CN113683722A - Polyacrylate elastomer, hybrid network system material thereof and display screen protection film prepared from polyacrylate elastomer and hybrid network system material - Google Patents
Polyacrylate elastomer, hybrid network system material thereof and display screen protection film prepared from polyacrylate elastomer and hybrid network system material Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The invention relates to the technical field of display screen protection, in particular to a polyacrylate elastomer, a hybrid network system material thereof and a display screen protection film prepared from the polyacrylate elastomer and the hybrid network system material. The polyacrylate elastomer of the present invention is a random copolymer composed of a butyl acrylate repeating unit and an acrylate repeating unit containing a UPy group. The invention further provides a hybrid network system material formed by the polyacrylate elastomer and other elastomers. The polyacrylate elastomer and the hybrid network system material can be used for preparing a display screen protective film, and the prepared display screen protective film has good flexibility, light transmission performance, impact resistance, elastic recovery capability and adhesiveness. The screen protection device can be used for protecting novel screens such as 2.5D screens, 3D screens, curved screens and flexible folding screens. In the use, this protection film can be folded and folding be difficult to the crease that appears, has compromise the good protection effect and the good use of user experience to the display screen, has fine application prospect.
Description
Technical Field
The invention relates to the technical field of display screen protection, in particular to a polyacrylate elastomer, a hybrid network system material thereof and a display screen protection film prepared from the polyacrylate elastomer and the hybrid network system material.
Background
With the advancement of technology and the improvement of experience and requirements of consumers on the performance of electronic devices, the screens of many electronic devices are gradually developed to 2.5D, 3D, curved screens and flexible folding screens. The performance requirements and structure of the corresponding display screen protective film also need to be changed.
The display screen protective film is initially a single PET film, and then develops into a TPU film, a TPU and PET multilayer film, and the like. Aiming at a flexible film, the Chinese patent application CN201710567238.6 provides a flexible explosion-proof protective film, which comprises an upper protective film, an H/C, TPU, a silica gel layer and a release film which are sequentially overlapped from top to bottom, wherein the H/C is a hardened layer/protective layer, and the TPU is a thermoplastic polyurethane elastomer.
However, these conventional protective films have disadvantages in terms of high hardness, low adhesion, poor impact resistance, and difficulty in folding. When these protective films are used for a screen such as a folding screen or a flexible screen, there are disadvantages that a fold is likely to occur, the elastic recovery is poor, and the film is difficult to be folded outward. This not only severely affects the use experience of the electronic device, but also does not protect the screen well (Tsujimura t. oled display functions and applications [ M ]. John Wiley & Sons, 2017). In order to better apply the display screen protective film to novel screens such as 2.5D screens, 3D screens, curved screens, flexible folding screens and the like, a new display screen protective film material is urgently needed, the contradiction between the rigid protection performance requirement and the flexible bending (or folding) performance of the protective film is solved, and the screens are well protected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a polyacrylate elastomer, a hybrid network system material thereof and a display screen protective film prepared from the polyacrylate elastomer, and aims to provide a flexible protective film with excellent light transmission performance, very good impact resistance and damping performance, good elastic recovery capability and good fitting performance, so that novel screens such as a 2.5D screen, a 3D screen, a curved screen and a flexible folding screen are well protected.
A polyacrylate elastomer is a random copolymer composed of butyl acrylate repeating units and acrylate repeating units containing UPy groups,
the repeating unit of the butyl acrylate is
The acrylate repeating unit containing the UPy group is as follows:
wherein n is 1, 2 or 3, R is selected from hydroxyl, halogen or C1-C3At least one of alkyl groups, wherein the alkyl group may be further substituted with hydroxyl or halogen.
Preferably, the acrylate repeating unit containing a UPy group is:
Preferably, the content of the butyl acrylate repeating unit is 60-90 mol%, and the content of the acrylate repeating unit containing the UPy group is 10-40 mol%; and/or the number average molecular weight of the polyacrylate elastomer is more than or equal to 30000 g/mol.
