CN109456716B - Optical composite film and preparation method thereof - Google Patents
Optical composite film and preparation method thereof Download PDFInfo
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- CN109456716B CN109456716B CN201811345625.6A CN201811345625A CN109456716B CN 109456716 B CN109456716 B CN 109456716B CN 201811345625 A CN201811345625 A CN 201811345625A CN 109456716 B CN109456716 B CN 109456716B
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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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- 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
- C09J2475/00—Presence of polyurethane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polyurethanes Or Polyureas (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses an optical composite film and a preparation method thereof. The optical composite film comprises an optical base film and a TPU glue layer arranged on the optical base film, wherein raw materials for preparing the TPU glue layer comprise polyol and at least two isocyanates with different molecular weights. The invention adopts at least two isocyanates with different molecular weights as the curing agents, the isocyanate with smaller molecular weight is easy to migrate to the surface of the adhesive layer in the heating process, so that the surface of the adhesive layer is firstly cured, and the isocyanate with large molecular weight is relatively slow in migration speed, limited by the cured adhesive layer and incapable of migrating upwards, and can be cured only below the cured adhesive layer, so that a TPU adhesive layer with more complete curing is obtained, and the performance of the optical composite film is more stable.
Description
Technical Field
The invention relates to an optical composite film and a preparation method thereof.
Background
Optical film materials benefit from their excellent optical properties and are widely used in the fields of optical material preparation, optoelectronic technology, and the like. However, the optical film has the defects of poor processability and mechanical property, and the like, and the application of the optical film in fields with high requirements on the processability of materials such as curved screens and foldability is greatly limited.
A thermoplastic polyurethane elastomer (TPU) film with better plasticity, flexibility and weather resistance is introduced and is attached to an optical film, so that the TPU optical composite film with excellent processing performance can be obtained. Because the TPU film has extremely strong viscosity, the single layer is easy to stick together when being curled in the laminating process, the later processing is not facilitated, and the TPU glue is coated on the surface of the optical film and solidified by adopting a coating mode, so that the problem can be effectively solved. However, when the coating thickness of the TPU paste is more than a certain critical value (e.g., 30 μm), the curing reaction of the TPU is difficult to be sufficiently performed, mainly because the difference between the curing degree of the surface layer and the curing degree of the primer layer is large. Therefore, when a TPU-optical film composite film material with a certain thickness is obtained by a coating mode, the problems of poor optical performance, incomplete curing, glue overflow and the like of a TPU glue layer exist.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an optical composite film and a preparation method thereof, which solve the problem of poor performance of a TPU glue layer caused by incomplete solidification of the TPU glue layer in the prior art.
According to one aspect of the invention, an optical composite film is provided, which comprises an optical base film and a TPU glue layer arranged on the optical base film, wherein the TPU glue layer is prepared from raw materials including polyol and at least two isocyanates with different molecular weights.
Further, the polyol is a diol and the isocyanate is a diisocyanate.
Further, in the raw materials for preparing the TPU glue layer, the molar ratio of isocyanate groups to hydroxyl groups is (0.8-1): 1.
further, the raw materials for preparing the TPU glue layer comprise at least three isocyanates with different molecular weights.
Further, the isocyanate is selected from at least two of: toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, lysine diisocyanate.
Further, the polyhydric alcohol comprises polyether glycol and polyester glycol, and the molar ratio of the polyether glycol to the polyester glycol is (0.5-2): 1.
further, the thickness of the TPU glue layer is 30-150 mu m.
Further, the optical base film is selected from one or more of the following films: polyethylene terephthalate, polycarbonate, polymethyl methacrylate, cellulose triacetate, cycloolefin polymer, super-birefringent polyester.
According to another aspect of the present invention, there is provided a method for preparing the above optical composite film, comprising the steps of:
s1, providing an optical base film;
and S2, coating the uniformly mixed polyol and at least two isocyanates with different molecular weights on the optical base film, and curing to form a TPU adhesive layer.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts at least two isocyanates with different molecular weights as curing agents, the isocyanates with smaller molecular weights are easy to migrate to the surface of the glue layer along with a solvent volatilization channel in the heating process, so that the surface of the glue layer is firstly cured, and the isocyanates with large molecular weights and slow migration speed are limited by the cured glue layer and can not migrate upwards any more, and can only be cured below the cured glue layer, thereby obtaining a TPU glue layer with more complete curing, and ensuring that the performance of the optical composite film is more stable.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The invention provides an optical composite film, which comprises an optical base film and a TPU adhesive layer arranged on the optical base film, wherein the raw materials for preparing the TPU adhesive layer comprise polyol and at least two isocyanates with different molecular weights.
