CN102391510A - Production method for synthesizing polypyrrole hollow spheres by self template process - Google Patents
Production method for synthesizing polypyrrole hollow spheres by self template process Download PDFInfo
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- CN102391510A CN102391510A CN2011101955798A CN201110195579A CN102391510A CN 102391510 A CN102391510 A CN 102391510A CN 2011101955798 A CN2011101955798 A CN 2011101955798A CN 201110195579 A CN201110195579 A CN 201110195579A CN 102391510 A CN102391510 A CN 102391510A
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- pyrroles
- polypyrrole hollow
- hollow ball
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Abstract
The invention relates to a production method for synthesizing polypyrrole hollow spheres by a self template process, belonging to the technical field of conducting polymer materials. The method comprises the following steps: dissolving mercuric chloride in deionized water, adding a pyrrole liquid, and uniformly stirring with a magnetic stirrer to obtain a pyrrole mercury salt solid sphere complex of which the diameter is 140-270nm; and adding the pyrrole mercury salt solid sphere complex into an ammonium persulfate solution, and stirring to react to obtain the polypyrrole hollow spheres of which the diameter is 250-450nm. The invention is simple to operate, and can easily obtain the product; and the invention saves the consumption of the surfactant, and does not need to modify the self template in the polypyrrole hollow sphere synthesis process or remove the template after the reaction finishes.
Description
Technical field
The invention belongs to the conducting polymer materials technical field.
Background technology
Polypyrrole as a kind of by the conductive polymers of broad research; Because characteristics such as its unique Doping Mechanism, higher environmental stability, good oxidation-reduction quality and raw material are easy to get; At battery material, anti-corrosion of metal, aspects such as electromagnetic shielding, molecular device, transmitter exist the potential application prospect, and the polypyrrole hollow ball can be used as the vehicle of pollutent; The controlled release of medicine, the carrier of catalyzer etc.As everyone knows, the pattern of material has decisive influence to its performance, and preparation polypyrrole and employing " firmly " template prepares the method that polypyrrole is common synthetic polypyrrole hollow ball specific morphology in the surfactant system.
Summary of the invention
The object of the invention is to propose a kind of working method of the convenient synthetic polypyrrole hollow ball of producing of self template.
Technical scheme of the present invention is: earlier mercury chloride is dissolved in the deionized water, adds pyrroles's liquid then, even with magnetic stirrer, obtaining diameter is the solid spherical complex compound of pyrroles's mercury salt of 140～270 nanometers; Then the solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, obtaining diameter is the polypyrrole hollow ball of 250～450 nanometers.
In the solid spherical complex compound of said pyrroles's mercury salt in pyrroles and the ammonium persulfate solution mol ratio of ammonium persulphate be 1 ︰ 1.
The present invention adopts pyrroles's mercury salt complex compound can prepare and control the polypyrrole hollow ball effectively as self template, for the compound method of polypyrrole hollow ball has been widened approach.
The present invention is easy and simple to handle, and product is easy to get, HgCl in the raw material
2Through reacting the back with Hg
2Cl
2Form doping polypyrrole in, environment is not caused secondary pollution; Hg in addition
2Cl
2The wide spectrum bacterium there is certain bacterinertness; Simultaneously also just because of Hg
2Cl
2Doping, make polypyrrole have hydrophobicity.What be worth proposition is that this compound method has been omitted the use of tensio-active agent on the one hand, in addition on the one hand, neither need modify self template in the synthetic polypyrrole hollow ball process, also need after reaction finishes, not remove template.
Tensio-active agent that has no in the reaction soln of the present invention or SiO
2Deng " firmly " template, need not the soft or hard template effect in any external world; Pyrroles and mercury chloride directly form spherical big or small homogeneous white complex compound emulsion in the aqueous solution, need not ultra-sonic dispersion, directly under agitation condition, add initiator ammonium persulfate solution and continue reaction, obtain the Hg that mixes
2Cl
2The polypyrrole hollow ball, the polypyrrole hollow ball pattern homogeneous good dispersion degree of processing, polypyrrole hollow ball controllable size.
The mass ratio that feeds intake of mercury chloride according to the invention and pyrroles's liquid is 1～4 ︰ 1～2, can be through the size of control pyrroles and mercury chloride amount of substance ratio regulation and control complex compound.
