CN117659467A - Humidity-resistant low-precipitation polyester film prepared by coating method and preparation method thereof - Google Patents
Humidity-resistant low-precipitation polyester film prepared by coating method and preparation method thereof Download PDFInfo
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- 238000001556 precipitation Methods 0.000 title claims abstract description 115
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 108
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 35
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000080 wetting agent Substances 0.000 claims abstract description 22
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims abstract description 18
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000007493 shaping process Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 238000007711 solidification Methods 0.000 claims abstract description 4
- 230000008023 solidification Effects 0.000 claims abstract description 4
- 239000010410 layer Substances 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 40
- 229920000728 polyester Polymers 0.000 claims description 29
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- -1 polyoxyethylene Polymers 0.000 claims description 12
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- 238000001125 extrusion Methods 0.000 claims description 9
- 239000012948 isocyanate Substances 0.000 claims description 9
- 150000002513 isocyanates Chemical class 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012792 core layer Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- IMSODMZESSGVBE-UHFFFAOYSA-N 2-Oxazoline Chemical compound C1CN=CO1 IMSODMZESSGVBE-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 3
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- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims description 3
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- 229920001634 Copolyester Polymers 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention discloses a wet-heat-resistant low-precipitation polyester film prepared by a coating method and a preparation method thereof, and relates to the technical field of polyester film processing. The surface of the polyester film is coated with an anti-precipitation coating by a coating technology, and the anti-precipitation coating is formed by double-sided coating, high-temperature drying, solidification and shaping of anti-precipitation coating liquid; the anti-precipitation coating liquid comprises water-soluble styrene-maleic anhydride copolymer, deionized water, a cross-linking agent, silica sol, a wetting agent and isopropanol. The invention has the advantages that: the anti-precipitation coating is coated on the surface of the polyester film, the main resin of the coating is styrene-maleic anhydride copolymer, the polymer has good affinity, the oligomer migrates into the low-precipitation coating in a high-temperature or high-temperature and high-humidity state, the anti-precipitation coating can effectively keep the oligomer in a dispersed state, the migrated oligomer is uniformly dispersed in the coating, aggregation, crystallization and whitening of the oligomer are prevented, the anti-precipitation performance is more excellent, and the material cost is lower.
Description
Technical Field
The invention relates to the technical field of polyester film processing, in particular to a wet-heat-resistant low-precipitation polyester film prepared by a coating method and a preparation method thereof.
Background
With the high-speed development of the photoelectric display industry, optical grade polyethylene terephthalate (PET) films are increasingly widely used, and the film processing modes are diversified. Oligomers, i.e. oligomers, molecular weight 10 4 Hereinafter, the oligomers are referred to as oligomers. In the production process of the raw materials of the polyester film, the oligomer is generated by side reaction. The molecular chain motion of PET becomes active in a high-temperature state (especially in a high-temperature and high-humidity environment), the coated oligomer can be transferred to the surface and form aggregation, and a visible whitening phenomenon is formed after crystallization, so that the coating, composite quality, printing and gold stamping quality of the post-processing of a polyester film are affected, and the application of PET in the high-end field (such as the ITO field, which needs long-time high-temperature treatment and high-temperature and high-humidity aging test) is severely limited. Therefore, the surface oligomers of optical polyester films are receiving more and more attention, and how to reduce the oligomers precipitated from the optical polyester base film is an important research topic.
At present, few domestic products with low precipitation performance are produced, and domestic polyester raw film manufacturers are few in terms of low precipitation biaxially oriented polyester film due to limitations in equipment and technology, most of the products depend on foreign import, and the foreign products are mainly from the United states, japan, korea and the like; on the other hand, in the electronic display industry which is increasingly rapidly developed, more and more products need to be subjected to multiple coating, compounding and other processing procedures, and high-temperature treatment needs to be carried out for multiple times, and in the processing process, the polyester base film needs to have the performance of high temperature, low precipitation and even no precipitation in order to ensure the quality of the products. Therefore, the high-temperature low-precipitation polyester film is a trend of development in the future.
