CN108794996A - A kind of Aluminum sol improves polythiophene conductive material and preparation method thereof - Google Patents
A kind of Aluminum sol improves polythiophene conductive material and preparation method thereof Download PDFInfo
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- CN108794996A CN108794996A CN201810578951.5A CN201810578951A CN108794996A CN 108794996 A CN108794996 A CN 108794996A CN 201810578951 A CN201810578951 A CN 201810578951A CN 108794996 A CN108794996 A CN 108794996A
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Abstract
The invention discloses a kind of Aluminum sols to improve polythiophene conductive material, it is made of the raw material of following weight parts：Oleamide 3-5, ferric chloride (FeCl36H2O) 2-4, acetylene carbon black 10-13, zinc stearate 0.7-1, tributyl tin trichloride 0.1-0.2, palm wax 3-5, silane coupling agent kh550 0.5-1, colloidal sol monomer 110-130, it polymerize under oxidant effect, by polymerization material using amino silane modified, the fine dispersion between each raw material is realized, to improve the mechanics and conductive stability of finished-product material.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of Aluminum sol improves polythiophene conductive material and preparation method thereof.
Background technology
The compound rare report of unsubstituted thiophene and inorganic material is all a bit in organic solvent (chloroform) or thiophene is straight
It connects compound in the progress of thiophene boiling point with montmorillonite；Unsubstituted polythiophene is because dissolubility is bad in water for it, usually in chloroform etc.
In organic solvent or pass through electrochemical polymerization.When thiophene polymerize in chloroform solvent, chloroform evaporated is finally generally required to fall,
Or disposed by other approach, which increase the time of reaction and cost, it is unfavorable for industrializing；And pass through electrochemical polymerization
When, it needs to seek suitable solvent, and variable factor is too many, obtains polythiophene quality and be difficult to ensure, industrialization is also limited
System；The compatibility of inorganic filler and polythiophene is poor, and the stability of finished product is low, therefore the purpose of the present invention is exactly to improve poly- thiophene
Pheno and inorganic filler stablize it is compatible on the basis of, assign composite material new function, to enhance its applicability in different field.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of Aluminum sols to improve polythiophene conductive
Material and preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of Aluminum sol improvement polythiophene conductive material, it is made of the raw material of following weight parts：
Oleamide 3-5, ferric chloride (FeCl36H2O) 2-4, acetylene carbon black 10-13, zinc stearate 0.7-1, tributyl tri-chlorination
Tin 0.1-0.2, palm wax 3-5, silane coupling agent kh5500.5-1, colloidal sol monomer 110-130.
What the colloidal sol monomer was made of the raw material of following weight parts：
Propandiol butyl ether 2-3, aluminium isopropoxide 20-27, thiophene 100-120, triethylamine 1-2.
The preparation method of the colloidal sol monomer, includes the following steps：
(1) thiophene is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs evenly, triethylamine is added, increases temperature
Degree is 50-55 DEG C, and insulated and stirred 10-30 minutes obtains amine aqueous solution；
(2) aluminium isopropoxide is taken, is added in the deionized water of 35-40 times of its weight, stirs evenly, it is mixed with above-mentioned amine aqueous solution
It closes, is stirred to react 3-4 hour, propandiol butyl ether is added, it is 65-70 DEG C to increase temperature, and insulated and stirred 10-20 minutes is to get institute
State colloidal sol monomer.
A kind of Aluminum sol improves the preparation method of polythiophene conductive material, includes the following steps：
(1) palm wax is taken, is added in the dimethylformamide of 6-9 times of its weight, 85-90 DEG C of water bath with thermostatic control is sent to
In, insulated and stirred 10-20 minutes, discharging is mixed with tributyl tin trichloride, is stirred to room temperature, is obtained amide solution；
(2) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly；
(3) acetylene carbon black is taken, in ethanol solution that be added to 30-40 times of its weight, 60-65%, oleamide is added,
It is 7-10 minutes ultrasonic, obtain carbon black dispersion liquid；
(4) above-mentioned amide solution, carbon black dispersion liquid mixing are taken, stirs evenly, above-mentioned colloidal sol monomer is added, is sent to reaction
In kettle, it is passed through nitrogen, it is 15-20 DEG C to adjust temperature of reaction kettle, and the aqueous solution of above-mentioned ferric chloride (FeCl36H2O), insulated and stirred is added
10-14 hours, silane coupling agent kh550 was added in discharging, and it is 60-65 DEG C to increase temperature, and insulated and stirred 1-2 hours filters, will
Filter cake is washed, and air drying obtains sol-gel modified polythiophene；
(5) above-mentioned sol-gel modified polythiophene is taken, mixes, stirs evenly with remaining each raw material, it is dry at 50-55 DEG C of vacuum
30-40 minutes, be cooled to room temperature to get.
