CN110343270A - A kind of preparation method of carbon nanotube anti-static material, slurry and film and film - Google Patents
A kind of preparation method of carbon nanotube anti-static material, slurry and film and film Download PDFInfo
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- CN110343270A CN110343270A CN201910602470.8A CN201910602470A CN110343270A CN 110343270 A CN110343270 A CN 110343270A CN 201910602470 A CN201910602470 A CN 201910602470A CN 110343270 A CN110343270 A CN 110343270A
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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
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
Abstract
The invention belongs to antistatic film technical fields, more particularly to a kind of carbon nanotube anti-static film and preparation method thereof, it include: carbon nanotube, resin and the solvent for obtaining pipe range and being 100~500 microns, the carbon nanotube, the resin and the solvent are uniformly mixed, carbon nanotube resin mixture is obtained；Roll-type milled processed is carried out to the carbon nanotube resin mixture, obtains grinding product；Curing agent and the solvent are obtained, the curing agent and the solvent are added in the grinding product, is configured to the carbon nanotube anti-static slurry that solid content is 70~85%；Carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry.Preparation process of the present invention can be such that long-chain carbon nanotube is evenly dispersed in slurry, without additionally adding dispersing agent, avoid influence of the dispersing agent to adhesion of thin film and surface resistivity, and the preparation method simple process, be suitable for industrialized production.
Description
Technical field
The invention belongs to antistatic film technical field more particularly to a kind of carbon nanotube anti-static film and its preparation sides
Method and a kind of carbon nanotube anti-static material, a kind of carbon nanotube anti-static slurry.
Background technique
With the development of science and technology current a large amount of high molecular material continues to bring out, the high score in people's production and life
Sub- material product is widely used in above many articles for daily use, such as varieties of food items packaging, electronic device etc., thus greatly
Improve people's production and life quality.It is conductive but since most macromolecule membranes have excellent insulation performance
Property it is very poor, it is quiet during production and transportation since the electrostatic charge that friction generates can not exclude in time and cause the accumulation of charge
The tired harm of electrodeposition is also increasingly prominent.The dust of Electrostatic Absorption includes many bacteriums and virus, is caused damages to people's health；Together
When static discharge abrupt release go out huge energy, static discharge can generate explosion and fire, can generate to electronic device accumulative
Injury until device failure.Therefore, to avoid harm caused by charge accumulated, have to the development of Antistatic type high molecular products
Great application prospect and the market demand.
Currently, promoting high molecular products antistatic property often by adding the carbon nanometers such as carbon nanotube in high molecular material
Material.But the method for high molecular material electric conductivity is improved there is also more defect by addition carbon nano-tube material at present,
Such as: carbon nanotube disperses unevenly, to be distributed not in high molecular material as antistatic agent in use, can have carbon nanotube
, the antistatic property for influencing high molecular material causes its antistatic effect to decline, and easy to fall off, makes high molecular material
Stability is poor.In order to increase the dispersibility of carbon nanotube, dispersing agent is often added in high molecular material, but dispersing agent meeting
Influence adhesion of thin film and surface resistivity.For the antistatic property for preferably improving high molecular material, generally require to add
More carbon nanotube, influences the light transmittance of high molecular material, also will appear a large amount of stains, and limit high molecular material applies model
It encloses.
Summary of the invention
Problems to be solved by the invention
The preparation method for being designed to provide a kind of carbon nanotube anti-static film of the embodiment of the present invention, it is intended to solve existing
There is the method dispersion effect for preparing carbon nanotube anti-static film bad, generally require addition dispersing agent, electric conductivity is bad etc.
Technical problem.
A further object of the embodiment of the present invention is to provide a kind of carbon nanotube anti-static slurry.
The another object of the embodiment of the present invention is to provide a kind of carbon nanotube anti-static film.
The means solved the problems, such as
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of preparation method of carbon nanotube anti-static film, comprising the following steps:
Obtaining pipe range is 100~500 microns of carbon nanotube, resin and solvent, by the carbon nanotube, the resin and
The solvent is uniformly mixed, and obtains carbon nanotube resin mixture；
Roll-type milled processed is carried out to the carbon nanotube resin mixture, obtains grinding product；
Curing agent is obtained, the curing agent is added in the grinding product, being configured to solid content is 70~85%
Carbon nanotube anti-static slurry；
Carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry.
Preferably, the mass ratio of the carbon nanotube, the resin and the curing agent is (0.01~0.5): (65~
80): (6~8).
