CN113136045A - PET single-side antistatic film and processing method thereof - Google Patents
PET single-side antistatic film and processing method thereof Download PDFInfo
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- CN113136045A CN113136045A CN202010083715.3A CN202010083715A CN113136045A CN 113136045 A CN113136045 A CN 113136045A CN 202010083715 A CN202010083715 A CN 202010083715A CN 113136045 A CN113136045 A CN 113136045A
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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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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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
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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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
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
Abstract
The invention discloses a PET single-side antistatic film and a processing method thereof. The processing method comprises the following steps: coating a polyethylene glycol terephthalate solution on the surface of a substrate, and drying to obtain a composite film; arranging uniformly dispersed carbon nanotubes on the surface of the polymer layer of the composite film; heating the polymer layer to enable at least the surface layer of the polymer layer to be in a viscous state and at least part of the carbon nanotubes distributed on the surface of the polymer layer to be automatically embedded into the polymer layer; and cooling the polymer layer, and crosslinking at least the polymer on the surface layer of the polymer layer by using a crosslinking agent, thereby obtaining the PET single-sided antistatic film. The invention has simple process, wide application range and easy large-scale preparation, and the formed antistatic film has excellent comprehensive performance, such as good light transmittance and conductivity, and simultaneously has excellent water resistance, alcohol resistance, wear resistance and the like.
Description
Technical Field
The invention relates to a PET single-side antistatic film and a processing method thereof, belonging to the technical field of nano materials.
Background
At present, in the production, storage and transportation processes of electronic products, in order to prevent the surface abrasion and pollution of the products, it is necessary to protect the surfaces of the products or related production and transportation equipment. One of the common ways is to cover the surface of such products with an antistatic protective film. Generally, in addition to being easily attached to the surface of an electronic product, a protective film used in an electronic product is required to have a certain antistatic function in order to prevent an excessive electrostatic voltage from being generated during the process of removing the protective film, which may even harm the safety of the electronic product.
In recent years, researchers have proposed various antistatic film products formed by using carbon nanotubes and polymer materials, but among these products, the defects of nonuniform dispersion and easy falling of the carbon nanotubes exist, so that the antistatic ability is limited, and the service life and the application range are severely limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a PET single-side antistatic film and a processing method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
in some embodiments, a method for processing a PET single-sided antistatic film is provided, which includes:
coating a polymer layer on the surface of the substrate to form a composite film,
uniformly dispersed carbon nanotubes are arranged on the surface of the polymer layer of the composite film,
heating the polymer layer to make at least the surface layer of the polymer layer in viscous state and at least partial carbon nanotubes distributed on the surface layer of the polymer layer automatically embedded into the polymer layer due to surface tension effect,
and cooling the polymer layer, and crosslinking at least the polymer on the surface layer of the polymer layer by using a crosslinking agent, thereby obtaining the PET single-sided antistatic film.
In some preferred embodiments, the processing method specifically includes:
coating a polymer solution on the surface of a substrate, drying to obtain a composite film,
coating the polymer layer surface of the composite film with carbon nanotube dispersion liquid, removing the solvent in the carbon nanotube dispersion liquid to uniformly distribute the carbon nanotubes on the polymer layer surface of the composite film,
heating the polymer layer to make at least the surface layer of the polymer layer in viscous state and at least part of the carbon nanotubes distributed on the surface layer of the polymer layer automatically embedded into the polymer layer,
and cooling the polymer layer, and crosslinking at least the polymer on the surface layer of the polymer layer by using a crosslinking agent, thereby obtaining the PET single-sided antistatic film.
In some embodiments, the substrate is selected from flexible substrates, in particular film-like flexible substrates.
For example, the material of the flexible substrate preferably includes a polyester material such as Polyethylene (PE), polypropylene (PP), Polystyrene (PS), Polycarbonate (PC), polymethyl methacrylate (PMMA), Polyimide (PI), or pet (pet), or a combination of any one or more of Polyether Sulfone (PEs), cellulose ester, polyvinyl chloride (PVC), benzocyclobutene (BCB), or acrylic resin, but is not limited thereto.
