CN109535463A - A kind of preparation method of TPU conductive film - Google Patents
A kind of preparation method of TPU conductive film Download PDFInfo
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- CN109535463A CN109535463A CN201811284659.9A CN201811284659A CN109535463A CN 109535463 A CN109535463 A CN 109535463A CN 201811284659 A CN201811284659 A CN 201811284659A CN 109535463 A CN109535463 A CN 109535463A
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/02—Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention discloses a kind of preparation methods of TPU conductive film, and using TPU as raw material, TPU film is made by hot extrusion briquetting technique；It is suitably swollen in xylene solvent；By the TPU film being moderately swollen, the ultrasound modification in the xylene solution of the functionalized multi-wall carbonnanotubes of different quality concentration, prepares the TPU conductive film of different conductive capabilities.The present invention is using carboxylic carbon nano-tube mitron as modifying agent, carbon nanotube has-COOH, and-OH isoreactivity functional group can form intermolecular hydrogen bonding with TPU polymeric matrix, active force between enhancing and TPU polymeric matrix, is conducive to the improvement of conductive network structure constructed with mechanical property.Make TPU film that appropriateness occur in a solvent at a suitable temperature to be swollen, so that cMWCNTs is not only uniformly modified in TPU membrane surface, and penetrates into film, be conducive to the formation and stabilization of conductive network, significantly improve the electric conductivity of TPU conductive film.
Description
Technical field
The present invention relates to field of material preparation, and in particular to a kind of preparation method of TPU conductive film.
Background technique
Conductive polymer material is achieving rapid development in the past few decades, obtains extensively in industries such as automobile, printing, electric appliances
General application.Conductive polymer material is broadly divided into conductive polymeric composite and structural conductive macromolecular material.It is compound
Type conductive polymer material will be by that will have compound (dispersion, the lamination or filling) system of the substance of conductive capability and high molecular material
, there are the advantages such as easy to form, at low cost.Currently, the preparation method of conductive polymeric composite mainly includes original position
Polymerization, melt-blending process, solution blending casting, ultrasonic vibration method etc..Ultrasonic vibration method makes conduction using high-energy ultrasound
Uniform particle is scattered in polymeric matrix, simple process, easy to operate.
Thermoplastic polyurethane (TPU) has the good characteristics such as hardness range is wide, high mechanical strength, processing performance are good, in electricity
It is used widely in the fields such as son, automobile, bulletproof glass.Multi-walled carbon nanotube (MWCNTs) has excellent electrical property, hot
Can, mechanical property, being widely used in preparation as ideal filler has superior electrical conductivity energy, thermal stability, mechanical performance
Composite material.Importantly, it is with excellent flexibility, sheared, the external forces such as ultrasound when performance it is not easily damaged.
Functionalized multi-wall carbonnanotubes (cMWCNTs) have-COOH ,-OH isoreactivity functional group can be poly- with polarity compared with MWCNTs
Close object matrix and form intermolecular hydrogen bonding, the active force between enhancing polymeric matrix, be conducive to conductive network structure construct and
The improvement of mechanical property.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of preparation methods of TPU conductive film, with TPU
For primary raw material, TPU film is prepared by hot extrusion briquetting technique, appropriateness swelling occurs in the xylene solvent of certain temperature,
And the ultrasound modification preparation TPU conductive film in the xylene solution of various concentration cMWCNTs.TPU produced by the present invention is conductive
Film not only has excellent electrical property and lower excess effusion value, and thermal stability and mechanical property are also changed compared with TPU membrane
It is kind.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of preparation method of TPU conductive film, steps are as follows:
(1) with thermoplastic polyurethane (TPU) for raw material, using vacuum hot pressing formation technology for TPU film；
(2) functionalized multi-wall carbonnanotubes of certain mass (cMWCNTs) are added in xylene solvent, preparation mixing is molten
Mixed solution is put into ultrasonic washing instrument by liquid, ultrasonic vibration 30-40 minutes in 70-80 DEG C of water-bath, obtains dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 75-85oThe dimethylbenzene of C
It is swollen 30-40 minutes in solvent, so that TPU film is moderately swollen；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue and taken out after ultrasonic vibration 20-40 minutes in 70-80 DEG C of water-bath, washed with dehydrated alcohol, naturally dry obtains different conductions
The TPU conductive film of ability.