In the prior art, the low-precipitation polyester film is usually prepared by adding a heat stabilizer into a common polyester chip during film production to reduce degradation in the processing process, so that the generated low-molecular-weight substances are fewer, and precipitation is reduced. The method has poor actual effect, can slightly reduce the educt, and can not meet the requirement of a conventional low-educt film in actual application; also, a low-precipitation polyester film is coated on the surface by gluing or resin coating with a certain thickness, for example, chinese patent CN202110196595.2 discloses a low-precipitation polyester film and a preparation method thereof, wherein the polyester film is coated with the same or different coating solutions on the two sides, and the coating solution is one or more of polyester coating solution, polyurethane coating solution or acrylic coating solution, so that the surface precipitate is reduced, but terephthalic acid and ethylene glycol are reacted to obtain a copolyester melt according to certain requirements during processing, and then polyester chips are obtained, so that the preparation requirements are higher; the prior art also has low precipitation polyester film products realized by adopting a polyester raw material modification and tackifying mode, but the precipitation resistance is still not ideal, and the material cost is high; chinese patent CN202111526407.4 discloses a polyester film with low precipitation and its preparation method, its coating is aqueous polyester, aqueous polyurethane, aqueous acrylic resin, etc., and does not have the function of low precipitation in high temperature or high temperature and high humidity environment.
Disclosure of Invention
The invention aims to solve the technical problems that the moisture-heat resistant low-precipitation polyester film prepared by a coating method and the preparation method thereof can solve the problems that the preparation method for reducing surface precipitates in the prior art needs to prepare polyester chips, the preparation requirement is high, the low-precipitation polyester film product realized by adopting a polyester raw material modification and tackifying mode is still not ideal in precipitation resistance, the material cost is high, and the existing coating does not have a high-temperature or high-temperature high-humidity environment low-precipitation function.
In order to solve the technical problems, the technical scheme of the invention is as follows: the anti-precipitation coating is coated on the surface of the polyester film by a coating technology, is formed by double-sided coating, high-temperature drying and solidification shaping of anti-precipitation coating liquid, and comprises a first anti-precipitation coating, a main film layer and a second anti-precipitation coating which are sequentially laminated, wherein the main film layer is an ABA three-layer co-extrusion structure polyester film;
the preparation steps of the anti-precipitation coating liquid are as follows:
a: adding water-soluble styrene-maleic anhydride copolymer into a stirring tank a, adding deionized water according to a proportion, starting stirring, controlling the temperature to be 15-35 ℃, controlling the rotating speed of a stirrer to be 500-3000rpm, and stirring for 15-30 min;
b: adding the cross-linking agent into a stirring tank b, adding deionized water according to the proportion, starting stirring, controlling the temperature to be 15-35 ℃, and stirring for 15-30 min at the rotating speed of 500-3000 rpm;
c: slowly adding the mixture in the stirring tank b into the stirring tank a, and continuously stirring for 15-30 min;
d: adding silica sol, wetting agent and isopropanol, continuously stirring for 15-30 min, and standing for 30-60 min after completion;
the weight fraction is as follows: 2 to 20 parts of water-soluble styrene-maleic anhydride copolymer, 40 to 90 parts of deionized water, 5 to 25 parts of isopropanol, 0.4 to 5 parts of cross-linking agent, 0.01 to 0.1 part of silica sol and 0.01 to 0.05 part of wetting agent;
the main film layer comprises 100 parts of polyester as the layer B, 30-95 parts of polyester and 5-70 parts of opening master batch as the layer A.
Further, the thicknesses of the first precipitation preventing coating and the second precipitation preventing coating are 20-150 nm, the total thickness of the main film layer is 25-360 mu m, the thickness of the layer A is 2-18 mu m, and the melting points of the polyester and the opening master batch are 255-265 ℃.
Further, the cross-linking agent is one or more of isocyanate cross-linking agent, carbodiimide cross-linking agent, oxazoline cross-linking agent and epoxy silane cross-linking agent;
the silica sol is aqueous silica sol, the aqueous silica sol is silicon dioxide, and the particle size is 30-120 nm;
the wetting agent is one or more of alkyl sulfate wetting agents, polyoxyethylene alkylphenol ether and silanol nonionic surfactants.