Preferably, include: to the step of carbon nanotube resin mixture progress roll-type milled processed
In the case where roller gap is 20~40 microns, the carbon nanotube resin mixture is carried out at roll-type grinding
Reason 5~10 minutes；Then by the roller gap adjustment be 0 micron roll-type milled processed 5~10 minutes；It again will be between the roller
Gap is adjusted to 5~10 microns of roll-type milled processeds 10~20 minutes.
Preferably, it is configured to the carbon nanotube anti-static slurry that solid content is 70~85%:
The curing agent is added in the grinding product after mixing evenly, Fruit storage is carried out, is obtained described
The carbon nanotube anti-static slurry that solid content is 70~85%.
Preferably, it is configured to the carbon nanotube anti-static slurry that solid content is 70~85%:
Curing agent and the solvent are obtained, the curing agent and the solvent are added in the grinding product and stirred
After even, Fruit storage is carried out, obtains the carbon nanotube anti-static slurry that the solid content is 70~85%.
Preferably, carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry: uses doctor blade process,
In the case that scraper spacing is 50~300 microns, the carbon nanotube anti-static slurry is coated on substrate, is obtained after dry
The carbon nanotube anti-static film.
Preferably, the carbon nanotube is selected from: single-walled carbon nanotube and/or multi-walled carbon nanotube；And/or
The resin is selected from: epoxy resin, acrylic resin, polyurethane, any one in organic siliconresin；And/or
The curing agent is selected from: triethylene tetramine, ethylenediamine, hexamethylene diamine, diethylenetriamine, in diethylaminopropylamine at least
It is a kind of；And/or
The solvent is selected from: at least one of acetone, dimethylbenzene, N-Methyl pyrrolidone；And/or
The substrate is selected from: polyester film, polyethylene film, polyvinyl chloride, a kind of in polypropylene screen.
Correspondingly, a kind of carbon nanotube anti-static material, with the gross mass of the carbon nanotube anti-static material for 100%
Meter, the raw material components including following mass percentage:
The carbon nanotube 0.01~0.5% that pipe range is 100~500 microns,
Resin 65~80%,
Curing agent 6~8%,
Surplus is solvent.
Correspondingly, a kind of carbon nanotube anti-static slurry, the carbon nanotube anti-static slurry include above-mentioned carbon nanotube
Anti-static material, and the solid content of the carbon nanotube anti-static slurry is 70~85%.
Correspondingly, a kind of carbon nanotube anti-static film, the carbon nanotube anti-static film are resisted by above-mentioned carbon nanotube
The preparation method of electrostatic film is made or the carbon nanotube anti-static film is made with above-mentioned carbon nanotube anti-static material
It is prepared for raw material or the carbon nanotube anti-static film is coated with by above-mentioned carbon nanotube anti-static slurry and is made.
Invention effect
The preparation method of carbon nanotube anti-static film provided by the invention, the carbon nanometer for being 100~500 microns with pipe range
Pipe, resin, curing agent and solution are raw material, wherein the long-chain carbon nanotube that pipe range is 100~500 microns, single-root carbon nano-tube
Or carbon nano pipe array has anisotropic electric conductivity, and can to form one layer of electric conductivity each for a small amount of carbon nanotube
To the high-transmittance of the same sex, the carbon nano tube transparent conductive thin-film of low areal resistance, to keep carbon nanotube anti-static obtained thin
Film has excellent electric conductivity, can conduct charge in time, avoid harm caused by charge accumulation.In addition, prepared by the present invention
Carbon nanotube anti-static film in due to pipe range be 100~500 microns carbon nanotube simultaneously there is excellent heat dissipation performance,
Thus carbon nanotube anti-static film prepared by the present invention not only has excellent antistatic property but also has preferable heat dissipation
Effect.The present invention is mixed carbon nanotube, resin, curing agent and each raw material of solution by mixing procedures such as roll-type milled processeds
The uniform organic whole of carbon nanotube anti-static slurry that solid content is 70~85% is formed, the slurry of the solid content has most suitable
Film forming, then carbon nanotube anti-static film is made in slurry.It can make pipe range 100~500 by roll-type milled processed technique
The long-chain carbon nanotube of micron, which is evenly dispersed in slurry, forms equably carbon nanotube anti-static slurry, without additional
Dispersing agent is added, influence of the dispersing agent to adhesion of thin film and surface resistivity, and the preparation method simple process are avoided,
Suitable for industrialized production.
