CN102219996B - 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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- CN102219996B CN102219996B CN 201110147887 CN201110147887A CN102219996B CN 102219996 B CN102219996 B CN 102219996B CN 201110147887 CN201110147887 CN 201110147887 CN 201110147887 A CN201110147887 A CN 201110147887A CN 102219996 B CN102219996 B CN 102219996B
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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, particularly poly-23 dimethyl aniline/polyaniline composite material of a kind of nucleocapsid structure and preparation method thereof.
Background technology
Electrically conductive polyaniline has unique chemistry, 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 sensor aspect, but because the existence of methyl, very easily oxidized in preparation process, therefore be difficult to make the poly-23 dimethyl aniline with electroconductibility, as: the 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) sensor, 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); The 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 prepared of prior art is too low, greatly limited it in the further research of the aspects such as other sensor, conductive element device and electrode active material.
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, is a kind of take poly-23 dimethyl aniline as nuclear, and 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 first, by obtaining its powder after suction filtration, washing, oven dry, the grinding; Take pulverous poly-23 dimethyl aniline as nuclear, carry out polymerization by solution polymerization process or emulsion polymerization on its surface again, form the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure.
These composite manufacture concrete steps are as follows:
1) preparation of nuclear:
In reactor A, add successively 25ml distilled water 8.2 * 10
-3Mol concentrated hydrochloric acid (commercially available content 36 ~ 38%) and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Then splash into 12.5ml 1.2mol/L oxidizing agent solution (oxygenant be in ammonium persulphate or the Sodium Persulfate a kind of), in 30 ℃ of lower stirring reaction 12h; Suction filtration, and colourless to filtrate with the distilled water wash filter cake; Filter cake takes out and grinds behind 60 ℃ of lower dry 12h, obtains Powdered poly-23 dimethyl aniline, as nuclear;
2) preparation of shell:
A. with step 1) the poly-23 dimethyl aniline end that makes moves in the reactor B, adds the hydrochloric acid soln of 1.2mol/L, stir 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, aniline and step 1) in the mol ratio of 23 dimethyl aniline be 1 ~ 4
:1;
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, at 0 ~ 30 ℃ of lower reaction 5 ~ 8h; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1
:1, 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, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8 ~ 12h.
Among the above-mentioned preparation method, the preparation of shell also can obtain as follows:
A: with step 1) the poly-23 dimethyl aniline powder that makes 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 subsequently aniline, stir lower emulsification 30min; Wherein, the mol ratio of emulsifying agent and aniline is 0.6 ~ 1:1, and emulsifying agent is Sodium dodecylbenzene sulfonate, and the volume ratio of hydrochloric acid soln and aniline is 50
:1, aniline and step 1) in the mol ratio of 23 dimethyl aniline be 1 ~ 4
:1;
B. the oxidizing agent solution with 0.58mol/L slowly splashes in the reactor B, at 0 ~ 30 ℃ of lower reaction 5 ~ 8h; Wherein, the mol ratio of oxygenant and aniline is 0.4 ~ 1
:1, 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 to filtrate with the hydrochloric acid soln washing leaching cake of 0.1mol/L; Filter cake after taking-up is ground, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower 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 it in the further applied research in the fields such as sensor, conductive element device, electrode active material.
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 successively 25ml distilled water 8.2 * 10
-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 lower stirring reaction 12h; Suction filtration, colourless to filtrate with the distilled water wash filter cake; Filter cake is pulverized after the taking-up at 60 ℃ of lower dry 12h, 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 lower stirring reaction 5h; Suction filtration, colourless to filtrate with 0.1mol/L hydrochloric acid soln washing leaching cake.Filter cake after taking-up is ground, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 12h, and recording specific conductivity with four probe method is 2.74 S/cm.
Experimental example 2:
In reactor A, add successively 25ml distilled water 8.2 * 10
-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 lower stirring reaction 12h; Suction filtration, colourless to filtrate with the distilled water wash filter cake; Filter cake is pulverized after the taking-up at 60 ℃ of lower dry 12h, 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 lower stirring reaction 8h; Suction filtration, colourless to filtrate with 0.1mol/L hydrochloric acid soln washing leaching cake.Filter cake after taking-up is ground, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8h, and recording specific conductivity with four probe method is 1.38S/cm.
Experimental example 3:
In reactor A, add successively 25ml distilled water 8.2 * 10
-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 lower stirring reaction 12h, suction filtration, colourless to filtrate with the distilled water wash filter cake; Filter cake is pulverized after the taking-up at 60 ℃ of lower dry 12h, 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; Then add successively 1.97 * 10
-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 lower stirring reaction 8h; After reaction finishes, in reactor B, add the saturated NaCl solution of 30ml, breakdown of emulsion 30min; Suction filtration, colourless to filtrate with 0.1mol/L hydrochloric acid soln washing leaching cake; Filter cake namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 12h, and recording specific conductivity with four probe method is 1.48 S/cm.
Experimental example 4:
In reactor A, add successively 25ml distilled water 8.2 * 10
-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 lower stirring reaction 12h, suction filtration, colourless to filtrate with the distilled water wash filter cake; Filter cake is pulverized after the taking-up at 60 ℃ of lower dry 12h, 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; Then add successively 1.96 * 10
-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 lower stirring reaction 7h; After reaction finishes, in reactor B, add the 30ml dehydrated alcohol, breakdown of emulsion 30min; Suction filtration, colourless to filtrate with 0.1mol/L hydrochloric acid soln washing leaching cake; Filter cake namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8h, and recording specific conductivity with four probe method is 0.65S/cm.