Further, the particle size of the open master batch is 0.5-5 μm, and the reason for selecting the particle size master batch is that the surface roughness is relatively low while providing good openness, the conditions of uneven dispersion and agglomeration when the master batch is used are reduced, and the film surface adhesiveness is relatively high.
A preparation method of a wet-heat resistant low-precipitation polyester film prepared by a coating method is characterized by comprising the following steps of: the method comprises the following steps:
s1: conveying the polyester of the polyester film main film layer B layer to a core layer extruder for melting according to the formula amount, conveying the polyester of the polyester film main film layer A layer and the uniform mixture of the opening master batch to the core layer extruder for melting, and co-extruding to obtain an ABA three-layer co-extrusion structure polyester film thick sheet;
s2: cooling and casting an extruded ABA three-layer co-extrusion structure polyester film thick sheet;
s3: preheating a polyester film thick sheet at 60-90 ℃ and then longitudinally stretching to form a main film layer, wherein the stretching multiple is 2.5-4.0 times;
s4: performing on-line coating, performing double-sided coating on the longitudinally stretched membrane, uniformly coating the prepared precipitation-preventing coating liquid on the surface of the main membrane layer, and performing wet coating with the amount of 3-10 g/m 2 ；
S5: drying the coated sheet film in an oven to remove surface moisture, transversely stretching the sheet film at a stretching rate of 3.0-4.0 times and a stretching temperature of 110-160 ℃, and shaping the sheet film at a shaping temperature of 200-255 ℃ by using high temperature after the stretching is finished;
s6: and cooling and rolling the film to obtain the polyester film with low moisture and heat resistance and precipitation by a coating method.
Further, in the step S4, in order to perform online coating and perform coating by using an offline coating method, steps S5 and S6 are directly performed after step S3, and after the winding in step S6 is completed, the winding is unwound again, and coating is performed by step S4, and then drying and winding are performed.
Further, in the S4 coating, the coating mode is one of gravure roll coating and D-bar coating.
Further, in the step S5, the coated sheet film is dried in an oven at a drying temperature of 90 ℃ to 120 ℃.
The invention has the advantages that:
(1) In order to obtain the polyester film with excellent heat and humidity resistance and low precipitation performance, the invention adopts a mode to coat the surface of the polyester film with an anti-precipitation coating, wherein the main resin of the coating is styrene-maleic anhydride copolymer, the coating has good oligomer affinity, the oligomer migrates into the low precipitation coating in a high-temperature or high-temperature and high-humidity state, the anti-precipitation coating can effectively keep the oligomer in a dispersed state, the migrated oligomer is uniformly dispersed in the coating, and the occurrence of aggregation, crystallization and whitening of the oligomer is prevented.
(2) The anti-precipitation coating disclosed by the invention is excellent in coating uniformity and optical performance, and the light transmittance of the polyester film can be improved by 1.5-3%;
(3) The invention has excellent processability, a coating process is added on the existing polyester film production process, special polyester raw materials are not needed, raw material transition is not needed, the preparation requirement is not high, and the processing process change is small;
(4) The optical property, mechanical property, shrinkage rate and the like of the polyester film can be adjusted according to requirements, meanwhile, the low precipitation performance is not influenced, the application range of the product is greatly increased, and the requirements of different applications are met.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. The following examples will provide those skilled in the art with a more complete understanding of the present invention and are not intended to limit the invention to the embodiments described.
The existing polyester inevitably generates a large amount of small molecular side reaction products and oligomers due to side reaction in the preparation process, so as to solve the problem of oligomer transfer precipitation in a high-temperature or high-temperature and high-humidity environment of a polyester film, meet the application of PET in the high-end field (such as the ITO field, which requires long-time high-temperature treatment and high-temperature high-humidity aging test), and provide a moisture-heat-resistant low-precipitation polyester film prepared by a coating method and a preparation method thereof.
The specific implementation mode adopts the following technical scheme: the surface of the polyester film is coated with an anti-precipitation coating by a coating technology, the anti-precipitation coating is formed by double-sided coating, high-temperature drying and solidification shaping of anti-precipitation coating liquid, and the polyester film comprises a first anti-precipitation coating, a main film layer and a second anti-precipitation coating which are sequentially laminated.