Carbon nanotube anti-static material provided by the invention, the gross mass with the carbon nanotube anti-static material are
100% meter, the carbon nanotube that the pipe range including 0.01~0.5% is 100~500 microns, 65~80% resin, 6~8%
Curing agent and solvent.Since the long-chain carbon for being 100~500 microns containing the pipe range for having conductivity excellent and preferable heat dissipation performance is received
Mitron, making the anti-static material equally has excellent electric conductivity, charge can be conducted in time, caused by avoiding charge accumulation
Harm, good heat dissipation effect, and content of carbon nanotubes is extremely low, material transmissivity is high.
Carbon nanotube anti-static slurry provided by the invention, on the one hand, due to including above-mentioned with excellent electric conductivity
Can, and the carbon nanotube anti-static material that content of carbon nanotubes is extremely low, thus, carbon nanotube anti-static slurry also has excellent
Electric conductivity can conduct charge in time, avoid harm caused by charge accumulation, and slurry light transmittance is good；On the other hand, of the invention
The solid content of carbon nanotube anti-static slurry is 70~85%, has preferable processability, can be directly prepared into antistatic film
Or the antistatic grinding tool of other forms, practicability is wide, convenient for utilizing.
Carbon nanotube anti-static film provided by the invention is due to containing the above-mentioned carbon nanotube anti-static material haveing excellent performance
Material is prepared as raw material, or is made by the coating of above-mentioned carbon nanotube anti-static slurry, or pass through above-mentioned carbon nanotube
The preparation method of antistatic film is made, thus has excellent electric conductivity, can conduct charge in time, avoid charge accumulation
Caused by endanger, good heat dissipation effect, and content of carbon nanotubes is extremely low, film light transmittance is high.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph for the carbon nanotube anti-static film surface that the embodiment of the present invention 6 provides.
Fig. 2 is the scanning electron microscope (SEM) photograph for the carbon nanotube anti-static film sections that the embodiment of the present invention 6 provides.
Fig. 3 is the test of the carbon nanotube anti-static film surface resistivity that the embodiment of the present invention 1~6 provides and light transmittance
Figure.
Specific embodiment
To keep the purpose, technical solution and technical effect of the embodiment of the present invention clearer, below in conjunction with of the invention real
The attached drawing in example is applied, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.In conjunction with the embodiment in the present invention, ordinary skill
Personnel's every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
The embodiment of the invention provides a kind of preparation methods of carbon nanotube anti-static film, comprising the following steps:
S10. carbon nanotube, resin and the solvent that pipe range is 100~500 microns are obtained, by the carbon nanotube, the tree
Rouge and the solvent are uniformly mixed, and obtain carbon nanotube resin mixture；
S20. the carbon nanotube resin mixture is ground, obtains grinding product；
S30. obtain curing agent, the curing agent be added in the grinding product, be configured to solid content be 70~
85% carbon nanotube anti-static slurry；
S40. carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry.
The preparation method of carbon nanotube anti-static film provided in an embodiment of the present invention is 100~500 microns with pipe range
Carbon nanotube, resin, curing agent and solution are raw material, wherein the long-chain carbon nanotube that pipe range is 100~500 microns, single carbon
Nanotube or carbon nano pipe array have anisotropic electric conductivity, and a small amount of carbon nanotube can form one layer of conduction
The carbon nano tube transparent conductive thin-film of the isotropic high-transmittance of performance, low areal resistance, to keep carbon nanotube obtained anti-
Electrostatic film has excellent electric conductivity, can conduct charge in time, avoid harm caused by charge accumulation.In addition, this hair
Since the carbon nanotube that pipe range is 100~500 microns has excellent dissipate simultaneously in the carbon nanotube anti-static film of bright preparation
Hot property, thus carbon nanotube anti-static film prepared by the present invention not only has excellent antistatic property but also has preferable
Heat dissipation effect.The embodiment of the present invention is by the mixing procedures such as roll-type milled processed, by carbon nanotube, resin, curing agent and molten
Each raw material of liquid is mixed to form the uniform organic whole of carbon nanotube anti-static slurry that solid content is 70~85%, the slurry of the solid content
Material has most suitable film forming, then carbon nanotube anti-static film is made in slurry.It can make pipe by roll-type milled processed technique
A length of 100~500 microns of long-chain carbon nanotube, which is evenly dispersed in slurry, forms equably carbon nanotube anti-static slurry,
Without additionally adding dispersing agent, influence of the dispersing agent to adhesion of thin film and surface resistivity, and the preparation are avoided
Method and process is simple, is suitable for industrialized production.
