CN107815045B - Wear-resistant polyvinylidene fluoride film - Google Patents
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- CN107815045B CN107815045B CN201710950475.0A CN201710950475A CN107815045B CN 107815045 B CN107815045 B CN 107815045B CN 201710950475 A CN201710950475 A CN 201710950475A CN 107815045 B CN107815045 B CN 107815045B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2433/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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Abstract
The invention relates to a wear-resistant polyvinylidene fluoride film and a preparation method thereof, belonging to the field of solar cells. The wear-resistant polyvinylidene fluoride film comprises the following components in parts by weight: 60-80 parts of polyvinylidene fluoride; 10-25 parts of polymethyl methacrylate; 1-15 parts of inorganic filler; 1-5 parts of a processing aid; 1-5 parts of wear-resistant auxiliary agent. The preparation method of the wear-resistant polyvinylidene fluoride film is an extrusion casting method. According to the invention, the organic modified silicone polymer is added as the wear-resistant auxiliary agent, so that the obtained vinylidene fluoride film has outstanding wear resistance, good mechanical property, weather resistance, cohesiveness and size stability, and is particularly suitable for being used on the back plate of the solar cell module packaging material.
Description
Technical Field
The invention relates to the field of solar cells, in particular to a wear-resistant polyvinylidene fluoride (PVDF) film for a solar cell back plate and a preparation method thereof.
Background
With the development of economic society, the traditional fossil energy sources such as coal, petroleum and natural gas are gradually reduced, and people are compelling to explore new energy sources. New energy sources such as solar energy, wind energy, biomass energy, hydroenergy, tidal energy and the like are increasingly paid more attention by people. Solar energy is energy generated by fusion of hydrogen atoms in the sun to release huge nuclear energy, is inexhaustible, clean and pollution-free, and is most concerned by a plurality of new energy sources.
In recent years, the solar power generation industry has developed explosively, but many problems have arisen, and among them, the quality of the back sheet has received much attention. Since the solar cell module is exposed to a severe outdoor environment for a long time, severe requirements are imposed on the performance of the solar cell backsheet, and high weather resistance, adhesion, barrier property, and the like are required. In addition, most of the centralized power station projects in China are located in western regions such as inner Mongolia, Qinghai, Ningxia and Xinjiang, the wind sand is generally large in the regions, sand can impact the back plate continuously under the action of wind, and the outer layer of the back plate can be abraded, cracked, perforated and shed after a long time. After the backplate skin is destroyed, the PET hydrolysis ageing of intermediate level will aggravate, and then causes whole backplate quality to receive serious damage, inside steam gets into the subassembly for subassembly generating efficiency greatly reduced, the life-span is discounted greatly, consequently, has proposed higher requirement to the wear resistance of backplate.
At present, the back plates in the market mainly comprise a TPT type and a KPK type, and the outer layers of the corresponding back plates are a PVF film and a PVDF film. Therefore, the key to improving the wear resistance of the back plate is to improve the wear resistance of the outer film. In the prior art, much attention is paid to mechanical properties, weather resistance and adhesive properties of a PVDF film, and the research on the wear resistance of the PVDF film is less, for example, patent CN102604274A discloses a modified PVDF film for a solar cell back panel and a preparation method thereof, a polyolefin graft is added to improve the adhesive property of the PVDF film, but the wear resistance of the PVDF film is not related.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a PVDF film with excellent adhesion and weather resistance and high wear resistance for a solar cell back plate and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
on one hand, the invention provides a wear-resistant polyvinylidene fluoride film, which comprises the following components in parts by weight: 60-80 parts of polyvinylidene fluoride; 10-25 parts of polymethyl methacrylate; 1-15 parts of inorganic filler; 1-5 parts of a processing aid; 1-5 parts of wear-resistant auxiliary agent.
Further, the melt index of the polyvinylidene fluoride is 5-30g/10min, and the test conditions are as follows: 230 ℃ and 5 kg.
Further, the melt index of the polymethyl methacrylate is 2-25g/10min, and the test conditions are as follows: 230 ℃ and 5 kg.