In the prior art, a single isocyanate is usually adopted as a curing agent for a TPU glue layer, and when the thickness of the TPU glue layer reaches more than 30 micrometers, the phenomenon of incomplete curing inside the TPU glue layer exists. The inventors have found that the main reason for incomplete internal curing of TPU is that small molecular isocyanates migrate to the surface when heated, resulting in complete surface curing and incomplete internal curing. The invention adopts at least two isocyanates with different molecular weights as curing agents, the isocyanate with smaller molecular weight is easy to migrate to the surface of the adhesive layer in the heating process, so that the surface of the adhesive layer is firstly cured, and the isocyanate with slower migration speed and larger molecular weight is limited by the cured adhesive layer, can not migrate upwards and can only be cured below the cured adhesive layer, thereby obtaining the TPU adhesive layer with more complete curing.
The thickness of the TPU glue layer can be more than 30 microns, and when the thickness of the TPU glue layer reaches more than 50 microns, the TPU glue layer can be used for preparing a foldable composite film; when the thickness of the TPU subbing layer is less than 50 μm, the effect is mainly to improve the flexibility and processability of the optical film.
The invention also provides a preparation method of the optical composite film, which comprises the following steps:
s1, providing an optical base film;
and S2, coating the uniformly mixed polyol and at least two isocyanates with different molecular weights on the optical base film, and curing to form the TPU glue layer.
The polyol and the isocyanate with different molecular weights are coated on the optical base film in a coating mode, so that the adhesive force between the TPU adhesive layer and the optical base film is enhanced, the process is simplified, and the production yield is greatly improved. The TPU glue layer is formed in a thick coating mode, and due to the excellent flexibility performance of the TPU glue layer, the flexibility of the optical composite film is good, and the TPU glue layer can be applied to the field of foldable optical films.
In some embodiments, the polyol is a diol and the isocyanate is a diisocyanate.
In some embodiments, in the raw materials for preparing the TPU adhesive layer, the molar ratio of isocyanate groups to hydroxyl groups is (0.8-1): 1.
in some embodiments, the starting materials for making the TPU subbing layer include at least three different molecular weight isocyanates. More than three kinds of isocyanate with different molecular weights are added, so that complete curing of the TPU glue layer can be further ensured.
In some embodiments, the aforementioned isocyanates are selected from, but not limited to, at least two of the following: toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), dicyclohexylmethane diisocyanate (HMDI), Hexamethylene Diisocyanate (HDI), Lysine Diisocyanate (LDI).
In some embodiments, the polyol includes polyether diol and polyester diol, wherein the molar ratio of the polyether diol to the polyester diol is (0.5-2): 1. the polyether TPU has the advantages of high strength, hydrolysis resistance, high resilience and good low-temperature property, and the polyester TPU has better tensile property, flexibility, wear resistance, solvent resistance and high-temperature resistance. The TPU adhesive layer with excellent comprehensive performance can be obtained by mixing the polyether diol and the polyester diol according to a certain proportion.
In some embodiments, the thickness of the TPU glue layer is 30-150 μm.
The optical base film includes, but is not limited to, a composite film composed of one or more of the following films: polyethylene terephthalate (PET), Polycarbonate (PC), polymethyl methacrylate (PMMA), cellulose Triacetate (TAC), cycloolefin polymer (COP), super-birefringent polyester (SRF).
[ example 1 ]
The optical composite film is prepared by the following steps:
(1) providing a PET optical base film;
(2) the preparation method comprises the steps of uniformly mixing polyethylene glycol and poly (hexamethylene adipate) glycol ester at a molar ratio of 0.5:1, TDI and IPDI at a weight ratio of 3:2, and a molar ratio of isocyanate groups to hydroxyl groups of 0.8:1, coating the raw materials on a PET optical base film, and curing to obtain a TPU adhesive layer with a thickness of 30 mu m.
[ example 2 ]
The optical composite film is prepared by the following steps:
(1) providing a PC optical base film;
(2) uniformly mixing IPDI, MDI and HMDI with a molar ratio of 0.6:1 and poly (hexamethylene adipate) of 3:3:2, and a molar ratio of isocyanate group to hydroxyl group of 0.85:1, coating the raw materials on a PC optical base film, and curing to obtain a TPU adhesive layer with a thickness of 50 microns.
[ example 3 ]
The optical composite film is prepared by the following steps:
(1) providing a PMMA optical base film;
(2) the preparation method comprises the steps of taking polyethylene glycol and poly (hexamethylene adipate) with a molar ratio of 0.8:1, MDI, HMDI and HDI with a weight ratio of 3:10:2, and the molar ratio of isocyanate groups to hydroxyl groups of 0.9:1, uniformly mixing the raw materials, coating the mixture on a PMMA optical base film, and curing to obtain a TPU adhesive layer with the thickness of 65 micrometers.
[ example 4 ]
The optical composite film is prepared by the following steps:
(1) providing a TAC optical base film;
(2) the preparation method comprises the steps of taking polyethylene glycol and poly (hexanediol adipate) at a molar ratio of 1:1, taking HMDI, HDI and LDI at a weight ratio of 3:3:2, and uniformly mixing the raw materials at a molar ratio of isocyanate group to hydroxyl group of 0.95:1, coating the mixture on a TAC optical base film, and curing to obtain a TPU adhesive layer with the thickness of 80 microns.
