CN105754093A - Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant - Google Patents
Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant Download PDFInfo
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- CN105754093A CN105754093A CN201610245420.5A CN201610245420A CN105754093A CN 105754093 A CN105754093 A CN 105754093A CN 201610245420 A CN201610245420 A CN 201610245420A CN 105754093 A CN105754093 A CN 105754093A
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- malic acid
- aniline
- conductive polyaniline
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
Abstract
The invention discloses a method for preparing a conductive polyaniline nano-rod by using malic acid as a template and a dopant.The method comprises the following steps: dispersing aniline in an aqueous solution containing the malic acid at different ratios, and fully stirring under the condition of ice water bath to obtain an even mixed solution; then dropwise adding ammonium persulfate as an oxidation initiator, initiating polymerization of aniline, and reacting for 12 hours under the condition of stirring; adding 2 mL of 1M hydrochloric acid solution in the solution so that polyaniline is fully doped; washing and carrying out suction filtration with deionized water until filtrate is neutral; and finally, drying at the temperature of 50 DEG C, and grinding and collecting to obtain the conductive polyaniline nano-rod.A preparation process of the invention is simple, environmentally friendly and reliable, sources of raw materials are extensive, cost is low, the method is suitable for industrial production, and compared with massive polyaniline, the obtained conductive polyaniline with the nano-rod-shaped structure has lower resistance and higher specific capacitance.
Description
Technical field
The invention belongs to electrically conductive polyaniline preparing technical field, particularly to a kind of method preparing conductive polyaniline nanometer rod for template and adulterant with malic acid.It particularly relates to one is with malic acid for template and adulterant, the method that aniline prepares the electrically conductive polyaniline with nano bar-shape structure by self assembly and in-situ polymerization.
Background technology
Polyaniline is as a kind of common conducting polymer, owing to its preparation is simple, with low cost, and there is good environmental stability and unique physics and chemical property, it is typically used to ultracapacitor, battery, sensor and corrosion-resistant field, obtains the concern energetically of countries in the world researcher.Particularly there is the electrically conductive polyaniline of nanostructured, owing to its particle diameter is minimum, the character such as specific surface area is big, the electron transfer rate that is exceedingly fast, imparts nano-conductive polyaniline material and there are the many special performances not available for conventional blocks.
Polyaniline nano-rod has big specific surface area, it is possible to be effectively improved the efficiency of ion and electrode generation redox reaction, receives concern and the research of researcher.Such as conductive polyaniline nanometer rod (X.D.Fu is prepared with soft template method, etal, Alignedpolyanilinenanorodsinsitugrownongasdiffusionlayer andtheirapplicationinpolymerelectrolytemembranefuelcells .InternationalJournalofHydrogenEnergy, 2016,41,3655-3663;Y.W.Chengetal,Branchedandphenazinizedpolyanilinenanorodpreparedinthepresenceofmeta-phenylenediamine.SyntheticMetals,2013,168,48-57;Y.Z.Li, etal, OrientedArraysofPolyanilineNanorodsGrownonGraphiteNanosh eetsforanElectrochemicalSupercapacitor.Langmuir, 2013,29,493-500.).Polyaniline nano-rod prepared by above-mentioned various soft template method has regular club shaped structure and has good chemical property.
Malic acid has good water solublity, and relative to any of the above method, there is wide material sources, the advantage such as cheap, especially there is substantial amounts of hydroxyl in its strand, substantial amounts of hydrogen bond can be formed with aniline molecule, be suitable as the template preparing nano bar-shape material；Meanwhile, malic acid can as the adulterant of polyaniline, it is possible to be effectively improved the chemical property of polyaniline.Make template with malic acid and adulterant to prepare polyaniline nano-rod be a kind of simple and environmental protection preparation method, the compound with regular structure of gained polyaniline nano-rod and there is good chemical property, it is a kind of desirably electrode material for super capacitor, is especially suitable for industrialized production.
Summary of the invention
It is an object of the invention to provide a kind of with malic acid be template and adulterant, method by self-assembling technique and the in-situ polymerization method of preparing the conductive polyaniline nanometer rod with ordered structure.
Concretely comprise the following steps:
Measure malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance ratio of described malic acid and aniline is 0.1 ~ 5:1；The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
The inventive method has the advantage that
The inventive method preparation process is simple and environmentally-friendly, reliable, and raw material sources are extensive, with low cost, is suitable for industrialized production, and the electrically conductive polyaniline of gained nano bar-shape structure has less resistance, higher ratio electric capacity than block polyaniline.