In some embodiments, the polymer may be selected from, but is not limited to, polyethylene terephthalate, for example, polyethylene terephthalate having a number average molecular weight of 2 to 10 ten thousand may be preferred.
In some embodiments, the concentration of the polymer solution is preferably 0.01 wt% to 5 wt%.
In some embodiments, the solvent of the polymer solution may be selected from water or any suitable organic solvent.
In some embodiments, the thickness of the polymer layer (dry film) is preferably 500nm to 50 μm.
In some embodiments, the concentration of the carbon nanotube dispersion is preferably 0.001 wt% to 10 wt%.
In some embodiments, the carbon nanotube dispersion may further include, but is not limited to, any one or a combination of two or more of water, alcohols, ethers, lipids, and alcohol ethers, which are mainly used as a carrier of the dispersion. The carbon nano tube can be any one of a single-wall carbon nano tube and a multi-wall carbon nano tube or any combination of a plurality of the single-wall carbon nano tube and the multi-wall carbon nano tube.
In some embodiments, the carbon nanotube dispersion is preferably coated on the polymer layer in an amount of 50mg/m 2-10 g/m 2.
In some embodiments, the processing method may further include: and coating the surface of the polymer layer of the composite film with carbon nanotube dispersion liquid, and then baking at low temperature to remove the solvent in the carbon nanotube dispersion liquid, thereby arranging uniformly dispersed carbon nanotubes on the surface of the polymer layer of the composite film.
Preferably, the low-temperature baking temperature is 50-80 ℃, and the heat preservation time is 10 min-10 h.
In some embodiments, the processing method may further include: and at least heating the polymer layer to the viscous state temperature of the polymer, so that at least the surface layer of the polymer layer is in a viscous state, and at least part of the carbon nanotubes distributed on the surface of the polymer layer are automatically embedded into the polymer layer.
In some embodiments, the polymer is polyethylene terephthalate, and the viscous state temperature of the polyethylene terephthalate is 80-140 ℃. Preferably, the polyethylene terephthalate layer can be heated to 80-140 ℃ at a heating rate of 50-300 ℃/min, and the temperature is kept for 5 s-5 min.
In some embodiments, the polymer solution can be coated on the surface of the substrate at least by any one of spraying, rolling, knife coating, and dipping.
In some embodiments, the carbon nanotube dispersion can be coated on the surface of the polymer layer by any one of spraying, rolling, blade coating, and screen printing.
In some embodiments, the polymer is selected from polyethylene terephthalate and the crosslinking agent is selected from polyethylene terephthalate crosslinking agents, which may be selected from the types known in the art (see "fine chemical technology", chemical industry press, publication date 2008/2/1), for example, may be selected from any one or a combination of two or more of sodium sulfate, zinc sulfate, boric acid, formaldehyde, butyraldehyde, glutaraldehyde, and commercial polyethylene terephthalate crosslinking agents.
Also provided in some embodiments is a PET single-sided antistatic film, which can be prepared by any of the methods described above.
Compared with the prior art, the invention has the advantages that: the carbon nano tubes are assembled and embedded into the polymer matrix and then are crosslinked, so that the effective distribution of the carbon nano tubes on the surface layer of the antistatic film can be maintained to the maximum extent, and good light transmittance and electric conductivity can be obtained; meanwhile, the water resistance, alcohol resistance, wear resistance and the like of the antistatic film can be obviously improved by adopting the polyethylene glycol terephthalate surface crosslinking process, so that the antistatic film has excellent comprehensive performance, and the process has the advantages of wide application range, simple method, easiness in large-scale preparation and the like.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, implementation process and principle of the present invention will be further explained with reference to several embodiments as follows.
