CN112831161A - High-transparency toughening master batch for polyester sheet and preparation method and application thereof - Google Patents
High-transparency toughening master batch for polyester sheet and preparation method and application thereof Download PDFInfo
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/04—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to rubbers
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- 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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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Abstract
The invention belongs to the technical field of polyester sheets, and provides a high-transparency toughening master batch for a polyester sheet, and a preparation method and application thereof; the high-transparency toughening master batch for the polyester sheet is prepared by taking 45-78 parts of PET resin as a carrier, compounding 5-20 parts of TPEE material, 3-12 parts of epoxidized soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin and adding 0.1-0.5 part of antioxidant; the high-transparency toughening master batch for the polyester sheet can increase the toughness of the PET polyester sheet under the condition of ensuring that the transparency of the PET polyester sheet is less influenced, so that the PET polyester sheet with the characteristics of high transparency and high toughness is obtained, the application requirements of the market on the high-transparency high-toughness PET polyester sheet are met, and the application range of the PET polyester sheet can be expanded.
Description
Technical Field
The invention relates to the technical field of polyester sheets, in particular to a high-transparency toughening master batch for a polyester sheet, and a preparation method and application thereof.
Background
PET polyester sheets are used for food-grade blister boxes, cosmetic folding boxes, printed sheets, gift packaging boxes, and the like because of their superior optical properties, such as high light transmittance, high smoothness, and low halo, outstanding printability, and low cost, ease of production, and the like. However, pure PET polyester sheets are brittle and have insufficient impact resistance, limiting their wider use. Based on the above, the conventional method is to improve the impact resistance of the PET by toughening and modifying the PET, but the toughening and modification almost affects the transparency of the PET polyester sheet, and although the toughness of the PET polyester sheet is improved, the optical performance of the PET polyester sheet is reduced, but the application of the PET polyester sheet in the optical field is limited. Therefore, there is a need to develop a master batch with high transparency and high toughness, which can be added into a PET polyester sheet to meet the market demand for the PET polyester sheet with high transparency and high toughness.
Disclosure of Invention
One of the purposes of the invention is to provide a high-transparency toughening master batch for a polyester sheet, which is added into a PET polyester sheet to overcome the defect that the existing PET polyester sheet cannot have high transparency and high toughness.
The invention also aims to provide a preparation method of the high-transparency toughening master batch for the polyester sheet, which has a stable preparation process and is suitable for large-scale production, aiming at the defects of the prior art.
The third purpose of the invention is to solve the defects of the prior art, and the high-transparency toughening master batch for the polyester sheet is applied to the preparation of the PET polyester sheet, so that the obtained PET polyester sheet has the characteristics of high transparency and high toughness, and the application range of the PET polyester sheet can be expanded.
Based on the above, the invention discloses a high-transparency toughening master batch for polyester sheets, which is prepared from the following raw materials in parts by weight: the composition is characterized by comprising the following raw materials in parts by weight:
in the invention, a TPEE (thermoplastic polyester elastomer for short) material with the refractive index of 1.58 is specially selected, and the TPEE material is a linear block copolymer containing PBT (polybutylene terephthalate) polyester (crystalline phase) hard segment and aliphatic polyester or polyether (amorphous phase) soft segment, and has the elasticity of rubber and the strength of engineering plastics; thus, the TPEE material has polyester hard segment component of polybutylene terephthalate, so that the TPEE material has good compatibility with PET polyester material and similar material refractive index; the soft segment of the aliphatic polyester or polyether ensures that the rubber-like elastomer has flexibility; therefore, the inventors used this TPEE material as an impact resistance-modifying material. The refractive index of the calcium carbonate is 1.60, which is similar to that of the PET material, and tests show that the 50-150 nm-grade nano calcium carbonate has a good nucleating effect on the PET material, can accelerate the uniform crystallization of the PET material, and further increases the toughness and strength of the PET material. The high-quality epoxidized soybean oil is a low-cost plasticizer, and the high-quality epoxidized soybean oil is colorless transparent liquid and can ensure the light transmittance. And the MBS resin is a terpolymer of methyl methacrylate (M)/butadiene (B)/styrene (S), can be used as a plastic toughening agent and also has transparency.
In conclusion, the invention takes 45-78 parts of PET resin as a carrier, 5-20 parts of TPEE material, 3-12 parts of epoxidized soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin are compounded, 0.1-0.5 part of antioxidant is added, and the high-transparency toughening master batch for the polyester sheet can be prepared, and can be added into the PET polyester sheet, so that the transparency and toughness of the PET polyester sheet can be improved, the toughness of the PET polyester sheet can be increased under the condition of ensuring that the influence of the transparency of the PET polyester sheet is small, and the PET polyester sheet with the characteristics of high transparency and high toughness can be further obtained, so that the application requirements of the market on the high-transparency high-toughness PET sheet can be met, and the application range of the PET polyester sheet can be further expanded.
Preferably, the PET resin is a film-grade or bottle-grade special PET resin with the viscosity of 0.6-0.85.
Preferably, the TPEE material is a thermoplastic polyester elastomer with Shore hardness of D45-D60.
Preferably, the particle size of the nano calcium carbonate is 50-150 nm.
Preferably, the antioxidant is a complex of a hindered phenol antioxidant and a phosphite antioxidant.
