CN108424539A - A kind of preparation method of heat-resisting layer/polyaniline conductive film - Google Patents
A kind of preparation method of heat-resisting layer/polyaniline conductive film Download PDFInfo
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- CN108424539A CN108424539A CN201810377796.0A CN201810377796A CN108424539A CN 108424539 A CN108424539 A CN 108424539A CN 201810377796 A CN201810377796 A CN 201810377796A CN 108424539 A CN108424539 A CN 108424539A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
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- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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Abstract
The invention discloses a kind of preparation method of heat-resisting layer/polyaniline conductive film, preparation process is：（1）The preparation of ammonium persulfate aqueous solution；（2）The preparation of phosphorus doping polymer emulsion；（3）The preparation of heat-resistant polymer；（4）The preparation of heat-resisting layer/polyaniline conductive film.The present invention is using phosphorus trichloride as modifying agent, by being doped to aniline monomer after hydrolysis, the good electric conductivity of polyaniline is not given only, and esterification is blended with bisphenol-A for it later, obtained bisphenol-A ester has good heat-resistant stability, improves the high-temperature capability of finished films；The Thin film conductive stability of the present invention is good, and mechanical strength is high, and heat-resistant stability is good, and comprehensive performance is superior.
Description
Technical field
The invention belongs to film applications, and in particular to a kind of preparation method of heat-resisting layer/polyaniline conductive film.
Background technology
Polyaniline as one of conducting polymer composite, because its chemical stability is good, weatherability is good, raw material is cheap and easy to get,
Synthetic method is simple and electric conductivity etc., it is considered to be the most structural conducting polymer of commercial application value, in life
There is great market demand in the fields such as object sensor, anti-corrosion material, absorbing material.But polyaniline conductivity is not high and post-production
It handles, the problem of stability difference makes it be a greater impact in popularization and application.
Simultaneously currently, greatly developing with polyaniline film, is proposed mechanical strength, the heat resistance etc. of film
New requirement, it is high, heat-resisting therefore, the purpose of the present invention is to how provide a kind of mechanical strength to adapt to different working environments
The good polyaniline film of performance.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of heat-resisting layer/polyaniline conductive films
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of heat-resisting layer/polyaniline conductive film, is made by following steps：
（1）Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, it is water-soluble that ammonium persulfate is made
Liquid；
（2）Phosphorus trichloride, glyceryl tristearate mixing are taken, is added in the deionized water of 10-17 times of mixture weight,
It is stirred 10-20 minutes at 50-55 DEG C, aniline is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjust reaction kettle temperature
Degree is 65-70 DEG C, and above-mentioned ammonium persulfate aqueous solution, insulated and stirred 4-5 hours is added, and discharging cooling obtains phosphorus doping polymer breast
Liquid；
（3）Bisphenol-A is taken, is added in above-mentioned phosphorus doping polymer emulsion, stirs evenly, it is 90-95 DEG C to increase temperature, and heat preservation is stirred
It mixes 1-2 hours, filters, filter cake is washed, air drying obtains heat-resistant polymer；
（4）Above-mentioned heat-resistant polymer is taken, is added in activated graphene dispersion liquid, stirs evenly, heat-resisting stabilizing agent, stirring is added
3-4 hours, spin-coating film was to get the heat-resisting layer/polyaniline conductive film.
Preferably, it counts in parts by weight, above-mentioned each raw material is：
130-150 parts of aniline, 3-4 parts of phosphorus trichloride, 5-7 parts of bisphenol-A, 1-2 parts of heat-resisting stabilizing agent, glyceryl tristearate
0.8-1 parts, 200-300 parts of activated graphene dispersion liquid, 3-4 parts of ammonium persulfate.
Preferably, the one kind of heat-resisting stabilizing agent of the present invention in stearate or dibutyl tin laurate.