The preparation method of the anti-precipitation coating liquid comprises the following steps:
a: adding water-soluble styrene-maleic anhydride copolymer into a stirring tank a, adding deionized water according to a proportion, starting stirring, controlling the temperature to be 15-35 ℃, controlling the rotation speed of a stirrer to be 500-3000rpm, and stirring for 15-30 min, wherein the main active ingredient of the coating liquid is water-soluble styrene-maleic anhydride copolymer (benzene-horse resin, SMA for short), has good precipitation resistance, can well prevent micromolecular oligomer from transferring, aggregating to form whitening, and is uniformly coated on the surface of a film by being prepared into aqueous coating liquid by matching with a cross-linking agent, a wetting agent, an opening agent and the like;
b: adding the cross-linking agent into a stirring tank b, adding deionized water according to the proportion, starting stirring, controlling the temperature to be 15-35 ℃, and stirring for 15-30 min at the rotating speed of 500-3000 rpm;
c: slowly adding the mixture in the stirring tank b into the stirring tank a, and continuously stirring for 15-30 min;
d: adding silica sol, wetting agent and isopropyl alcohol (IPA), continuously stirring for 15-30 min, and standing for 30-60 min after completion.
The weight fraction is as follows: 2 to 20 parts of water-soluble styrene-maleic anhydride copolymer, 40 to 90 parts of deionized water, 5 to 25 parts of isopropanol, 0.4 to 5 parts of cross-linking agent, 0.01 to 0.1 part of silica sol and 0.01 to 0.05 part of wetting agent.
The cross-linking agent is one or more of isocyanate cross-linking agent, carbodiimide cross-linking agent, oxazoline cross-linking agent and epoxy silane cross-linking agent; the silica sol is aqueous silica sol, the aqueous silica sol is silicon dioxide, and the particle size is 30-120 nm; the wetting agent is one or more of alkyl sulfate wetting agent, polyoxyethylene alkylphenol ether and silanol nonionic surfactant.
The main film layer is an ABA three-layer co-extrusion structure polyester film, the thickness of the first anti-precipitation coating and the second anti-precipitation coating is 20-150 nm, the B layer in the main film layer is 100 parts of polyester, the A layer is 30-95 parts of polyester and 5-70 parts of opening master batch, the total thickness of the main film layer is 25-360 mu m, the thickness of the A layer is 2-18 mu m, the melting point of the polyester and the opening master batch is 255-265 ℃, the particle size of the opening master batch is 0.5-5 mu m, the particle size master batch is selected because the good opening property is provided, the surface roughness is relatively low, the uneven dispersion and agglomeration of the master batch in use are reduced, and the film surface adhesiveness is relatively high.
A preparation method of a wet-heat resistant low-precipitation polyester film prepared by a coating method comprises the following steps:
s1: conveying the polyester of the polyester film main film layer B layer to a core layer extruder for melting according to the formula amount, conveying the polyester of the polyester film main film layer A layer and the uniform mixture of the opening master batch to the core layer extruder for melting, and co-extruding to obtain an ABA three-layer co-extrusion structure polyester film thick sheet;
s2: cooling and casting an extruded ABA three-layer co-extrusion structure polyester film thick sheet;
s3: preheating a polyester film thick sheet at 60-90 ℃ and then longitudinally stretching to form a main film layer, wherein the stretching multiple is 2.5-4.0 times;
s4: performing on-line coating, performing double-sided coating on the longitudinally stretched membrane, uniformly coating the prepared precipitation-preventing coating liquid on the surface of the main membrane layer, and performing wet coating with the amount of 3-10 g/m 2 The coating mode is one of gravure roll coating and D-bar coating; preferably, the wet coating amount of the on-line coating is 4-6 g/m 2 Too high a liquid carrying amount is not easy to dry, and too low a liquid carrying amount does not give a sufficient coating thickness.
S5: the coated sheet film enters an oven for drying, the drying temperature is 90-120 ℃, surface moisture is removed, then transverse stretching is carried out, the stretching multiplying power is 3.0-4.0 times, the stretching temperature is 110-160 ℃, the sheet film is shaped by high temperature after the stretching is finished, and the shaping temperature is 200-255 ℃;
s6: and cooling and rolling the film to obtain the polyester film with low moisture and heat resistance and precipitation by a coating method.