Example 1, a method for processing a PET single-sided antistatic film provided in this example includes:
(1) providing an aqueous polyethylene terephthalate solution having a concentration of about 0.01 weight percent, wherein the polyethylene terephthalate has a molecular weight of about 10 million (number average molecular weight, unless otherwise specified below); and providing a carbon nanotube dispersion at a concentration of about 0.01 wt%, wherein the carbon nanotubes may be single-walled carbon nanotubes and/or multi-walled carbon nanotubes, and the solvent may be water;
(2) coating the polyethylene terephthalate solution on the surface of a PET (PET) film (with visible light transmittance of about 89%) in a spraying mode, and drying to obtain a composite film, wherein the thickness of the polyethylene terephthalate dry film is about 500 nm;
(3) coating the carbon nano tube dispersion liquid on the surface of the polyethylene glycol terephthalate layer of the composite film, keeping the temperature for 5 hours at the temperature of about 50 ℃ to volatilize and remove the solvent in the carbon nano tube dispersion liquid, and then cooling;
(4) rapidly heating to viscous state temperature (about 140 deg.C) of polyethylene terephthalate at a heating rate of about 50 deg.C/min, maintaining for about 3min to automatically embed the carbon nanotubes into the polyethylene terephthalate layer, and cooling;
(5) and then soaking the film in a polyethylene terephthalate cross-linking agent solution (wherein the cross-linking agent can be sodium sulfate, zinc sulfate and the like) for about 15min to cross-link the polyethylene terephthalate on the surface layer, and then washing and drying with water to obtain the PET single-side antistatic film with a stable structure.
Example 2: the processing method of the PET single-sided antistatic film provided in this embodiment includes the following steps:
(1) providing a 5 wt% aqueous solution of polyethylene terephthalate, wherein the polyethylene terephthalate has a molecular weight of about 2 million; and providing a carbon nanotube dispersion having a concentration of about 0.001 wt%, wherein the carbon nanotubes may be single-walled carbon nanotubes and/or multi-walled carbon nanotubes, and the solvent may be a mixed solvent of water and ethanol;
(2) coating a polyethylene terephthalate solution on the surface of a polyethylene film (with visible light transmittance of about 70%) in a dip-coating mode, and drying to obtain a composite film, wherein the thickness of a polyethylene terephthalate dry film is about 5 mu m;
(3) coating the carbon nano tube dispersion liquid on the surface of the polyethylene glycol terephthalate layer of the composite film, keeping the temperature for about 10min at the temperature of about 80 ℃ to volatilize and remove the solvent in the carbon nano tube dispersion liquid, and then cooling;
(4) rapidly heating to viscous state temperature (about 80 ℃) of the polyethylene glycol terephthalate at a heating rate of 100 ℃/min, keeping the temperature for about 5 seconds, automatically embedding the carbon nano tube into the polyethylene glycol terephthalate layer, and then cooling;
(5) and then soaking the film in a polyethylene terephthalate cross-linking agent solution (wherein the cross-linking agent can be boric acid, formaldehyde or butyraldehyde and the like) for about 15min to cross-link the polyethylene terephthalate on the surface layer, and then washing and drying with water to obtain the PET single-side antistatic film with a stable structure.
Example 3: the processing method of the PET single-sided antistatic film provided in this embodiment includes the following steps:
(1) providing an aqueous polyethylene terephthalate solution having a concentration of about 1 weight percent, wherein the polyethylene terephthalate has a molecular weight of about 5 million; and providing a carbon nanotube dispersion with a concentration of about 1 wt%, wherein the carbon nanotubes can be single-walled carbon nanotubes and/or multi-walled carbon nanotubes, and the solvent can be a mixed solvent of water and ethanol in any proportion;
(2) coating a polyethylene terephthalate solution on the surface of a polypropylene film (with visible light transmittance of about 75%) in a dip-coating manner, and drying to obtain a composite film, wherein the thickness of the polyethylene terephthalate dry film is about 50 mu m;
(3) coating the carbon nano tube dispersion liquid on the surface of the polyethylene glycol terephthalate layer of the composite film, preserving the heat for about 2 hours at the temperature of about 80 ℃ to volatilize and remove the solvent in the carbon nano tube dispersion liquid, and then cooling;
(4) rapidly heating to viscous state temperature (about 120 ℃) of the polyethylene glycol terephthalate at the heating rate of 300 ℃/min, preserving the heat for about 1min, automatically embedding the carbon nano tube into the polyethylene glycol terephthalate layer, and then cooling;
(5) and then soaking the film in a polyethylene terephthalate cross-linking agent solution (wherein the cross-linking agent can be a commercially available polyethylene terephthalate cross-linking agent) for about 15min to cross-link the polyethylene terephthalate on the surface layer, and then washing with water and drying to obtain the PET single-sided antistatic film with stable structure.