Specifically, in above-mentioned steps S10, carbon nanotube, resin and solvent that pipe range is 100~500 microns are obtained, by institute
It states carbon nanotube, the resin and the solvent to be uniformly mixed, obtains carbon nanotube resin mixture.The embodiment of the present invention is with pipe
A length of 100~500 microns of long-chain carbon nanotube be raw material, by stirring etc. hybrid modes, by long-chain carbon nanotube, resin and
Solvent is uniformly mixed, and obtains mixture.Wherein, the excellent electric conductivity of long-chain carbon nanotube, can effectively improve antistatic film
Electric conductivity, charge in timely conducting membranes prevents static charge accumulation in film from causing damages.
In some embodiments, after obtaining carbon nanotube, resin and the solvent that pipe range is 100~500 microns, using magnetic force
The mode of stirring stir process 30~60 minute, the carbon nanotube, the resin and the solvent is uniformly mixed, obtained
Carbon nanotube resin mixture.In some embodiments, the pipe range of the carbon nanotube can be 100~200 microns, 200~
300 microns, 300~400 microns or 400~500 microns.
As a preferred embodiment, the mass ratio of the carbon nanotube and the resin is (0.01~0.5): (65~80).
The embodiment of the present invention is with mass ratio for (0.01~0.5): (65~80) obtain pipe range be 100~500 microns carbon nanotube with
Resin, since carbon nanotube used in the embodiment of the present invention is the long-chain carbon nanotube that pipe range is 100~500 microns, relative to
Short chain carbon nanotube has better electric conductivity, and under the requirement of same electric conductivity, the embodiment of the present invention only needs to add
The long-chain carbon nanotube that minimal amount of pipe range is 100~500 microns can make film have excellent electric conductivity, antistatic
Performance.The cost of material of antistatic film is not only reduced, and minimal amount of carbon nanotube is to antistatic film transmitance shadow
Sound is small, is also beneficial to slurry and is uniformly dispersed.
In some implementation columns, the carbon nanotube is selected from: single-walled carbon nanotube or multi-walled carbon nanotube, Huo Zhedan
The mixture of wall carbon nano tube and multi-walled carbon nanotube.
As a preferred embodiment, the resin is selected from: epoxy resin, polyurethane, is appointed in organic siliconresin at acrylic resin
It anticipates one kind.The resins such as epoxy resin, acrylic resin, polyurethane and organic siliconresin used in the embodiment of the present invention have preferable
Adhesive strength and chemical-resistance, and it is colorless and transparent, be conducive to the antistatic film that high transparency is made.
As a preferred embodiment, the solvent is selected from: at least one of acetone, dimethylbenzene, N-Methyl pyrrolidone.This hair
Acetone, dimethylbenzene, the N-Methyl pyrrolidone solvent of bright embodiment selection have preferable dissolution to resin and carbon nanotube, point
Dissipate effect.
Specifically, in above-mentioned steps S20, roll-type milled processed is carried out to the carbon nanotube resin mixture, is ground
Grind product.The embodiment of the present invention carries out grinding distribution processing to carbon nanotube resin mixture using roll-type milled processed technique,
Carbon nanotube, resin and solvent is set to form the ground grinding product that is uniformly dispersed.
In some embodiments, the roll-type milled processed specifically can use two roller milled processeds, three roller milled processeds,
Four-roller milled processed or multiple roll milled processed.
As a preferred embodiment, the step of being ground to the carbon nanotube resin mixture includes: in roller
In the case that gap is 20~40 microns, the carbon nanotube resin mixture is carried out roll-type milled processed 5~10 minutes；So
Afterwards by the roller gap adjustment be 0 micron roll-type milled processed 5~10 minutes；It is again 5~10 by the roller gap adjustment
Micron roll-type milled processed 10~20 minutes.The embodiment of the present invention carries out roller to the carbon nanotube resin mixture in three stages
Formula milled processed, the shearing force ground by roll-type open carbon nanotube removing, the tearing reunited together, make every carbon nanometer
Guan Gengen disperses in the slurry, each component in the mixture of carbon nanotube, resin and solvent to be made to be uniformly dispersed, and is formed organic uniform
The grinding product of dispersion preferably plays the electric conductivity of carbon nanotube.Firstly, the case where roller gap is 20~40 microns
Under, the carbon nanotube resin mixture is carried out roll-type milled processed 5~10 minutes, it will be at the beginning of carbon nanotube, resin and solvent
Step is uniformly dispersed, and allows the components such as resin to soften, is more advantageous to roll-type milled processed.It then is 0 micro- by the roller gap adjustment
Rice milled processed 5~10 minutes, by gapless roll-type milled processed, the strong E Fande destroyed between carbon nanotube
Hua Li is evenly dispersed in carbon nanotube root root in slurry.It is again 5~10 microns of roll-type grindings by the roller gap adjustment
Processing 10~20 minutes, makes further to be uniformly dispersed between each component in mixture, especially carbon nanotube is whole in the mixture
Body is uniformly dispersed.
