CN107201035A - A kind of preparation method of conductive automatically cleaning polyamidoimide/polyaniline film - Google Patents
A kind of preparation method of conductive automatically cleaning polyamidoimide/polyaniline film Download PDFInfo
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- CN107201035A CN107201035A CN201710479137.3A CN201710479137A CN107201035A CN 107201035 A CN107201035 A CN 107201035A CN 201710479137 A CN201710479137 A CN 201710479137A CN 107201035 A CN107201035 A CN 107201035A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/02—Polyamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The invention discloses a kind of preparation method of conductive automatically cleaning polyamidoimide/polyaniline film, belong to polymer modification and the preparing technical field of nano composite material.Multi-functional polyamidoimide/polyaniline film of the present invention is prepared as follows：Synthesized polyaniline, is then adulterated with camphorsulfonic acid first, obtains the polyaniline of camphorsulfonic acid doping, and the polyaniline that camphorsulfonic acid adulterates is dispersed in polyamideimide solution by high speed emulsification and ultrasonic vibration.Polyamidoimide/polyaniline composite material can be prepared by solvent cast membrane formation process.Polyamidoimide/polyaniline composite material that the present invention is provided has automatically cleaning and superior electrical conductivity energy and certain mechanical strength, and electrical conductivity reaches 50 more than S/m, and water contact angle is 120oMore than, the multiple fields such as electrostatic screen and sapecial coating can be used in.
Description
Technical field：
The present invention relates to a kind of conductive automatically cleaning polyamidoimide/polyaniline film and preparation method thereof, belong to high
The preparing technical field of molecular material blending and modifying and nano composite material.
Background technology：
In recent years, relative to the nano material of one-component, Multifunctional composite nanometer material is gradually by scientists
Extensive concern.The characteristics of composite nano materials not only have the nano materials such as quantum size effect, surface and interface effect, also has
There is the synergistic function effect that composite construction is brought, so that composite nano materials are multi-field with wide in light, electricity, magnetic etc.
Application prospect.
Polyamidoimide with good mechanical property, heat endurance and machinability due to turning into industrial and daily
Wide variety of high polymer material in life.But the high-insulativity of polyamidoimide makes it easily produce, accumulates electrostatic, and this is big
Its application field is limited greatly.On the other hand, polyaniline has preferable electrical property, optical property, and environmental stability, is
Most there is one of conducting polymer of actual application prospect, thus with wide in terms of conductive plastics, nano composite material
Application prospect.
The present invention passes through regulation using the good mechanical property of polyamidoimide and the excellent conductive characteristic of polyaniline
The ratio of polyamidoimide and polyaniline, obtaining that electrical conductivity is controllable and polyamidoimide of excellent in mechanical performance/poly-
Aniline composite nano materials.Meanwhile, nano material is small due to the nano-particles size of its composition material, what microparticle surfaces were occupied
Non-nano particle of the atom number far more than phase homogenous quantities.Therefore, the present invention utilizes the surface and interface effect of nano-particle,
The polyamidoimide with rough surface structure/layer/polyaniline conductive composite nano materials are constructed, with preferable electric conductivity
While with mechanical strength, there is self-cleaning function again.
The content of the invention
It is an object of the invention to by simple solvent cast method, prepare the electrical-conductive nanometer with self-cleaning function and be combined
Material.
The preparation method of multi-functional polyamidoimide/polyaniline composite material, is carried out as steps described below：
(1) preparation of polyaniline
The aniline newly distilled is added in 0.2mol/L hydrochloric acid solution, is stirred at 0-5 DEG C after 0.5-2h, slowly
The aqueous solution of (1-3s often drips) ammonium persulfate is added dropwise, then 6-10h is reacted at 0-5 DEG C.Reaction solution suction filtration is obtained into green solid
Body, then methanol, n-hexane, chloroform surname extraction are used respectively, 60 DEG C of vacuum drying 12h obtain the green powder of doped hydrochloride
Polyaniline.
