CN117924782A - Preparation method of antistatic polyester film - Google Patents
Preparation method of antistatic polyester film Download PDFInfo
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- CN117924782A CN117924782A CN202311781564.9A CN202311781564A CN117924782A CN 117924782 A CN117924782 A CN 117924782A CN 202311781564 A CN202311781564 A CN 202311781564A CN 117924782 A CN117924782 A CN 117924782A
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 267
- 238000002360 preparation method Methods 0.000 title claims description 6
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 179
- 239000002344 surface layer Substances 0.000 claims abstract description 94
- 238000001035 drying Methods 0.000 claims abstract description 72
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 230000008961 swelling Effects 0.000 claims abstract description 50
- 239000007800 oxidant agent Substances 0.000 claims abstract description 46
- 230000001590 oxidative effect Effects 0.000 claims abstract description 44
- 239000000178 monomer Substances 0.000 claims abstract description 31
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 22
- 239000010410 layer Substances 0.000 claims abstract description 17
- 238000007664 blowing Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 126
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims description 88
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 claims description 80
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 44
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 40
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 24
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000010926 purge Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 13
- 229920001940 conductive polymer Polymers 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000007654 immersion Methods 0.000 description 48
- 229920000139 polyethylene terephthalate Polymers 0.000 description 12
- 229920000728 polyester Polymers 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 4
- 239000002216 antistatic agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- -1 pyrrole small molecules Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000010129 solution processing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
A method for preparing an antistatic polyester film comprising the steps of: step a: immersing the polyester film in an expansion tank filled with swelling liquid for 5-60 minutes at 50-100 ℃, wherein the swelling liquid gradually swells the surface layer of the polyester film; step b: soaking the swelled polyester film in soaking tank with pyrrole-containing soaking liquid at 60-120 deg.c for 5-90 min to diffuse pyrrole monomer to make the polyester film surface layer molecule chain; step c: b, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film; step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 10-180 minutes, so that oxidant molecules penetrate into the surface layer of the polyester film, and the pyrrole is subjected to oxidation reaction and polymerized into polypyrrole, thereby forming an antistatic layer on the surface layer of the polyester film. Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. One or both sides of the obtained polyester film are provided with polypyrrole conductive polymers, and a conductive network with even distribution is formed, so that the polyester film has a good charge dredging effect.
Description
Technical Field
The invention relates to a preparation method of an antistatic polyester film.
Background
The polyester film has good comprehensive performance and is widely applied to the fields of electronics, optics and the like. However, the PET film is used as a polymer insulating material, has higher self-resistivity, is easy to generate static electricity due to friction in the production and use processes, brings a plurality of inconveniences to the application of the PET film, and particularly leads to the failure of a semiconductor due to the electrostatic discharge phenomenon when the PET film is applied to the field of electronic and electric appliances, thereby influencing the performance of products. Therefore, the antistatic modification of the PET film has very important practical significance.
The antistatic property represents a property of discharging charges accumulated on the surface of the insulating material by an appropriate method. In order to improve the antistatic property of the polyester film, an antistatic layer or conductive layer may be generally formed on the surface of the polyester film, or a conductive or antistatic substance (e.g., metal, carbon powder, antistatic agent, etc.) may be added to the polyester material matrix so that the charges accumulated on the surface are effectively discharged.
Small molecules and polymers containing anions and cations such as surfactants are used as antistatic agents to form the antistatic coating, and the antistatic agents can play an antistatic function according to the humidity in the atmosphere. However, such ionic antistatic agents have disadvantages of not being resistant to washing with water and limited antistatic effect.
The conductive polymer can also be used for improving the antistatic property of the polyester film, and has the advantages of excellent conductivity, water resistance and the like. However, the polymer has conjugated pi bond in molecular chain, and has strong conjugation effect, so that the polymer has strong interaction between rigidity and chain, is insoluble and infusible under general conditions, and has poor processability. It is difficult to apply to the current melting and solution processing of polymers.
Disclosure of Invention
In order to overcome the defects of the antistatic polyester film in the prior art, the invention provides a preparation method for improving the dispersion of a conductive polymer in the polyester film and a polyester matrix so as to obtain the polyester film with excellent antistatic performance.