Example 4: the processing method of the PET single-sided antistatic film provided in this embodiment includes the following steps:
(1) providing a 2 wt% aqueous solution of polyethylene terephthalate having a molecular weight of about 5 to 8 million; and providing a carbon nanotube dispersion liquid with the concentration of 8 wt% -10 wt%, wherein the carbon nanotubes can be single-walled carbon nanotubes and/or multi-walled carbon nanotubes, and the solvent can be a mixed solvent of water and ethanol in any proportion;
(2) coating the polyethylene terephthalate solution on the surface of a polystyrene film (with visible light transmittance of about 85%) in a dip-coating mode, and drying to obtain a composite film, wherein the thickness of the polyethylene terephthalate dry film is 10 microns;
(3) coating the carbon nano tube dispersion liquid on the surface of the polyethylene glycol terephthalate layer of the composite film, preserving the heat for about 5 hours at the temperature of about 70 ℃ to volatilize and remove the solvent in the carbon nano tube dispersion liquid, and then cooling;
(4) rapidly heating to viscous state temperature (about 100 ℃) of the polyethylene glycol terephthalate at a heating rate of 200 ℃/min, preserving heat for about 5min, automatically embedding the carbon nano tube into the polyethylene glycol terephthalate layer, and then cooling;
(5) and then soaking the film in a polyethylene terephthalate cross-linking agent solution (wherein the cross-linking agent can be a commercial polyethylene terephthalate cross-linking agent) for about 15min to cross-link the polyethylene terephthalate on the surface layer, and then washing and drying the film by water to obtain the PET single-sided antistatic film with stable structure.
Comparative example 1: the starting materials used in this comparative example were the same as those used in example 1, and the procedure was as follows: mixing polyethylene glycol terephthalate aqueous solution and carbon nano tube dispersion liquid according to a ratio of about 1: 1, coating the mixture on a PET film, and curing to form a coating with the thickness of about 500 nm.
When the light transmittance, the electric conductivity, the water resistance, the alcohol resistance and the abrasion resistance of the products obtained in examples 1 to 4 and comparative example 1 are respectively tested, it can be found that the carbon nanotubes directly dispersed in the polyethylene terephthalate matrix in comparative example 1 need a higher conductive threshold, and the content of the carbon nanotubes in the solid film-forming material needs to be more than 1 wt% to obtain a better antistatic property, but the light transmittance is sharply reduced. In examples 1 to 4, the carbon nanotubes are partially embedded in the surface, and the amount of the carbon nanotubes required is greatly reduced, so that both conductivity and transmittance can be achieved, and the surface-crosslinked polyethylene terephthalate has excellent overall stability.
In summary, it can be seen that, by adopting a route of assembling and embedding the carbon nanotubes into the matrix first and then cross-linking, the process of the present invention can maximally maintain the effective distribution of the carbon nanotubes on the surface layer of the antistatic film, thereby obtaining a good balance between the light transmittance and the electrical conductivity of the antistatic film. Meanwhile, the polyethylene glycol terephthalate surface crosslinking process is adopted, so that the water resistance, alcohol resistance, wear resistance and the like of the antistatic film can be obviously improved, and the antistatic film has excellent comprehensive performance. The method has the advantages of wide process application range, simple and convenient method, easy large-scale preparation and the like, and has wide application prospect.