(2) camphorsulfonic acid doped polyaniline
Polyaniline powder is added under 10% ammoniacal liquor, normal temperature and stirred after 12-16h, is washed with water to neutrality, 60 DEG C true
Sky dries 12h, obtains polyaniline in eigenstate, and its character is purple powder.Camphorsulfonic acid doping is obtained with solution-mechanical milling method
Polyaniline, i.e., first camphorsulfonic acid is ground, polyaniline in eigenstate is added afterwards, be fully ground 15min, a first is then added dropwise
Phenol, and continue to grind 30min, then 30min is emulsified with high-speed emulsifying machine, camphorsulfonic acid doping is finally dried to obtain at 90 DEG C
Polyaniline.
(3) preparation of polyamidoimide/polyaniline composite material
The polyaniline that camphorsulfonic acid is adulterated is put into the polyamidoimide m-cresol solution prepared in advance, and is added
Enter compatilizer hydroquinones, the polyaniline that camphorsulfonic acid adulterates is homogeneously dispersed in by polyamides by high speed emulsification and ultrasonic vibration
In amine imide solution.Then polyamidoimide/polyaniline multifunctional composite is prepared by solvent cast method.
The mol ratio of aniline, ammonium persulfate and hydrochloric acid is 1 wherein in step (1):1:0.2；
The mass ratio of polyaniline and ammoniacal liquor is 1 wherein in step (2):20；
The mass ratio of polyaniline and camphorsulfonic acid is 1 wherein in step (2):1.5
The content for the polyaniline that camphorsulfonic acid adulterates is polyamidoimide/polyaniline composite material wherein in step (3)
The 10%-40% of gross mass；
The content of hydroquinones is polyamidoimide/polyaniline composite material gross mass wherein in step (3)
0.5%-2%；
The structural formula of the polyaniline of wherein affiliated camphorsulfonic acid doping is as follows：
Wherein 0<y<1；
Wherein 10<n<200.
The structural formula of wherein described polyamide-imide resin is shown below：
Wherein 10<n<200.
Using the above method, with following technological merit：
Polymer/polymer Quito functional composite material is mostly using the complicated technique such as electrospinning, LBL self-assembly.We
Using the interaction of hydrogen bond and the surface and interface effect of nano-particle between polyamidoimide and polyaniline, using letter
Single solvent casting methods can greatly shorten the time of multifunctional composite preparation, and reduce the system of multifunctional composite
Cause this.
Brief description of the drawings
Fig. 1 is composite material film automatically cleaning schematic diagram of the present invention.
Embodiment
With reference to embodiments, the present invention will be described in further detail, and specific embodiment described herein is only used
To explain the present invention, it is not intended to limit the present invention.
Embodiment 1
(1) preparation of polyaniline
It is added in 0.2mol/L hydrochloric acid solution 120ml, the aniline 11.16g (0.12mol) newly distilled at 0-5 DEG C
After lower stirring 0.5-2h, (1-3s often drips) ammonium persulfate 27.36g (0.12mol) the 180ml aqueous solution, Ran Hou is slowly added dropwise
6-10h is reacted at 0-5 DEG C.Reaction solution suction filtration is obtained into green solid, then uses methanol, n-hexane, chloroform surname extraction, 60 respectively
DEG C vacuum drying 12h, obtain the green powder polyaniline of doped hydrochloride.
(2) camphorsulfonic acid doped polyaniline
In the 100ml ammoniacal liquor that 5g polyaniline powders are added to 10%, after stirring at normal temperature 12-16h, it is washed with water to neutrality, 60
DEG C vacuum drying 12h, obtain polyaniline in eigenstate, its character be purple powder.Camphor sulphur is obtained with solution-mechanical milling method
The polyaniline of acid doping, i.e., first grind camphorsulfonic acid, and the polyaniline in eigenstate (mass ratio of polyaniline and camphorsulfonic acid is added afterwards
For 1:1.5), be fully ground 15min, after be added dropwise metacresol, and continue to grind 30min, then emulsified with high-speed emulsifying machine
30min, is finally dried to obtain the polyaniline of camphorsulfonic acid doping at 90 DEG C.