Advantages of the present invention：
Using aluminium isopropoxide as presoma, the thiophene being modified with amine is blended the present invention, hydrolyzes in aqueous solution, it is molten to obtain amination
Glue monomer, is also added into propandiol butyl ether in hydrolytic process, can effectively improve the stability of colloidal sol, the present invention is with second
Alkynes carbon black is conductive material, is gathered under oxidant effect with amination colloidal sol monomer blend using oleamide aqueous dispersion
It closes, polymerization is expected that use is amino silane modified, the fine dispersion between each raw material is realized, to improve the mechanics of finished-product material
And conductive stability.
Specific implementation mode
Embodiment 1
A kind of Aluminum sol improvement polythiophene conductive material, it is made of the raw material of following weight parts：
Oleamide 5, ferric chloride (FeCl36H2O) 4, acetylene carbon black 13, zinc stearate 1, tributyl tin trichloride 0.2, palm wax
5, silane coupling agent kh5501, colloidal sol monomer 130.
What the colloidal sol monomer was made of the raw material of following weight parts：
Propandiol butyl ether 3, aluminium isopropoxide 27, thiophene 120, triethylamine 2.
The preparation method of the colloidal sol monomer, includes the following steps：
(1) thiophene is taken, is added in the absolute ethyl alcohol of 20 times of its weight, stirs evenly, triethylamine is added, increasing temperature is
55 DEG C, insulated and stirred 30 minutes obtains amine aqueous solution；
(2) aluminium isopropoxide is taken, is added in the deionized water of 40 times of its weight, stirs evenly, mixed with above-mentioned amine aqueous solution,
It is stirred to react 4 hours, propandiol butyl ether is added, it is 70 DEG C to increase temperature, and insulated and stirred 20 minutes is to get the colloidal sol monomer.
A kind of Aluminum sol improves the preparation method of polythiophene conductive material, includes the following steps：
(1) palm wax is taken, is added in the dimethylformamide of 9 times of its weight, is sent in 90 DEG C of water bath with thermostatic control, is protected
Temperature stirring 20 minutes, discharging are mixed with tributyl tin trichloride, are stirred to room temperature, are obtained amide solution；
(2) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
(3) acetylene carbon black is taken, is added in 40 times of its weight, 65% ethanol solution, oleamide, ultrasound 10 is added
Minute, obtain carbon black dispersion liquid；
(4) above-mentioned amide solution, carbon black dispersion liquid mixing are taken, stirs evenly, above-mentioned colloidal sol monomer is added, is sent to reaction
In kettle, it is passed through nitrogen, it is 20 DEG C to adjust temperature of reaction kettle, the aqueous solution of above-mentioned ferric chloride (FeCl36H2O) is added, insulated and stirred 14 is small
When, silane coupling agent kh550 is added in discharging, and it is 65 DEG C to increase temperature, and insulated and stirred 2 hours is filtered, filter cake washed, room temperature
It is dry, obtain sol-gel modified polythiophene；
(5) above-mentioned sol-gel modified polythiophene is taken, mixes, stirs evenly with remaining each raw material, it is 40 points dry at 55 DEG C of vacuum
Clock, be cooled to room temperature to get.
Embodiment 2
A kind of Aluminum sol improvement polythiophene conductive material, it is made of the raw material of following weight parts：
Oleamide 3, ferric chloride (FeCl36H2O) 2, acetylene carbon black 10, zinc stearate 0.7, tributyl tin trichloride 0.1, palm
Wax 3, silane coupling agent kh5500.5, colloidal sol monomer 110.
