 2
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it at room temperature disperses 0.51g sodium acetate in 500ml deionized water, magnetic is dispersed with stirring uniformly；Add 0.86g
Mixed solution is continued magnetic stirring 60min by aniline monomer；It disperses the ammonium persulfate of 2.34g in 500ml deionized water；Instead
It answers temperature control at 25 DEG C, ammonium persulfate solution is added dropwise to the mixed solution of sodium acetate and aniline；After being added dropwise, continue anti-
10h is answered, is stood；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 70 DEG C of vacuum drying 10h to get to netted polyaniline nano piece nano material；
3) product for obtaining step 2) is scattered in 0.2mol/L hydrochloric acid solution, and magnetic stirs for 24 hours, is then filtered, and is washed,
10h is dried in vacuo under the conditions of 70 DEG C to get the netted polyaniline nano piece nano material of acidification is arrived.
Embodiment 3
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it at room temperature disperses 0.85g sodium acetate in 500ml deionized water, magnetic is dispersed with stirring uniformly；Add 0.86g
Mixed solution is continued magnetic stirring 60min by aniline monomer；It disperses the ammonium persulfate of 2.34g in 500ml deionized water；Instead
It answers temperature control at 30 DEG C, ammonium persulfate solution is added dropwise to the mixed solution of sodium acetate and aniline；After being added dropwise, continue anti-
15h is answered, is stood；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 60 DEG C of vacuum drying for 24 hours to get arriving netted polyaniline nano piece nano material；
3) product for obtaining step 2) is scattered in 0.3mol/L hydrochloric acid solution, and magnetic stirs for 24 hours, is then filtered, and is washed,
It is dried in vacuo under the conditions of 60 DEG C for 24 hours to get the netted polyaniline nano piece nano material for arriving acidification.
Embodiment 4
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it at room temperature disperses 0.51g sodium acetate in 500ml deionized water, magnetic is dispersed with stirring uniformly；Add 1.40g
Mixed solution is continued magnetic stirring 60min by aniline monomer；It disperses the ammonium persulfate of 3.78g in 500ml deionized water；Instead
It answers temperature control at 25 DEG C, ammonium persulfate solution is added dropwise to the mixed solution of sodium acetate and aniline；After being added dropwise, continue anti-
20h is answered, is stood；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 60 DEG C of vacuum drying for 24 hours to get arriving netted polyaniline nano piece nano material；
3) product for obtaining step 2) is scattered in 0.1mol/L sodium chloride solution, and magnetic stirs for 24 hours, is then filtered, is washed
It washs, is dried in vacuo under the conditions of 60 DEG C for 24 hours to get the netted polyaniline nano piece nano material for arriving acidification.As shown in Figure 3
Netted polyaniline nano piece cycle charge-discharge curve graph, using 1Ag-1When electric current carries out cyclic charging and discharging test to it, ratio
Capacitor can reach 473.6Fg-1。
Embodiment 5
A kind of preparation method of netted polyaniline nano piece, comprising the following steps:
1) it at room temperature disperses 0.51g sodium acetate in 500ml deionized water, magnetic is dispersed with stirring uniformly；Add 1.94g
Mixed solution is continued magnetic stirring 60min by aniline monomer；It disperses the ammonium persulfate of 5.22g in 500ml deionized water；Instead
It answers temperature control at 25 DEG C, ammonium persulfate solution is added dropwise to the mixed solution of sodium acetate and aniline；After being added dropwise, continue anti-
20h is answered, is stood；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 60 DEG C of vacuum drying for 24 hours to get arriving netted polyaniline nano piece nano material；
3) product for obtaining step 2) is scattered in 0.1mol/L Klorvess Liquid, and magnetic stirs for 24 hours, is then filtered, is washed
It washs, is dried in vacuo under the conditions of 60 DEG C for 24 hours to get the netted polyaniline nano piece nano material for arriving acidification.
Comparative example
1) 0.01mol/L hydrochloric acid solution 500ml is prepared at room temperature, and 1.40g aniline monomer is added, mixed solution is continued into magnetic
Stir 60min；It disperses the ammonium persulfate of 3.78g in 500ml deionized water；Reaction temperature is controlled at 25 DEG C, by persulfuric acid
Ammonium salt solution is added dropwise to the mixed solution of hydrochloric acid and aniline；After being added dropwise, the reaction was continued 20h, standing；
2) filtered after product that step 1) obtains being removed supernatant liquor, respectively with deionized water and dehydrated alcohol wash to
Filtrate in colourless, then in vacuum drying oven 60 DEG C of vacuum drying for 24 hours to get arriving common polyaniline nano material.Fig. 2 is shown
Dendritic structure polyaniline, average diameter are 50~200nm, and average length is 10~20 μm.Fig. 4 is that common polyaniline circulation is filled
Discharge curve, specific capacitance value maximum only have 288.1F/g；Fig. 6 is that common polyaniline electromagnetic wave in 2-18GHz frequency range is anti-
Loss (R-L) curve graph is penetrated, reflection loss maximum value only has -13.6dB.It is found that doped hydrochloride prepares common dendroid polyphenyl
Amine pattern is disorderly and unsystematic, and its specific capacitance value and electromagnetic wave absorption performance are also poor.
Claims (2)
1. a kind of preparation method of netted polyaniline nano piece, it is characterised in that: the following steps are included:
1) it disperses sodium acetate in deionized water, aniline monomer blending is added after being uniformly dispersed, reaction temperature is 20~40
DEG C, ammonium persulfate aqueous solution is added dropwise, after being added dropwise, the reaction was continued 5~20h, standing；Wherein, the sodium acetate, aniline and
The mass ratio of ammonium persulfate is 1:1~5.1:2.8~13.2；
2) after the product for obtaining step 1) filters, it is to obtain netted polyaniline to receive after vacuum drying that washing to filtrate, which is in colourless,
Rice piece；Wherein, product step 2) obtained is scattered in chloride solution, and magnetic stirring filters, washing, is dried in vacuo to obtain the final product
Netted polyaniline nano piece nano material after doping；The chloride is hydrochloric acid, sodium chloride or potassium chloride, mole dense
Degree is 0.01~0.05mol/L；The vacuum drying oven temperature is 50~70 DEG C, and the time is 10~30h；The polyaniline
Nanometer sheet average diameter is 5~6 microns, and average thickness is 180~220nm.
2. the preparation method of netted polyaniline nano piece according to claim 1, it is characterised in that: described in step 1)
Sodium acetate, aniline and ammonium persulfate mass ratio be 1:2.75:7.4.
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| CN107556474A (en) * | 2017-09-30 | 2018-01-09 | 江苏瑞腾涂装科技有限公司 | A kind of high-specific surface area polyaniline and preparation method thereof |
| CN108003604B (en) * | 2017-12-27 | 2020-09-25 | 兀帅帅 | Photothermal effect type self-repairing cable insulating material and preparation method thereof |
| CN108641080B (en) * | 2018-04-02 | 2020-12-15 | 陶玉仑 | High-yield and green synthesis method of conductive polyaniline |
| CN110723918A (en) * | 2019-10-15 | 2020-01-24 | 沈阳大学 | Nano material for freeze-thaw resistant concrete and use method thereof |
| CN112490450B (en) * | 2020-10-26 | 2022-05-10 | 温州大学 | Adhesive for microbial fuel cell, application, cathode and microbial fuel cell |
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