The technical scheme for solving the technical problems is as follows: a method for preparing an antistatic polyester film comprising the steps of:
Step a: immersing the polyester film in an expansion tank filled with swelling liquid for 5-60 minutes at 50-100 ℃, wherein the swelling liquid gradually swells the surface layer of the polyester film;
Step b: soaking the swelled polyester film in soaking tank with pyrrole-containing soaking liquid at 60-120 deg.c for 5-90 min to diffuse pyrrole monomer to make the polyester film surface layer molecule chain;
Step c: b, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film;
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 10-180 minutes, so that oxidant molecules penetrate into the surface layer of the polyester film, and the pyrrole is subjected to oxidation reaction and polymerized into polypyrrole, thereby forming an antistatic layer on the surface layer of the polyester film.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film.
Preferably, in the step a, the swelling liquid is one or a combination of several of toluene, paraxylene, metaxylene and 1, 2-tetrachloroethane.
Preferably, the swelling liquid consists of toluene, paraxylene, m-xylene and 1, 2-tetrachloroethane, and the mass ratio of the swelling liquid is 1 (0.5-1): 0.2-0.5): 0.5-1.5.
Preferably, the mass of pyrrole contained in the impregnating solution in the impregnating tank accounts for 50% -90% of the total impregnating solution mass, and the rest components are one or a combination of more of toluene, paraxylene and metaxylene.
Preferably, the components except pyrrole in the impregnating solution are toluene, paraxylene, metaxylene, toluene, paraxylene and metaxylene, and the mass ratio of the components is 1 (0.5-1) to 0.2-0.5.
Preferably, in the step c, the drying temperature of the drying oven is 115-130 ℃ and the drying time is 10-60 minutes.
Preferably, in the step d, the oxidant is a composition formed by mixing ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.5-5.0 mol/liter, the concentration of the ammonium persulfate is 0-2.0 mol/liter, and the concentration of the hydrogen peroxide is 0-3.9 mol/liter.
Preferably, in step e, the moisture content of the dry clean air is less than 0.06 g/cubic meter and the air purge speed is 10 meters/second; the temperature of the hot oven is 130-250 ℃, and the residence time of the polyester film in the hot oven is 10-90 seconds.
The invention has the beneficial effects that: after swelling the surface layer of the polyester film by using a proper swelling agent, pyrrole small molecules can penetrate into the surface layer of the polyester film, and then the surface layer of the polyester film is modified by an oxidizing agent to initiate polymerization of pyrrole monomers, so that a conductive polymer polypyrrole is formed in the surface layer of the polyester film, thereby reducing the surface resistance of the polyester film and realizing an antistatic effect. Since polypyrrole cannot be melt processed, the method of blending polyester with polypyrrole cannot uniformly disperse polypyrrole in polyester to form a uniform polyester/polypyrrole blend film. The present method can solve this problem. One or both sides of the obtained polyester film are provided with polypyrrole conductive polymers, and a conductive network with even distribution is formed, so that the polyester film has a good charge dredging effect.
Description of the embodiments
The present invention will be described in further detail with reference to the following embodiments.
In one embodiment, the method for preparing the antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 30 minutes at 80 ℃ (the temperature is not controlled to 80 ℃ accurately and only controlled within 80+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. The swelling liquid in this example was toluene.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 60 minutes at 100 ℃ (the temperature can not be accurately controlled at 100 ℃ and only needs to be controlled within 100+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this example, the impregnating solution consisted of pyrrole and p-xylene, wherein pyrrole accounted for 70% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 120℃and the drying time was 30 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 60 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. The oxidant in this example is ferric chloride.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 200℃and the residence time of the polyester film in the hot oven was 30 seconds.
In a second embodiment, the method for preparing the antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid for 20 minutes at 50 ℃ (the temperature is not controlled to be 50 ℃ accurately and can be controlled within 50+/-3 ℃ only), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. The swelling liquid in this example is p-xylene.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 90 minutes at 70 ℃ (the temperature is not controlled to be 70 ℃ accurately and only controlled to be within 70+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this example, the impregnating solution consisted of pyrrole and toluene, wherein pyrrole accounted for 65% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 115℃and the drying time was 20 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 100 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. The oxidant in this example is ammonium persulfate.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 140℃and the residence time of the polyester film in the hot oven was 80 seconds.
