CN109096756A - Polyaniline-polyamidoimide single-sided conductive nano compound film preparation method and application - Google Patents
Polyaniline-polyamidoimide single-sided conductive nano compound film preparation method and application Download PDFInfo
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- CN109096756A CN109096756A CN201810705058.4A CN201810705058A CN109096756A CN 109096756 A CN109096756 A CN 109096756A CN 201810705058 A CN201810705058 A CN 201810705058A CN 109096756 A CN109096756 A CN 109096756A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
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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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Abstract
The invention belongs to the preparation technical fields of polymer modification and nanocomposite, disclose a kind of high-intensitive, high-modulus single-sided conductive film and preparation method thereof based on polyamidoimide.Single-sided conductive method for manufacturing thin film of the invention are as follows: synthesizing soluble polyaniline (polyortho methylaniline and Polyanisidine) first is doped to obtain fusible conductive polyaniline with organic acid (p-methyl benzenesulfonic acid) afterwards.Then, fusible conductive polyaniline is cast in polyamidoimide upper surface and prepares polyaniline-polyamidoimide single-sided conductive laminated film.Polyaniline provided by the invention-polyamidoimide single-sided conductive laminated film conductivity with higher and mechanical property, may be used as electric contact material.
Description
Technical field
The invention belongs to the preparation technical fields of nanocomposite, and in particular to a kind of polyaniline-polyamidoimide
The preparation method and application of single-sided conductive nano compound film.
Background technique
Conductive metal material is oxidizable under high temperature, wet environment, be easy to cause overheat and open circuit, influences electronic product portion
The service life of part simultaneously causes safety accident；And metal product heavier mass, price is more expensive, and resource is limited.As society rapidly develops,
Single conductive metal material is no longer satisfied the high request of high-precision end industry, and more and more electrically conductive height polymerize
Object material is found.Macromolecule conducting material have been widely used space flight and aviation, communications and transportation, medical treatment and industrial equipment, automobile,
In household electrical appliances, electronic market.Wherein electrically conductive polyaniline has a stable chemical property, not oxidizable, high-low temperature resistant, electric conductivity is high,
The advantages that easy processing.
Most representative in electric contact material at present is Cu-W alloy and Ag base slider material (AgSnO2、AgCdO、Ag-
W system etc.) two major class.Since W, Ag etc. belong to noble metal, resource reserve is limited, and such noble metal is used to make as raw material
The cost of electric contact material is prohibitively expensive, is unfavorable for promoting and applying.In addition, such slider material wear-resisting property is poor, it is difficult to use
On sliding contact.
Summary of the invention
The present invention uses soluble polyaniline (polyortho methylaniline or Polyanisidine) for conductive material, polyamide
Acid imide is that flexible high-intensity high-modulus mechanics material prepares single-sided conductive laminated film, to reduce cost and avoid the occurrence of gold
Belong to the problems such as contact resistance occurred in material electric contact use process increases.Wherein soluble polyaniline chemical property is stablized,
Not oxidizable, light weight, good conductivity, it is cheap.Polyamidoimide is flexible material, can be bonded any surface, and
High strength and modulus.The two is combined and prepares polyaniline-polyamidoimide single-sided conductive nano compound film by the present invention, can be with
It is used to prepare not oxidizable, any surface, the key electric contact material of light weight can be bonded.
Polyaniline provided by the invention-polyamidoimide single-sided conductive nano compound film is by nonconducting polyamide
The acid imide double layer material compound with conductive polyaniline.
Polyaniline provided by the invention-polyamidoimide single-sided conductive nano compound film preparation method, under
State step progress:
(1) selection of polyamidoimide
The polyamidoimide material of selection high intensity, high-modulus.
(2) preparation of polyaniline
It respectively by the o-toluidine newly distilled or o-aminoanisole, is added in the hydrochloric acid solution of 0.2mol/L, in 0-5
After stirring 0.5-2h at DEG C, it is slowly dropped in the aqueous solution of ammonium persulfate with the speed of the every drop of 1-3s, in 0-5 DEG C of reaction 6-
10h；Reaction solution filters to obtain green solid, uses methanol, n-hexane, chloroform Soxhlet extraction respectively later, and chloroform is taken to dissolve part；
60 DEG C of vacuum drying 12h obtain the polyortho methylaniline (POT) or Polyanisidine (POMA) of doped hydrochloride, i.e., solvable
Property polyaniline, their character is green powder.