Preferably, activated graphene dispersion liquid of the present invention is made from the raw material by following weight parts：
30-40 parts of graphene, 0.1-0.2 parts of polysorbate, 6-9 parts of potassium permanganate, 2-4 parts of chlorosulfonic acid, barium naphthanate 0.7-1
Part, 100-120 parts of dimethylformamide.
Preferably, activated graphene dispersion liquid of the present invention, is made by following steps：
（1）Barium naphthanate is taken, is added in dimethylformamide, is stirred evenly, amide solution is obtained；
（2）Graphene is taken, it is 6-10 hours ultrasonic in sulfuric acid solution that be added to 20-30 times of its weight, 96-98%, it is added high
Potassium manganate, it is 65-70 DEG C to increase temperature, insulated and stirred 1-2 hours, and chlorosulfonic acid, stirring to room temperature is added, and filtering will precipitate water
It washes, air drying obtains activated graphene；
（3）Above-mentioned Activated Graphite alkene is taken, is added in amide solution, polysorbate, the insulated and stirred 20- at 40-50 DEG C is added
30 minutes to get the graphite alkene dispersion liquid.
Advantages of the present invention：
In the activated graphene dispersion liquid of the present invention, oxidation processes are carried out to graphene first, then chlorosulfonic acid is used to be modified, changed
It has been apt to its surface-active, has improved the stable composition intensity of graphene and polyaniline；The present invention using phosphorus trichloride as modifying agent,
By being doped to aniline monomer after hydrolysis, do not give only the good electric conductivity of polyaniline, and later by its with it is double
Esterification is blended in phenol A, and obtained bisphenol-A ester has good heat-resistant stability, improves the high-temperature capability of finished films；The present invention
Thin film conductive stability it is good, mechanical strength is high, and heat-resistant stability is good, and comprehensive performance is superior.
Specific implementation mode
The present invention is further described through with reference to embodiment.
Embodiment 1
1）The preparation of activated graphene dispersion liquid
It counts in parts by weight, weighs the following raw material：40 parts of graphene, 0.2 part of polysorbate, 9 parts of potassium permanganate, 4 parts of chlorosulfonic acid,
1 part of barium naphthanate, 120 parts of dimethylformamide；
Specifically preparation method step is：
（1）Barium naphthanate is taken, is added in dimethylformamide, is stirred evenly, amide solution is obtained；
（2）Graphene is taken, is added in 30 times of its weight, 98% sulfuric acid solution, potassium permanganate is added in ultrasound 10 hours, rises
High-temperature is 70 DEG C, insulated and stirred 2 hours, and chlorosulfonic acid, stirring to room temperature is added, and precipitation is washed in filtering, and air drying obtains
Activated graphene；
（3）Above-mentioned Activated Graphite alkene is taken, is added in amide solution, addition polysorbate, insulated and stirred 30 minutes at 50 DEG C,
Up to the graphite alkene dispersion liquid.
2）The preparation of heat-resisting layer/polyaniline conductive film
It counts in parts by weight, weighs the following raw material：150 parts of aniline, 4 parts of phosphorus trichloride, 7 parts of bisphenol-A, 2 parts of odium stearate, three
1 part of tristerin, 300 parts of activated graphene dispersion liquid, 4 parts of ammonium persulfate；
Specifically preparation method step is：
（1）Ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly；
（2）Phosphorus trichloride, glyceryl tristearate mixing are taken, is added in the deionized water of 17 times of mixture weight, at 55 DEG C
Lower stirring 20 minutes, is added aniline, stirs evenly, be sent in reaction kettle, is passed through nitrogen, and it is 70 DEG C to adjust temperature of reaction kettle,
Above-mentioned ammonium persulfate aqueous solution, insulated and stirred 5 hours is added, discharging cooling obtains phosphorus doping polymer emulsion；
（3）Bisphenol-A is taken, is added in above-mentioned phosphorus doping polymer emulsion, stirs evenly, it is 95 DEG C to increase temperature, insulated and stirred 2
Hour, it filters, filter cake is washed, air drying obtains heat-resistant polymer；
（4）Above-mentioned heat-resistant polymer is taken, is added in activated graphene dispersion liquid, stirs evenly, odium stearate, stirring 4 is added
Hour, spin-coating film is to get the heat-resisting layer/polyaniline conductive film.