[ example 5 ]
The optical composite film is prepared by the following steps:
(1) providing a COP optical base film;
(2) the preparation method comprises the steps of taking polyethylene glycol and poly (hexamethylene adipate) with a molar ratio of 1.2:1, taking HDI, LDI and TDI with a weight ratio of 3:10:2, taking the molar ratio of isocyanate groups to hydroxyl groups as 1:1, uniformly mixing the raw materials, coating the mixture on a COP optical basal membrane, and curing to obtain a TPU adhesive layer with the thickness of 90 mu m.
[ example 6 ]
The optical composite film is prepared by the following steps:
(1) providing an SRF optical base film;
(2) uniformly mixing and coating the raw materials of 1.5:1 polyethylene glycol and polyhexamethylene adipate with the weight ratio of LDI, TDI, IPDI and HDI of 3:3:2:2 and the molar ratio of isocyanate group to hydroxyl group of 0.9:1 on an SRF optical base film, and curing to obtain a TPU adhesive layer with the thickness of 120 mu m.
[ example 7 ]
The optical composite film is prepared by the following steps:
(1) providing a PET optical base film;
(2) the preparation method comprises the steps of taking polyethylene glycol and poly (hexamethylene adipate) with a molar ratio of 1.8:1, taking TDI, HDI and MDI with a weight ratio of 3:3:2, and taking the molar ratio of isocyanate groups to hydroxyl groups as 0.95:1, uniformly mixing the raw materials, coating the mixture on a PET optical base film, and curing to obtain a TPU adhesive layer with the thickness of 135 microns.
[ example 8 ]
The optical composite film is prepared by the following steps:
(1) providing a PMMA optical base film;
(2) uniformly mixing IPDI, HMDI, LDI and TDI which are used in a weight ratio of 3:3:2:2, and a molar ratio of isocyanate group to hydroxyl group is 0.85:1, coating the raw materials on a PMMA optical base film, and curing to obtain a TPU adhesive layer, wherein the thickness of the TPU adhesive layer is 150 microns.
The optical composite films prepared in examples 1 to 8 were subjected to the relevant performance tests, and the test results are shown in table 1.
TABLE 1
| Glue line thickness/mum | Light transmittance | Haze degree | △b/QUV 96h | High-temperature high-humidity grid | Water boiling grid | Hundred grids | |
| Example 1 | 30 | 91.8％ | 0.8％ | 0.7 | 100％ | 100％ | 100％ |
| Example 2 | 50 | 92.3％ | 0.5％ | 0.7 | 100％ | 100％ | 100％ |
| Example 3 | 65 | 91.6％ | 0.8％ | 0.9 | 100％ | 100％ | 100％ |
| Example 4 | 80 | 91％ | 0.7％ | 0.6 | 100％ | 100％ | 100％ |
| Example 5 | 90 | 91.2％ | 0.6％ | 0.5 | 100％ | 100％ | 100％ |
| Example 6 | 120 | 90.5％ | 0.8％ | 0.8 | 100％ | 100％ | 100％ |
| Example 7 | 135 | 90.7％ | 0.7％ | 0.9 | 100％ | 100％ | 100％ |
| Example 8 | 150 | 90％ | 0.9％ | 0.8 | 100％ | 100％ | 100％ |
Note that △ b/QUV 96h indicates the yellowing index of the material before and after 96 hours of QUV testing;
"high temperature and high humidity lattice" means: after being placed for 72 hours at the temperature of 60 ℃ and the humidity of 90 percent, a hundred-grid test is carried out;
"poaching hundreds grid" means: treating in boiling water for 60min, and performing a hundred-grid test;
"hundred lattices" means: the optical composite prepared was subjected to a hundred grid test.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (4)
1. An optical composite film is characterized by comprising an optical base film and a TPU glue layer arranged on the optical base film in a coating mode, wherein raw materials for preparing the TPU glue layer comprise polyol and isocyanate with different molecular weights;
the isocyanate is the combination of toluene diisocyanate, isophorone diisocyanate, dicyclohexylmethane diisocyanate and lysine diisocyanate; wherein the weight ratio of isophorone diisocyanate, dicyclohexylmethane diisocyanate, lysine diisocyanate and toluene diisocyanate is 3:3:2: 2;
the polyhydric alcohol comprises polyether dihydric alcohol and polyester dihydric alcohol, and the molar ratio of the polyether dihydric alcohol to the polyester dihydric alcohol is 2: 1;
the thickness of the TPU glue layer is 150 mu m.
2. The optical composite film according to claim 1, wherein the molar ratio of isocyanate group to hydroxyl group in the raw materials for preparing the TPU glue layer is (0.8-1): 1.
3. an optical composite film according to any of claims 1-2 wherein the optical base film is selected from one or more of the following: polyethylene terephthalate, polycarbonate, polymethyl methacrylate, cellulose triacetate, cycloolefin polymer, super-birefringent polyester.
4. A method of making an optical composite film according to any of claims 1-3 comprising the steps of:
s1, providing an optical base film;
and S2, coating the uniformly mixed polyol and isocyanate with different molecular weights on the optical base film, and curing to form a TPU adhesive layer.
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