CN102337030A - Polypyrrole compound nanosphere possessing electromagnetic function and its preparation method - Google Patents
Polypyrrole compound nanosphere possessing electromagnetic function and its preparation method Download PDFInfo
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- CN102337030A CN102337030A CN2011101546160A CN201110154616A CN102337030A CN 102337030 A CN102337030 A CN 102337030A CN 2011101546160 A CN2011101546160 A CN 2011101546160A CN 201110154616 A CN201110154616 A CN 201110154616A CN 102337030 A CN102337030 A CN 102337030A
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Abstract
The invention provides a polypyrrole/gamma-Fe2O3 compound nanosphere possessing an electromagnetic function, the appearance of the nanosphere is in a spherical shape, the particle size is 50-290nm, the conductivity ratio is 39.56S/cm-66.7S/cm, and the saturation magnetization intensity is 0.658 emu/g-5.85 emu/g. The preparation method comprises the following steps: adding pyrrole into an ammonia aqueous solution, adding a ferrous chloride aqueous solution, adding an iron chloride aqueous solution drop by drop under stirring, then adding a dopant aqueous solution, wherein the mol ratio of dopant to pyrrole is 0.001-3:1, controlling the reaction temperature at 0-5 DEG C, electromagnetically stirring and reacting to generate blackish green deposition; filtering the deposition, washing by successively using distilled water, ethanol and ether, vacuum drying. According to the invention, the addition of the dopant realizes high electrical property and synchronous increase of electrical property and magnetic property, wherein both of electrical property and magnetic property could reach the maximum value; the preparation method has simple operation which realizes a large-scale production.
Description
Technical field
The invention belongs to technical field of nano material, particularly relate to polypyrrole/γ-Fe that a kind of absorbing material has function solenoid
2O
3Mixture nanometer ball and preparation method thereof.
Background technology
The conductive polymer composite that has electricity, magnetic function concurrently has special light, electricity, magnetic properties, has the potential application prospect at aspects such as electromagnetic shielding, electrochromic device, microwave absorbing and nonlinear opticses.In recent years, the micro nano structure conducting polymer materials of function solenoidization becomes the research focus of conductive polymer micro-nano rice field of materials.Recently, successfully synthesize the conductive polymer composite of the micro of function solenoidization, such as polyaniline/Fe
3O
4Nanotube (Zhang, Z.M.; Wan, M.X.Synth.Met.2003,132,205.), polyaniline/γ-Fe
2O
3Nano wire (Zhang, Z.M.; Wan, M.X.; Wei, Y. Nanotechnology 2005,16,2827.).The preparation of the micro conductive polymer composite of these two kinds of function solenoidizations all needs two-step reaction to accomplish, i.e. the good magnetic nano-particle of prepared beforehand is like Fe
3O
4Or γ-Fe
2O
3Nano particle, the Fe that is preparing then
3O
4Or γ-Fe
2O
3Under the existence of nanoparticle, generate conductive polymers, generate the conductive polymers with micro of function solenoidization through the method for self-assembly.Yet this method is because the characteristics that magnetic nano-particle is reunited easily cause magnetic nano-particle in mixture, to disperse uneven problem easily.Recently, a kind of " chemical single stage method " (Zhang, Z.M.; Deng, J.Y.; Shen, J.Y.; Wan, M.X.; Chen, Z.J.Macromol.Rapid Commun.2007,28,585) proposition realized that successfully a step of conductive polymers and magnetic particle generates, overcome the defective that above-mentioned two-step approach exists.The preparation method of " chemical single stage method " is following:
1) 0.2mL aniline is joined in the ammonia soln (1M) of 10mL, ultra-sonic dispersion forms white homogeneous phase solution.
2) with a certain amount of FeCl
2.4H
2O (10mg, 20mg, 30mg, 40mg) joins in the zero(ppm) water of 5mL, pours in the aniline solution after the dissolving fully.In aniline solution, drip the FeCl of 10mL then
3.6H
2The aqueous solution (the FeCl of O
3.6H
2O is respectively 1.08g, 3.24g, 5.4g, 8.1g, 10.8g and 16.2g).The pH value of reaction soln is respectively 10 and 2 before and after dripping.
3) the induction stirring reaction finished after 12 hours under the normal temperature.
4) (30rpm 5min), respectively with zero(ppm) water, ethanol and three final vacuum oven dry of ether washing, promptly obtains the polyaniline/γ-Fe of function solenoidization with the product spinning
2O
3The mixture nano wire.