(3) preparation of the fusible conductive polyaniline of p-methyl benzenesulfonic acid doping
Soluble polyaniline powder is added in the ammonium hydroxide that mass concentration is 10%, then stirring at normal temperature 12-16h is used
It is washed to neutrality, 60 DEG C of vacuum drying 12h obtain the soluble polyaniline of eigenstate, and character is purple powder.Then it uses
Solution blending obtains the soluble polyaniline of p-methyl benzenesulfonic acid doping, i.e., grinds p-methyl benzenesulfonic acid (TSA), eigenstate is added
Metacresol is added in soluble polyaniline, and continues to stir 60min at 90 DEG C, is finally dried to obtain at 90 DEG C to toluene sulphur
The fusible conductive polyaniline of acid doping.
(4) soluble polyaniline-polyamidoimide single-sided conductive nano compound film preparation
The fusible conductive polyaniline of p-methyl benzenesulfonic acid doping and chloroform are prepared to be poured into after solution and pre-selected
Then polyamidoimide upper surface dries at 80-95 DEG C and soluble polyaniline-polyamidoimide single-sided conductive nanometer is made
Laminated film.
Wherein, step (1) polyamidoimide is flexible material, can be bonded arbitrary surfaces；It is described high-intensitive high
The polyamide imide of modulus is with a thickness of 0.2mm.The structural formula of polyamide-imide resin is shown below:
Wherein, 10 < n < 200.
The molar ratio of step (2) o-toluidine or o-aminoanisole and ammonium persulfate is 1:1；Polyphenyl obtained
Amine chemical property is stablized, not oxidizable, light weight, good conductivity.
The soluble polyaniline of the doping of p-methyl benzenesulfonic acid described in step (3) is polyortho methylaniline (POT-TSA) or gathers
The structural formula of o-aminoanisole (POMA-TSA) is as follows.
Wherein, 0 < y < 1；Wherein 10 < n.
The mass ratio of soluble polyaniline described in step (3) and ammonium hydroxide is 1:20.
Soluble polyaniline described in step (3) and the mass ratio of p-methyl benzenesulfonic acid doping are 1:0.8-1:2.
The present invention also provides the application of polyaniline obtained-polyamidoimide single-sided conductive nano compound film, systems
Polyaniline-polyamidoimide single-sided conductive the nano compound film obtained is used as electric contact material.
The utility model has the advantages that
The polyamidoimide that the present invention selects is flexible high-intensity high-modulus mechanics material, and processing is facilitated to be die cut, can be with
It is attached at any surface and curved surface；Using the feature that the materials chemistry property is stable, can make at relatively high temperatures for a long time
With；The light weight of the material has higher conductivity, can be used as the electric contact material being used for a long time under higher temperature.
The polyaniline of preparation-polyamidoimide single-sided conductive nano compound film is applied to wherein polyaniline when electric contact
Conductive layer energy high temperature resistant and good in oxidation resistance, it is possible to reduce the formation of oxide layer reduces total contact resistance, reduces in use process
Fever, increase the reliability and service life of electric contact material.
Detailed description of the invention
Fig. 1 is soluble polyaniline-polyamidoimide single-sided conductive nano compound film schematic diagram.
Specific 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.