The technical process of vacuum hotpressing preparation TPU film is as follows in the step (1): using the mould of the cm size of 5 cm × 5
Tool, by the hot-forming preparation TPU film of TPU pellet.Hot-forming includes two stages of precompressed and hot pressing: in 180-200oC is pre-
After 5 min of heat, the precompressed 1-3 min under 1300-1500 kg pressure；The hot pressing 3-5 min under 1600-1800 kg pressure.
TPU conductive film with a thickness of 0.02-1 mm in the step (1).
The concentration of dispersion liquid is 0.05-0.30 mg/mL in the step (2).
The degree that TPU film is swollen in the step (3) increases 15-20% as standard using TPU film length.
The beneficial effects of the present invention are: (1) present invention conducts a research by raw material of thermoplastic polyurethane, with polyaniline, poly-
The intrinsic conducting polymers such as thiophene, polypyrrole are compared, at low cost, easily processed into type, applied widely；(2) present invention utilizes
Carboxylic carbon nano-tube mitron (cMWCNTs) is used as modifying agent, and carbon nanotube has-COOH, and-OH isoreactivity functional group can be with
TPU polymeric matrix forms intermolecular hydrogen bonding, and the active force between enhancing and TPU polymeric matrix is conducive to conductive network structure
The improvement constructed with mechanical property；(3) make TPU film that appropriateness occur in a solvent at a suitable temperature to be swollen, so that
CMWCNTs is not only uniformly modified in TPU membrane surface, and is penetrated into film, is conducive to the formation and stabilization of conductive network, significantly
Improve the electric conductivity of TPU conductive film；(4) when conductive modification, TPU film carries out in the xylene solution of cMWCNTs
Temperature when ultrasound modification is lower than the temperature of TPU film swelling, has not only guaranteed that TPU film kept the state of swelling, but also will not destroy
The surface texture of TPU film.
Detailed description of the invention
Fig. 1 is the SEM figure of TPU conductive film prepared by embodiment 1；
Fig. 2 is the resistivity curve of TPU conductive film prepared by embodiment 1；
Fig. 3 is the load-deformation curve of TPU conductive film prepared by embodiment 1.
Specific embodiment
Below with reference to the embodiment of the present invention, technical solution of the present invention is clearly and completely described.Obviously, it is retouched
The embodiment stated is only a part of the embodiment of the present invention, instead of all the embodiments.Based on implementation disclosed in this invention
Example, those of ordinary skill in the art can carry out partial modification or equivalent replacement to technical solution of the present invention, not pay
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
The preparation method of the present embodiment TPU conductive film, steps are as follows:
(1) with thermoplastic polyurethane (TPU) for raw material, using vacuum hot pressing formation technology for TPU film, hot press forming technology mistake
Journey is as follows: 5 cm × 5 cm × 0.5mm size mold is used, 200oAfter preheating 5 min under C mold temperature, in 1300
2 min of precompressed under kg pressure；5 min of hot pressing under 1600 kg pressure；Prepare TPU film with a thickness of 0.5mm；
(2) claim the cMWCNTs of certain mass in xylene solvent, preparing 50 mL mass concentrations is respectively 0.05 mgmL-1、0.10 mg·mL-1、0.15 mg·mL-1、0.20 mg·mL-1、0.25 mg·mL-1、0.30 mg·mL-1Mixing it is molten
Liquid, in 80o30 min of C ultrasonic disperse, obtains dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 85oThe dimethylbenzene of C is molten
It is swollen 30 minutes in agent, so that TPU film is moderately swollen, the length of film is increased to original 20%；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue and taken out after ultrasonic vibration 30 minutes in 80 DEG C of water-baths, washed with dehydrated alcohol, naturally dry obtains different conductive capabilities
TPU conductive film.For simplicity, the corresponding TPU conductive film of various concentration carbon nanotube is represented with x-TPU.
The scanning electron microscope diagram of TPU conductive film manufactured in the present embodiment is as shown in Figure 1.As seen from the figure, when
When cMWCNTs concentration is lower, the surface TPU film (Fig. 1 a) smoother, cMWCNTs is evenly dispersed in film surface, but still
Not formed conductive network, TPU film are non-conductive.(>=0.10 mgmL when carbon nanotube concentration is higher-1), TPU film surface
It is obvious roughening, increase with cMWCNTs concentration, film surface degree of roughness is also higher and higher.At this point, cMWCNTs is uniformly modified
Conductive network structure is constituted in TPU film surface.When cMWCNTs concentration increases to 0.25 mgmL-1With 0.30 mgmL-1
When, occur a small amount of reunion in TPU laminated film, but the size reunited is smaller (< 1 μm).Illustrate to utilize ultrasound modification
Method can avoid the reunion of carbon nanotube, promote carbon nanotube in the uniform modification on TPU membrane surface.In addition, can be clear by SEM figure
It observes to Chu, carbon nanotube is not only uniformly modified in TPU membrane surface, but also is penetrated into film, is conducive to construct stable
Conductive network structure enhances the interface binding power between carbon nanotube and TPU matrix.