Embodiment more preferably, the step of being ground to the carbon nanotube resin mixture include: in roller
In the case that wheel gap is 20~40 microns, the carbon nanotube resin mixture is carried out three roller milled processeds 5~10 minutes；
Then by the roller gap adjustment be 0 micron three roller milled processed 5~10 minutes；Again by the roller gap adjustment be 5~
10 micron three roller milled processed 10~20 minutes.
Specifically, in above-mentioned steps S30, curing agent is obtained, the curing agent is added in the grinding product, prepared
The carbon nanotube anti-static slurry for being 70~85% at solid content.The embodiment of the present invention is solidified by adding in grinding product
Agent, the carbon nanotube anti-static slurry that hybrid modulation is 70~85% at solid content, there is paste carbon nanotubes antistatic slurry
Most suitable film-formation result.
As a preferred embodiment, the step of being configured to the carbon nanotube anti-static slurry that solid content is 70~85% packet
It includes: the curing agent being added in the grinding product after mixing evenly, Fruit storage is carried out, it is anti-to obtain carbon nanotube
Electrostatic slurry.Curing agent is distributed to and is ground with being uniformly dispersed by agitating modes such as magnetic force, machinery by the embodiment of the present invention
In product, then by vacuum outgas by the removal of bubbles in slurry, avoid the bubble in slurry in film manufacturing process
Stomata is formed on film influences film integrity energy.
In some embodiments, the step of being configured to the carbon nanotube anti-static slurry that solid content is 70~85% packet
It includes: obtaining curing agent and the solvent, the curing agent and the solvent are added in the grinding product after mixing evenly,
Fruit storage is carried out, the carbon nanotube anti-static slurry that the solid content is 70~85% is obtained.The embodiment of the present invention exists
Obtain curing agent while being adjusted, can obtain according to actual needs solvent and be added in grinding product to grinding product,
The carbon nano tube paste obtained is set to have optimal solid content and filming performance.
As a preferred embodiment, the mass ratio of the carbon nanotube, the resin and the curing agent be (0.01~
0.5): (65~80): (6~8).The mass ratio of carbon nanotube of the embodiment of the present invention, the resin and the curing agent makes slurry
There is optimal film forming solidification effect, stablizes film performance obtained.
As a preferred embodiment, the curing agent is selected from: triethylene tetramine, ethylenediamine, hexamethylene diamine, diethylenetriamine, two
At least one of ethylamino propylamine.Triethylene tetramine used in the embodiment of the present invention, ethylenediamine, hexamethylene diamine, diethylenetriamine and
Diethylaminopropylamine curing agent has preferable crosslinking curing to make epoxy resin, acrylic resin, polyurethane or organic siliconresin
With the netted three-dimensional structured polymeric films of formation, by carbon nanotube, equably envelope is among the reticulate body of resin, enhanced film
For stability, electric conductivity.
Specifically, in above-mentioned steps S40, carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry.
As a preferred embodiment, the carbon nanotube is resisted in the case where scraper spacing is 50~300 microns using doctor blade process
Electrostatic slurry is coated on substrate, obtains the carbon nanotube anti-static film after dry.The embodiment of the present invention passes through blade coating
Carbon nanotube anti-static film, flexible operation aspect is made in carbon nanotube anti-static slurry by mode.
As a preferred embodiment, the substrate is selected from: polyester film, polyethylene film, polyvinyl chloride, a kind of in polypropylene screen.
The embodiment of the present invention, as substrate, has excellent physical mechanical using polyester film, polyethylene film, polyvinyl chloride, polypropylene screen
Performance, chemical property and dimensionally stable, the optical properties such as transparency.