The structural formula of selected polyamide-imide resin (PAI-AU) is as follows:
The following institute of structural formula of selected polyortho methylaniline (POT-TSA) or Polyanisidine (POMA-TSA)
Show:
Embodiment 1
(1) selection of polyamidoimide
The polyamidoimide material of selection high intensity, high-modulus；
(2) preparation of polyaniline
The o-toluidine that will newly distill respectively, is added in the hydrochloric acid solution of 0.2mol/L, after stirring 2h at 0 DEG C, with
The speed of the every drop of 1-3s is slowly added dropwise in the aqueous solution of ammonium persulfate, in 0 DEG C of reaction 10h；The green that reaction solution filters is solid
Body uses methanol, n-hexane, chloroform Soxhlet extraction respectively, and chloroform is taken to dissolve part, and 60 DEG C of vacuum drying 12h obtain doped hydrochloride
Polyortho methylaniline (POT)；
(3) preparation of fusible conductive polyaniline (soluble polyaniline and organic acid doped)
Soluble polyaniline powder is added in 10% ammonium hydroxide, stirring at normal temperature 12h, is then washed with water to neutrality, 60
DEG C vacuum drying 12h, obtains the soluble polyaniline of eigenstate, character is purple powder.Use solution blending by poly- neighbour afterwards
Methylaniline and p-methyl benzenesulfonic acid 1:0.8 in mass ratio adulterate to obtain soluble polyaniline, i.e., first grind p-methyl benzenesulfonic acid (TSA)
The soluble polyaniline of eigenstate is added in mill later, and metacresol is added, and continues to stir 60min at 90 DEG C, finally at 90 DEG C
Under be dried to obtain p-methyl benzenesulfonic acid doping fusible conductive polyaniline；
(4) soluble polyaniline-polyamidoimide single-sided conductive nano compound film preparation
The fusible conductive polyaniline that p-methyl benzenesulfonic acid adulterates is dissolved in chloroformic solution, prepares the solution of 10mg/ml, is stirred
It is poured on the polyamidoimide film of 0.2mm thickness and dries after 12h, obtain conductive polyaniline with a thickness of 0.02mm.It is soluble
Polyaniline-polyamidoimide single-sided conductive nano compound film conductivity is 3.02S/m；Its tensile strength is 63.5MPa,
Young's modulus is 1.9GPa.
Embodiment 2
The present embodiment is the difference from embodiment 1 is that soluble polyaniline-polyamidoimide single-sided conductive is nano combined
Polyortho methylaniline and p-methyl benzenesulfonic acid 1:1.1 in mass ratio in the preparation step of film, other processing means with embodiment 1
Unanimously, conductive polyaniline is obtained with a thickness of 0.02mm.Soluble polyaniline-polyamidoimide single-sided conductive is nano combined thin
The conductivity of film is 2.51S/m；Its tensile strength intensity is 59.6MPa, Young's modulus 1.7GPa.
Embodiment 3
The present embodiment is the difference from embodiment 1 is that soluble polyaniline-polyamidoimide single-sided conductive is nano combined
Polyortho methylaniline and p-methyl benzenesulfonic acid 1:0.9 in mass ratio and it is dissolved in chloroformic solution in the preparation step of film, configured
The solution of 40mg/ml, other processing means are consistent with embodiment 1, obtain conductive polyaniline with a thickness of 0.03mm.It is soluble
Polyaniline-polyamidoimide single-sided conductive nano compound film conductivity is 5.10S/m；Its tensile strength is 58.4MPa,
Young's modulus is 1.6GPa.
Embodiment 4
The present embodiment is the difference from embodiment 1 is that soluble polyaniline-polyamidoimide single-sided conductive is nano combined
Polyortho methylaniline is substituted for Polyanisidine in the preparation step of film, other processing means with embodiment 1 one
It causes, obtains conductive polyaniline with a thickness of 0.02mm.Soluble polyaniline-polyamidoimide single-sided conductive nano compound film
Conductivity be 72.02S/m；Its tensile strength is 62.1MPa, Young's modulus 1.8GPa.
Embodiment 5
The present embodiment is the difference from embodiment 1 is that soluble polyaniline-polyamidoimide single-sided conductive is nano combined
Polyortho methylaniline is substituted for Polyanisidine in the preparation step of film and is dissolved in chloroformic solution, configures 40mg/
The solution of ml, other processing means are consistent with embodiment 1, obtain conductive polyaniline with a thickness of 0.03mm.Soluble polyphenylene
Amine-polyamidoimide single-sided conductive nano compound film conductivity is 103.22S/m；Its tensile strength is 58.1MPa, poplar
Family name's modulus is 1.3GPa.
As can be known from Table 1: the material that embodiment 4 and embodiment 5 obtain is relative to 1~embodiment of embodiment 3, conductivity
It is very high, and resistance is very low, illustrates that the conductivity for the laminated film conductive layer that the present invention obtains can control.
