CN102219996A - Electric conduction composite material with poly-2, 3-dimethylaniline/polyaniline core shell structure and preparation method of electric conduction composite material - Google Patents
Electric conduction composite material with poly-2, 3-dimethylaniline/polyaniline core shell structure and preparation method of electric conduction composite material Download PDFInfo
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- CN102219996A CN102219996A CN 201110147887 CN201110147887A CN102219996A CN 102219996 A CN102219996 A CN 102219996A CN 201110147887 CN201110147887 CN 201110147887 CN 201110147887 A CN201110147887 A CN 201110147887A CN 102219996 A CN102219996 A CN 102219996A
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Abstract
The invention relates to an electric conduction composite material with a poly-2, 3-dimethylaniline/polyaniline core shell structure, and a preparation method of the electric conduction composite material. In the composite material, the poly-2, 3-dimethylaniline is used as a core, and the polyaniline is used as a shell. The preparation method comprises the following steps: the poly-2,3-dimethylaniline is firstly prepared by a solution polymerization process, and then is filtered, washed, dried and ground to obtain the powdered poly-2,3-dimethylaniline; and the powered poly-2, 3-dimethylaniline is used as the core, polymerization is carried out to the surface of the powered poly-2, 3-dimethylaniline by the solution polymerization process or emulsion polymerization process, and then a product is filtered, washed, dried and ground to obtain the electric conduction composite material with the poly-2, 3-dimethylaniline/polyaniline core shell structure. In the electric conduction composite material with the poly-2, 3-dimethylaniline/polyaniline core shell structure, the electric conductivity of the poly-2, 3-dimethylaniline/polyaniline is remarkably improved, thereby being beneficial to being applied to the field of sensors, electric conductive devices, electrode active materials and the like.
Description
Technical field
The invention belongs to field of compound material, poly-23 dimethyl aniline/polyaniline composite material of particularly a kind of nucleocapsid structure and preparation method thereof.
Background technology
Electrically conductive polyaniline has unique chemical, electricity, optics and thermal property because of it, and reversible doping/dedoping process, has a wide range of applications at aspects such as smart window, electrochromic device, stealth material, electrode materials, protective systems.
Poly-2, the 3-xylidine is a kind of as outbalance in the electrically conductive polyaniline ring substitutive derivative, at present, about poly-2, the research of 3-xylidine mainly concentrates on the transmitter aspect, but because the existence of methyl, very easily oxidized in preparation process, therefore be difficult to make poly-23 dimethyl aniline with electroconductibility, as: people such as Anjali have prepared poly-2 by solution polymerization process, the 3-xylidine, and studied its application in the Fatty Alcohol(C12-C14 and C12-C18) transmitter, but the poly-23 dimethyl aniline resistance of preparing only has 10
6Ω (Polyaniline and its substituted derivatives as sensor for aliphatic alcohols[J] .Sensors and Actuators B, 2000,67:173-177); People such as Milind have also prepared poly-2 in solution system, the 3-xylidine, (Poly (2 to find its relative humidity to air to have the sensing effect, 3-dimethylaniline) as a competent material for humidity sensor[J]. Journal of Applied Polymer Science, 2001,81:1382-1387), but the poly-23 dimethyl aniline resistance of preparing all 10
7This scope of Ω has entered the category of isolator.Because the poly-23 dimethyl aniline specific conductivity that goes out of prior art for preparing is too low, greatly limited its further research at aspects such as other transmitter, conductive element device and electrode active materials.
Summary of the invention
Purpose of the present invention is exactly in order to overcome above-mentioned the deficiencies in the prior art, and a kind of poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure with high conductance and preparation method thereof is provided.
A kind of nucleocapsid structure involved in the present invention gathers 23 dimethyl aniline/polyaniline composite material, be a kind of be nuclear with poly-23 dimethyl aniline, polyaniline is the core-shell structural conductive matrix material of shell.
This matrix material is to make poly-23 dimethyl aniline with solution polymerization process earlier, by obtaining its powder after suction filtration, washing, oven dry, the grinding; Be nuclear with pulverous poly-23 dimethyl aniline again, carry out polymerization on its surface, form the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure by solution polymerization process or emulsion polymerization.