In some embodiments, the carbon nanotube is selected from: single-walled carbon nanotube and/or multi-walled carbon nanotube；The tree
Rouge is selected from: epoxy resin, acrylic resin, polyurethane, any one in organic siliconresin；The curing agent is selected from: triethylene
At least one of tetramine, ethylenediamine, hexamethylene diamine, diethylenetriamine, diethylaminopropylamine；The solvent is selected from: acetone, diformazan
At least one of benzene, N-Methyl pyrrolidone；The substrate is selected from: polyester film, polyethylene film, polyvinyl chloride, in polypropylene screen
It is a kind of.
The embodiment of the invention also provides a kind of carbon nanotube anti-static materials, with the carbon nanotube anti-static material
Gross mass is 100% meter, the raw material components including following mass percentage:
The carbon nanotube 0.01~0.5% that pipe range is 100~500 microns,
Resin 65~80%,
Curing agent 6~8%,
Surplus is solvent.Gross mass is 100% meter, and the carbon that the pipe range including 0.01~0.5% is 100~500 microns is received
Mitron, 65~80% resin, 6~8% curing agent and solvent.Excellent and preferable heat dissipation performance is had conductivity due to containing
The long-chain carbon nanotube that pipe range is 100~500 microns, making the anti-static material equally has excellent electric conductivity, Neng Gouji
When conduct charge, avoid harm caused by charge accumulation, good heat dissipation effect, and content of carbon nanotubes is extremely low, energy saving and cost lowering.
In some embodiments, in terms of by the gross mass of the carbon nanotube anti-static material for 100%, including following quality
The raw material components of percentage composition:
The single-walled carbon nanotube and/or multi-walled carbon nanotube that 0.01~0.5% pipe range is 100~500 microns,
65~80% any one resin in epoxy resin, acrylic resin, polyurethane, organic siliconresin,
6~8% at least one in triethylene tetramine, ethylenediamine, hexamethylene diamine, diethylenetriamine, diethylaminopropylamine
The curing agent of kind,
And the solvent selected from least one of acetone, dimethylbenzene, N-Methyl pyrrolidone of surplus.
Correspondingly, the embodiment of the invention also provides a kind of carbon nanotube anti-static slurries, which is characterized in that the carbon is received
Mitron antistatic slurry includes above-mentioned carbon nanotube anti-static material, and the solid content of the carbon nanotube anti-static slurry is 70
~85%.
Carbon nanotube anti-static slurry provided in an embodiment of the present invention, on the one hand, due to including above-mentioned with excellent
Electric conductivity, and the carbon nanotube anti-static material that content of carbon nanotubes is extremely low, thus, carbon nanotube anti-static slurry also has
Excellent electric conductivity can conduct charge in time, avoid harm caused by charge accumulation, and slurry light transmittance is good；On the other hand,
The solid content of carbon nanotube anti-static slurry of the embodiment of the present invention is 70~85%, has preferable processability, can directly make
At the antistatic grinding tool of antistatic film or other forms, practicability is wide, convenient for utilizing.
The embodiment of the invention also provides a kind of carbon nanotube anti-static film, the carbon nanotube anti-static film is by upper
The preparation method for stating carbon nanotube anti-static film is made or the carbon nanotube anti-static film is with above-mentioned carbon nanotube
Anti-static material is prepared as raw material or the carbon nanotube anti-static film is starched by above-mentioned carbon nanotube anti-static
Material coating is made.
Carbon nanotube anti-static film provided in an embodiment of the present invention is by the above-mentioned carbon nanotube anti-static material haveing excellent performance
Material is prepared as raw material, or is made by the coating of above-mentioned carbon nanotube anti-static slurry, or pass through above-mentioned carbon nanotube
The preparation method of antistatic film is made, thus has excellent electric conductivity, can conduct charge in time, avoid charge accumulation
Caused by endanger, good heat dissipation effect, and content of carbon nanotubes is extremely low, film light transmittance is high.
To make, the above-mentioned implementation detail of the present invention and operation can be clearly readily appreciated by one skilled in the art and the present invention is real
The progress performance for applying a carbon nanotube anti-static film significantly embodies, and above-mentioned skill is illustrated below by way of multiple embodiments
Art scheme.
