CN112322208A - Preparation process of high-end release protection polyester base film for OCA (optical clear adhesive) - Google Patents
Preparation process of high-end release protection polyester base film for OCA (optical clear adhesive) Download PDFInfo
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- CN112322208A CN112322208A CN202011242241.9A CN202011242241A CN112322208A CN 112322208 A CN112322208 A CN 112322208A CN 202011242241 A CN202011242241 A CN 202011242241A CN 112322208 A CN112322208 A CN 112322208A
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- 230000003287 optical effect Effects 0.000 title claims abstract description 59
- 229920000728 polyester Polymers 0.000 title claims abstract description 36
- 239000000853 adhesive Substances 0.000 title claims abstract description 19
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 19
- 230000004224 protection Effects 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 19
- 239000010410 layer Substances 0.000 claims abstract description 17
- 239000012790 adhesive layer Substances 0.000 claims abstract description 7
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- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000013329 compounding Methods 0.000 claims abstract 2
- 239000004568 cement Substances 0.000 claims description 37
- 238000004519 manufacturing process Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
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- 238000005266 casting Methods 0.000 claims description 10
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 8
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- 229920000642 polymer Polymers 0.000 claims description 7
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- 229920005989 resin Polymers 0.000 claims description 6
- 238000009864 tensile test Methods 0.000 claims description 6
- 238000002834 transmittance Methods 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 5
- -1 polyethylene terephthalate Polymers 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 5
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a preparation process of a high-end release protection polyester base film for OCA optical adhesive, which comprises the OCA optical adhesive, wherein the OCA optical adhesive is produced in an ABA three-layer structure mode, when the OCA optical adhesive is adhered to a film, the thickness of a light release film is generally required to be 25-55 mu m, the release force is 5-20mm/g, the thickness of a heavy release film is 50-100 mu m, the release force is 30-110mm/g, the thickness of an adhesive layer is 45-100 mu m, and the Shore hardness is 40D-50D, when a customer needs electrostatic treatment, the viscosity of one surface of the film before coating is about 0mps and the solid content is about 95%, the obtained OCA optical adhesive has a better effect on the basis of ensuring the complete curing of each adhesive layer through compounding and superposing a plurality of adhesive layers, the invention has excellent optical appearance performance, excellent transparency and haze, impurities such as crystal points and white spots are not generated, and defects such as bubbles and foreign matters in the OCA can be observed without removing the protective film.
Description
Technical Field
The invention belongs to the technical field of liquid crystal display, and particularly relates to a preparation process of a high-end release protective polyester base film for OCA (optical clear adhesive).
Background
The OCA optical adhesive is one of raw materials of the touch screen, is the best adhesive of the touch screen, the optical acrylic pressure-sensitive adhesive is made into a base material, then the upper bottom layer and the lower bottom layer are respectively adhered with a layer of optical release film to form a double-sided adhesive tape, so that the normal image display of the liquid crystal panel has irreplaceable effect, and the OCA optical adhesive has the advantages of high cleanliness, high light transmittance, low haze, high adhesion, no crystal point, no bubble, water resistance, high temperature resistance, ultraviolet resistance and the like, has uniform thickness and high flatness, has the refractive index close to that of glass and PC, can not generate yellowing, aging, fogging, falling off of an adhered surface, bubble generation and the like after long-time use, greatly improves the adhering efficiency, reduces the production cost, and fundamentally solves the bottleneck of the difficult adhering problem of the touch screen panel and a large-size panel.
The high-end release type protective polyester base film material for OCA optical cement is monopolized by foreign enterprises for a long time due to high technology barriers, the brands established by fully pasting OCA optical cement of liquid crystal display enterprises and the like in China only comprise Japan and American companies at present, the market occupancy of the full pasting of the two brands is about more than 85 percent, the corresponding film material for OCA is monopolized by Korea, Japan and the like, but with the rapid increase of the OCA market, domestic OCA film material processing enterprises are also greatly popularized, mainly in Guangdong, Zhejiang, Jiangsu and the like, the national industry for protecting the polyester base film by the high-end release type polyester base film is at the stage, the strength is weak and is dispersed, basic research and development and aiming at optical performance are not yet developed, most domestic polyester film base film manufacturers are lack of key links and experience of manufacturing technical conditions, and the difference of raw materials makes the product only meet the low-end, in addition, the explosive growth of global smart phones, wearable intelligent products and touch screens brings unprecedented development space for OCA optical cement products. Therefore, the preparation process of the liquid crystal display screen needs to be improved, and the preparation process of the high-end release type protection polyester base film for the OCA optical cement is provided, so that the problems are solved better.