The preparation concrete steps of this matrix material are as follows:
1) He preparation:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L oxidizing agent solution (oxygenant be in ammonium persulphate or the Sodium Persulfate a kind of) then, in 30 ℃ of following stirring reaction 12h; Suction filtration, and colourless with the distilled water wash filter cake to filtrate; Filter cake takes out and grinds behind dry 12h under 60 ℃, obtains Powdered poly-23 dimethyl aniline, as nuclear;
2) preparation of shell:
A. the poly-23 dimethyl aniline end that step 1) is made moves in the reactor B, adds the hydrochloric acid soln of 1.2mol/L, stirs it is uniformly dispersed; In reactor B, add aniline, stir 30min and make its mixing; Wherein, the volume ratio of hydrochloric acid soln and aniline is 50:1, and the mol ratio of 23 dimethyl aniline is 1 ~ 4:1 in aniline and the step 1);
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, reacts 5 ~ 8h down at 0 ~ 30 ℃; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1:1, and oxygenant is a kind of in ammonium persulphate or the Sodium Persulfate;
C. suction filtration is colourless to filtrate with the hydrochloric acid soln washing leaching cake of 0.1mol/L; Filter cake after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of down dry 8 ~ 12h.
Among the above-mentioned preparation method, the preparation of shell also can obtain as follows:
A: the poly-23 dimethyl aniline powder that step 1) is made moves in the reactor B; After emulsifying agent being dissolved in the hydrochloric acid soln of 1.2mol/L, join in the reactor B, add aniline subsequently, stir emulsification 30min down; Wherein, the mol ratio of emulsifying agent and aniline is 0.6 ~ 1:1, and emulsifying agent is a Sodium dodecylbenzene sulfonate, and the volume ratio of hydrochloric acid soln and aniline is 50:1, and the mol ratio of 23 dimethyl aniline is 1 ~ 4:1 in aniline and the step 1);
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, reacts 5 ~ 8h down at 0 ~ 30 ℃; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1:1, and oxygenant is a kind of in ammonium persulphate or the Sodium Persulfate;
C: add the 30ml emulsion splitter, breakdown of emulsion 30min; Wherein, emulsion splitter is a kind of in acetone, dehydrated alcohol or the saturated NaCl solution; Suction filtration, colourless with the hydrochloric acid soln washing leaching cake of 0.1mol/L to filtrate; Filter cake after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of down dry 8 ~ 12h.
Nucleocapsid structure provided by the present invention gathers 23 dimethyl aniline/polyaniline composite material, has significantly improved the specific conductivity of poly-2.3-xylidine, is beneficial to its further applied research in fields such as transmitter, conductive element device, electrode active materials.
Description of drawings
Fig. 1 is the structural representation of matrix material of the present invention
Wherein 1 is the polyaniline shell, and 2 are poly-23 dimethyl aniline nuclear.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described.
The structure of the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure provided by the present invention as shown in Figure 1, wherein 1 be the polyaniline shell, 2 examine for poly-23 dimethyl aniline.Embodiment 1 to embodiment 5 is the concrete preparation example of matrix material of the present invention.
Experimental example 1:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L ammonium persulfate solution, 30 ℃ of following stirring reaction 12h; Suction filtration, colourless with the distilled water wash filter cake to filtrate; Filter cake is dry 12h under 60 ℃, pulverizes after the taking-up, obtains Powdered poly-23 dimethyl aniline.This powder is moved in the reactor B, add 150ml 1.2mol/L hydrochloric acid soln, stirring is uniformly dispersed it; Add 3.29 * 10
-2Mol aniline (3ml) stirs 30min; In system, slowly splash into 22.7ml 0.58mol/L ammonium persulfate solution, 30 ℃ of following stirring reaction 5h; Suction filtration, colourless with 0.1mol/L hydrochloric acid soln washing leaching cake to filtrate.Filter cake is dry 12h under 60 ℃, after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure, and recording specific conductivity with four probe method is 2.74 S/cm.
Experimental example 2:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L Sodium Persulfate solution, 30 ℃ of following stirring reaction 12h; Suction filtration, colourless with the distilled water wash filter cake to filtrate; Filter cake is dry 12h under 60 ℃, pulverizes after the taking-up, obtains Powdered poly-23 dimethyl aniline.This powder is moved in the reactor B, add 37.5ml 1.2mol/L hydrochloric acid soln, stirring is uniformly dispersed it; Add 8.15 * 10
-3Mol aniline (0.75ml) stirs 30min; In system, slowly splash into 14.1ml 0.58mol/L Sodium Persulfate solution, 0 ℃ of following stirring reaction 8h; Suction filtration, colourless with 0.1mol/L hydrochloric acid soln washing leaching cake to filtrate.Filter cake is dry 8h under 60 ℃, after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure, and recording specific conductivity with four probe method is 1.38S/cm.