Embodiment 1
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.01%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.015g (0.01%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 2
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.03%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.045g (0.03%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 3
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.04%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.06g (0.04%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 4
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.05%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.075g (0.05%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 5
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.06%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.09g (0.06%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 6
The embodiment of the present invention provides a kind of antistatic film that content of carbon nanotubes is 0.07%, by following steps system
:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.105g (0.07%), are added in the epoxy resin of 100g,
12.5g acetone solvent is added, is put into beaker, uniform using magnetic agitation, mixing time 30min or so, has visually seen herein
Uniformly, to obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. by grinding product, the triethylene tetramine curing agent of 10g and the acetone solvent of 27.5g is added.It is configured to solid
Carbon nanotube/resin compound that content is 80%, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
Embodiment 7
The embodiment of the present invention provides a kind of carbon nanotube anti-static film, is made by following steps:
S10. 200 μm of long multi-walled carbon nanotubes for weighing 0.5g, are added in the epoxy resin of 100g, are added a small amount of third
Ketone solvent is put into beaker, uniform using magnetic agitation, herein mixing time 30min or so, is visually seemed uniformly,
Obtain carbon nanotube resin mixture.
S20. uniformly mixed carbon nanotube resin mixture is put into three-roll grinder, first arrives three roller gap adjustments
30 μm of operation 5min；Then, gap 0 μm is adjusted to run 30 times；Finally, adjusting to 5 μm of 10min that rerun, ground
Product.
S30. the grinding product after taking 10g to disperse, is added the epoxy resin of 40g, then 5g is added in mechanical stirring 10min
Triethylene tetramine curing agent and 13.75g acetone solvent.It is configured to carbon nanotube/resin mixing that solid content is 80%
Object, deaeration 30min, obtains carbon nanotube anti-static slurry under vacuum conditions.
S40. to the carbon nanotube anti-static slurry after above-mentioned dispersion, using doctor blade process, scraper gap is 50 μm, coating
In in PET film, 30min is once then toasted at 120 DEG C, obtains carbon nanotube anti-static film.
The grinding product of the carbon nanotube resin of elder generation of embodiment of the present invention compounding high concentration, leads to again when practical application
It crosses addition resin and high concentration grinding product is diluted to suitable concentration, carbon nanotube anti-static film is then made, eliminate big
The operation of scale dispersion, easy to use and flexible.
In order to further verify the progressive of carbon nanotube anti-static film provided in an embodiment of the present invention, the present invention is to upper
The antistatic film for stating embodiment preparation has carried out performance test.
Test case 1
The surface and section for the carbon nanotube anti-static film that the embodiment of the present invention is prepared embodiment 6 using scanning electron microscope
Pattern test is carried out, as a result as shown in attached drawing 1~2.
As shown in attached drawing 1~2, the surface and section of the carbon nanotube anti-static film of preparation of the embodiment of the present invention are considerable
Equally distributed carbon nanotube is observed, carbon nanotube forms fine and close conducting function reticular structure in antistatic film.
Test case 2
The surface resistivity and light transmittance for the carbon nanotube anti-static film that the embodiment of the present invention prepares Examples 1 to 6
It is tested, as a result as shown in Fig. 3.
As shown in Fig. 3, the carbon nanotube anti-static film that prepared by the embodiment of the present invention 1~6 all has higher light transmission
Rate and lower surface resistivity.As the surface resistivity of the increase antistatic film of content of carbon nanotubes reduces, transmitance
Also corresponding to reduce, when continuing growing, transmitance and surface resistivity tend towards stability.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of preparation method of carbon nanotube anti-static film, which comprises the following steps:
Obtaining pipe range is 100~500 microns of carbon nanotube, resin and solvent, by the carbon nanotube, the resin and described
Solvent is uniformly mixed, and obtains carbon nanotube resin mixture；
Roll-type milled processed is carried out to the carbon nanotube resin mixture, obtains grinding product；
Curing agent is obtained, the curing agent is added in the grinding product, the carbon that solid content is 70~85% is configured to and receives
Mitron antistatic slurry；
Carbon nanotube anti-static film is made in the carbon nanotube anti-static slurry.
2. the preparation method of carbon nanotube anti-static film as described in claim 1, which is characterized in that the carbon nanotube,
The mass ratio of the resin and the curing agent is (0.01~0.5): (65~80): (6~8).
3. the preparation method of carbon nanotube anti-static film as claimed in claim 1 or 2, which is characterized in that received to the carbon
Mitron resin compound carry out roll-type milled processed the step of include:
In the case where roller gap is 20~40 microns, roll-type milled processed 5 is carried out to the carbon nanotube resin mixture
~10 minutes；Then by the roller gap adjustment be 0 micron roll-type milled processed 5~10 minutes；Again by the roller gap
It is adjusted to 5~10 microns of roll-type milled processeds 10~20 minutes.