Preferably, the polyacrylate elastomer is contained in an amount of 98 wt% or more, and the filler is selected from at least one of silica and white carbon black.
The invention also provides a polyacrylate elastomer hybrid network system material, which is a hybrid network system material formed by the polyacrylate elastomer and the damping elastomer material.
Preferably, the damping elastomer material is selected from at least one of polydimethylsiloxane, polysulfide elastomer or polyurethane elastomer, and/or the damping elastomer has a number average molecular weight of more than 30000 g/mol.
Preferably, the feed additive is prepared from the following raw materials in parts by weight: 50-95 parts of polyacrylate elastomer, 50-5 parts of damping elastomer material and a curing agent; the amount of the curing agent is 0.5-3 wt% of the damping elastomer material; the curing agent is at least one of DCP, silane coupling agent, bis-di-penta or platinum metal catalyst.
The invention also provides a display screen protective film which is prepared from the raw materials comprising the polyacrylate elastomer or the hybrid network system material.
Preferably, the transparent substrate layer comprises an elastomer layer and a transparent substrate layer; the elastomer layer is prepared from the polyacrylate elastomer or the hybrid network system material; the elastomer layer is compounded with one transparent substrate layer, or the elastomer layer is positioned between two transparent substrate layers.
Preferably, the thickness of the elastomer layer is 10 to 200 μm; and/or the thickness of the transparent substrate layer is 20-100 mu m; and/or the material for preparing the transparent substrate layer film is selected from at least one of polyethylene terephthalate, thermoplastic polyurethane or polycarbonate.
The invention also provides a preparation method of the display screen protective film, which is obtained by processing the polyacrylate elastomer or the hybrid network system material into an elastomer layer by a coating method or a mould pressing method and compounding the elastomer layer with a transparent substrate layer;
the solvent adopted by the coating method is at least one selected from methanol, ethanol, tetrahydrofuran, dichloromethane, chloroform, toluene or ethyl acetate.
In the invention, the specific steps of the coating method are as follows: the polyacrylate elastomer or the hybrid network system material is dissolved in an organic solvent to obtain a uniform and stable solution, and the solution is independently placed in a mold to volatilize the solvent to form a protective film, or the solution is placed on a layer of base material or between two layers of base materials to volatilize the solvent to form the protective film.
The mould pressing method comprises the following specific steps: the polyacrylate elastomer or the hybrid network system material is uniformly blended through a mechanical device, an elastomer layer with a single-layer structure is formed in a mould pressing mode, and then the elastomer layer is placed on a transparent substrate layer to form a protective film with a double-layer structure, or the elastomer layer is placed between two transparent substrate layers to form a protective film with a three-layer structure. The mechanical device for blending can be a double-roller machine, a three-roller machine, a kneader or an internal mixer, and the mechanical device for molding can be a molding press or a vulcanizing press.
The polyacrylate elastomer provided by the invention contains a large amount of UPy groups, and a large amount of hydrogen bonds in the UPy groups dissipate energy, so that the polyacrylate elastomer can play a role in buffering and impact resistance, and the material has good impact resistance, damping performance, elastic recovery capability and fitting property.
After the polyacrylate elastomer and the hybrid network system material formed by the polyacrylate elastomer are introduced into the flexible protective film, the obtained protective film has good flexibility, light transmission performance, impact resistance, elastic recovery capability and adhesiveness. In the use, this protection film can be folded and folding be difficult to the crease that appears, has compromise the good protection effect and the good use experience of user to the display screen.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 shows the result of the change of loss factor with temperature in DMA test of polyacrylate elastomer. It can be seen from the figure that the temperature range of the material with the loss factor of more than 0.3 is-40 ℃ to 60 ℃, the temperature range is wider, and the material shows excellent damping characteristics.