Disclosure of Invention
The invention aims to: in order to solve the problems, the preparation process of the high-end release protection polyester base film for the OCA optical cement is provided.
The technical scheme adopted by the invention is as follows:
the preparation process of the high-end release protection polyester base film for the OCA optical cement comprises the OCA optical cement, wherein the OCA optical cement is produced in an ABA three-layer structure mode, if a customer needs antistatic treatment, one surface of the OCA optical cement is subjected to online coating treatment, and the OCA optical cement is produced and operated as follows:
step one, preparing 90% FG600 (master batch) and 10% FG611 (additive) by a host machine, and preparing 45% FG804 (master batch) and 55% FG611 (opening agent) by a slave machine;
step two, preparing the optical cement (namely OCA) without a base material by the formula, and then respectively attaching a layer of release film to the upper bottom layer and the lower bottom layer;
and step three, the OCA glue exists in a semi-solid film form and is processed in a bonding mode.
In a preferred embodiment, when the OCA optical adhesive film is applied, the thickness of the light release film is generally 25 μm to 55 μm, the release force is 5 to 20mm/g, the thickness of the heavy release film is 50 μm to 100 μm, the release force is 30 to 110mm/g, the thickness of the adhesive layer is 45 μm to 100 μm, and the shore hardness is 40D to 50D, when a customer needs electrostatic treatment, the viscosity of one side of the film before coating is about 5500mps, the solid content is about 95%, the light transmittance is greater than 99%, and the haze is about 0.5 to 1%.
In a preferred embodiment, the technical performance index of the OCA optical cement is as follows: the heat shrinkage performance MD is less than or equal to 1.0%, the TD is less than or equal to 0.3%, the haze is less than or equal to 0.6% (38-125 um), the clarity is more than or equal to 93%, the roughness Ra is less than or equal to 45 um, the Rz is less than or equal to 650 um, and the Rmax is less than or equal to 850 um.
In a preferred embodiment, the production method of the high-end release protective polyester base film for the OCA optical cement requires the following experimental equipment during experimental operation: quartz glass plate, microscopic hot bench HS82 (thermal analysis bench + polarizing display mirror), digital measurement projector CPT-3025A, haze light transmittance tester AT-4725, darkness meter 6801, glossiness meter 4454-45, electronic thickness meter C1216; the device comprises a polarizer 9020, a research-grade microscope DM700M, a tensile testing machine, a silica gel roller, a Shore hardness tester, a friction coefficient instrument MXD-02, an electrostatic tester FMX-003, a double-light-source color matching platform SPS-80T, a drying box JGX-9146MBE, a high-pressure defoaming machine and a cut-off knife JDC-15M-10.
In a preferred embodiment, the high-end release-type protective polyester-based film resin slice for OCA optical cement is provided with a high polymer with a moisture absorption tendency, and the high polymer is subjected to pre-crystallization and drying treatment before biaxial stretching, so that the softening property of the polymer is improved, the resin particles are prevented from being adhered to each other and agglomerated in the drying, melting and extruding process, the moisture in the resin is removed, the polymer containing the base ester is prevented from being subjected to hydrolytic degradation and bubble generation in the melting and extruding process, the crystallization and drying temperature is 160-180 ℃, the crystallization time is 10-20min, the drying time is 4-8H, the dried polyethylene terephthalate polyester slice has the pre-crystallization degree of 35-42%, and the moisture content W (H, W) of the dried polyethylene terephthalate polyester slice2O)<30PPm。
In a preferred embodiment, the melt extrusion of the OCA optical adhesive high-end release protection polyester base film comprises an extruder, a melt metering pump and a melt filter, wherein the extruder mainly comprises a screw and a heated barrel, a crystallized and dried polyethylene terephthalate polyester chip enters the twin-screw extruder to be heated and melted, the temperature of the extruder is 210-280 ℃, the melt metering is realized by a high-precision gear pump, and the heating temperature of the metering pump is 270-280 ℃.