Yet, no matter above-mentioned two-step approach, still " chemical single stage method ", the specific conductivity of resulting function solenoid conductive polymer composite all lower (10
-2～100S/cm).Though, polypyrrole/FeooH mixture nanometer ball (Xiao, H.M. with high conductivity (16.1S/cm); Zhang, W. D.; Fu, S.Y. Composites Science and Technology 2010,70,909) existing report, but its saturation magnetization has only 0.11emu/g.Up to the present, the electric property and the magnetic performance that obtain the conductive polymer composite of function solenoidization all can not be taken into account.
Summary of the invention
The object of the present invention is to provide a kind of polypyrrole/γ Fe with function solenoid
2O
3Mixture nanometer ball and preparation method thereof, it is low that it can overcome the specific conductivity that exists in the prior art, the shortcoming that electricity and magnetic performance can not be taken into account.
A kind of polypyrrole/γ Fe with function solenoid
2O
3The mixture nanometer ball, the pattern that it is characterized in that this mixture nanometer ball is a spheroidal, and particle diameter is 50～290nm, and specific conductivity is 39.56S/cm～66.7S/cm, and saturation magnetization is 0.658emu/g～5.85emu/g.
Above-mentioned polypyrrole/γ-Fe with function solenoid
2O
3The preparation method of mixture nanometer ball is characterized in that at first adding the pyrroles, ultrasonic formation white emulsion to concentration in the ammonia soln of (0.8～1.2) mol/L; In this white emulsion, adding (8～10) mL concentration afterwards is the ferrous chloride aqueous solution of (0.0168～0.0699) mol/L; Obtain containing chlorination ferrous solution, under the ice-water bath condition, stir, dripped the ferric chloride in aqueous solution of concentration for (0.5～0.6) mol/L introversive above-mentioned containing in the chlorination ferrous solution at 15～30 minutes; Dropwise the back and add the doping agent aqueous solution; This doping agent and pyrroles's mol ratio is 0.001～3: 1, and after the interpolation of the doping agent aqueous solution finished, control reaction temperature was at 0～5 ℃; Induction stirring reaction 10～12 hours produces the blackish green deposition; Leach the blackish green deposition at last, with 8～10ml zero(ppm) water, ethanol and the oven dry of ether washing final vacuum, obtain polypyrrole/γ-Fe successively
2O
3The mixture nanometer ball.
The present invention overcome magnetic particle that traditional method exists disperse inhomogeneous, the defective that low and electricity of mixture specific conductivity and magnetic performance can not taken into account.Through the adding of doping agent, improved the electric property of product greatly, specific conductivity can improve 10
3～60 times; When realizing high electric property, realized the simultaneous growth of electricity and magnetic performance through the control of iron protochloride consumption, and reached peak simultaneously; The preparation method is simple to operate, can realize mass production.
Description of drawings
Fig. 1 is the polypyrrole/γ-Fe of instance 1 preparation of the present invention
2O
3The sem photograph of mixture nanometer ball.
Fig. 2 is the polypyrrole/γ-Fe of instance 2 preparations of the present invention
2O
3The sem photograph of mixture nanometer ball.
Fig. 3 is the polypyrrole/γ-Fe of instance 1,2 preparation of the present invention
2O
3The X-diffractogram of mixture nanometer ball.
Fig. 4 is polypyrrole/γ-Fe
2O
3Magnetic hysteresis loop (the FeCl of mixture nanometer ball
2Amount a:30mg; B:75mg; C:100mg; D:125mg).
Embodiment
Polypyrrole/γ-Fe with function solenoid of the present invention
2O
3The mixture nanometer ball, the pattern that it is characterized in that this mixture nanometer ball is a spheroidal, and particle diameter is 50～290nm, and specific conductivity is 39.56S/cm～66.7S/cm, and saturation magnetization is 0.658emu/g～5.85emu/g.During preparation, at first add the pyrroles, ultrasonic formation white emulsion in the ammonia soln of (0.8～1.2) mol/L to concentration; In this white emulsion, adding (8～10) mL concentration afterwards is the ferrous chloride aqueous solution of (0.0168～0.0699) mol/L; Obtain containing chlorination ferrous solution, under the ice-water bath condition, stir, dripped the ferric chloride in aqueous solution of concentration for (0.5～0.6) mol/L introversive above-mentioned containing in the chlorination ferrous solution at 15～30 minutes; Dropwise the back and add the doping agent aqueous solution; This doping agent and pyrroles's mol ratio is 0.001～3: 1, and after the interpolation of the doping agent aqueous solution finished, control reaction temperature was at 0～5 ℃; Induction stirring reaction 10～12 hours produces the blackish green deposition; Leach the blackish green deposition at last, with 8～10ml zero(ppm) water, ethanol and the oven dry of ether washing final vacuum, obtain polypyrrole/γ-Fe successively
2O
3The mixture nanometer ball.