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 |
| Conductivity (S/m) | 3.02 | 2.51 | 5.10 | 72.02 | 103.22 |
| Resistivity (Ω m) | 3.31×10-1 | 3.98×10-1 | 1.96×10-1 | 1.39×10-2 | 9.69×10-3 |
| Tensile strength (MPa) | 63.5 | 59.6 | 58.4 | 62.1 | 58.1 |
| Young's modulus (GPa) | 1.9 | 1.7 | 1.6 | 1.8 | 1.3 |
The various embodiments described above are merely to illustrate the present invention, wherein the parameter of each step, implementation condition etc. is all can be
Variation, all equivalent variationss and improvement carried out based on the technical solution of the present invention should not be excluded of the invention
Except protection scope.
In conclusion the polyamideimide-based single-sided conductive composite material that the present invention is shown, has excellent conduction
Performance and mechanical strength, can be applied to electric contact material.
Claims (8)
1. a kind of polyaniline-polyamidoimide single-sided conductive nano compound film, it is characterised in that: the single-sided conductive nanometer
Laminated film is the double layer material compound by nonconducting polyamide imide and conductive polyaniline.
2. a kind of polyaniline according to claim 1-polyamidoimide single-sided conductive nano compound film preparation side
Method, it is characterised in that: the preparation method includes the following steps:
(1) selection of polyamidoimide
The polyamidoimide material of selection high intensity, high-modulus；
(2) preparation of polyaniline
It respectively by the o-toluidine newly distilled or o-aminoanisole, is added in the hydrochloric acid solution of 0.2mol/L, at 0-5 DEG C
After stirring 0.5-2h, it is slowly dropped in the aqueous solution of ammonium persulfate with the speed of the every drop of 1-3s, in 0-5 DEG C of reaction 6-10h；Instead
The green solid for answering liquid to filter uses methanol, n-hexane, chloroform Soxhlet extraction respectively, and chloroform is taken to dissolve part, 60 DEG C of vacuum
Dry 12h, obtains the polyortho methylaniline or Polyanisidine of doped hydrochloride, i.e., soluble polyaniline powder；
(3) preparation of the fusible conductive polyaniline of p-methyl benzenesulfonic acid doping
Soluble polyaniline powder is added in 10% ammonium hydroxide, stirring at normal temperature 12-16h, is then washed with water to neutrality, 60 DEG C
It is dried in vacuo 12h, obtains the soluble polyaniline of eigenstate；Then p-methyl benzenesulfonic acid is ground, later be added eigenstate can
Metacresol is added in dissolubility polyaniline, and continues to stir 60min at 50 DEG C, is finally dried to obtain p-methyl benzenesulfonic acid at 90 DEG C
The fusible conductive polyaniline of doping；
(4) soluble polyaniline-polyamidoimide single-sided conductive nano compound film preparation
It is configured to fusible conductive polyaniline and the chloroform of p-methyl benzenesulfonic acid doping to be poured into step (1) after solution selected
Then polyamidoimide upper surface dries and soluble polyaniline-polyamidoimide single-sided conductive nano compound film is made.
3. polyaniline according to claim 2-polyamidoimide single-sided conductive nano compound film preparation method,
Be characterized in that: polyamidoimide described in step (1) is the flexible material with a thickness of 0.2mm, and structural formula is shown below:
Wherein 10 < n < 200.
4. polyaniline according to claim 2-polyamidoimide single-sided conductive nano compound film preparation method,
Be characterized in that: the molar ratio of o-toluidine or o-aminoanisole and ammonium persulfate is 1:1 in step (2).
5. polyaniline according to claim 2-polyamidoimide single-sided conductive nano compound film preparation method,
Be characterized in that: the mass ratio of soluble polyaniline and ammonium hydroxide is 1:20 in step (3).
6. polyaniline according to claim 2-polyamidoimide single-sided conductive nano compound film preparation method,
Be characterized in that: soluble polyaniline and the mass ratio of p-methyl benzenesulfonic acid doping are 1:0.8-1:2 in step (3).
7. polyaniline according to claim 2-polyamidoimide single-sided conductive nano compound film preparation method,
Be characterized in that: the fusible conductive polyaniline layer being poured in step (4) with a thickness of 0.02-0.03mm.
8. a kind of application of polyaniline according to claim 1-polyamidoimide single-sided conductive nano compound film,
Be characterized in that: the polyaniline-polyamidoimide single-sided conductive nano compound film is used as electric contact material.
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