FIG. 2 shows the results of the storage modulus and loss modulus of polyacrylate elastomer with temperature change in the rheological test, and at normal temperature, the storage modulus of the material is 0.3MPa, showing good flexibility.
Fig. 3 shows the critical height of impact resistance of each of the display screen protective films of examples and comparative examples.
Fig. 4 is a graph showing the percentage improvement of the impact resistance of the protective films of the examples and comparative examples.
Detailed Description
The reagents and materials used in the following examples are not particularly limited and are commercially available.
EXAMPLE 1 polyacrylate elastomer
This example provides a random copolymer of butyl acrylate repeat units and acrylate repeat units containing a UPy-type group. The molecular structural formula is as follows:
wherein m is 45 and n is 104
The preparation method of the polyacrylate elastomer of this example is: an acrylate elastomer was synthesized by radical polymerization, and 70 parts of butyl acrylate, 30 parts of Upy monomer, 0.001 part of AIBN, and 0.2 part of ethyl acetate solvent were reacted at 70 ℃ for 12 hours. The molecular formula of Upy monomer is as follows:
the damping performance of the polyacrylate elastomer described in this example is tested by the method specified in ASTM E756-1993 standard, and the result is shown in fig. 1, wherein the temperature range of the loss factor higher than 0.3 is-50 ℃ to 60 ℃, and the temperature range is wider, which indicates that the material has excellent damping characteristics in a wide temperature range, and the test result indicates that the material has excellent damping performance. Meanwhile, the results of the change of the storage modulus and the loss modulus along with the temperature in the rheological test of the polyacrylate elastomer are shown in fig. 2, and the results show that the shear modulus of the material is lower, only 0.3MPa is obtained at normal temperature, and the material shows ultrahigh flexibility. The light transmittance and the haze of the material are tested by using the method specified in ASYM D1003-2007 standard, the light transmittance of the material is 95%, the haze is 1%, and the material has excellent transparent characteristics. The result of the bonding strength test was 12N/2.5 mm.
Example 2 protective film for display Screen
In this example, the polyacrylate elastomer of example 1 was used, 2g of the polyacrylate elastomer material was dissolved in 1ml of tetrahydrofuran solvent to obtain a polyacrylate elastomer tetrahydrofuran solution, the polyacrylate elastomer solution was poured onto a 50 μm-thick transparent PET plastic film (AQ 2ST31HC, St. Ex. electronics Co., Ltd., Suzhou) to obtain a protective film having a dry film thickness of 50 μm by precision coating, and the protective film was dried and cured in a vacuum oven at 80 ℃ for 2 to 3 hours with a release PET film (AQ-LX 3T, St. Ex. electronics Co., Suzhou) having a thickness of 50 μm attached to the surface of the coating to obtain a protective film for a display screen.
The critical height of the toughened glass with the thickness of 0.5mm, which is protected by the protective film, which can bear the free falling body of a small steel ball (the diameter is 10mm, and the weight is 4g) is 115 cm.
Example 3 protective film for display Screen
In this example, the polyacrylate elastomer of example 1 was used, 1g of the polyacrylate elastomer was dissolved in 1ml of tetrahydrofuran solvent together with 1g of polydimethylsiloxane (number average molecular weight 80000g/mol) and a small amount of curing agent DCP to obtain a mixed solution, the mixed solution was poured onto a 50 μm-thick transparent PET plastic film (AQ 2ST31HC, Inc.: Isuzu Elastu electronics Co., Ltd., product number: AQ2ST 31), a protective film having a dry film thickness of 50 μm was obtained by precision coating, and dried and cured in a vacuum oven at 80 ℃ for 2 to 3 hours, and a 50 μm-thick release PET (AQ-LX 3T, Inc.: Isuzu Elastu electronics Co., Ltd., product number: AQ-LX3T) was attached to the coating surface to obtain a display screen protective film.