It should be noted that the various products and related parameters, various reaction participants and process conditions adopted in the above embodiments are typical examples, but through a great deal of experimental verification by the present inventors, other different types of reaction participants and other process conditions listed above are applicable and can achieve the claimed technical effects.
Therefore, it should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. A processing method of a PET single-side antistatic film is characterized by comprising the following steps:
coating a polymer solution on the surface of a substrate, and drying to obtain a composite film, wherein the polymer is polyethylene terephthalate;
coating a carbon nanotube dispersion liquid on the surface of the polymer layer of the composite film, and removing the solvent in the carbon nanotube dispersion liquid to uniformly distribute the carbon nanotubes on the surface of the polymer layer of the composite film;
heating the polymer layer to the viscous state temperature of the polymer so as to enable at least the surface layer of the polymer layer to be in a viscous state and further enable at least part of the carbon nanotubes distributed on the surface of the polymer layer to be automatically embedded into the polymer layer;
and cooling the polymer layer, and crosslinking at least the polymer on the surface layer of the polymer layer by using a crosslinking agent, so as to obtain the PET single-sided antistatic film, wherein the crosslinking agent is selected from polyethylene terephthalate crosslinking agents.
2. The processing method according to claim 1, characterized in that: the substrate is selected from flexible substrates, and the material of the flexible substrates is selected from any one or the combination of more than two of polyethylene, polypropylene, polystyrene, polycarbonate, polyimide, PET, polyether sulfone, cellulose ester, polyvinyl chloride and acrylic resin.
3. The processing method of the PET single-sided antistatic film according to claim 1, characterized in that: the polymer is selected from polyethylene terephthalate with the number average molecular weight of 2-10 ten thousand, and the concentration of the polymer solution is 0.01-5 wt%.
4. The processing method according to claim 1, characterized in that: the thickness of the polymer layer is 500 nm-50 mu m, the concentration of the carbon nano tube dispersion liquid is 0.001 wt% -10 wt%, and the carbon nano tube dispersion liquid contains any one or the combination of more than two of water, alcohols, ethers, lipids and alcohol ethers.
5. The processing method according to claim 1, characterized in that: the coating amount of the carbon nano tube dispersion liquid on the polymer layer is 50mg/m 2-10 g/m2, the carbon nano tube dispersion liquid is coated on the surface of the polymer layer of the composite film, then the solvent in the carbon nano tube dispersion liquid is removed through low-temperature baking, so that the uniformly dispersed carbon nano tubes are arranged on the surface of the polymer layer of the composite film, the low-temperature baking temperature is 50-80 ℃, the heat preservation time is 10 min-10 h, the polyethylene glycol terephthalate layer is heated to 80-140 ℃ at the heating rate of 50-300 ℃/min, and the heat preservation time is 5 s-5 min.
6. The process of claim 1, comprising: the viscous state temperature of the polyethylene glycol terephthalate is 80-140 ℃, and the polymer solution is coated on the surface of the substrate by any one of spraying, rolling, blade coating and dip coating.
7. The process of claim 1, comprising: and coating the carbon nano tube dispersion liquid on the surface of the polymer layer by any one of spraying, rolling, blade coating and screen printing.
8. The processing method of the PET single-sided antistatic film according to claim 1, characterized in that: the cross-linking agent is selected from any one or the combination of more than two of sodium sulfate, zinc sulfate, boric acid, formaldehyde, butyraldehyde and glutaraldehyde.
9. A PET single-sided antistatic film prepared by the method of any one of claims 1 to 8.
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| CN114854139A (en) * | 2022-04-06 | 2022-08-05 | 万华化学（宁波）有限公司 | Conductive polymer composite material and preparation method thereof |
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| CN114854139A (en) * | 2022-04-06 | 2022-08-05 | 万华化学（宁波）有限公司 | Conductive polymer composite material and preparation method thereof |
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