CN104119530A - Method for preparing conducting polyaniline nanotube - Google Patents
Method for preparing conducting polyaniline nanotube Download PDFInfo
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- CN104119530A CN104119530A CN201410376418.2A CN201410376418A CN104119530A CN 104119530 A CN104119530 A CN 104119530A CN 201410376418 A CN201410376418 A CN 201410376418A CN 104119530 A CN104119530 A CN 104119530A
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- polyaniline
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- aniline
- urea
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 55
- 239000002071 nanotube Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title abstract description 15
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 30
- 239000005457 ice water Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000012065 filter cake Substances 0.000 claims description 16
- 239000013067 intermediate product Substances 0.000 claims description 16
- 239000004160 Ammonium persulphate Substances 0.000 claims description 8
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 230000017105 transposition Effects 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005287 template synthesis Methods 0.000 description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Abstract
The invention discloses a method for preparing a conducting polyaniline nanotube. The method comprises the following steps: dispersing aniline in water solutions containing different proportions of urea, fully stirring under conditions of ice-water bath to obtain a uniform mixed solution, dropwise adding oxidation initiator-ammonium persulfate to initiate aniline polymerization, reacting for 12 hours while stirring and doping the product by using 2ml of 1mol/L hydrochloric acid solution to obtain the conducting polyaniline nanotube with a tubular structure. The specific capacitance of the polyaniline nanotube prepared by adopting the method disclosed by the invention is much greater than that of polyaniline and the polyaniline nanotube has a regular tubular structure and good electrochemical performances, so that the polyaniline nanotube is an ideal supercapacitor electrode material and is particularly suitable for industrial production; moreover, the urea is low in cost and wide in source; the polyaniline nanotube is simple in preparation process; the method is easy in large-scale popularization.
Description
Technical field
The invention belongs to conductive nanotube preparing technical field, particularly a kind ofly take urea as template, aniline is prepared the method for the Preparation of conductive polyaniline nanotubes with ordered structure by self-assembly and in-situ polymerization.
Background technology
Polyaniline is as a kind of common conductive polymers, because its preparation is simple, with low cost, and there is good environmental stability and unique physics and chemistry character, usually be used to ultracapacitor, battery, sensor and corrosion-resistant field, obtained the concern energetically of countries in the world researchers.The electrically conductive polyaniline particularly with nanostructure, due to the character such as electron transfer rate that its particle diameter is minimum, specific surface area large, be exceedingly fast, has given nano-conductive polyaniline material and has had the not available many special performances of conventional blocks.
Polyaniline nanotube, owing to shortening the distance of ion transportation, thereby improve the efficiency of ion and electrode generation redox reaction for diffusion and the mobile passage easily that provides of electrolyte ion, has been subject to concern and the research of researcher.For example with soft template method, prepare Preparation of conductive polyaniline nanotubes (Z.J. Gu, et al, Synthesis of polyaniline nanotubes with controlled rectangular or square pore shape. Mater. Lett. 2014,121,12-14, H.J. Yin, et al, Synthesis of high-performance one-dimensional polyaniline nanostructures using dodecylbenzene sulfonic acid as soft template. Mater. Lett. 2011,65,850-853, M.M. Sk, et al, Synthesis of polyaniline nanotubes using the self-assembly behavior of vitamin C:a mechanistic study and application in electrochemical supercapacitors. J. Mater. Chem. A 2014, 2, 2830-2838.) and without template synthesis Preparation of conductive polyaniline nanotubes (Z.Z. Huang, et al, Preparation of polyaniline nanotubes by a template-free self-assembly method. Mater. Lett. 2011, 65, 2015-2018.), polyaniline nanotube prepared by above-mentioned various soft template method has regular tubular structure and has good chemical property, but in suitability for industrialized production, there is certain difficulty.Without template synthesis polyaniline, there is environmental protection, the advantage such as simple, but the pipe diameter size of gained polyaniline nanotube cannot controlled and irregularity, affected to a certain extent the chemical property of polyaniline.
Urea has good water-soluble, and wide material sources, and especially it intermolecularly forms a large amount of hydrogen bonds, is suitable as the template of preparation nano material.With urea, as template, prepare the preparation method that polyaniline nanotube is a kind of simple and environmental protection, this thinking has no bibliographical information at present.
Summary of the invention
The object of this invention is to provide and a kind ofly take urea as template, by the method for self-assembling technique and in-situ polymerization, prepare the method for the Preparation of conductive polyaniline nanotubes with ordered structure.
Concrete steps are:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 0 ~ 2:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind and collect, make Preparation of conductive polyaniline nanotubes.