The critical height of a 0.5mm thick tempered glass protected with the display screen protective film, which can withstand free fall of a small steel ball (diameter 10mm, weight 4g), is 101 cm.
Example 4 protective film for display Screen
In this example, the polyacrylate elastomer of example 1 was used, 1.99g of the polyacrylate elastomer and 0.01g of white carbon black were dissolved in 1ml of tetrahydrofuran solvent to obtain a mixed solution, the mixed solution was poured onto a 50 μm-thick transparent PET plastic film (AQ 2ST31HC, St. Ex. electronic Co., Ltd., Suzhou) to obtain a protective film having a dry film thickness of 50 μm by precision coating, and the protective film was dried and cured in a vacuum oven at 80 ℃ for 2 to 3 hours with a release PET (AQ-LX 3T, St. Ex. electronic Co., Ltd., Suzhou) having a coating thickness of 50 μm attached to the surface of the protective film to obtain a display screen protective film.
The critical height of 0.5mm of toughened glass protected with the display screen protective film, which can withstand the free fall of a small steel ball (diameter 10mm, weight 4g), is 109 cm.
Example 5 protective film for display Screen
In this example, the polyacrylate elastomer of example 1 was used, 10g of the polyacrylate elastomer was molded at 90 ℃ under a pressure of 10MPa for 20 minutes using a flat vulcanization machine to obtain a 50 μm-thick protective film, and the protective film was interposed between two 50 μm-thick transparent PET plastic films (manufactured by AQ2ST31HC, Ichho electronics Co., Ltd., Suzhou) to form a three-layer-structured protective film for a display screen.
The critical height of a 0.5mm thick tempered glass protected with the display screen protective film, which can withstand free fall of a small steel ball (diameter 10mm, weight 4g), is 121 cm.
Example 6 protective film for display Screen
In this example, the polyacrylate elastomer of example 1 was used, 5g of the polyacrylate elastomer, 5g of polydimethylsiloxane (number average molecular weight: 80000g/mol), and 0.01g of curing agent DCP were uniformly blended by a kneader, and then a 50 μm protective film was obtained by press molding at 120 ℃ and 10MPa for 20min by a flat vulcanizer, and was interposed between two 50 μm transparent PET plastic films (product model: AQ2ST31HC, Inc.: Suzhou Ituo electronics Co., Ltd.) to form a three-layer display screen protective film.
The critical height of a 0.5mm thick tempered glass protected with the display screen protective film, which can withstand free fall of a small steel ball (diameter 10mm, weight 4g), is 103 cm.
Comparative example 1 display screen protective film
2g of polyurethane elastomer material (number average molecular weight of 50000g/mol) is dissolved in 1ml of tetrahydrofuran solvent to obtain a polyurethane tetrahydrofuran solution, the solution is poured on a 50 mu m transparent PET plastic film (the company: Suzhou Eltu electronics Co., Ltd., product model: AQ2ST31HC), a precise coating mode is adopted to obtain a protective film with the dry film thickness of 50 mu m, the protective film is dried and cured for 2-3h in a vacuum oven at 80 ℃, and a release PET film (the company: Suzhou Eltu electronics Co., Ltd., product model: AQ-LX3T) with the thickness of 50 mu m is attached to the coating surface to obtain the polyurethane protective film.
The critical height of the toughened glass with the thickness of 0.5mm, which is protected by the protective film, which can bear the free falling body of a small steel ball (the diameter is 10mm, and the weight is 4g) is 86 cm.
Comparative example 2 display screen protective film
2g of polydimethylsiloxane material (number average molecular weight of 80000g/mol) and 0.004g of curing agent DCP are dissolved in 1ml of tetrahydrofuran solvent to obtain polydimethylsiloxane tetrahydrofuran solution, the polydimethylsiloxane solution is poured on a transparent PET plastic film (product model: AQ2ST31HC, Techno Eltrom electronics Co., Ltd.) with the thickness of 50 mu m, a protective film with the thickness of 50 mu m is obtained by adopting a precise coating mode, the protective film is dried and cured for 2 to 3 hours in a vacuum oven at the temperature of 80 ℃, and a release PET film (product: AQ-LX3T, Techno Eltrom electronics Co., Ltd.) with the thickness of 50 mu m is attached on the coating surface to obtain the polydimethylsiloxane protective film.