4. the preparation method of carbon nanotube anti-static film as claimed in claim 3, which is characterized in that described to be configured to contain admittedly
The carbon nanotube anti-static slurry that amount is 70~85%:
The curing agent is added in the grinding product after mixing evenly, Fruit storage is carried out, obtains described containing admittedly
The carbon nanotube anti-static slurry that amount is 70~85%.
5. the preparation method of carbon nanotube anti-static film as described in claim 1, which is characterized in that described to be configured to contain admittedly
The carbon nanotube anti-static slurry that amount is 70~85%:
Curing agent and the solvent are obtained, the curing agent and the solvent are added in the grinding product and stirred evenly
Afterwards, Fruit storage is carried out, the carbon nanotube anti-static slurry that the solid content is 70~85% is obtained.
6. the preparation method of the carbon nanotube anti-static film as described in claim 4 or 5 is any, which is characterized in that will be described
Carbon nanotube anti-static film is made in carbon nanotube anti-static slurry: using doctor blade process, is 50~300 microns in scraper spacing
In the case where, the carbon nanotube anti-static slurry is coated on substrate, it is thin to obtain the carbon nanotube anti-static after dry
Film.
7. the preparation method of carbon nanotube anti-static film as claimed in claim 6, which is characterized in that the carbon nanotube choosing
From: single-walled carbon nanotube and/or multi-walled carbon nanotube；And/or
The resin is selected from: epoxy resin, acrylic resin, polyurethane, any one in organic siliconresin；And/or
The curing agent is selected from: triethylene tetramine, ethylenediamine, hexamethylene diamine, diethylenetriamine, at least one in diethylaminopropylamine
Kind；And/or
The solvent is selected from: at least one of acetone, dimethylbenzene, N-Methyl pyrrolidone；And/or
The substrate is selected from: polyester film, polyethylene film, polyvinyl chloride, a kind of in polypropylene screen.
8. a kind of carbon nanotube anti-static material, which is characterized in that the gross mass with the carbon nanotube anti-static material is
100% meter, the raw material components including following mass percentage:
The carbon nanotube 0.01~0.5% that pipe range is 100~500 microns,
Resin 65~80%,
Curing agent 6~8%,
Surplus is solvent.
9. a kind of carbon nanotube anti-static slurry, which is characterized in that the carbon nanotube anti-static slurry includes such as claim 8
The carbon nanotube anti-static material, and the solid content of the carbon nanotube anti-static slurry is 70~85%.
10. a kind of carbon nanotube anti-static film, which is characterized in that the carbon nanotube anti-static film is by such as claim 1
The preparation method of carbon nanotube anti-static film described in~7 any one is made or the carbon nanotube anti-static film
It is prepared using carbon nanotube anti-static material as claimed in claim 8 as raw material or the carbon nanotube anti-static
Film is coated with by carbon nanotube anti-static slurry as claimed in claim 9 and is made.
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| CN111825952A (en) * | 2020-07-14 | 2020-10-27 | 国家纳米科学中心 | Super-ordered carbon nanotube epoxy resin composite material and preparation method and application thereof |
| CN113912876A (en) * | 2021-11-03 | 2022-01-11 | 江西铜业技术研究院有限公司 | Carbon nanotube mother solution for modified acrylic resin and preparation method thereof |
| CN116179015A (en) * | 2023-02-10 | 2023-05-30 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
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| CN111825952A (en) * | 2020-07-14 | 2020-10-27 | 国家纳米科学中心 | Super-ordered carbon nanotube epoxy resin composite material and preparation method and application thereof |
| CN111825952B (en) * | 2020-07-14 | 2023-02-10 | 国家纳米科学中心 | Super-ordered carbon nanotube epoxy resin composite material and preparation method and application thereof |
| CN113912876A (en) * | 2021-11-03 | 2022-01-11 | 江西铜业技术研究院有限公司 | Carbon nanotube mother solution for modified acrylic resin and preparation method thereof |
| CN116179015A (en) * | 2023-02-10 | 2023-05-30 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
| CN116179015B (en) * | 2023-02-10 | 2023-12-01 | 深圳烯湾科技有限公司 | Polyurethane composite material, preparation method thereof and product |
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Application publication date: 20191018 |