CN102140249B - Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method - Google Patents
Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method Download PDFInfo
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- CN102140249B CN102140249B CN 201010607616 CN201010607616A CN102140249B CN 102140249 B CN102140249 B CN 102140249B CN 201010607616 CN201010607616 CN 201010607616 CN 201010607616 A CN201010607616 A CN 201010607616A CN 102140249 B CN102140249 B CN 102140249B
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- silver
- silver nitrate
- polypyrrole composite
- pyrrole monomer
- polypyrrole
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Abstract
The invention discloses a method for quickly preparing silver/polypyrrole composite sol. An oxidation-reduction reaction between a silver salt and a pyrrole monomer is a simple and effective method for preparing a silver/polypyrrole composite material, but has the defect of low dynamic reaction speed. In the invention, a method for adding a microwave external field irradiation solution into a reaction system is provided, so that the reaction speed is effectively increased, and the silver/polypyrrole composite sol is formed within 15-270 minutes.
Description
Technical field
The present invention relates to the preparation method of a kind of silver/polypyrrole complex sol, be specifically related to utilize microwave technology to improve the method for the kinetic reaction speed between silver salt and the pyrrole monomer.
Background technology
Precious metal/conducting polymer composite is an important branch of metal/polymer composite material, all has important application at aspects such as biology, storage, electronics and catalysis.Utilizing the redox reaction between precious metal and the monomer is a kind of simple and effective method for preparing precious metal/conductive polymer composite, at present, utilize this method to prepare matrix materials such as comprising gold/polypyrrole, gold/polyaniline, silver/polypyrrole and silver/polyaniline.Yet, when preparation silver/Pt/Polypyrrole composite material, although find that the reaction between silver ions and the pyrrole monomer is feasible at thermodynamics, but very slow [the Matthew C.Henry of kinetics speed that should react, Chen-Chan Hsueh, Brian P.Timko, Michael S.Freund, Reaction of pyrrole and chlorauric acid,: a new route to composite colloids, J.Electrochem.Soc.148 (11) (2001) D155-D161.], for example, do not having under the condition of illumination, forming silver/polypyrrole film in 0.5M Silver Nitrate+0.5M pyrroles's aqueous solution needs 48 hours [M.A.Breimer, G.Yevgeny, S.Sy, O.A.Sadik, Incorporation of metal nanoparticles in photopolymerized organic conducting polymers:A mechanistic insight, Nano Lett.1 (2001) 305-308.].Although ultraviolet light irradiation can shorten the required time of this process to a certain extent, still needs a few hours, and the rarely seen report of method of relevant this reaction kinetics speed of other Effective Raise.
Summary of the invention
The object of the invention is intended to propose a kind of method that simply and effectively prepares fast silver/polypyrrole complex sol, in order to effectively solve the kinetics speed issue in the matrix material forming process.
Preparation method of the present invention comprises the steps:
(1) respectively Silver Nitrate and pyrrole monomer are dissolved in N, among the N '-dimethyl formamide (or ethylene glycol), then mixed nitrate silver and pyrrole monomer solution; Or successively Silver Nitrate and pyrrole monomer are dissolved in N, among the N '-dimethyl formamide (or ethylene glycol), to form the mixing solutions of Silver Nitrate and pyrrole monomer.The concentration of Silver Nitrate and pyrrole monomer is controlled at 0.01-2.0M.
(2) power range with microwave is set in 200-900W, and Temperature Setting is at 30-150 ℃, and the time was set in 15 minutes-270 minutes, and the mixing solutions of step (1) is carried out microwave exposure, until form the silver of homogeneous/polypyrrole complex sol;
Organic solvent N, N '-dimethyl formamide, or all have good solubility for Silver Nitrate and pyrrole monomer in the ethylene glycol, simultaneously microwave is had good sorption, therefore be conducive to the uniform contact of two kinds of reactants, thereby improve homogeneity and the speed of response of product.This microwave method has the advantages such as simple to operate, that speed of response is fast.
Description of drawings
Fig. 1 the inventive method is utilized the UV-Vis absorption spectrum of the Ag/PPy complex sol of microwave technology preparation, (A) in DMF solution; (B) in ethylene glycol solution.
Embodiment
Embodiment 1
Such as above-mentioned step, take by weighing the Silver Nitrate of 300mg and the pyrrole monomer of 0.55ml, be dissolved in respectively among the DMF of 40ml, then two kinds of solution are mixedly configured into Silver Nitrate+pyrroles's mixing solutions.After stirring, this mixing solutions being placed microwave device, is 500W at power, and temperature is under 70 ℃ of conditions, and microwave exposure obtains the Ag/PPy complex sol after 20 minutes, and its UV-Vis absorption spectrum figure is seen Figure 1A.