As, when the mass ratio that feeds intake of said mercury chloride and pyrroles's liquid is 1 ︰ 2, obtain the solid spherical complex compound of pyrroles's mercury salt; Then the solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, the outside diameter of available polypyrrole hollow ball are 400 nm, about 200 nm of interior diameter, thick 100 nm of shell.
As, when the mass ratio that feeds intake of said mercury chloride and pyrroles's liquid is 1 ︰ 1, obtain the solid spherical complex compound of pyrroles's mercury salt; The solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, about 250 nm of the outside diameter of available polypyrrole hollow ball, about 160 nm of interior diameter, thickness 45 nm of shell.
As, when the mass ratio that feeds intake of said mercury chloride and pyrroles's liquid is 2 ︰ 1, obtain the solid spherical complex compound of pyrroles's mercury salt; The solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, outside diameter 450 nm of polypyrrole hollow ball, about 300 nm of interior diameter, about 75 nm of thickness of the shell.
For another example, when the mass ratio that feeds intake of said mercury chloride and pyrroles's liquid is 4 ︰ 1, the solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, the outside diameter 380nm of polypyrrole hollow ball, about 300 nm of interior diameter, about 40 nm of thickness of the shell.
Description of drawings
Among Fig. 1, A is the ESEM of pyrroles's mercury salt complex compound; B is a transmission electron microscope picture.
Among Fig. 2, A is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the sem photograph of the polypyrrole hollow ball that obtained of 1 ︰ 2; B is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the transmission electron microscope picture of the polypyrrole hollow ball that obtained of 1 ︰ 2.
Among Fig. 3, A is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the sem photograph of the polypyrrole hollow ball that obtained of 1 ︰ 1; B is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the transmission electron microscope picture of the polypyrrole hollow ball that obtained of 1 ︰ 1.
Among Fig. 4, A is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the sem photograph of the polypyrrole hollow ball that obtained of 2 ︰ 1; B is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the transmission electron microscope picture of the polypyrrole hollow ball that obtained of 2 ︰ 1.
Among Fig. 5, A is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the sem photograph of the polypyrrole hollow ball that obtained of 4 ︰ 1; B is that the mass ratio that feeds intake of mercury chloride and pyrroles's liquid is the transmission electron microscope picture of the polypyrrole hollow ball that obtained of 4 ︰ 1.
Embodiment
One, embodiment 1:
1, preparation pyrroles mercury salt complex compound
Take by weighing 0.080 g HgCl
2Be dissolved in the 50 ml deionized waters, under the agitation condition, add 0.020 g (26.4 μ l) pyrroles's liquid, solution promptly becomes the milk sap of white.Continue to stir, react and take out seldom a part of white milk sap after 1 hour, centrifugal (3000 r/min) separates, deionized water wash three times, and ethanol washes twice, then product is placed 60 ° of C vacuum drying ovens 24 hours.The white product that obtains is done ESEM and transmission electron microscope, sees shown in Figure 1.
2, preparation polypyrrole hollow ball
Direct adding is the APS solution of 1:1 with pyrroles's mol ratio in the solid sphere pyrroles mercury salt complex solution of employing method for preparing, and solution is grey black then by white fast transition.Continued stirring reaction 8 hours.The product spinning is washed three times, and ethanol is washed twice.The black solid that obtains is placed 60 ℃ of vacuum-dryings 12 hours.
3, analyze
Utilized sem and transmission electron microscope that the product pattern is observed in the pyrroles's mercury salt complex compound solid sphere for preparing.
Utilize x-ray photoelectron spectroscopy and nucleus magnetic resonance H spectrum to the complex molecules structural analysis.Measure polypyrrole hollow ball molecular structure through Fourier infrared spectrograph and nucleus magnetic resonance H spectrum, and x-ray diffractometer is measured pyrroles's mercury salt complex compound and polypyrrole hollow ball crystallinity.Measure the surperficial contact angle of its water and polypyrrole hollow ball all greater than 130o through the video contact angle measurement, electroconductibility is good.
The outside diameter of the polypyrrole hollow ball that 4, obtains is 380 nm, about 300 nm of interior diameter, thick 40 nm of shell.As shown in Figure 5.
Two, embodiment 2:
Other method just when preparation pyrroles mercury salt complex compound, drops into 0.080g HgCl with embodiment 1
2, 0.160g pyrroles's liquid.