Embodiment 2
1）The preparation of activated graphene dispersion liquid
It counts in parts by weight, weighs the following raw material：30 parts of graphene, 0.1 part of polysorbate, 6 parts of potassium permanganate, 2 parts of chlorosulfonic acid,
0.7 part of barium naphthanate, 100 parts of dimethylformamide；
Specifically preparation method step is：
（1）Barium naphthanate is taken, is added in dimethylformamide, is stirred evenly, amide solution is obtained；
（2）Graphene is taken, is added in 20 times of its weight, 96% sulfuric acid solution, potassium permanganate is added in ultrasound 6 hours, rises
High-temperature is 65 DEG C, insulated and stirred 1 hour, and chlorosulfonic acid, stirring to room temperature is added, and precipitation is washed in filtering, and air drying obtains
Activated graphene；
（3）Above-mentioned Activated Graphite alkene is taken, is added in amide solution, addition polysorbate, insulated and stirred 20 minutes at 40 DEG C,
Up to the graphite alkene dispersion liquid.
2）The preparation of heat-resisting layer/polyaniline conductive film
It counts in parts by weight, weighs the following raw material：130 parts of aniline, 3 parts of phosphorus trichloride, 5 parts of bisphenol-A, 1 part of barium stearate, three
0.8 part of tristerin, 200 parts of activated graphene dispersion liquid, 3 parts of ammonium persulfate.
Specifically preparation method step is：
（1）Ammonium persulfate is taken, is added in the deionized water of 20 times of its weight, stirs evenly；
（2）Phosphorus trichloride, glyceryl tristearate mixing are taken, is added in the deionized water of 10 times of mixture weight, at 50 DEG C
Lower stirring 10 minutes, is added aniline, stirs evenly, be sent in reaction kettle, is passed through nitrogen, and it is 65 DEG C to adjust temperature of reaction kettle,
Above-mentioned ammonium persulfate aqueous solution, insulated and stirred 4 hours is added, discharging cooling obtains phosphorus doping polymer emulsion；
（3）Bisphenol-A is taken, is added in above-mentioned phosphorus doping polymer emulsion, stirs evenly, it is 90 DEG C to increase temperature, insulated and stirred 1
Hour, it filters, filter cake is washed, air drying obtains heat-resistant polymer；
（4）Above-mentioned heat-resistant polymer is taken, is added in activated graphene dispersion liquid, stirs evenly, barium stearate, stirring 3 is added
Hour, spin-coating film is to get the heat-resisting layer/polyaniline conductive film.
Performance test：
The heat-resisting layer/polyaniline conductive film of embodiment 1：
Thickness 2.0mm；
Tensile strength 12.7Mpa；It is heat-treated 10 hours at 100 DEG C, tensile strength reduced rate is 0.13%；
Conductivity is tested using four probe method, result 0.90S/cm；
The heat-resisting layer/polyaniline conductive film of embodiment 2：
Thickness 2.2mm；
Tensile strength 13.1Mpa；It is heat-treated 10 hours at 100 DEG C, tensile strength reduced rate is 0.20%；
Conductivity is tested using four probe method, result 0.97S/cm.