Embodiment 2
Such as above-mentioned step, take by weighing the Silver Nitrate of 300mg and the pyrrole monomer of 0.55ml, be dissolved in respectively among the DMF of 40ml, then two kinds of solution are mixedly configured into Silver Nitrate+pyrroles's mixing solutions.After stirring, this mixing solutions being placed microwave device, is 600W at power, and temperature is under 70 ℃ of conditions, and microwave exposure obtains the Ag/PPy complex sol after 30 minutes, and its UV-Vis absorption spectrum figure is seen Figure 1B.
Embodiment 3
Such as above-mentioned step, take by weighing the Silver Nitrate of 1.36g and the pyrrole monomer of 5.7ml, be dissolved in respectively among the DMF of 40ml, then two kinds of solution are mixedly configured into Silver Nitrate+pyrroles's mixing solutions.After stirring, this mixing solutions being placed microwave device, is 900W at power, and temperature is under 80 ℃ of conditions, and microwave exposure obtains the Ag/PPy complex sol after 5 minutes;
Embodiment 4
Such as above-mentioned step, take by weighing the Silver Nitrate of 68mg and the pyrrole monomer of 0.29ml, be dissolved in respectively in the ethylene glycol of 20ml, then two kinds of solution are mixedly configured into Silver Nitrate+pyrroles's mixing solutions.After stirring, this mixing solutions being placed microwave device, is 900W at power, and temperature is under 90 ℃ of conditions, and microwave exposure obtains the Ag/PPy complex sol after 60 minutes.
Embodiment 5
Such as above-mentioned step, take by weighing the Silver Nitrate of 680mg and the pyrrole monomer of 2.8ml, be dissolved in respectively in the ethylene glycol of 20ml, then two kinds of solution are mixedly configured into Silver Nitrate+pyrroles's mixing solutions.After stirring, this mixing solutions being placed microwave device, is 900W at power, and temperature is under 30 ℃ of conditions, and microwave exposure obtains the Ag/PPy complex sol after 60 minutes.
Claims (1)
1. a method for preparing fast silver/polypyrrole complex sol is characterized in that it comprises the steps:
(1) respectively Silver Nitrate and pyrrole monomer are dissolved in N, in N '-dimethyl formamide;
Or
Respectively Silver Nitrate and pyrrole monomer are dissolved in the ethylene glycol;
The concentration range of Silver Nitrate is at 0.01-2.0M, and the scope of pyrroles's concentration is at 0.01-2.0M;
(2) above-mentioned silver nitrate solution and pyrroles's solution are mixed;
(3) mixing solutions with step (2) carries out microwave exposure, until the silver of formation homogeneous/polypyrrole complex sol; The power range of microwave is at 200-900W, and temperature range is set in 30-150 ℃, and time range is set in 15-270 minute.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010607616 CN102140249B (en) | 2010-12-23 | 2010-12-23 | Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method |
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| CN 201010607616 CN102140249B (en) | 2010-12-23 | 2010-12-23 | Method for quickly preparing silver/polypyrrole composite sol by adopting microwave method |
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| CN102140249A CN102140249A (en) | 2011-08-03 |
| CN102140249B true CN102140249B (en) | 2013-04-03 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102614933B (en) * | 2012-03-20 | 2013-12-18 | 南京大学 | Noble metal silver deposition-polypyrrole sensitization hollow titanium dioxide nano photocatalyst and preparation method thereof |
| CN103319740B (en) * | 2013-07-18 | 2015-10-28 | 华东理工大学 | A kind of method of rapid-assembling Ag/PPy nano compound film |
| CN110105569A (en) * | 2019-04-23 | 2019-08-09 | 太仓萃励新能源科技有限公司 | A kind of silver loads the synthetic method of poly- 3,4- ethyl dioxypyrrole |
| CN113491509A (en) * | 2021-06-17 | 2021-10-12 | 西安理工大学 | Preparation method of flexible electronic sensor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040105980A1 (en) * | 2002-11-25 | 2004-06-03 | Sudarshan Tirumalai S. | Multifunctional particulate material, fluid, and composition |
| CN1631982A (en) * | 2004-11-17 | 2005-06-29 | 中国科学院上海光学精密机械研究所 | Process for preparing silver/polypyrrole composite nano materials |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040105980A1 (en) * | 2002-11-25 | 2004-06-03 | Sudarshan Tirumalai S. | Multifunctional particulate material, fluid, and composition |
| CN1631982A (en) * | 2004-11-17 | 2005-06-29 | 中国科学院上海光学精密机械研究所 | Process for preparing silver/polypyrrole composite nano materials |
Non-Patent Citations (1)
| Title |
|---|
| 任祥忠.反胶束体系中聚吡咯/氯化银纳米复合粒子的合成与表征.《材料科学与工程学报》.2008,第26卷(第2期),181-184. * |
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