The present invention utilizes the hydroxyl on malic acid molecule and carboxyl and aniline molecule formation hydrogen bond to prepare the electrically conductive polyaniline with nano bar-shape structure, nano bar-shape structure can for the diffusion of electrolyte ion with mobile provide good passage, enable ion that redox reaction to occur fully with electrode material, increase the ratio electric capacity of material, reduce internal resistance, thus obtaining the nano bar-shape structure polyaniline with good electrical chemical property, it it is a kind of desirably electrode material for super capacitor.
Accompanying drawing explanation
Fig. 1 is the cyclic voltammogram of the conductive polyaniline nanometer rod that the embodiment of the present invention 1 prepares.
Fig. 2 is the constant current charge-discharge figure of the conductive polyaniline nanometer rod that the embodiment of the present invention 1 prepares.
Fig. 3 is the scanning electron microscope (SEM) photograph of the conductive polyaniline nanometer rod that the embodiment of the present invention 1 prepares.
Detailed description of the invention
Embodiment 1:
Weigh 0.074g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Embodiment 2:
Weigh 0.186g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Embodiment 3:
Weigh 0.372g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Embodiment 4:
Weigh 0.744g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Embodiment 5:
Weigh 1.861g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Embodiment 6:
Weigh 3.721g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared.
The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
Claims (1)
1. the method preparing conductive polyaniline nanometer rod for template and adulterant with malic acid, it is characterised in that concretely comprise the following steps:
Measure malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then the aniline and the 2mL concentration that add 0.5mL in flask are the hydrochloric acid solution of 1mol/L, 1h is stirred under the condition of ice-water bath, prepare mixed liquor, then in mixed liquor, it is added dropwise over ammonium persulfate solution, 12h is stirred when ice-water bath, add the hydrochloric acid solution that 2mL concentration is 1mol/L, finally wash with deionized water, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely conductive polyaniline nanometer rod is prepared；
The amount of substance ratio of described malic acid and aniline is 0.1 ~ 5:1；The amount of substance of described Ammonium persulfate. and aniline is than for 1:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610245420.5A CN105754093A (en) | 2016-04-20 | 2016-04-20 | Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant |
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| CN201610245420.5A CN105754093A (en) | 2016-04-20 | 2016-04-20 | Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant |
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| CN105754093A true CN105754093A (en) | 2016-07-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625484A (en) * | 2020-10-20 | 2021-04-09 | 兰州理工大学 | Preparation method and application of conductive polysiloxane-polyaniline anticorrosive coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302293A (en) * | 2008-07-04 | 2008-11-12 | 西北工业大学 | Preparation of polyaniline nano-rods |
| US7713446B2 (en) * | 2004-06-28 | 2010-05-11 | The Ohio State Univeristy | Synthesis of nanofibers of polyaniline and substituted derivatives |
| CN105037718A (en) * | 2015-08-27 | 2015-11-11 | 桂林理工大学 | Method for preparing conductive polyaniline nano tube by taking D-tartaric acid as template |
-
2016
- 2016-04-20 CN CN201610245420.5A patent/CN105754093A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7713446B2 (en) * | 2004-06-28 | 2010-05-11 | The Ohio State Univeristy | Synthesis of nanofibers of polyaniline and substituted derivatives |
| CN101302293A (en) * | 2008-07-04 | 2008-11-12 | 西北工业大学 | Preparation of polyaniline nano-rods |
| CN105037718A (en) * | 2015-08-27 | 2015-11-11 | 桂林理工大学 | Method for preparing conductive polyaniline nano tube by taking D-tartaric acid as template |
Non-Patent Citations (1)
| Title |
|---|
| LIJUAN ZHANG ET AL.: ""The effect of hydrogen bonding on self-assembled polyaniline nanostructures"", 《ADVANCED FUNCTIONAL MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625484A (en) * | 2020-10-20 | 2021-04-09 | 兰州理工大学 | Preparation method and application of conductive polysiloxane-polyaniline anticorrosive coating |
| CN112625484B (en) * | 2020-10-20 | 2021-12-31 | 兰州理工大学 | Preparation method and application of conductive polysiloxane-polyaniline anticorrosive coating |
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Application publication date: 20160713 |
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