Experimental example 5:
In reactor A, add successively 25ml distilled water 8.2 * 10
-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 lower stirring reaction 12h, suction filtration, colourless to filtrate with the distilled water wash filter cake; Filter cake is pulverized after the taking-up at 60 ℃ of lower dry 12h, 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; Then add successively 8.15 * 10
-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 lower stirring reaction 5h; After reaction finishes, in reactor B, add 30ml acetone, breakdown of emulsion 30min; Suction filtration, colourless to filtrate with 0.1mol/L hydrochloric acid soln washing leaching cake; Filter cake namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 10h, 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 it in the application in the fields such as sensor, conductive element device, electrode active material.
Claims (3)
1. a nucleocapsid structure gathers 23 dimethyl aniline/polyaniline composite material, and particularly take poly-23 dimethyl aniline as nuclear, polyaniline is the conducing composite material of shell, and its preparation method is:
1) preparation of nuclear:
In reactor A, add successively 25ml distilled water, 8.2 * 10
-3The commercially available content of mol is 36 ~ 38% concentrated hydrochloric acid and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Then splash into 12.5ml 1.2mol/L ammonium persulphate or Sodium Persulfate solution, in 30 ℃ of lower stirring reaction 12h; Suction filtration, and colourless to filtrate with the distilled water wash filter cake; Filter cake takes out and grinds behind 60 ℃ of lower dry 12h, obtains Powdered poly-23 dimethyl aniline, as nuclear;
2) preparation of shell:
A. with step 1) the poly-23 dimethyl aniline powder that makes moves in the reactor B, adds the hydrochloric acid soln of 1.2mol/L, stir 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, aniline and step 1) in the mol ratio of 23 dimethyl aniline be 1 ~ 4
:1;
B. ammonium persulphate or the Sodium Persulfate solution with 0.58mol/L slowly splashes in the reactor B, at 0 ~ 30 ℃ of lower reaction 5 ~ 8h; Wherein, the mol ratio of ammonium persulphate or Sodium Persulfate and aniline is 0.4 ~ 1
:1;
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, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8 ~ 12h.
2. one kind prepares the method that nucleocapsid structure as claimed in claim 1 gathers 23 dimethyl aniline/polyaniline composite material, it is characterized in that:
1) preparation of nuclear:
In reactor A, add successively 25ml distilled water, 8.2 * 10
-3The commercially available content of mol is 36 ~ 38% concentrated hydrochloric acid and 8.15 * 10
-3The mol 23 dimethyl aniline stirs 30min and makes its mixing; Then splash into 12.5ml 1.2mol/L ammonium persulphate or Sodium Persulfate solution, in 30 ℃ of lower stirring reaction 12h; Suction filtration, and colourless to filtrate with the distilled water wash filter cake; Filter cake takes out and grinds behind 60 ℃ of lower dry 12h, obtains Powdered poly-23 dimethyl aniline, as nuclear;
2) preparation of shell:
A. with step 1) the poly-23 dimethyl aniline powder that makes moves in the reactor B, adds the hydrochloric acid soln of 1.2mol/L, stir 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, aniline and step 1) in the mol ratio of 23 dimethyl aniline be 1 ~ 4
:1;
B. ammonium persulphate or the Sodium Persulfate solution with 0.58mol/L slowly splashes in the reactor B, at 0 ~ 30 ℃ of lower reaction 5 ~ 8h; Wherein, the mol ratio of ammonium persulphate or Sodium Persulfate and aniline is 0.4 ~ 1
:1;
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, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8 ~ 12h.
3. method as claimed in claim 2 is characterized in that: step 2) preparation process of shell is as follows,
A. with step 1) the poly-23 dimethyl aniline powder that makes moves in the reactor B; After Sodium dodecylbenzene sulfonate being dissolved in the hydrochloric acid soln of 1.2mol/L, join in the reactor B, add subsequently aniline, stir lower emulsification 30min; Wherein, the mol ratio of Sodium dodecylbenzene sulfonate and aniline is 0.6 ~ 1:1, and the volume ratio of hydrochloric acid soln and aniline is 50
:1, aniline and step 1) in the mol ratio of 23 dimethyl aniline be 1 ~ 4
:1;
B. ammonium persulphate or the Sodium Persulfate solution with 0.58mol/L slowly splashes in the reactor B, at 0 ~ 30 ℃ of lower reaction 5 ~ 8h; Wherein, the mol ratio of ammonium persulphate or Sodium Persulfate and aniline is 0.4 ~ 1
:1;
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 to filtrate with the hydrochloric acid soln washing leaching cake of 0.1mol/L; Filter cake after taking-up is ground, namely gets the poly-23 dimethyl aniline/polyaniline composite material of nucleocapsid structure at 60 ℃ of lower dry 8 ~ 12h.
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| 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 |
| CN115411259B (en) * | 2022-10-13 | 2023-04-25 | 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 |
|---|---|---|---|---|
| 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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| 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 |
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