In step S4, for on-line coating, when coating is performed by an off-line coating method, steps S5 and S6 are directly performed after step S3, and after winding in step S6 is completed, the coating is performed by step S4 by unreeling again, and then drying and winding are performed.
The invention aims to obtain better high-temperature low-precipitation performance, wherein the high-temperature low-precipitation performance is mainly provided by an anti-precipitation coating, namely, corresponding anti-precipitation coating liquid is prepared, and the invention is described in detail below with reference to specific embodiments.
Example 1:
the preparation method of the coating method of the embodiment is the same as the steps, wherein the anti-precipitation coating liquid is prepared according to the following method:
a: adding 2 parts of water-soluble styrene-maleic anhydride copolymer into a stirring tank a, adding 80 parts of deionized water, starting stirring, controlling the temperature to be 15-35 ℃, controlling the rotating speed of a stirrer to be 500-3000rpm, and stirring for 15-30 min;
b: adding 0.4 part of commercial closed isocyanate cross-linking agent into a stirring tank b, adding 7.45 parts of deionized water according to the proportion, starting stirring, controlling the temperature to be 15-35 ℃, controlling the rotating speed of a stirrer to be 500-3000rpm, and stirring for 15-30 min;
c: slowly adding the mixture in the stirring tank b into the stirring tank a, and continuously stirring for 15-30 min;
d: adding 0.1 part of commercial silica sol with the particle size of 70nm, 0.05 part of polyoxyethylene alkylphenol ether wetting agent and 10 parts of isopropanol, continuously stirring for 15-30 min, and standing for 30-60 min after completion.
Namely, a water-soluble styrene-maleic anhydride copolymer: deionized water: blocked isocyanate-based crosslinking agent: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=2: 87.45:0.4:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of a surface low-precipitation coating of 25-30nm is prepared by a coating method in the preparation process of the moisture-heat resistant low-precipitation polyester film.
Example 2:
this example differs from example 1 in that the water-soluble styrene-maleic anhydride copolymer: deionized water: blocked isocyanate-based crosslinking agent: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=5: 83.85:1:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of 55-60nm is prepared by a coating method and a wet heat resistance low-precipitation polyester film preparation process.
Example 3:
this example differs from example 1 in that the water-soluble styrene-maleic anhydride copolymer: deionized water: blocked isocyanate-based crosslinking agent: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=8: 80.25:1.6:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of 85-90nm is prepared by a coating method in the preparation process of the moisture-heat resistant low-precipitation polyester film.
Example 4:
this example differs from example 1 in that the water-soluble styrene-maleic anhydride copolymer: deionized water: blocked isocyanate-based crosslinking agent: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=10: 77.85:2:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of 100-110nm is prepared by a coating method and a wet heat resistance low-precipitation polyester film preparation process.
Example 5:
this example differs from example 3 in that the cross-linking agent is removed, the water-soluble styrene-maleic anhydride copolymer: deionized water: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=8: 81.85:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of 85-90nm is prepared by a coating method in the preparation process of the moisture-heat resistant low-precipitation polyester film.
Example 6:
this example differs from example 3 in that the amount of crosslinking agent is increased, the water-soluble styrene-maleic anhydride copolymer: deionized water: blocked isocyanate-based crosslinking agent: silica sol: polyoxyethylene alkylphenol ether wetting agent: isopropanol=8: 78.65:3.2:0.1:0.05:10.
according to the embodiment, the low-precipitation polyester film with the thickness of 85-90nm is prepared by a coating method in the preparation process of the moisture-heat resistant low-precipitation polyester film.
In the above embodiments, silica sol, polyoxyethylene alkylphenol ether wetting agent, and isopropyl alcohol are coating aids for improving the openness and wettability, and the types and amounts are not specifically required, and belong to the types and amounts notified by those skilled in the art.
Comparative example 1:
the comparative example was made into a 125 μm polyester film according to the above polyester film production process, the film, the surface was not coated with an anti-bleeding coating.
Comparative example 2:
this comparative example was a commercially available raw material type anti-precipitation product, and the thickness was selected to be 125. Mu.m.