What the colloidal sol monomer was made of the raw material of following weight parts：
Propandiol butyl ether 2, aluminium isopropoxide 20, thiophene 100, triethylamine 1.
The preparation method of the colloidal sol monomer, includes the following steps：
(1) thiophene is taken, is added in the absolute ethyl alcohol of 17 times of its weight, stirs evenly, triethylamine is added, increasing temperature is
50 DEG C, insulated and stirred 10 minutes obtains amine aqueous solution；
(2) aluminium isopropoxide is taken, is added in the deionized water of 35 times of its weight, stirs evenly, mixed with above-mentioned amine aqueous solution,
It is stirred to react 3 hours, propandiol butyl ether is added, it is 65 DEG C to increase temperature, and insulated and stirred 10- minutes is to get the colloidal sol monomer.
A kind of Aluminum sol improves the preparation method of polythiophene conductive material, includes the following steps：
(1) palm wax is taken, is added in the dimethylformamide of 6 times of its weight, is sent in 85 DEG C of water bath with thermostatic control, is protected
Temperature stirring 10 minutes, discharging are mixed with tributyl tin trichloride, are stirred to room temperature, are obtained amide solution；
(2) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 17 times of its weight, stirs evenly；
(3) acetylene carbon black is taken, is added in 30 times of its weight, 60% ethanol solution, oleamide, ultrasonic 7- is added
Minute, obtain carbon black dispersion liquid；
(4) above-mentioned amide solution, carbon black dispersion liquid mixing are taken, stirs evenly, above-mentioned colloidal sol monomer is added, is sent to reaction
In kettle, it is passed through nitrogen, it is 15 DEG C to adjust temperature of reaction kettle, the aqueous solution of above-mentioned ferric chloride (FeCl36H2O) is added, insulated and stirred 10 is small
When, silane coupling agent kh550 is added in discharging, and it is 60 DEG C to increase temperature, and insulated and stirred 1 hour is filtered, filter cake washed, room temperature
It is dry, obtain sol-gel modified polythiophene；
(5) above-mentioned sol-gel modified polythiophene is taken, mixes, stirs evenly with remaining each raw material, it is 30 points dry at 50 DEG C of vacuum
Clock, be cooled to room temperature to get.
Performance test：
It is shown according to document (influence of the polythiophene preparation condition to its structure and electric conductivity)：Wang Hongmin etc. passes through chemistry
Oxidizing process is prepared for polythiophene and is tested to its conductivity, made when reaction temperature is respectively 0 DEG C, 18 DEG C, 55 DEG C
The conductivity of standby polythiophene is respectively 15.8 × 10-8S/cm、5.28×10-8S/cm、1.02×10-8S/cm；
The conductivity of the finished-product material of the embodiment of the present invention 1 is 0.33S/cm；The conductivity of the finished-product material of embodiment 2 is
0.32S/cm；
The tensile strength of the finished-product material of the embodiment of the present invention 1 is 34.4Mpa, the stretching of the finished-product material of embodiment 2 is strong
Degree is 35.1Mpa.
Claims (4)
1. a kind of Aluminum sol improves polythiophene conductive material, which is characterized in that it is made of the raw material of following weight parts：
Oleamide 3-5, ferric chloride (FeCl36H2O) 2-4, acetylene carbon black 10-13, zinc stearate 0.7-1, tributyl tin trichloride
0.1-0.2, palm wax 3-5, silane coupling agent kh550 0.5-1, colloidal sol monomer 110-130.
2. a kind of Aluminum sol according to claim 1 improves polythiophene conductive material, which is characterized in that the colloidal sol list
Body is made of the raw material of following weight parts：
Propandiol butyl ether 2-3, aluminium isopropoxide 20-27, thiophene 100-120, triethylamine 1-2.