The outside diameter of the polypyrrole hollow ball that obtains is 400 nm, about 200 nm of interior diameter, and thick 100 nm of shell, as shown in Figure 2.
Three, embodiment 3:
Other method just when preparation pyrroles mercury salt complex compound, drops into 0.080g HgCl with embodiment 1
2, 0.080g pyrroles's liquid.
About 250 nm of the outside diameter of the polypyrrole hollow ball that obtains, about 160 nm of interior diameter, thickness 45 nm of shell, as shown in Figure 3.
Four, embodiment 4:
Other method just when preparation pyrroles mercury salt complex compound, drops into 0.080g HgCl with embodiment 1
2, 0.040g pyrroles's liquid.
Outside diameter 450 nm of the polypyrrole hollow ball that obtains, about 300 nm of interior diameter, about 75 nm of thickness of the shell, as shown in Figure 4.
Claims (2)
1. the working method of the synthetic polypyrrole hollow ball of self template; It is characterized in that earlier mercury chloride being dissolved in the deionized water; Add pyrroles's liquid then, even with magnetic stirrer, obtaining diameter is the solid spherical complex compound of pyrroles's mercury salt of 140～270 nanometers; Then the solid spherical complex compound of pyrroles's mercury salt is added ammonium persulfate solution, stirring reaction, obtaining diameter is the polypyrrole hollow ball of 250～450 nanometers.
2. according to the working method of the synthetic polypyrrole hollow ball of said self template of claim 1, the mass ratio that feeds intake that it is characterized in that said mercury chloride and pyrroles's liquid is 1～4 ︰ 1～2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117074A (en) * | 2013-04-27 | 2014-10-29 | 北京大学 | Therapy diagnosis preparation based on polypyrrole compound and preparation method of preparation |
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| US6929764B2 (en) * | 2000-11-17 | 2005-08-16 | William Marsh Rice University | Polymers having ordered, monodisperse pores and their corresponding ordered, monodisperse colloids |
| CN101165092A (en) * | 2006-10-16 | 2008-04-23 | 中南大学 | Method for preparing electric polypyrrole nano hollow sphere |
| CN101177253A (en) * | 2006-11-07 | 2008-05-14 | 中国科学院理化技术研究所 | Method for preparing hollow micrometre carbon ball with structured size |
-
2011
- 2011-07-13 CN CN 201110195579 patent/CN102391510B/en not_active Expired - Fee Related
Patent Citations (3)
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|---|---|---|---|---|
| US6929764B2 (en) * | 2000-11-17 | 2005-08-16 | William Marsh Rice University | Polymers having ordered, monodisperse pores and their corresponding ordered, monodisperse colloids |
| CN101165092A (en) * | 2006-10-16 | 2008-04-23 | 中南大学 | Method for preparing electric polypyrrole nano hollow sphere |
| CN101177253A (en) * | 2006-11-07 | 2008-05-14 | 中国科学院理化技术研究所 | Method for preparing hollow micrometre carbon ball with structured size |
Non-Patent Citations (6)
| Title |
|---|
| 《Synthetic Metals》 20030905 Lingyun Hao,et.al Fabrication of silica core-conductive polymer polypyrrole shell composite particles and polypyrrole capsule on monodispersed silica templates 391-396页 1~2 第139卷, 第2期 * |
| DAMING CHENG,ET.AL: "Fabrication of polymeric hollow nanospheres, hollow nanocubes and hollow plates", 《NANOTECHNOLOGY》 * |
| JUN ZHANG,ET.AL: "Polypyrrole-Coated SnO2 Hollow Spheres and Their Application for Ammonia Sensor", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| LINGYUN HAO,ET.AL: "Fabrication of silica core–conductive polymer polypyrrole shell composite particles and polypyrrole capsule on monodispersed silica templates", 《SYNTHETIC METALS》 * |
| 吕秋丰: "聚吡咯纳米粒子及聚吡咯－木质素磺酸空心球的制备", 《高分子材料科学与工程》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104117074A (en) * | 2013-04-27 | 2014-10-29 | 北京大学 | Therapy diagnosis preparation based on polypyrrole compound and preparation method of preparation |
| CN104117074B (en) * | 2013-04-27 | 2016-09-28 | 北京大学 | A kind for the treatment of diagnostic preparation based on polypyrrole complex and preparation method thereof |
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