The thickness of the polyester film in the above examples and comparative examples is not limited, and the polyester film is applicable to any common thickness specification.
Performance tests were conducted on the low-precipitation polyester base films prepared in examples 1 to 6 and comparative examples 1 to 2; the test method of the correlation performance is as follows:
1. baking test at 150℃for 3X 1h
The polyester films of examples 1 to 6 and comparative examples 1 to 2 were subjected to a BYK haze test by a haze meter, baked at 150℃for 1 hour in an oven, taken out of the oven, subjected to a room temperature test by a haze test, baked at 150℃for 1 hour in an oven again, taken out of the oven, subjected to a haze test by a film test, and repeated 3 times to calculate a difference DeltaH from the initial haze.
The bake test data are shown in table 1.
Table 1:
according to the data in the table, the haze change values before and after baking of the comparative examples 1 to 6 and the comparative example 1 can obtain better high-temperature anti-precipitation performance by coating the anti-precipitation coating on the surface of the polyester film, the haze increase caused by precipitation of the oligomer on the surface of the film is reduced, and meanwhile, the light transmittance is obviously increased after the coating is applied.
The haze change values before and after baking of comparative examples 1 to 6 and comparative example 2 are remarkably superior to those of the polyester film with low precipitation resistance to wet heat by the coating method and high temperature precipitation resistance by the coating method to those of the polyester film with high precipitation resistance by the commercially available raw materials.
The haze change values before and after baking in comparative examples 1 to 4 increased the thickness of the anti-precipitation coating, improved the high temperature anti-precipitation property to some extent, and the increase width became smaller after the coating reached a certain thickness.
The haze change values before and after baking in comparative examples 3 and 5 are improved to a certain extent by adding the crosslinking agent; comparative example 3 and example 6 show haze change values before and after baking, and excessive addition of the crosslinking agent is not beneficial to improving high temperature anti-precipitation performance.
2. Dual 85 environmental test
The polyester films of examples 1 to 6 and comparative examples 1 to 2 were bonded with an acrylic adhesive film, and then placed in a high and low temperature damp-heat test box for Beijing Zhongke ring test, the temperature was set at 85℃and the humidity was set at 85%, and the polyester films were taken out every 24 hours to see whether or not dot-like precipitation occurred on the bonding surface of the film surface and the acrylic adhesive film.
Double 85 environmental test data are shown in table 2.
Table 2:
according to the data in the table, the double-85-loop test precipitation results of comparative examples 1-6 and comparative example 1 show that the coating method prepared by the invention has excellent wet heat resistance and low precipitation polyester film wet heat resistance; according to the double-85-ring test precipitation results of comparative examples 1-6 and comparative example 2, the wet heat resistant low-precipitation polyester film prepared by the coating method disclosed by the invention has remarkably better wet heat resistant precipitation performance than that of a commercially available raw material type anti-precipitation polyester base film.
According to the test results of double-85 rings in comparative examples 1-4, the thickness of the anti-precipitation coating is increased, and the wet heat resistance is correspondingly improved.
Comparing the results of the double 85 loop test of example 3 and example 5, the addition of the crosslinking agent can help to increase the wet heat resistance; comparative example 3 and example 6 double 85 ring test precipitation results, excessive addition of the crosslinking agent was not beneficial to improving wet heat resistance precipitation performance.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A wet-heat resistant low-precipitation polyester film prepared by a coating method is characterized in that: the anti-precipitation coating is coated on the surface of the polyester film by a coating technology, is formed by double-sided coating, high-temperature drying and solidification shaping of anti-precipitation coating liquid, and comprises a first anti-precipitation coating, a main film layer and a second anti-precipitation coating which are sequentially laminated, wherein the main film layer is an ABA three-layer co-extrusion structure polyester film;
the preparation steps of the anti-precipitation coating liquid are as follows:
a: adding water-soluble styrene-maleic anhydride copolymer into a stirring tank a, adding deionized water according to a proportion, starting stirring, controlling the temperature to be 15-35 ℃, controlling the rotating speed of a stirrer to be 500-3000rpm, and stirring for 15-30 min;
b: adding the cross-linking agent into a stirring tank b, adding deionized water according to the proportion, starting stirring, controlling the temperature to be 15-35 ℃, and stirring for 15-30 min at the rotating speed of 500-3000 rpm;
c: slowly adding the mixture in the stirring tank b into the stirring tank a, and continuously stirring for 15-30 min;
d: adding silica sol, wetting agent and isopropanol, continuously stirring for 15-30 min, and standing for 30-60 min after completion;
the weight fraction is as follows: 2 to 20 parts of water-soluble styrene-maleic anhydride copolymer, 40 to 90 parts of deionized water, 5 to 25 parts of isopropanol, 0.4 to 5 parts of cross-linking agent, 0.01 to 0.1 part of silica sol and 0.01 to 0.05 part of wetting agent;
the main film layer comprises 100 parts of polyester as the layer B, 30-95 parts of polyester and 5-70 parts of opening master batch as the layer A.