Fig. 2 is the resistivity curve of TPU conductive film.As seen from the figure, increase with cMWCNTs concentration, the electricity of TPU conductive film
Resistance rate reduces, and conductive capability improves.When cMWCNTs mass concentration is 0.05 mgmL-1When, resistivity is 2972.5 Ω m,
Film is non-conductive.When cMWCNTs concentration is 0.10 mgmL-1When, cMWCNTs is uniformly modified in film surface and is formed conductive network,
The resistivity bust of TPU film is 206.3 Ω m.It is continued growing with cMWCNTs concentration, resistivity reduces slow.cMWCNTs
Concentration be respectively 0.20 mgmL-1、0.25 mg·mL-1With 0.30 mgmL-1When, resistivity is reduced to 48.9 respectively
Ω m, 53.6 Ω m and 45.4 Ω m.Compared with result reported in the literature, the TPU conductive film of this research preparation
Excess effusion value significantly reduces.
Fig. 3 is the load-deformation curve of TPU conductive film.As seen from the figure: compared with TPU membrane, the drawing of TPU conductive film
It stretches intensity and Young's modulus is significantly improved, and increase with the increase of cMWCNTs concentration.Wherein, 0.20-TPU film
Tensile strength increases 40.2 % compared with TPU membrane, and Young's modulus increases 22.6 %.Since cMWCNTs has excellent power
Performance is learned, specific strength and specific modulus are higher, the evenly dispersed film stretching intensity and modulus of being conducive in TPU conductive composite film
Increase.In addition, reduced stress-strain curve surround the area is it is found that low cMWCNTs concentration (0.05 mgmL-1) TPU conductive thin
The area that membrane stress-strain curve surrounds is almost unchanged.When cMWCNTs concentration is higher, TPU conductive film stress-strain is bent
The area that line surrounds is noticeably greater than TPU membrane, and toughness improves.This is because when cMWCNTs concentration is higher, carbon nanometer after ultrasound modification
Pipe is not only dispersed in TPU membrane surface, but also penetrates into and form stable conductive network structure inside film, is conducive to
Interface binding power enhances between cMWCNTs and TPU matrix, promotes stress transfer.
Embodiment 2
The preparation method of the present embodiment TPU conductive film, steps are as follows:
(1) with thermoplastic polyurethane (TPU) for raw material, using vacuum hot pressing formation technology for TPU film, hot press forming technology mistake
Journey is as follows: 5 cm × 5 cm × 1mm size mold is used, 200oAfter preheating 5 min under C mold temperature, in 1300 kg
3 min of precompressed under pressure；5 min of hot pressing under 1600 kg pressure, prepare TPU film with a thickness of 1mm；
(2) claim the cMWCNTs of certain mass in xylene solvent, preparing 50 mL mass concentrations is respectively 0.07 mgmL-1、0.12 mg·mL-1、0.17 mg·mL-1、0.22 mg·mL-1、0.27 mg·mL-1Mixed solution, in 70oC ultrasound
Disperse 30 min, obtains dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 75oThe dimethylbenzene of C is molten
It is swollen 30 minutes in agent, so that TPU film is moderately swollen, the length of film is increased to original 15%；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue and taken out after ultrasonic vibration 30 minutes in 70 DEG C of water-baths, washed with dehydrated alcohol, naturally dry obtains different conductive capabilities
TPU conductive film.
Embodiment 3
The preparation method of the present embodiment TPU conductive film, steps are as follows:
(1) with thermoplastic polyurethane (TPU) for raw material, using vacuum hot pressing formation technology for TPU film, hot press forming technology mistake
Journey is as follows: 5 cm × 5 cm × 0.02mm size mold is used, 180oAfter preheating 5 min under C mold temperature, in 1300
1 min of precompressed under kg pressure；The hot pressing 3min under 1600 kg pressure, prepare TPU film with a thickness of 0.02 mm；
(2) claim the cMWCNTs of certain mass in xylene solvent, preparing 50 mL mass concentrations is respectively 0.05mgmL-1、
0.075 mg·mL-1、0.10 mg·mL-1、0.125mg·mL-1Mixed solution, in 70o30 min of C ultrasonic disperse, obtains
Dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 75oThe dimethylbenzene of C is molten
It is swollen 30 minutes in agent, so that TPU film is moderately swollen；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue the ultrasonic vibration in 70 DEG C of water-baths to take out after twenty minutes, be washed with dehydrated alcohol, naturally dry obtains different conductive capabilities
TPU conductive film.