3. a kind of Aluminum sol according to claim 2 improves polythiophene conductive material, which is characterized in that the colloidal sol list
The preparation method of body, includes the following steps：
(1) thiophene is taken, is added in the absolute ethyl alcohol of 17-20 times of its weight, stirs evenly, triethylamine is added, increasing temperature is
50-55 DEG C, insulated and stirred 10-30 minutes obtains amine aqueous solution；
(2) aluminium isopropoxide is taken, is added in the deionized water of 35-40 times of its weight, stirs evenly, is mixed with above-mentioned amine aqueous solution,
It is stirred to react 3-4 hours, propandiol butyl ether is added, it is 65-70 DEG C to increase temperature, and insulated and stirred 10-20 minutes is to get described molten
Glue monomer.
4. a kind of Aluminum sol as described in claim 1 improves the preparation method of polythiophene conductive material, which is characterized in that including with
Lower step：
(1) palm wax is taken, is added in the dimethylformamide of 6-9 times of its weight, is sent in 85-90 DEG C of water bath with thermostatic control,
Insulated and stirred 10-20 minutes, discharging, mixes with tributyl tin trichloride, stirs to room temperature, obtains amide solution；
(2) ferric chloride (FeCl36H2O) is taken, is added in the deionized water of 17-20 times of its weight, stirs evenly；
(3) acetylene carbon black is taken, in ethanol solution that be added to 30-40 times of its weight, 60-65%, oleamide, ultrasound is added
7-10 minutes, obtain carbon black dispersion liquid；
(4) above-mentioned amide solution, carbon black dispersion liquid mixing are taken, stirs evenly, above-mentioned colloidal sol monomer is added, is sent to reaction kettle
In, it is passed through nitrogen, it is 15-20 DEG C to adjust temperature of reaction kettle, and the aqueous solution of above-mentioned ferric chloride (FeCl36H2O), insulated and stirred 10- is added
14 hours, silane coupling agent kh550 was added in discharging, and it is 60-65 DEG C to increase temperature, and insulated and stirred 1-2 hours filters, by filter cake
Washing, air drying obtain sol-gel modified polythiophene；
(5) above-mentioned sol-gel modified polythiophene is taken, mixes, stirs evenly with remaining each raw material, dry 30-40 at 50-55 DEG C of vacuum
Minute, be cooled to room temperature to get.
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| KR20140086516A (en) * | 2012-12-28 | 2014-07-08 | 삼성전기주식회사 | Conductive polymer composition and conductive film prepared from the composition |
| CN105977448A (en) * | 2016-07-13 | 2016-09-28 | 广东工业大学 | Ferric fluoride/conducting polymer composite material, preparation method thereof and lithium secondary battery |
| CN107629453A (en) * | 2017-10-18 | 2018-01-26 | 温州市赢创新材料技术有限公司 | A kind of polypyrrole conductive sol film and preparation method thereof |
| CN107841231A (en) * | 2017-11-07 | 2018-03-27 | 常州福隆工控设备有限公司 | A kind of preparation method of wear-resistance and anti-corrosion coating material |
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2018
- 2018-06-07 CN CN201810578951.5A patent/CN108794996A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101722049A (en) * | 2009-11-25 | 2010-06-09 | 武汉理工大学 | Catalyst modified by proton conductor and using conductive polymer as carrier and preparation method thereof |
| CN103412019A (en) * | 2012-11-20 | 2013-11-27 | 中国科学院合肥物质科学研究院 | Bioelectrode formed by three-dimensional ordered porous oxide modified conductive film and preparation method of bioelectrode |
| KR20140086516A (en) * | 2012-12-28 | 2014-07-08 | 삼성전기주식회사 | Conductive polymer composition and conductive film prepared from the composition |
| CN105977448A (en) * | 2016-07-13 | 2016-09-28 | 广东工业大学 | Ferric fluoride/conducting polymer composite material, preparation method thereof and lithium secondary battery |
| CN107629453A (en) * | 2017-10-18 | 2018-01-26 | 温州市赢创新材料技术有限公司 | A kind of polypyrrole conductive sol film and preparation method thereof |
| CN107841231A (en) * | 2017-11-07 | 2018-03-27 | 常州福隆工控设备有限公司 | A kind of preparation method of wear-resistance and anti-corrosion coating material |
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