The inventive method has the following advantages:
(1) the inventive method, by changing the mol ratio of urea and aniline, can obtain internal diameter and the different polyaniline nano tube material of length-to-diameter ratio of surface roughness, pipe.
(2) much larger than capacity ratio polyaniline of the polyaniline nanotube that prepared by the present invention, prepared polyaniline nanotube has regular tubular structure and good chemical property, be a kind of desirable electrode material for super capacitor, be especially applicable to suitability for industrialized production.
(3) with low cost, the wide material sources of urea, polyaniline nanotube preparation technology is simple, and the method is easy to large-scale promotion.
Accompanying drawing explanation
Fig. 1 is SEM figure and the TEM figure of the Preparation of conductive polyaniline nanotubes of the embodiment of the present invention 4 preparations, and wherein (a) is SEM figure, is (b) TEM figure.
Fig. 2 is the cyclic voltammetry curve that the Preparation of conductive polyaniline nanotubes of the embodiment of the present invention 1 preparation and the electrically conductive polyaniline of embodiment 6 preparations are tested when scanning speed is 5mV/s; Wherein UREA-PANI is the cyclic voltammetry curve that the Preparation of conductive polyaniline nanotubes of embodiment 1 preparation is tested when scanning speed is 5mV/s, and PANI is the cyclic voltammetry curve that the electrically conductive polyaniline of embodiment 6 preparations is tested when scanning speed is 5mV/s.
Embodiment
embodiment 1:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 2:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
embodiment 2:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 1:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
embodiment 3:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 0.5:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
embodiment 4:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 0.25:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
embodiment 5:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 0.1:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
embodiment 6:
(1) by the flask that fills 30 ml deionized water from room temperature transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stir 12 hours, make intermediate product; In the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding.
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
Claims (1)
1. a preparation method for Preparation of conductive polyaniline nanotubes, is characterized in that concrete steps are:
(1) taking urea joins in the flask that fills 30 ml deionized water, after stirring at room 0.5 hour, by flask transposition in ice-water bath, then to the hydrochloric acid soln that adds 0.5 milliliter of aniline of having purified and 2 milliliter of 1 mol/L in flask, under the condition of ice-water bath, stir 1 hour, finally ammonium persulfate solution is dropwise added drop-wise in flask, under the condition of ice-water bath, stirs 12 hours, make intermediate product; The urea taking is 0 ~ 2:1 with the mol ratio of the aniline adding, and in the ammonium persulfate solution dripping, ammonium persulphate is 1:1 with the mol ratio of the aniline adding;
(2) the intermediate product filtering and washing with deionized water, step (1) being made, until filtrate is neutral, again to the hydrochloric acid soln that adds 2 milliliter of 1 mol/L in filter cake, polyaniline is fully adulterated, finally filter cake is inserted in the vacuum drying oven of 50 ℃ dry 24 hours, grind, make Preparation of conductive polyaniline nanotubes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892935A (en) * | 2015-05-21 | 2015-09-09 | 安徽大学 | Method for synthesizing polyaniline nanotubes |
| CN105037717A (en) * | 2015-08-27 | 2015-11-11 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking glucose as template |
| CN105131281A (en) * | 2015-10-09 | 2015-12-09 | 桂林理工大学 | Method for manufacturing conductive polyaniline nanotube by using xylitol as template |
| CN105131282A (en) * | 2015-10-09 | 2015-12-09 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking sucrose as template |
| CN105906805A (en) * | 2016-04-28 | 2016-08-31 | 桂林理工大学 | Method for preparing conductive polyaniline nanotubes by taking niacin as template and dopant |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892935A (en) * | 2015-05-21 | 2015-09-09 | 安徽大学 | Method for synthesizing polyaniline nanotubes |
| CN104892935B (en) * | 2015-05-21 | 2017-03-01 | 安徽大学 | A kind of method of synthesized polyaniline nanotube |
| CN105037717A (en) * | 2015-08-27 | 2015-11-11 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking glucose as template |
| CN105131281A (en) * | 2015-10-09 | 2015-12-09 | 桂林理工大学 | Method for manufacturing conductive polyaniline nanotube by using xylitol as template |
| CN105131282A (en) * | 2015-10-09 | 2015-12-09 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking sucrose as template |
| CN105906805A (en) * | 2016-04-28 | 2016-08-31 | 桂林理工大学 | Method for preparing conductive polyaniline nanotubes by taking niacin as template and dopant |
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| CN104119530B (en) | 2016-04-06 |
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