1), concentration adds the pyrroles in being the ammonia soln of 1mol/L, ultrasonic formation white emulsion, and wherein, the volume ratio of pyrroles and ammonia soln is 0.0133;
2) in above-mentioned solution, adding concentration is 0.0168mol/L solution of ferrous chloride 10mL;
3) under the ice-water bath condition, under whipped state, in 20 minutes to above-mentioned steps 2) dropwise drip the ferric chloride Solution(38 that concentration is 0.599mol/L in the solution that obtains; Dropwise the back and add tosic acid solution; Wherein tosic acid and pyrroles's mol ratio is 2, and after the interpolation of tosic acid solution finished, temperature of reaction was controlled at 0～5 ℃; Induction stirring reaction 12 hours obtains the blackish green deposition;
4) with above-mentioned steps 3) sedimentation and filtration that obtains, successively with 10ml zero(ppm) water, ethanol and ether washing, the final vacuum oven dry obtains having the polypyrrole/γ-Fe of function solenoid
2O
3The mixture nanometer ball.
Fig. 1 has provided the prepared function solenoid polypyrrole/γ-Fe of instance of the present invention 1
2O
3The sem photograph of mixture nanometer ball.As can be seen from the figure, polypyrrole/γ-Fe
2O
3The particle diameter of mixture nanometer ball is even, the about 260nm of its mean diameter, and its specific conductivity is 42.86S/cm, saturation magnetization is 0.958emu/g.Through X-ray diffraction its structure is analyzed, as shown in Figure 3.Except ° locating to occur belonging to the characteristic peak of polypyrrole in 2 θ=25.1; Also in 2 θ=30.4 °, 35.7 °, 43.4 °, 53.8 °, 57.3 ° and 62.9 ° locate to occur a plurality of diffraction peaks; These diffraction peaks and the standard diffraction peak in full accord, can prove through preparation method of the present invention successfully to have prepared polypyrrole/γ-Fe
2O
3The mixture nanometer ball.
The test of absorbing property:
Adopt the arch bridge antenna method respectively 1～18GHz, 18～26.5GHz, three frequency range absorption of electromagnetic wave of 26.5～40GHz effect to be measured; Measuring result show material that present embodiment makes in the attenuation by absorption value at 7～16GHz, 26～40GHz place all above-5dB; Attenuation by absorption value at 8～12GHz, 28～35GHz place reaches-more than the 10dB; And the maximum absorption decay can reach-11dB in the ripple frequency scope of 1～18GHz, explains that the material that present embodiment makes all has assimilation effect preferably to hertzian wave in the wideband section.
Embodiment 2
1), concentration adds the pyrroles in being the ammonia soln of 0.96mol/L, ultrasonic formation white emulsion, and wherein, the volume ratio of pyrroles and ammonia soln is 0.0135;
2) in above-mentioned solution, adding concentration is 0.0559mol/L solution of ferrous chloride 10mL;
3) under the ice-water bath condition, under whipped state, in 20 minutes to above-mentioned steps 2) dropwise to drip concentration in the solution that obtains be the 0.585mol/L ferric chloride Solution(38; Dropwise the back and add tosic acid solution; Wherein tosic acid and pyrroles's mol ratio is 1.8, and after the interpolation of tosic acid solution finished, temperature of reaction was controlled at 0-5 ℃; Induction stirring reaction 11 hours obtains the blackish green deposition;
4) with above-mentioned steps 3) sedimentation and filtration that obtains, with zero(ppm) water, ethanol and three the final vacuums oven dry of ether washing of 9ml, obtain function solenoid polypyrrole/γ-Fe successively
2O
3The mixture nanometer ball.