Embodiment 4
The preparation method of the present embodiment TPU conductive film, steps are as follows:
(1) with thermoplastic polyurethane (TPU) for raw material, using vacuum hot pressing formation technology for TPU film, hot press forming technology mistake
Journey is as follows: 5 cm × 5 cm × 1mm size mold is used, 200oAfter preheating 5 min under C mold temperature, in 1300 kg
2 min of precompressed under pressure；5 min of hot pressing under 1600 kg pressure, prepare TPU film with a thickness of 1mm；
(2) claim the cMWCNTs of certain mass in xylene solvent, preparing 50 mL mass concentrations is respectively 0.07 mgmL-1、0.12 mg·mL-1、0.17 mg·mL-1、0.22 mg·mL-1、0.27 mg·mL-1Mixed solution, in 80oC ultrasound
Disperse 40 min, obtains dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 85oThe dimethylbenzene of C is molten
It is swollen 40 minutes in agent, so that TPU film is moderately swollen；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue the ultrasonic vibration in 80 DEG C of water-baths to take out after forty minutes, be washed with dehydrated alcohol, naturally dry obtains different conductive capabilities
TPU conductive film.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of preparation method of TPU conductive film, it is characterised in that steps are as follows:
(1) using thermoplastic polyurethane as raw material, using vacuum hot pressing formation technology for TPU film；
(2) functionalized multi-wall carbonnanotubes of certain mass are added in xylene solvent, prepare mixed solution, will mixed molten
Liquid is put into ultrasonic washing instrument, ultrasonic vibration 30-40 minutes in 70-80 DEG C of water-bath, obtains dispersion liquid；
(3) batten that the TPU film prepared in step (1) is cut into the cm size of 5 cm × 1 is placed in 75-85oThe dimethylbenzene of C
It is swollen 30-40 minutes in solvent, so that TPU film is moderately swollen；
(4) TPU film for occurring moderately to be swollen in step (3) is taken out, is immediately placed in the dispersion liquid that step (2) obtains, after
Continue and taken out after ultrasonic vibration 20-40 minutes in 70-80 DEG C of water-bath, washed with dehydrated alcohol, naturally dry obtains different conductions
The TPU conductive film of ability.
2. the preparation method of TPU conductive film according to claim 1, it is characterised in that: Vacuum Heat in the step (1)
The technical process for suppressing standby TPU film is as follows: the mold of the cm size of 5 cm × 5 is used, by the hot-forming preparation TPU of TPU pellet
Film, hot-forming includes two stages of precompressed and hot pressing: in 180-200oAfter C preheats 5 min, pressed in 1300-1500 kg
Precompressed 1-3 min under power；The hot pressing 3-5 min under 1600-1800 kg pressure.
3. the preparation method of TPU conductive film according to claim 1, it is characterised in that: TPU is thin in the step (1)
Film with a thickness of 0.02-1 mm.
4. the preparation method of TPU conductive film according to claim 1, it is characterised in that: dispersion liquid in the step (2)
Concentration be 0.05-0.30 mg/mL.
5. the preparation method of TPU conductive film according to claim 1, it is characterised in that: TPU is thin in the step (3)
The degree that film is swollen increases 15-20% as standard using TPU film length.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600197A (en) * | 2019-09-19 | 2019-12-20 | 浙江佳阳塑胶新材料有限公司 | Preparation method of TPU conductive film |
| CN112111145A (en) * | 2020-08-21 | 2020-12-22 | 东莞市雄林新材料科技股份有限公司 | Conductive TPU film and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600197A (en) * | 2019-09-19 | 2019-12-20 | 浙江佳阳塑胶新材料有限公司 | Preparation method of TPU conductive film |
| CN112111145A (en) * | 2020-08-21 | 2020-12-22 | 东莞市雄林新材料科技股份有限公司 | Conductive TPU film and preparation method thereof |
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Application publication date: 20190329 |