Claims (5)
1. a kind of preparation method of heat-resisting layer/polyaniline conductive film, it is characterised in that：Preparation process is as follows：
（1）Ammonium persulfate is taken, is added in the deionized water of 20-30 times of its weight, stirs evenly, it is water-soluble that ammonium persulfate is made
Liquid；
（2）Phosphorus trichloride, glyceryl tristearate mixing are taken, is added in the deionized water of 10-17 times of mixture weight,
It is stirred 10-20 minutes at 50-55 DEG C, aniline is added, stirs evenly, is sent in reaction kettle, be passed through nitrogen, adjust reaction kettle temperature
Degree is 65-70 DEG C, and above-mentioned ammonium persulfate aqueous solution, insulated and stirred 4-5 hours is added, and discharging cooling obtains phosphorus doping polymer breast
Liquid；
（3）Bisphenol-A is taken, is added in above-mentioned phosphorus doping polymer emulsion, stirs evenly, it is 90-95 DEG C to increase temperature, and heat preservation is stirred
It mixes 1-2 hours, filters, filter cake is washed, air drying obtains heat-resistant polymer；
（4）Above-mentioned heat-resistant polymer is taken, is added in activated graphene dispersion liquid, stirs evenly, heat-resisting stabilizing agent, stirring is added
3-4 hours, spin-coating film was to get the heat-resisting layer/polyaniline conductive film.
2. a kind of preparation method of heat-resisting layer/polyaniline conductive film according to claim 1, it is characterised in that：By weight
Number meter, each raw material are：130-150 parts of aniline, 3-4 parts of phosphorus trichloride, 5-7 parts of bisphenol-A, 1-2 parts of heat-resisting stabilizing agent, three tristearin
0.8-1 parts of acid glyceride, 200-300 parts of activated graphene dispersion liquid, 3-4 parts of ammonium persulfate.
3. a kind of preparation method of heat-resisting layer/polyaniline conductive film according to claim 1 or 2, it is characterised in that：It is described
One kind in stearate or dibutyl tin laurate of heat-resisting stabilizing agent.
4. a kind of preparation method of heat-resisting layer/polyaniline conductive film according to claim 1 or 2, which is characterized in that described
Activated graphene dispersion liquid be made from raw material by following weight parts：
30-40 parts of graphene, 0.1-0.2 parts of polysorbate, 6-9 parts of potassium permanganate, 2-4 parts of chlorosulfonic acid, barium naphthanate 0.7-1
Part, 100-120 parts of dimethylformamide.
5. a kind of preparation method of heat-resisting layer/polyaniline conductive film according to claim 4, which is characterized in that the work
Graphite alkene dispersion liquid, is made by following steps：
（1）Barium naphthanate is taken, is added in dimethylformamide, is stirred evenly, amide solution is obtained；
（2）Graphene is taken, it is 6-10 hours ultrasonic in sulfuric acid solution that be added to 20-30 times of its weight, 96-98%, it is added high
Potassium manganate, it is 65-70 DEG C to increase temperature, insulated and stirred 1-2 hours, and chlorosulfonic acid, stirring to room temperature is added, and filtering will precipitate water
It washes, air drying obtains activated graphene；
（3）Above-mentioned Activated Graphite alkene is taken, is added in amide solution, polysorbate, the insulated and stirred 20- at 40-50 DEG C is added
30 minutes to get the graphite alkene dispersion liquid.
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| US20090092747A1 (en) * | 2007-10-04 | 2009-04-09 | Aruna Zhamu | Process for producing nano-scaled graphene platelet nanocomposite electrodes for supercapacitors |
| CN106866961A (en) * | 2017-03-25 | 2017-06-20 | 山东本源晶体科技有限公司 | A kind of preparation method of polyaniline composite ganoine conductive graphene material |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
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- 2018-04-25 CN CN201810377796.0A patent/CN108424539A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090092747A1 (en) * | 2007-10-04 | 2009-04-09 | Aruna Zhamu | Process for producing nano-scaled graphene platelet nanocomposite electrodes for supercapacitors |
| CN106866961A (en) * | 2017-03-25 | 2017-06-20 | 山东本源晶体科技有限公司 | A kind of preparation method of polyaniline composite ganoine conductive graphene material |
| CN107722264A (en) * | 2017-11-23 | 2018-02-23 | 清远初曲智能科技有限公司 | A kind of colloidal sol polyaniline composite graphite alkene conductive material and preparation method thereof |
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