Fig. 2 has provided the prepared polypyrrole/γ with function solenoid-Fe of instance of the present invention 2
2O
3The sem photograph of mixture nanometer ball, the about 80nm of its mean diameter, specific conductivity is 64.4S/cm, saturation magnetization is 4.85emu/g.Through X-ray diffraction its structure is analyzed, as shown in Figure 3.Except ° locating to occur belonging to polypyrrole/γ-Fe in 2 θ=25.1
2O
3Characteristic peak outside; Also in 2 θ=30.4 °, 35.7 °, 43.4 °, 53.8 °, 57.3 ° and 62.9 ° locate to occur a plurality of diffraction peaks; These diffraction peaks and the standard diffraction peak in full accord, can prove through preparation method of the present invention successfully to have prepared polypyrrole/γ-Fe
2O
3The mixture nanometer ball.
The test of absorbing property:
Adopt the arch bridge antenna method respectively 1～18GHz, 18～26.5GHz, three frequency range absorption of electromagnetic wave of 26.5～40GHz effect to be measured; Measuring result show material that present embodiment makes in the attenuation by absorption value at 6～18GHz, 24～40GHz place all above-5dB; Attenuation by absorption value at 10～15GHz, 27～36GHz place reaches-more than the 10dB; And the maximum absorption pad value can reach-12dB in the ripple frequency scope of 1～18GHz, explains that the material that present embodiment makes all has assimilation effect preferably to hertzian wave in the wideband section.
Embodiment 3
1), concentration adds the pyrroles in being the ammonia soln of 1mol/L, ultrasonic formation white emulsion, and wherein, the volume ratio of pyrroles and ammonia soln is 0.0133;
2) in above-mentioned solution, adding concentration is 0.0559mol/L solution of ferrous chloride 10mL;
3) under the ice-water bath condition, under whipped state, in 20 minutes to above-mentioned steps 2) dropwise drip the ferric chloride Solution(38 that concentration is 0.600mol/L in the solution that obtains; Dropwise the back and add phosphoric acid solution; Wherein phosphoric acid and pyrroles's mol ratio is 2.1, and after the phosphoric acid solution interpolation finished, temperature of reaction was controlled at 0-5 ℃; Induction stirring reaction 12 hours obtains the blackish green deposition;
4) with above-mentioned steps 3) sedimentation and filtration that obtains, with zero(ppm) water, ethanol and three the final vacuums oven dry of ether washing of 10ml, obtain function solenoid polypyrrole/γ-Fe successively
2O
3The mixture nanometer ball.ESEM and X-ray diffraction prove and have successfully prepared polypyrrole/γ-Fe
2O
3The mixture nanometer ball.
The test of absorbing property:
Adopt the arch bridge antenna method respectively 1～18GHz, 18～26.5GHz, three frequency range absorption of electromagnetic wave of 26.5～40GHz effect to be measured; Measuring result show material that present embodiment makes in the attenuation by absorption value at 8～17GHz, 25～38GHz place all above-5dB; Attenuation by absorption value at 9～13GHz, 29～37GHz place reaches-more than the 10dB; And the maximum absorption pad value can reach-9dB in the ripple frequency scope of 1～18GHz, explains that the material that present embodiment makes all has assimilation effect preferably to hertzian wave in the wideband section.
The volume ratio of pyrroles described in the present invention and ammonia soln is 0.0102～0.0145: 1.Described doping agent is tosic acid, phosphoric acid, acetate or trifluoroacetic acid.
Claims (4)
1. polypyrrole/γ-Fe with function solenoid
2O
3The mixture nanometer ball, the pattern that it is characterized in that this mixture nanometer ball is a spheroidal, and particle diameter is 50～290nm, and specific conductivity is 39.56S/cm～66.7S/cm, and saturation magnetization is 0.658emu/g～5.85emu/g.
2. the described polypyrrole/γ-Fe of claim 1 with function solenoid
2O
3The preparation method of mixture nanometer ball is characterized in that at first adding the pyrroles, ultrasonic formation white emulsion to concentration in the ammonia soln of (0.8～1.2) mol/L; In this white emulsion, adding (8～10) mL concentration afterwards is the ferrous chloride aqueous solution of (0.0168～0.0699) mol/L; Obtain containing chlorination ferrous solution, under the ice-water bath condition, stir, dripped the ferric chloride in aqueous solution of concentration for (0.5～0.6) mol/L introversive above-mentioned containing in the chlorination ferrous solution at 15～30 minutes; Dropwise the back and add the doping agent aqueous solution; This doping agent and pyrroles's mol ratio is 0.001～3: 1, and after the interpolation of the doping agent aqueous solution finished, control reaction temperature was at 0～5 ℃; Induction stirring reaction 10～12 hours produces the blackish green deposition; Leach the blackish green deposition at last, with 8～10ml zero(ppm) water, ethanol and the oven dry of ether washing final vacuum, obtain polypyrrole/γ-Fe successively
2O
3The mixture nanometer ball.