Experimental example 3:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L Sodium Persulfate solution, 30 ℃ of following stirring reaction 12h, suction filtration, colourless with the distilled water wash filter cake to filtrate; Filter cake is dry 12h under 60 ℃, pulverizes after the taking-up, obtains Powdered poly-23 dimethyl aniline.This powder is moved in the reactor B, add 150ml 1.2mol/L hydrochloric acid soln, stirring is uniformly dispersed it; Add 1.97 * 10 successively then
-2Mol Sodium dodecylbenzene sulfonate and 3.29 * 10
-2Mol aniline (3ml), emulsification 30min; In system, slowly splash into 22.7ml 0.58mol/L Sodium Persulfate solution, 30 ℃ of following stirring reaction 8h; After reaction finishes, in reactor B, add the saturated NaCl solution of 30ml, breakdown of emulsion 30min; Suction filtration, colourless with 0.1mol/L hydrochloric acid soln washing leaching cake to filtrate; Filter cake is dry 12h under 60 ℃, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure, and recording specific conductivity with four probe method is 1.48 S/cm.
Experimental example 4:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L Sodium Persulfate solution, 30 ℃ of following stirring reaction 12h, suction filtration, colourless with the distilled water wash filter cake to filtrate; Filter cake is dry 12h under 60 ℃, pulverizes after the taking-up, obtains Powdered poly-23 dimethyl aniline.This powder is moved in the reactor B, add 115ml 1.2mol/L hydrochloric acid soln, stirring is uniformly dispersed it; Add 1.96 * 10 successively then
-2Mol Sodium dodecylbenzene sulfonate and 2.45 * 10
-2Mol aniline (2.3ml), emulsification 30min; In system, slowly splash into 33.8ml 0.58mol/L Sodium Persulfate solution, 0 ℃ of following stirring reaction 7h; After reaction finishes, in reactor B, add 30ml dehydrated alcohol, breakdown of emulsion 30min; Suction filtration, colourless with 0.1mol/L hydrochloric acid soln washing leaching cake to filtrate; Filter cake is dry 8h under 60 ℃, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure, and recording specific conductivity with four probe method is 0.65S/cm.
Experimental example 5:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L ammonium persulfate solution, 30 ℃ of following stirring reaction 12h, suction filtration, colourless with the distilled water wash filter cake to filtrate; Filter cake is dry 12h under 60 ℃, pulverizes after the taking-up, obtains Powdered poly-23 dimethyl aniline.This powder is moved in the reactor B, add 37.5ml 1.2mol/L hydrochloric acid soln, stirring is uniformly dispersed it; Add 8.15 * 10 successively then
-3Mol Witco 1298 Soft Acid ammonium and 8.15 * 10
-3Mol aniline (0.75ml), emulsification 30min; In system, slowly splash into 5.6ml 0.58mol/L Sodium Persulfate solution, 20 ℃ of following stirring reaction 5h; After reaction finishes, in reactor B, add 30ml acetone, breakdown of emulsion 30min; Suction filtration, colourless with 0.1mol/L hydrochloric acid soln washing leaching cake to filtrate; Filter cake is dry 10h under 60 ℃, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure, and recording specific conductivity with four probe method is 0.17S/cm.
As can be seen from the above embodiments, a kind of nucleocapsid structure provided by the present invention poly-2,3-xylidine/polyaniline composite material has significantly improved the specific conductivity of poly-2.3-xylidine, is beneficial to its application in fields such as transmitter, conductive element device, electrode active materials.
Claims (3)
1. a nucleocapsid structure gathers 23 dimethyl aniline/polyaniline composite material, and it is characterized in that: this matrix material is a nucleocapsid structure, and the material of nuclear is poly-23 dimethyl aniline, and the material of shell is a polyaniline.