(3) preparation of polyamidoimide/polyaniline composite material
The polyaniline (0.1g) that camphorsulfonic acid is adulterated is added to the 25ml polyamidoimide metacresols prepared in advance
In solution (0.036g/ml), compatilizer hydroquinones 10mg is added, camphorsulfonic acid is adulterated by high speed emulsification and ultrasonic vibration
Polyaniline be homogeneously dispersed in polyamideimide solution；Then solvent cast method film forming can be passed through.Polyamidoimide/
The electrical conductivity of polyaniline film is 0.00021S/m, and contact angle is 92 °, tensile strength 40.1MPa, Young's modulus 3.1GPa.Fig. 1
For composite material film automatically cleaning schematic diagram of the present invention.
Embodiment 2
The present embodiment and the difference of embodiment 1 are in the preparation process of polyamidoimide/polyaniline composite material, incite somebody to action
The polyaniline of 0.4g camphorsulfonic acid doping is added to the polyamidoimide m-cresol solution that 25mL is prepared in advance
In (0.024g/mL), other processing means are consistent with embodiment 1.The electrical conductivity of polyamidoimide/polyaniline film is
40S/m, 98 ° of contact angle, tensile strength 25.8MPa, the GPa of Young's modulus 1.8.
Embodiment 3
The present embodiment and the difference of embodiment 1 are in the preparation process of polyamidoimide/polyaniline material, by 0.2g
Camphorsulfonic acid doping polyaniline be added to the polyamidoimide m-cresol solution (0.032g/mL) that 25mL is prepared in advance
In, other processing means are consistent with embodiment 1.The electrical conductivity of polyamidoimide/polyaniline film is 10S/m, contact angle
102 °, tensile strength 32.1MPa, Young's modulus 2.4GPa.
Embodiment 4
The present embodiment and the difference of embodiment 3 are in the preparation process of polyamidoimide/polyaniline material, to benzene two
Phenol is 5mg, and other processing means are consistent with embodiment 3.The electrical conductivity of polyamidoimide/polyaniline film is 0.98S/m,
104 ° of contact angle, tensile strength 31.3MPa, Young's modulus 2.1GPa.
Embodiment 5
The present embodiment and the difference of embodiment 3 are in the preparation process of polyamidoimide/polyaniline material, to benzene two
Phenol is 20mg, and other processing means are consistent with embodiment 3.The electrical conductivity of polyamidoimide/polyaniline film is
0.0067S/m, 101 ° of contact angle, tensile strength 30.9MPa, Young's modulus 1.9GPa.
Embodiment 6
The present embodiment and the difference of embodiment 1 are in the preparation process of polyamidoimide/polyaniline material, by 0.3g
Camphorsulfonic acid doping polyaniline be added to the polyamidoimide m-cresol solution (0.028g/ that 17.5mL is prepared in advance
ML in).The electrical conductivity of polyamidoimide/polyaniline film is 24S/m, 120 ° of contact angle, tensile strength 29.1MPa, Young
Modulus 1.5GPa.
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Electrical conductivity (S/m) | 0.00021 | 40 | 10 | 0.98 | 0.067 | 24 |
| Water contact angle (°) | 92 | 98 | 102 | 104 | 101 | 120 |
| Tensile strength (MPa) | 40.1 | 25.8 | 32.1 | 31.1 | 30.9 | 29.1 |
| Young's modulus (GPa) | 3.1 | 1.8 | 2.4 | 2.1 | 1.9 | 1.5 |
The various embodiments described above are merely to illustrate the present invention, wherein the parameter of each step, implementation condition etc. are all can be
Change, every equivalent variations carried out on the basis of technical solution of the present invention and improvement should not be excluded the present invention's
Outside protection domain.
In summary, polyamidoimide/polyaniline composite material involved in the present invention not only has good conduction
Property, it is automatical cleaning ability also with preferable hydrophobicity, and mechanical strength, electrostatic screen and sapecial coating neck can be used in
Domain.