The critical height of 0.5mm of toughened glass protected by the protective film, which can bear the free fall of a small steel ball (diameter 10mm, weight 4g), is 96 cm.
Comparative example 3 display screen protective film
10g of a polyurethane elastomer material (number average molecular weight of 50000g/mol) was molded with a flat vulcanization press to obtain a 50 μm-thick protective film, and this was interposed between two 50 μm-thick transparent PET plastic films (manufactured by AQ2ST31HC, Isuzu electronics Co., Ltd., Suzhou) to form a three-layer-structured protective film.
The critical height of toughened glass with the thickness of 0.5mm, which is protected by the protective film, capable of bearing free fall of small steel balls (the diameter is 10mm, and the weight is 4g) is 89 cm.
Comparative example 4 display screen protective film
10g of polydimethylsiloxane material (number average molecular weight of 80000g/mol) elastomer material and 0.02g of curing agent DCP were uniformly blended by a kneader, and then a 50 μm-thick protective film was obtained by press molding using a flat vulcanizing machine, and was placed between two 50 μm transparent PET plastic films (manufactured by AQ2ST31HC, Isuzu electronics Co., Ltd.) to form a three-layer structure protective film.
The critical height of 0.5mm of toughened glass protected by the protective film, which can bear the free fall of a small steel ball (diameter 10mm, weight 4g), is 98 cm.
The impact resistance of the display screen protective films obtained in examples 2 to 6 and comparative examples 1 to 4 was tested by a method specified in ASTM D5628-2010, specifically, a falling steel ball (diameter 10mm, 4g) was used to impact a tempered glass with a thickness of 0.5mm, and the lowest height of the tempered glass at which cracks appear was used as the impact resistance critical height of the protective film to characterize the impact resistance of the display screen protective film.
The result shows that the toughened glass without any protective measures can bear the impact of a small steel ball falling freely at the position of 62cm at the maximum, and the critical height of the toughened glass is 62 cm; the test results of the display screen protective films obtained in examples 2 to 6 and comparative examples 1 to 4 are shown in fig. 3, 4 and the following table:
as can be seen from comparison of the impact resistance of the samples of example 2 and comparative examples 1 to 2, the impact resistance of the display screen protective film made of the polyacrylate elastomer of the present invention is significantly superior to that of the display screen protective film made of other elastomer materials. In addition, the impact resistance of the display screen protective film made of the material (example 2) added with other elastomers to form a hybrid network system and the material (example 3) added with fillers is also remarkably superior to that of the display screen protective film made of other elastomer materials. On the other hand, from the viewpoint of the manufacturing process, the impact resistance of the display screen protective film manufactured by the mold pressing process has better impact resistance than the display screen protective film manufactured by the coating process for the same material.
As can be seen from the above examples and comparative examples, the present invention provides a novel polyacrylate elastomer and a hybrid network system material formed by the polyacrylate elastomer and other elastomer materials, which can be used for preparing a display screen protective film having good flexibility, light transmission performance, impact resistance, elastic recovery capability and adhesion. The screen protection device can be used for protecting novel screens such as 2.5D screens, 3D screens, curved screens and flexible folding screens. In the use, this protection film can be folded and folding be difficult to the crease that appears, has compromise the good protection effect and the good use of user experience to the display screen, has fine application prospect.