Further, the inorganic filler is titanium dioxide, and the particle size of the inorganic filler is 0.1-1 mu m. Preferably, the particle size of the titanium dioxide is controlled to be 0.1 to 0.5 μm, for example: 0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, or the like.
Further, the processing aid is an acrylic ester impact modifier, and specifically includes: methyl methacrylate-butadiene-styrene terpolymer (MBS); and a core-shell copolymer (ACR) in which a crosslinked alkyl acrylate is used as a core and a polyalkylmethacrylate is used as a shell, but the present invention is not limited to the above-mentioned acrylate polymers, and other acrylate polymers commonly used in the art to achieve the same effect may be used in the present invention.
Further, the wear-resistant auxiliary agent is an organic modified silicone polymer. The organic modified silicone polymer is a silicone polymer containing organic modified groups on the side groups or the tail ends of the main chain of the silicone chain.
Preferably, the organo-modified silicone based polymer has a comb-type or linear structure. The comb-type or linear structure contains a plurality of modified groups on the main chain, which is beneficial to anchoring the silicone molecular chain.
Wherein, the comb type structure is as follows:
the linear structure is shown below:
wherein R is an organic modifying group; x, y, z and n are 1-5000.
Furthermore, the organic modifying group is one or more of acrylic group, hydroxyl group, carboxyl group, epoxy group, alkyl group and amino group.
Preferably, the organic modifying group is one or both of a hydroxyl group and an alkyl group.
On the other hand, the invention also provides a preparation method of the wear-resistant polyvinylidene fluoride film, which comprises the following steps:
(1) respectively adding 60-80 parts of polyvinylidene fluoride, 10-25 parts of polymethyl methacrylate, 1-15 parts of inorganic filler, 1-5 parts of processing aid and 1-5 parts of wear-resistant aid into a high-speed mixer for mechanical mixing;
(2) melting and granulating the mixed materials through a double-screw extruder to obtain master batches;
(3) and extruding and casting the master batch by a single screw to obtain the wear-resistant polyvinylidene fluoride film.
Further, the mechanical mixing conditions in the step (1) are as follows: the mixing time is controlled to be 30min, and the rotating speed of the mixer is 800 r/min.
Further, the granulation conditions in the step (2) are as follows: the temperature of the extruder head is 180-240 ℃, and the screw rotating speed is 250 r/min.
Further, the extrusion casting conditions described in the step (3) are: the temperature of the die head of the extruder is 190-230 ℃, and the rotating speed of the screw is 30 r/min.
Definition of terms
All ranges cited herein are inclusive, unless expressly stated to the contrary. For example, the temperature of the extruder head is 180-240 ℃, which means that the value range of the extrusion temperature is more than or equal to 180 ℃ and less than or equal to 240 ℃.
The terms "a" or "an" are used herein to describe elements and components described herein. This is done merely for convenience and to provide a general sense of the scope of the invention. Such description should be understood to include one or at least one and the singular also includes the plural unless it is obvious that it is meant otherwise.
The numbers in this disclosure are approximate, regardless of whether the word "about" or "approximately" is used. The numerical value of the number may have differences of 1%, 2%, 5%, 7%, 8%, 10%, etc. Whenever a number with a value of N is disclosed, any number with a value of N +/-1%, N +/-2%, N +/-3%, N +/-5%, N +/-7%, N +/-8% or N +/-10% is explicitly disclosed, wherein "+/-" means plus or minus, and a range between N-10% and N + 10% is also disclosed.
The following definitions, as used herein, should be applied unless otherwise indicated. For the purposes of the present invention, the chemical elements are in accordance with the CAS version of the periodic Table of elements, and the 75 th version of the handbook of chemistry and Physics, 1994. In addition, general principles of Organic Chemistry can be found in the descriptions of "Organic Chemistry", Thomas Sorrell, University Science Books, Sausaltito: 1999, and "March's Advanced Organic Chemistry" by Michael B.Smith and JerryMarch, John Wiley & Sons, New York:2007, the entire contents of which are incorporated herein by reference.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although methods and materials similar or equivalent to those described herein can also be used in the practice or testing of embodiments of the present invention, suitable methods and materials are described below. All publications, patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety, unless a specific paragraph is cited. In case of conflict, the present specification, including definitions, will control. In addition, the materials, methods, and examples are illustrative only and not intended to be limiting.