2. the method for the poly-23 dimethyl aniline/polyaniline composite material of the nucleocapsid structure for preparing claim 1:
1) He preparation:
In reactor A, add 25ml distilled water 8.2 * 10 successively
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Splash into 12.5ml 1.2mol/L oxidizing agent solution (oxygenant be in ammonium persulphate or the Sodium Persulfate a kind of) then, in 30 ℃ of following stirring reaction 12h; Suction filtration, and colourless with the distilled water wash filter cake to filtrate; Filter cake takes out and grinds behind dry 12h under 60 ℃, obtains Powdered poly-23 dimethyl aniline, as nuclear;
2) preparation of shell:
A. the poly-23 dimethyl aniline end that step 1) is made moves in the reactor B, adds the hydrochloric acid soln of 1.2mol/L, stirs it is uniformly dispersed; In reactor B, add aniline, stir 30min and make its mixing; Wherein, the volume ratio of hydrochloric acid soln and aniline is 50:1, and the mol ratio of 23 dimethyl aniline is 1 ~ 4:1 in aniline and the step 1);
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, reacts 5 ~ 8h down at 0 ~ 30 ℃; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1:1, and oxygenant is a kind of in ammonium persulphate or the Sodium Persulfate;
C. suction filtration is colourless to filtrate with the hydrochloric acid soln washing leaching cake of 0.1mol/L; Filter cake after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of down dry 8 ~ 12h.
3. a kind of nucleocapsid structure as claimed in claim 2 gathers 23 dimethyl aniline/polyaniline composite material preparation method, it is characterized in that: step 2) preparation process of shell is as follows,
A. the poly-23 dimethyl aniline powder that step 1) is made moves in the reactor B; After emulsifying agent being dissolved in the hydrochloric acid soln of 1.2mol/L, join in the reactor B, add aniline subsequently, stir emulsification 30min down; Wherein, the mol ratio of emulsifying agent and aniline is 0.6 ~ 1:1, and emulsifying agent is a Sodium dodecylbenzene sulfonate, and the volume ratio of hydrochloric acid soln and aniline is 50:1, and the mol ratio of 23 dimethyl aniline is 1 ~ 4:1 in aniline and the step 1);
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, reacts 5 ~ 8h down at 0 ~ 30 ℃; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1:1, and oxygenant is a kind of in ammonium persulphate or the Sodium Persulfate;
C. add the 30ml emulsion splitter, breakdown of emulsion 30min; Wherein, emulsion splitter is a kind of in acetone, dehydrated alcohol or the saturated NaCl solution; Suction filtration, colourless with the hydrochloric acid soln washing leaching cake of 0.1mol/L to filtrate; Filter cake after taking-up is ground, promptly gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of down dry 8 ~ 12h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862398A (en) * | 2016-06-23 | 2016-08-17 | 四川大学 | Polymer fiber-based conductive composite material and preparation method thereof |
| CN107603465A (en) * | 2017-09-20 | 2018-01-19 | 扬州大学 | The preparation method of the modified poly- high antiseptic property material of 2,3 dimethylaniline |
| CN115411259A (en) * | 2022-10-13 | 2022-11-29 | 广东比沃新能源有限公司 | High-pressure low-temperature lithium iron phosphate material and lithium battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US6059999A (en) * | 1997-03-03 | 2000-05-09 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Conducting compositions of matter |
| CN101225127A (en) * | 2007-12-13 | 2008-07-23 | 厦门大学 | Method for preparing size monodispersed core-shell structural conductive polymer microspheres |
| CN101892530A (en) * | 2010-07-15 | 2010-11-24 | 东华大学 | Preparation of polyaniline/polypyrrole composite nano fiber electrode materials with core-shell structure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6059999A (en) * | 1997-03-03 | 2000-05-09 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Conducting compositions of matter |
| CN101225127A (en) * | 2007-12-13 | 2008-07-23 | 厦门大学 | Method for preparing size monodispersed core-shell structural conductive polymer microspheres |
| CN101892530A (en) * | 2010-07-15 | 2010-11-24 | 东华大学 | Preparation of polyaniline/polypyrrole composite nano fiber electrode materials with core-shell structure |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862398A (en) * | 2016-06-23 | 2016-08-17 | 四川大学 | Polymer fiber-based conductive composite material and preparation method thereof |
| CN107603465A (en) * | 2017-09-20 | 2018-01-19 | 扬州大学 | The preparation method of the modified poly- high antiseptic property material of 2,3 dimethylaniline |
| CN115411259A (en) * | 2022-10-13 | 2022-11-29 | 广东比沃新能源有限公司 | High-pressure low-temperature lithium iron phosphate material and lithium battery |
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Address after: 400044 Shapingba street, Shapingba District, Chongqing, No. 174 Patentee after: Chongqing University Patentee after: Chemical Limited by Share Ltd Address before: 400044 Shapingba street, Shapingba District, Chongqing, No. 174 Patentee before: Chongqing University Patentee before: BSM Chemical Co., Ltd. |