In a preferred embodiment, the polyester-based film casting system for high-end release protection of OCA optical cement comprises:
firstly, the die head directly determines the shape and thickness uniformity of the cast sheet, which is the key for casting the cast sheet, and the temperature of the die head is controlled at 260 ℃ and 280 ℃.
Secondly, the surface temperature of the quenching roller is uniform, the cooling effect is good, and secondly, the rotating speed of the quenching roller is required to be uniform and stable, and cooling water with the temperature of about 25-30 ℃ is introduced into the casting sheet roller to ensure that the casting sheet is cooled to 60 ℃.
And thirdly, longitudinal stretching, namely longitudinally stretching the polyester base film thick sheet from a sheet casting machine by 3.0-3.8 times through the speed difference between a slow drawing roller and a fast drawing roller in a heating state.
Transverse stretching, wherein the transverse stretching is carried out at a stretching ratio of 3.0-3.8, and the heat setting temperature is 190-210 ℃.
And fifthly, drawing and winding, wherein the film passes through a control pressure roller, a spreading auxiliary roller and a guide roller to finally complete winding.
Sixthly, cutting, packaging and warehousing.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, the high-end release type polyester base film for OCA optical cement adopts an ABA three-layer structure, creatively, a layer of OCA optical cement is added into the middle layer, and a layer of PET release film is respectively attached to two sides of the OCA adhesive. The PET release film actually plays a role in protection, and is a protective release film. According to the production requirement of the product, the PET release films on two sides can be made into a light release force film and a heavy release force film. Thickness of OCA is from type membrane for optical cement has 38, 50, 75, 100, 125um, and wherein 50um is given first place to, and upper and lower two-layer difference has again. The release force of the release film made according to different customer requirements is also of various types, from heavy type to extremely light type.
2. In the invention, the high-end release type protective polyester base film for OCA optical cement belongs to an upstream product in the technical field of liquid crystal display, in production, the performance structure of a product can be reasonably researched and developed according to the requirement of a downstream market on the performance index of the product, and the release film for OCA also strictly controls the production environment in the processing process, so that the phenomenon that external impurities and dust are adhered to the film to further influence the production of OCA is avoided. Meanwhile, the quality of the polyester film is also an important factor, and impurities and foreign matters in the film need to be strictly controlled in quantity and size. In addition, OCA high-end is also required to have fine light transmissivity and definition from type base film to whether have various defects in the inspection OCA glue. OCA optical cement high-end is from type protection base film can reduce the influence through the cleanliness factor of strict control processing workshop in the course of working on the one hand, and on the other hand also can be through improving the characteristic of film for example endowing antistatic properties, makes it difficult adhesion powder in the course of working to this performance that improves the product.
Drawings
FIG. 1 is a structural diagram of an OCA optical cement of the present invention;
FIG. 2 is a flow chart of the OCA-based membrane of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Visual inspection of
Test apparatus and method
A microscopic hot stage HS82 (thermal analysis stage + polarizing display mirror), a digital measurement projector CPT-3025A, and a black plate.
Visually detected, colorless and transparent, and has no any defects.
The sample is inclined by 20-45 degrees by visual inspection by using an illuminating lamp and a black plate, and the sample is observed to have the phenomena of foreign matters, concave-convex, bending, scratching and the like, if the phenomena can not be judged by visual inspection, a magnifying glass and the like can be used.
Example two
Lightness, chroma, haze test
Test apparatus and method
Testing the apparatus: quartz glass plate, microscopic hot stage, haze light transmittance tester AT-4725, and darkness meter 6801; a gloss meter 4454-45; electronic thickness gauge C1216; cut-off knife JDC-15M-10
The glass washed with the solution was calibrated with a spectrophotometer and a haze meter, and then the heavy release film was peeled off at 30mm of the peeled light release film on the laminated glass plate, and the lightness, chroma and haze were measured.