Embodiment three, the preparation method of the antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 10 minutes at 100 ℃ (the temperature is not precisely controlled at 100 ℃ and can be controlled within 100+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. The swelling liquid in this example is meta-xylene.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 20 minutes at 90 ℃ (the temperature can not be controlled at 90 ℃ accurately and only needs to be controlled within 90+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this example, the impregnating solution consisted of pyrrole and meta-xylene, wherein pyrrole accounted for 50% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 130℃and the drying time was 50 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 10 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In this embodiment, the oxidizing agent is hydrogen peroxide.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 130℃and the residence time of the polyester film in the hot oven was 20 seconds.
In a fourth embodiment, the method for preparing an antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid for 5 minutes at 90 ℃ (the temperature is not precisely controlled at 90 ℃ and can be controlled within 90+/-3 ℃ as needed), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. The swelling liquid in this example was 1, 2-tetrachloroethane.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 80 minutes at 60 ℃ (the temperature can not be controlled at 60 ℃ accurately and only needs to be controlled within 60+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole, toluene and meta-xylene, and the mass ratio of toluene to meta-xylene is 1:1, wherein pyrrole accounts for 83% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 125℃and the drying time was 40 minutes.
Step d: c, immersing the polyester film treated in the step c into a bath containing an oxidant for 30 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, and the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, thereby forming an antistatic layer on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride and ammonium persulfate, wherein the concentration of the ferric chloride is 1mol/L, and the concentration of the ammonium persulfate is 0.5mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 180℃and the residence time of the polyester film in the hot oven was 10 seconds.
Example five, a method of making an antistatic polyester film, comprising the steps of:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 60 minutes at 60 ℃ (the temperature is not controlled to be 60 ℃ accurately and only controlled within 60+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition composed of toluene and meta-xylene, and the mass ratio of toluene to meta-xylene was 1:0.5.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 100 minutes at 120 ℃ (the temperature can not be accurately controlled at 120 ℃ and only needs to be controlled within 120+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In the embodiment, the impregnating solution consists of pyrrole, paraxylene and metaxylene, wherein the mass ratio of the paraxylene to the metaxylene is 5:2, and the pyrrole accounts for 60% of the total mass of the impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 120℃and the drying time was 45 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 150 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.5mol/L, and the concentration of the hydrogen peroxide is 2mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 150℃and the residence time of the polyester film in the hot oven was 90 seconds.
In a sixth embodiment, the method for preparing an antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 40 minutes at 70 ℃ (the temperature is not controlled to be 70 ℃ accurately and only controlled within 70+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane was 1:0.5:0.2:1.5.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 70 minutes at 80 ℃ (the temperature can not be accurately controlled at 80 ℃ and only needs to be controlled within 80+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:0.5:0.5, wherein pyrrole accounts for 90% of the total impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 125℃and the drying time was 10 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 50 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.5mol/L, the concentration of the ammonium persulfate is 1mol/L, and the concentration of the hydrogen peroxide is 2mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 210℃and the residence time of the polyester film in the hot oven was 50 seconds.
Embodiment seven, a method for preparing an antistatic polyester film, comprising the steps of:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid for 50 minutes at 65 ℃ (the temperature is not controlled to 65 ℃ accurately and only controlled within 65+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, 1, 2-tetrachloroethane was 1:1:0.5:0.5
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 5 minutes at 110 ℃ (the temperature is not controlled to be 110 ℃ accurately and only controlled to be within 110+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:1:0.2, wherein pyrrole accounts for 62% of the total impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 115℃and the drying time was 60 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 180 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 5mol/L, the concentration of the ammonium persulfate is 0.1mol/L, and the concentration of the hydrogen peroxide is 3.9mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 250℃and the residence time of the polyester film in the hot oven was 60 seconds.