Claims (8)
1. the preparation method of multi-functional polyamidoimide/polyaniline composite material, it is characterised in that carry out as steps described below：
(1) preparation of polyaniline
The aniline newly distilled is added in 0.2mol/L hydrochloric acid solution, stirs after 0.5-2h, be slowly added dropwise at 0-5 DEG C
The aqueous solution of (1-3s often drips) ammonium persulfate, then reacts 6-10h at 0-5 DEG C；Reaction solution suction filtration is obtained into green solid, then
Methanol, n-hexane, chloroform surname extraction are used respectively, and 60 DEG C of vacuum drying 12h obtain the green powder polyphenyl of doped hydrochloride
Amine；
(2) camphorsulfonic acid doped polyaniline
Polyaniline powder is added under 10% ammoniacal liquor, normal temperature and stirred after 12-16h, is washed with water to neutrality, 60 DEG C of vacuum drying
12h, obtains polyaniline in eigenstate, and its character is purple powder；The polyphenyl of camphorsulfonic acid doping is obtained with solution-mechanical milling method
Amine, i.e., first grind camphorsulfonic acid, and polyaniline in eigenstate is added afterwards, is fully ground 15min, and metacresol is then added dropwise, and
30min is persistently ground, then 30min is emulsified with high-speed emulsifying machine, the polyphenyl of camphorsulfonic acid doping is finally dried to obtain at 90 DEG C
Amine；
(3) preparation of polyamidoimide/polyaniline composite material
The polyaniline that camphorsulfonic acid is adulterated is put into the polyamidoimide m-cresol solution prepared in advance, and adds phase
Hold agent hydroquinones, the polyaniline that camphorsulfonic acid adulterates is homogeneously dispersed in by polyamide acyl by high speed emulsification and ultrasonic vibration
In imide liquor；Then polyamidoimide/polyaniline multifunctional composite is prepared by solvent cast method.
2. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
The mol ratio of aniline, ammonium persulfate and hydrochloric acid is 1 in wherein step (1):1:0.2.
3. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
The mass ratio of polyaniline and ammoniacal liquor is 1 in wherein step (2):20.
4. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
The mass ratio of polyaniline and camphorsulfonic acid is 1 in wherein step (2):1.5.
5. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
The content for the polyaniline that camphorsulfonic acid adulterates is polyamidoimide/polyaniline composite material gross mass in wherein step (3)
10%-40%.
6. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
The content of hydroquinones is the 0.5%-2% of polyamidoimide/polyaniline composite material gross mass in wherein step (3).
7. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
It is as follows in the structural formula of the polyaniline of wherein affiliated camphorsulfonic acid doping：
Wherein 0<y<1
Wherein 10<n<200.
8. the preparation method of multi-functional polyamidoimide/polyaniline composite material according to claim 1, its feature exists
It is shown below in the structural formula of wherein described polyamide-imide resin：
Wherein 10<n<200.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109096756A (en) * | 2018-07-01 | 2018-12-28 | 常州大学 | Polyaniline-polyamidoimide single-sided conductive nano compound film preparation method and application |
| CN109134894A (en) * | 2018-07-01 | 2019-01-04 | 常州大学 | The preparation method of the bilayer film of hydrophilic insulation while hydrophobic conductive |
| CN109135279A (en) * | 2018-07-11 | 2019-01-04 | 常州大学 | A kind of preparation method based on polyamidoimide high-strength high-conductivity film |
| CN113355107A (en) * | 2021-07-05 | 2021-09-07 | 合肥中聚合臣电子材料有限公司 | Liquid crystal orientation agent |
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| CN109135279A (en) * | 2018-07-11 | 2019-01-04 | 常州大学 | A kind of preparation method based on polyamidoimide high-strength high-conductivity film |
| CN113355107A (en) * | 2021-07-05 | 2021-09-07 | 合肥中聚合臣电子材料有限公司 | Liquid crystal orientation agent |
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