3. polypyrrole/the γ of function solenoid as claimed in claim 2-Fe
2O
3The preparation method of mixture nanometer ball, the volume ratio that it is characterized in that described pyrroles and ammonia soln is 0.0102～0.0145: 1.
4. polypyrrole/the γ of function solenoid as claimed in claim 2-Fe
2O
3The preparation method of mixture nanometer ball is characterized in that described doping agent is tosic acid, phosphoric acid, acetate or trifluoroacetic acid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102593454A (en) * | 2012-03-02 | 2012-07-18 | 合肥工业大学 | Preparation method for headspace iron trioxide and polypyrrole composite electrode material |
| CN104140674A (en) * | 2014-07-22 | 2014-11-12 | 中国海洋大学 | Polypyrrole-polyaniline/Fe3O4 compound and preparation method thereof |
| CN112533466A (en) * | 2020-12-02 | 2021-03-19 | 中国人民解放军火箭军工程大学 | MOFs derived porous carbon coated sheet carbonyl iron composite wave-absorbing material and preparation method thereof |
| CN112689452A (en) * | 2020-12-02 | 2021-04-20 | 中国人民解放军火箭军工程大学 | Co/C/carbonyl iron fiber composite wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN113527677A (en) * | 2021-07-20 | 2021-10-22 | 兰州理工大学 | P-toluenesulfonic acid doped polypyrrole/multi-walled carbon nanotube composite material |
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| CN1515629A (en) * | 2003-01-10 | 2004-07-28 | 中国科学院成都有机化学研究所 | Nano high-molecular microsphere with conductivity and magnetism and its preparation method |
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2011
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| CN1515629A (en) * | 2003-01-10 | 2004-07-28 | 中国科学院成都有机化学研究所 | Nano high-molecular microsphere with conductivity and magnetism and its preparation method |
Non-Patent Citations (4)
| Title |
|---|
| 《Macromolecules》 20110526 Zhiming Zhang et al "Highly Conductive Polypyrrole/gamma-Fe2O3 Nanospheres with Good Magnetic Properties Obtained through an Improved Chemical One-Step Method" 4610-4615 1-4 第44卷, * |
| 《高分子材料科学与工程》 20040731 邓建国等 "纳米Fe3O4-聚吡咯的相互作用" 149-152 1-4 第20卷, 第4期 * |
| ZHIMING ZHANG ET AL: ""Highly Conductive Polypyrrole/γ-Fe2O3 Nanospheres with Good Magnetic Properties Obtained through an Improved Chemical One-Step Method"", 《MACROMOLECULES》 * |
| 邓建国等: ""纳米Fe3O4-聚吡咯的相互作用"", 《高分子材料科学与工程》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102593454A (en) * | 2012-03-02 | 2012-07-18 | 合肥工业大学 | Preparation method for headspace iron trioxide and polypyrrole composite electrode material |
| CN102593454B (en) * | 2012-03-02 | 2014-12-03 | 合肥工业大学 | Preparation method for headspace iron trioxide and polypyrrole composite electrode material |
| CN104140674A (en) * | 2014-07-22 | 2014-11-12 | 中国海洋大学 | Polypyrrole-polyaniline/Fe3O4 compound and preparation method thereof |
| CN112533466A (en) * | 2020-12-02 | 2021-03-19 | 中国人民解放军火箭军工程大学 | MOFs derived porous carbon coated sheet carbonyl iron composite wave-absorbing material and preparation method thereof |
| CN112689452A (en) * | 2020-12-02 | 2021-04-20 | 中国人民解放军火箭军工程大学 | Co/C/carbonyl iron fiber composite wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN112689452B (en) * | 2020-12-02 | 2022-07-22 | 中国人民解放军火箭军工程大学 | Co/C/carbonyl iron fiber composite wave-absorbing material derived from metal organic framework and preparation method thereof |
| CN113527677A (en) * | 2021-07-20 | 2021-10-22 | 兰州理工大学 | P-toluenesulfonic acid doped polypyrrole/multi-walled carbon nanotube composite material |
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Application publication date: 20120201 |