The invention has the beneficial effects that:
(1) according to the invention, the organically modified silicone polymer is used as the wear-resistant auxiliary agent, on one hand, the main chemical structure of silicone is a silicon-oxygen bond, the stability of the silicon-oxygen bond is very high, and the film can have good wear resistance; on the other hand, after the silicone is organically modified, the organic modification group enhances the compatibility of the silicone and the PVDF resin matrix, and is beneficial to the dispersion of the silicone in the PVDF resin matrix, and meanwhile, the organic modification group can play a role in anchoring the silicone, so that the silicone is not migrated or precipitated, and the wear resistance of the film is further improved;
(2) the processing technology used by the invention is simple and is easy for industrialized continuous production.
Detailed Description
The following are preferred embodiments of the present invention, and the present invention is not limited to the following preferred embodiments. It should be noted that, for those skilled in the art, on the basis of the inventive concept herein, several variations and modifications are possible which fall within the scope of the invention, and for further description of the invention, reference is made to the following description of specific embodiments.
Description of materials:
polyvinylidene fluoride: HEVER201, melt index 25g/10min, test conditions: 5kg of milk origin Dongguang fluororesin Co., Ltd at 230 ℃;
polymethyl methacrylate: VDR, melt index 2.0g/10min test conditions: 230 ℃, 5kg, arkema;
titanium dioxide: r103, dupont, usa;
impact modifier: EXL2313, rocheus; m-701, Kazuno chemical industries, Japan;
wear-resistant auxiliary agent: TEGOMER H-Si6440P, TEGOMER 6848, winning Industrial group Co
Examples 1 to 4
A wear resistant polyvinylidene fluoride film was prepared according to the formulation in table 1 by the following steps:
(1) adding the components in the formula into a high-speed mixer, and mechanically stirring for 30min at the rotating speed of 800 r/min;
(2) melting and granulating the mixed materials through a double-screw extruder to obtain master batches, wherein the temperature of a machine head of the extruder is 180-240 ℃, and the rotating speed of a screw is 250 r/min;
(3) and extruding and casting the master batch by a single screw to obtain the wear-resistant polyvinylidene fluoride film, wherein the temperature of an extruder die head is 190-230 ℃, and the rotating speed of the screw is 30 r/min.
TABLE 1 examples 1-4 compositions of polyvinylidene fluoride film formulations and forming temperatures
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Polyvinylidene fluoride | 80 | 60 | 75 | 66 |
| Polymethyl methacrylate | 12 | 25 | 13 | 10 |
| Titanium dioxide | 5 | 10 | 5 | 15 |
| EXL2313 | 2 | 2 | 1 | 0 |
| M-701 | 0 | 0 | 1 | 5 |
| TEGOMER H-Si6440P | 1 | 3 | 0 | 2 |
| TEGOMER 6848 | 0 | 0 | 5 | 2 |
| Head temperature/deg.C of double screw extruder | 180 | 195 | 240 | 220 |
| Die temperature/. degree.C.for single screw extruders | 230 | 210 | 190 | 215 |
Example 5 Performance testing
Tensile strength, PCT 96h aging yellowing index, wear resistance, thermal shrinkage and cohesiveness of commercially available PVDF films and the PVDF films obtained in examples 1-4 are tested, and the test results are shown in Table 2.
The tensile strength is tested according to the ASTM D882 standard, the aging yellowing index of PCT 96h is tested by adopting a spectroscopic tester, the wear resistance is tested according to the ASTM D968-15 standard after the sample is aged for PCT 96h, and the adhesion test is to test the peel strength after the PVDF and the PET adhesive are bonded and compounded.