2. The low precipitation polyester film resistant to damp heat prepared by the coating method according to claim 1, wherein the low precipitation polyester film resistant to damp heat is characterized in that: the thickness of the first precipitation preventing coating and the second precipitation preventing coating is 20-150 nm, the total thickness of the main film layer is 25-360 mu m, the thickness of the layer A is 2-18 mu m, and the melting point of the polyester and the opening master batch is 255-265 ℃.
3. The low precipitation polyester film resistant to damp heat prepared by the coating method according to claim 1, wherein the low precipitation polyester film resistant to damp heat is characterized in that: the cross-linking agent is one or more of isocyanate cross-linking agent, carbodiimide cross-linking agent, oxazoline cross-linking agent and epoxy silane cross-linking agent;
the silica sol is aqueous silica sol, the aqueous silica sol is silicon dioxide, and the particle size is 30-120 nm;
the wetting agent is one or more of alkyl sulfate wetting agents, polyoxyethylene alkylphenol ether and silanol nonionic surfactants.
4. The low precipitation polyester film resistant to damp heat prepared by the coating method according to claim 2, wherein the low precipitation polyester film resistant to damp heat is characterized in that: the particle size of the open master batch is 0.5-5 mu m.
5. A method for preparing a coating-method humidity-heat-resistant low-precipitation polyester film, which is characterized in that: the method comprises the following steps:
s1: conveying the polyester of the polyester film main film layer B layer to a core layer extruder for melting according to the formula amount, conveying the polyester of the polyester film main film layer A layer and the uniform mixture of the opening master batch to the core layer extruder for melting, and co-extruding to obtain an ABA three-layer co-extrusion structure polyester film thick sheet;
s2: cooling and casting an extruded ABA three-layer co-extrusion structure polyester film thick sheet;
s3: preheating a polyester film thick sheet at 60-90 ℃ and then longitudinally stretching to form a main film layer, wherein the stretching multiple is 2.5-4.0 times;
s4: performing on-line coating, performing double-sided coating on the longitudinally stretched membrane, uniformly coating the prepared precipitation-preventing coating liquid on the surface of the main membrane layer, and performing wet coating with the amount of 3-10 g/m 2 ；
S5: drying the coated sheet film in an oven to remove surface moisture, transversely stretching the sheet film at a stretching rate of 3.0-4.0 times and a stretching temperature of 110-160 ℃, and shaping the sheet film at a shaping temperature of 200-255 ℃ by using high temperature after the stretching is finished;
s6: and cooling and rolling the film to obtain the polyester film with low moisture and heat resistance and precipitation by a coating method.
6. The method for preparing the wet heat resistant low precipitation polyester film prepared by the coating method according to claim 5, wherein the method is characterized in that: in the step S4, for performing online coating, when coating is performed by adopting an offline coating method, steps S5 and S6 are directly performed after step S3, and after winding in step S6, the coating is performed by unreeling and passing through step S4 again, and then drying and winding are performed.
7. The method for preparing the wet heat resistant low precipitation polyester film prepared by the coating method according to claim 5, wherein the method is characterized in that: in the S4 coating, the coating mode is one of gravure roll coating and D-bar coating.
8. The method for preparing the wet heat resistant low precipitation polyester film prepared by the coating method according to claim 5, wherein the method is characterized in that: in the step S5, the coated sheet film enters an oven for drying, and the drying temperature is 90-120 ℃.
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