In embodiment eight, the method for preparing the antistatic polyester film comprises the following steps:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and soaked for 55 minutes at 85 ℃ (the temperature can not be controlled at 85 ℃ accurately and can be controlled within 85+/-3 ℃ only), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane was 1:0.8:0.3:1.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 30 minutes at 85 ℃ (the temperature can not be controlled at 85 ℃ accurately and only within 85+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:0.6:0.4, wherein pyrrole accounts for 55% of the total impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 120℃and the drying time was 35 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 80 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 3mol/L, the concentration of the ammonium persulfate is 0.5mol/L, and the concentration of the hydrogen peroxide is 0.1mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 220 ℃ and the residence time of the polyester film in the hot oven was 70 seconds.
Example nine, a method of making an antistatic polyester film, comprising the steps of:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 25 minutes at 95 ℃ (the temperature is not controlled to be 95 ℃ accurately and can be controlled within 95+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane was 1:0.7:0.4:0.6.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 40 minutes at 90 ℃ (the temperature can not be controlled at 90 ℃ accurately and only needs to be controlled within 90+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:0.8:0.3, wherein pyrrole accounts for 85% of the total impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 115℃and the drying time was 55 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 120 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.8mol/L, the concentration of the ammonium persulfate is 2mol/L, and the concentration of the hydrogen peroxide is 1mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 230℃and the residence time of the polyester film in the hot oven was 55 seconds.
Example ten, a method for preparing an antistatic polyester film, comprising the steps of:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and soaked for 45 minutes at 55 ℃ (the temperature is not controlled to 55 ℃ accurately and only controlled within 55+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane was 1:0.9:0.3:1.2.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 50 minutes at 100 ℃ (the temperature can not be accurately controlled at 100 ℃ and only needs to be controlled within 100+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:0.7:0.2, wherein pyrrole accounts for 75% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 120℃and the drying time was 25 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 130 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 1.2mol/L, the concentration of the ammonium persulfate is 0.2mol/L, and the concentration of the hydrogen peroxide is 0.5mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 200℃and the residence time of the polyester film in the hot oven was 15 seconds.
Example eleven, a method of making an antistatic polyester film comprising the steps of:
Step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 30 minutes at 80 ℃ (the temperature is not controlled to 80 ℃ accurately and only controlled within 80+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane, and the mass ratio of toluene, paraxylene, metaxylene, and 1, 2-tetrachloroethane was 1:0.6:0.5:0.8.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 65 minutes at 75 ℃ (the temperature can not be controlled at 75 ℃ accurately and only needs to be controlled within 75+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In this embodiment, the impregnating solution is composed of pyrrole and toluene, paraxylene and metaxylene, and the mass ratio of toluene, paraxylene and metaxylene is 1:0.9:0.4, wherein pyrrole accounts for 80% of the total impregnating solution mass.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 130℃and the drying time was 15 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 115 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.6mol/L, the concentration of the ammonium persulfate is 0.8mol/L, and the concentration of the hydrogen peroxide is 3mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 200℃and the residence time of the polyester film in the hot oven was 60 seconds.
Example twelve, the method of making an antistatic polyester film, comprising the steps of:
step a: the PET polyester film is immersed in an expansion tank filled with swelling liquid, and is soaked for 15 minutes at 60 ℃ (the temperature is not controlled to be 60 ℃ accurately and only controlled within 60+/-3 ℃), and the swelling liquid enables the surface layer of the polyester film to be gradually swelled. In this example, the swelling liquid was a composition comprising metaxylene and 1, 2-tetrachloroethane, and the mass ratio of metaxylene to 1, 2-tetrachloroethane was 0.4:1.3.
Step b: the swollen polyester film is immersed in an immersion tank, the immersion tank is filled with an immersion liquid containing pyrrole, and the immersion tank is immersed for 60 minutes at 70 ℃ (the temperature is not controlled to be 70 ℃ accurately and only controlled to be within 70+/-3 ℃), so that pyrrole monomers are diffused among the molecular chains on the surface layer of the polyester film. In the embodiment, the impregnating solution consists of pyrrole, toluene, paraxylene and the mass ratio of toluene to paraxylene is 2:1, wherein the pyrrole accounts for 60% of the total mass of the impregnating solution.
Step c: and c, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film. The drying temperature of the drying oven in this example was 130℃and the drying time was 15 minutes.