TABLE 2 Performance testing of polyvinylidene fluoride films
| Test items | Commercial PVDF backsheet films | Example 1 | Example 2 | Example 3 | Example 4 |
| Thickness/mum | 25 | 25 | 25 | 25 | 25 |
| Tensile strength/MPa | 40 | 52 | 45 | 48 | 44 |
| PCT 96h aging yellowing index | 2.5 | 1.5 | 1.3 | 2.1 | 1.8 |
| Abrasion resistance/L | 78 | 92 | 104 | 115 | 108 |
| Thermal shrinkage/% | 1.4 | 1.1 | 0.8 | 1.2 | 0.6 |
| Peel strength/N/15 mm | 11.3 | 12.1 | 12.9 | 11.6 | 12.5 |
From the test results in table 2, it can be seen that after the wear-resistant auxiliary is added, the wear resistance of the PVDF films prepared in examples 1 to 4 is significantly better than that of the commercially available PVDF backsheet film, and the PVDF films are excellent in tensile strength, aging resistance, heat shrinkage and adhesiveness.
Claims (7)
1. The wear-resistant polyvinylidene fluoride film is characterized by comprising the following components in parts by weight: 60-80 parts of polyvinylidene fluoride; 10-25 parts of polymethyl methacrylate; 1-15 parts of inorganic filler; 1-5 parts of a processing aid; 1-5 parts of a wear-resistant auxiliary agent;
the wear-resistant auxiliary agent is an organic modified silicone polymer, and the organic modified silicone polymer has a comb-shaped or linear structure; wherein the content of the first and second substances,
the comb-shaped structure is as follows:
the linear structure is:
wherein R is an organic modifying group; x, y, z and n are 1-5000;
the organic modified group is one or more of acrylic group, hydroxyl group, carboxyl group and amino group.
2. The abrasion-resistant polyvinylidene fluoride film of claim 1, wherein the polyvinylidene fluoride has a melt index of 5 to 30g/10min, at 230 ℃ and 5 kg.
3. The abrasion-resistant polyvinylidene fluoride film of claim 1, wherein the polymethyl methacrylate has a melt index of 2 to 25g/10min, at 230 ℃ and 5 kg.
4. The abrasion-resistant polyvinylidene fluoride film of claim 1, wherein the inorganic filler is titanium dioxide having a particle size of 0.1 to 1 μm.
5. The abrasion-resistant polyvinylidene fluoride film of claim 1, wherein the processing aid is an acrylic impact modifier.
6. The method of making an abrasion resistant polyvinylidene fluoride film of any of claims 1-5, comprising:
(1) respectively adding 60-80 parts of polyvinylidene fluoride, 10-25 parts of polymethyl methacrylate, 1-15 parts of inorganic filler, 1-5 parts of processing aid and 1-5 parts of wear-resistant aid into a high-speed mixer for mechanical mixing;
(2) melting and granulating the mixed materials through a double-screw extruder to obtain master batches;
(3) and extruding and casting the master batch by a single screw to obtain the wear-resistant polyvinylidene fluoride film.
7. The method of preparing an abrasion-resistant polyvinylidene fluoride film according to claim 6, wherein the mechanical mixing in step (1) is performed under the following conditions: the mixing time is controlled to be 30min, and the rotating speed of the mixer is 800 r/min; the granulation conditions in the step (2) are as follows: the temperature of the extruder head is 180-240 ℃, and the screw rotating speed is 250 r/min; the extrusion casting conditions in the step (3) are as follows: the temperature of the die head of the extruder is 190-230 ℃, and the rotating speed of the screw is 30 r/min.
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| CN104231496A (en) * | 2014-09-05 | 2014-12-24 | 东莞市长安东阳光铝业研发有限公司 | Method for preparing polyvinylidene fluoride film |
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| CN102796334A (en) * | 2012-09-12 | 2012-11-28 | 常州荣晟新材料科技有限公司 | Flame-retardant polyvinylidene fluoride film and preparation method thereof |
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