Claims (10)
1. A polyacrylate elastomer which is a random copolymer comprising a repeating unit of butyl acrylate and a repeating unit of acrylate containing a UPy group,
the repeating unit of the butyl acrylate is
The acrylate repeating unit containing the UPy group is as follows:
wherein n is 1, 2 or 3, R is selected from hydroxyl, halogen or C1-C3At least one of alkyl groups, wherein the alkyl group may be further substituted with hydroxyl or halogen.
2. The polyacrylate elastomer according to claim 1, wherein: the acrylate repeating unit containing the UPy group is as follows:
3. The polyacrylate elastomer according to claim 1, wherein: the content of the butyl acrylate repeating unit is 60-90 mol%, and the content of the acrylate repeating unit containing the UPy group is 10-40 mol%; and/or the number average molecular weight of the polyacrylate elastomer is more than or equal to 30000 g/mol;
and/or, the polyacrylate elastomer is contained in an amount of more than or equal to 98 wt%, and the filler is selected from at least one of silicon dioxide or white carbon black.
4. A polyacrylate elastomer hybrid network system material is characterized in that: it is a hybrid network system material formed by the polyacrylate elastomer and the damping elastomer material according to any one of claims 1 to 3.
5. The hybrid network system material according to claim 4, wherein: the damping elastomer material is selected from at least one of polydimethylsiloxane, polysulfide elastomer or polyurethane elastomer, and/or the number average molecular weight of the damping elastomer is more than 30000 g/mol.
6. The hybrid network system material according to claim 4, which is prepared from the following raw materials in parts by weight: 50-95 parts of polyacrylate elastomer, 50-5 parts of damping elastomer material and a curing agent; the amount of the curing agent is 0.5-3 wt% of the damping elastomer material; the curing agent is at least one of DCP, silane coupling agent, bis-di-penta or platinum metal catalyst.
7. A display screen protective film is characterized in that: it is prepared from a raw material comprising the polyacrylate elastomer of any one of claims 1 to 3 or the hybrid network system material of any one of claims 4 to 6.
8. The display screen protective film according to claim 7, wherein: comprises an elastomer layer and a transparent substrate layer; the elastomer layer is prepared from the polyacrylate elastomer or the hybrid network system material; the elastomer layer is compounded with one transparent substrate layer, or the elastomer layer is positioned between two transparent substrate layers.
9. The display screen protective film according to claim 8, wherein: the thickness of the elastomer layer is 10-200 μm; and/or the thickness of the transparent substrate layer is 20-100 mu m; and/or the material for preparing the transparent substrate layer film is selected from at least one of polyethylene terephthalate, thermoplastic polyurethane or polycarbonate.
10. The method for producing a display screen protective film according to any one of claims 7 to 8, wherein: processing the polyacrylate elastomer or the hybrid network system material into an elastomer layer by a coating method or a mould pressing method, and compounding the elastomer layer with a transparent substrate layer to obtain the polyacrylate elastomer or the hybrid network system material;
the solvent adopted by the coating method is at least one selected from methanol, ethanol, tetrahydrofuran, dichloromethane, chloroform, toluene or ethyl acetate.
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| CN202110944094.8A CN113683722A (en) | 2021-08-17 | 2021-08-17 | Polyacrylate elastomer, hybrid network system material thereof and display screen protection film prepared from polyacrylate elastomer and hybrid network system material |
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| CN202110944094.8A CN113683722A (en) | 2021-08-17 | 2021-08-17 | Polyacrylate elastomer, hybrid network system material thereof and display screen protection film prepared from polyacrylate elastomer and hybrid network system material |
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| CN110105896A (en) * | 2019-06-18 | 2019-08-09 | 佛山固泰明科技有限公司 | A kind of curve screens protective film and preparation method thereof |
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| CN110105896A (en) * | 2019-06-18 | 2019-08-09 | 佛山固泰明科技有限公司 | A kind of curve screens protective film and preparation method thereof |
| CN111534244A (en) * | 2020-05-12 | 2020-08-14 | 江西蓝海芯科技集团有限公司 | Protective film applied to curved surface display screen |
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