Step d: and c, immersing the polyester film treated in the step c into a bath containing an oxidant for 100 minutes, so that the oxidant molecules infiltrate into the surface layer of the polyester film, the pyrrole undergoes an oxidation reaction and is polymerized into polypyrrole, and an antistatic layer is formed on the surface layer of the polyester film. In the embodiment, the oxidant is a composition composed of ferric chloride and ammonium persulfate, wherein the concentration of the ferric chloride is 1mol/L, and the concentration of the ammonium persulfate is 2mol/L.
Step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film. In the embodiment, the water content of the dry clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the hot oven temperature was 150℃and the residence time of the polyester film in the hot oven was 30 seconds.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the antistatic polyester film is characterized by comprising the following steps:
Step a: immersing the polyester film in an expansion tank filled with swelling liquid for 5-60 minutes at 50-100 ℃, wherein the swelling liquid gradually swells the surface layer of the polyester film;
Step b: soaking the swelled polyester film in soaking tank with pyrrole-containing soaking liquid at 60-120 deg.c for 5-90 min to diffuse pyrrole monomer to make the polyester film surface layer molecule chain;
Step c: b, after the polyester film treated in the step b leaves the impregnating solution, the polyester film enters a drying box for drying, the micromolecular solvent permeated into the surface layer of the polyester film gradually evaporates, and the pyrrole monomer remains on the surface layer of the polyester film;
Step d: c, immersing the polyester film treated in the step c into a bath containing an oxidant for 10-180 minutes, so that oxidant molecules penetrate into the surface layer of the polyester film, and the pyrrole is subjected to oxidation reaction and polymerized into polypyrrole, thereby forming an antistatic layer on the surface layer of the polyester film;
step e: and d, blowing the two sides of the polyester film treated in the step d by using dry clean air, and then, entering a hot oven for heat treatment to densify the surface structure of the polyester film, thereby finally forming the antistatic polyester film.
2. The method for producing an antistatic polyester film according to claim 1, wherein: in the step a, the swelling liquid is one or a combination of more of toluene, paraxylene, metaxylene and 1, 2-tetrachloroethane.
3. The method for producing an antistatic polyester film according to claim 2, wherein: the swelling liquid consists of toluene, paraxylene, m-xylene and 1, 2-tetrachloroethane, and the mass ratio of the swelling liquid is 1 (0.5-1): 0.2-0.5): 0.5-1.5.
4. The method for producing an antistatic polyester film according to claim 1, wherein: the mass of pyrrole contained in the impregnating solution in the impregnating tank accounts for 50% -90% of the total impregnating solution, and the rest components are one or a combination of more of toluene, paraxylene and metaxylene.
5. The method for producing an antistatic polyester film according to claim 4, wherein: the components except pyrrole in the impregnating solution are toluene, paraxylene and metaxylene, and the mass ratio of the toluene to the paraxylene to the metaxylene is 1 (0.5-1) to 0.2-0.5.
6. The method for producing an antistatic polyester film according to claim 1, wherein: in the step c, the drying temperature of the drying box is 115-130 ℃ and the drying time is 10-60 minutes.
7. The method for producing an antistatic polyester film according to claim 1, wherein: in the step d, the oxidant is one or a combination of more of ferric chloride, ammonium persulfate and hydrogen peroxide.
8. The method for producing an antistatic polyester film according to claim 1, wherein: the oxidant is a composition formed by mixing ferric chloride, ammonium persulfate and hydrogen peroxide, wherein the concentration of the ferric chloride is 0.5-5.0 mol/liter, the concentration of the ammonium persulfate is 0.1-2.0 mol/liter, and the concentration of the hydrogen peroxide is 0.1-3.9 mol/liter.
9. The method for producing an antistatic polyester film according to claim 1, wherein: in step e, the water content of the dried clean air is less than 0.06 g/cubic meter, and the air purging speed is 10 m/s; the temperature of the hot oven is 130-250 ℃, and the residence time of the polyester film in the hot oven is 10-90 seconds; the temperature of the hot oven is 130-250 ℃, and the residence time of the polyester film in the hot oven is 10-90 seconds.
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