EXAMPLE III
Adhesion test
Test apparatus and method
Testing the equipment: quartz glass plate, tensile testing machine, silica gel roller, Shore hardness instrument, cut-off knife JDC-15M-10
Cutting 15mm of the sample, peeling off the light release film, attaching the light release film to a cleaned glass plate, peeling off the heavy release film, attaching a supporting body film, pressing a pressure roller three times by hand, and carrying out adhesion test by a tensile machine after 30min in a room under the test conditions of 180 degrees of peeling angle and 100mm/min of tensile speed.
Example four
Release force test
Test apparatus and method
Testing the equipment: quartz glass plate, tensile testing machine, silica gel roller, Shore hardness instrument, cut-off knife JDC-15M-10
And (3) peeling off the light release film, cutting off the sample by 20mm, attaching the film surface to a glass plate by using double-sided adhesive tape, and testing the peeling force of the light release film by using a tensile testing machine. Heavy release type stripping, cutting off a sample by 20mm, attaching a film surface to a glass plate by using double faced adhesive tape, and testing the stripping force of the light release type film by using a tensile testing machine under the testing conditions: the peeling angle is 180 degrees, and the pulling speed is 300 mm/min.
EXAMPLE five
Structural testing
Test apparatus and method
Testing the equipment: quartz glass plate, friction coefficient meter MXD-02; static tester FMX-003; the double-light source color matching stand SPS-80T; drying oven JGX-9146 MBE; a high-pressure defoaming machine, a silica gel roller and a cutter JDC-15M-10.
Cutting a sample with the size of 50 multiplied by 100mm, stripping a light release film, attaching the light release film to a glass plate cleaned by a solution, cutting redundant samples along the edge of the glass plate, stripping a heavy release film, attaching the heavy release film to the stripping plate cleaned by the solution, cutting redundant samples along the edge of the glass plate, putting the prepared AA sample structure sample into a high-pressure defoaming machine, keeping the temperature at 50 ℃, keeping the pressure at 6kg, defoaming for 30min, determining whether the sample has residual bubbles after defoaming, if not, keeping still for 12h, observing whether new bubbles are generated, and if not, filling OK at the corresponding glue section.
EXAMPLE six
The high-end release protective polyester base film for the OCA optical adhesive product of the invention is subjected to product test in downstream enterprises at home and abroad, and the test values are shown in tables 1-3:
table 1 shows the test values of SFP20 product in certain company of korea, which completely meet the use requirements of users.
TABLE 2 Guangdong client test results
Table 2 shows that the product SFP21 model completely meets the use requirements of users.
TABLE 3 Zhejiang customer test values, test product SFP22 product
The high-end release type protective polyester base film for the OCA optical cement of the invention needs to have the following characteristics:
the optical film has excellent optical appearance performance, excellent transparency and good haze, has no impurities such as crystal points and white points, and can realize that the defects such as bubbles and foreign matters in the OCA can be observed under the condition of not removing the protective film;
the release film has good adhesion performance to OCA glue, and the protective film cannot warp and fall off in the material transportation or processing process;
the weather resistance and the permanent adhesion stability are not obvious in peeling force increase for several days or longer, the OCA adhesive is easy to tear, no wire is drawn on the surface of the OCA adhesive, and the surface of the OCA is not damaged;
according to the requirements of products and different customers, the antistatic material can have antistatic performance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. The utility model provides a preparation technology of OCA optical cement is with high-end release protection polyester base film, includes OCA optical cement, its characterized in that: the OCA optical cement is produced in an ABA three-layer structure mode, if a customer needs antistatic treatment, one surface of the OCA optical cement is subjected to online coating treatment, and the OCA optical cement is produced as follows:
step one, preparing 90% FG600 (master batch) and 10% FG611 (additive) by a host machine, and preparing 45% FG804 (master batch) and 55% FG611 (opening agent) by a slave machine;
step two, preparing the optical cement (namely OCA) without a base material by the formula, and then respectively attaching a layer of release film to the upper bottom layer and the lower bottom layer;
and step three, the OCA glue exists in a semi-solid film form and is processed in a bonding mode.
2. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: when the OCA optical adhesive film is used, the thickness of a light release film is generally required to be 25-55 μm, the release force is 5-20mm/g, the thickness of a heavy release film is 50-100 μm, the release force is 30-110mm/g, the thickness of an adhesive layer is 45-100 μm, and the Shore hardness is 40D-50D, when a customer needs electrostatic treatment, the viscosity of one surface of the film before coating is about 5500mps, the solid content is about 95%, the light transmittance is greater than 99%, and the haze is about 0.5-1%, and the obtained OCA optical adhesive has a good effect by compounding and superposing multiple adhesive layers on the basis of ensuring that all the adhesive layers are completely cured.
3. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: the technical performance indexes of the OCA optical cement are as follows: the heat shrinkage performance MD is less than or equal to 1.0%, the TD is less than or equal to 0.3%, the haze is less than or equal to 0.6% (38-125 um), the clarity is more than or equal to 93%, the roughness Ra is less than or equal to 45 um, the Rz is less than or equal to 650 um, and the Rmax is less than or equal to 850 um.
4. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: the production method of the high-end release protective polyester base film for the OCA optical cement needs the following experimental equipment during experimental operation: quartz glass plate, microscopic hot bench HS82 (thermal analysis bench + polarizing display mirror), digital measurement projector CPT-3025A, haze light transmittance tester AT-4725, darkness meter 6801, glossiness meter 4454-45, electronic thickness meter C1216; the device comprises a polarizer 9020, a research-grade microscope DM700M, a tensile testing machine, a silica gel roller, a Shore hardness tester, a friction coefficient instrument MXD-02, an electrostatic tester FMX-003, a double-light-source color matching platform SPS-80T, a drying box JGX-9146MBE, a high-pressure defoaming machine and a cut-off knife JDC-15M-10.
5. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: the high-end release type protective polyester base film resin slice for the OCA optical adhesive has a moisture absorption tendency of high polymer, pre-crystallization and drying treatment are carried out before biaxial stretching, the softening property of the polymer is improved, the resin particles are prevented from being mutually adhered and agglomerated in the drying, melting and extruding process, the moisture in the resin is removed, the polymer containing base ester is prevented from being hydrolyzed and degraded and generating air bubbles in the melting and extruding process, the crystallization and drying temperature is 160-180 ℃, the crystallization time is 10-20min, and the drying time is 4-8H, the pre-crystallization degree reaches 35-42% and the moisture content W (H) of the dried polyethylene terephthalate polyester slice2O)<30PPm。
6. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: the melt extrusion of the high-end release protection polyester base film for the OCA optical adhesive comprises an extruder, a melt metering pump and a melt filter, wherein the extruder mainly comprises a screw and a heated barrel, a crystallized and dried polyethylene terephthalate polyester slice enters the twin-screw extruder to be heated and melted, the temperature of the extruder is 210-280 ℃, the melt metering is realized by a high-precision gear pump, and the heating temperature of the metering pump is 270-280 ℃.
7. The process for preparing the high-end release protective polyester base film for the OCA optical cement as claimed in claim 1, wherein: OCA optical cement is with high-end protection polyester base film system of casting of leaving type includes:
firstly, a die head directly determines the uniformity of the shape and the thickness of a cast sheet, which is the key for casting the cast sheet, and the temperature of the die head is controlled at 260 ℃ and 280 ℃;
secondly, the surface temperature of the quenching roller is uniform, the cooling effect is good, the rotating speed of the quenching roller is required to be uniform and stable, and cooling water with the temperature of about 25-30 ℃ is introduced into the casting sheet roller to ensure that the casting sheet is cooled to 60 ℃;
longitudinal stretching, wherein the longitudinal stretching is to longitudinally stretch the polyester base film thick sheet from a sheet casting machine by 3.0-3.8 times through the speed difference between a slow drawing roller and a fast drawing roller in a heating state;
transverse stretching, wherein the stretching ratio is 3.0-3.8, and the heat setting temperature is 190-210 ℃;
traction and winding, wherein the film passes through a control pressure roller, a spreading auxiliary roller and a guide roller to finally complete winding work;
sixthly, cutting, packaging and warehousing.
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CN202011242241.9A CN112322208A (en) | 2020-11-09 | 2020-11-09 | Preparation process of high-end release protection polyester base film for OCA (optical clear adhesive) |
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CN113071122A (en) * | 2021-04-06 | 2021-07-06 | 山东胜通光学材料科技有限公司 | Preparation process and equipment of base film for polarizer protective film |
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