The invention also discloses a preparation method of the high-transparency toughening master batch for the polyester sheet, which comprises the following preparation steps:
step S1, adding the PET resin, the TPEE material and the epoxidized soybean oil into a stirring barrel, and uniformly stirring at a low speed;
step S2, adding the nano calcium carbonate, the MBS resin and the antioxidant into the stirring barrel, and uniformly stirring at a low speed to obtain a mixed material;
and step S3, putting the mixed material into a discharging barrel of an extruder, starting feeding the mixed material, extruding, granulating, homogenizing and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
Preferably, in step S1, the low-speed stirring speed is 300 rpm, and the stirring time is 5 minutes.
Preferably, in step S2, the low-speed stirring speed is 300 rpm, and the stirring time is 10 minutes.
Preferably, in step S3, the extrusion granulation process parameters are as follows: the temperatures in the extruder zones were: the temperature of the first zone is 50 +/-10 ℃, the temperature of the second zone is 210 +/-10 ℃, the temperature of the third zone is 250 +/-10 ℃, the temperature of the fourth zone is 260 +/-10 ℃, the temperature of the fifth zone to the sixth zone is 270 +/-10 ℃, the temperature of the seventh zone is 265 +/-10 ℃, the temperature of the eighth zone to the ninth zone is 260 +/-10 ℃, the temperature of the tenth zone is 250 +/-10 ℃, the temperature of the eleventh zone is 255 +/-10 ℃ and the temperature of the head is 270 +/-10 ℃; the rotating speed of the screw is 350 +/-15 revolutions per minute, the feeding rotating speed is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before entering water is 15-20mm, the length of the material strip before entering water is 3-6m, and the temperature of the water front tank is 40 +/-10 ℃.
The invention also discloses an application of the high-transparency toughening master batch for the polyester sheet, and particularly relates to an application of the high-transparency toughening master batch for the polyester sheet in preparation of the PET polyester sheet.
Preferably, the polyester sheet is added with the high transparent toughening master batch at a weight percentage of 5% to prepare the PET polyester sheet.
Compared with the prior art, the invention at least comprises the following beneficial effects:
the invention utilizes the characteristics that the TPEE material and the PET polyester material have good compatibility and similar material refractive index; the nano calcium carbonate has a refractive index similar to that of the PET material, can play a good nucleating role on the PET material, and can increase the toughness and strength of the PET material; the plasticizing effect and the colorless and transparent characteristics of the high-quality epoxidized soybean oil; and the MBS resin has the characteristics of good toughening effect and transparency; the preparation method comprises the steps of compounding 5-20 parts of TPEE material, 3-12 parts of epoxidized soybean oil, 1-5 parts of nano calcium carbonate and 1-5 parts of MBS resin by using 45-78 parts of PET resin as a carrier, adding 0.1-0.5 part of antioxidant, and performing compound modification and concentrated granulation to obtain the high-transparency toughening master batch for the polyester sheet, wherein after the high-transparency toughening master batch for the polyester sheet is added into the PET material and is produced by an extrusion process to obtain the PET polyester sheet, the toughness of the PET polyester sheet product can be greatly improved, and the influence of the master batch on the transparency of the product is very small (the influence of the light transmittance is less than or equal to 1%).
Specifically, after the high-transparency toughening master batch for the polyester sheet is prepared by adding and extruding 5 weight percent of PET raw material into a PET sheet with the thickness of 300um, the light transmittance is 87.6 percent, the haze is 1.3 percent, the definition is 99 percent, and the PET sheet is not cracked by a ball drop test of 300g/1 m; after the high-transparency toughening master batch for the polyester sheet is added with an injection molding sample bar according to 5 weight percent of the PET raw material, the impact strength is 10.8KJ/M through testing2The elongation at break was 384%. In conclusion, in the PET polyester sheet product with the light transmittance of more than or equal to 85%, the falling ball test data and the impact test data are higher than the data requirements of the current market products, so that the application requirements of the market on the high-transparency high-toughness PET polyester sheet can be met.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the above objects, features and advantages more apparent and understandable.
Examples 1 to 4
The formulation of the high transparent toughening master batch for polyester sheets of examples 1-4 is shown in the following table 1:
TABLE 1
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 |
| PET resin | 45 portions of | 57 portions | 70.8 portions | 78 portions of |
| TPEE material | 5 portions of | 9 portions of | 18 portions of | 20 portions of |
| Epoxidized soybean oil | 3 portions of | 5 portions of | 5 portions of | 12 portions of |
| Nano calcium carbonate | 1 part of | 2 portions of | 3 portions of | 5 portions of |
| MBS resin | 1 part of | 2 portions of | 2 portions of | 5 portions of |
| Antioxidant agent | 0.2 part | 0.1 part | 0.2 part | 0.5 portion |
Wherein the PET resin is special PET resin with viscosity of 0.6-0.85 for film grade or bottle grade.
Wherein the TPEE material is thermoplastic polyester elastomer with Shore hardness of D45-D60.
Wherein the particle size of the nano calcium carbonate is 50-150 nm.
Wherein the antioxidant is a compound of hindered phenol antioxidant and phosphite antioxidant.
The preparation method of the highly transparent toughening master batch for the polyester sheets of the embodiments 1 to 4 includes the following preparation steps:
step one, mixing materials: adding PET resin, TPEE material and epoxy soybean oil into a stirring barrel, and stirring for 5 minutes at 300 revolutions per minute; adding nano calcium carbonate, MBS resin and antioxidant, and continuously stirring for 10 minutes at 300 revolutions per minute to obtain a mixed material;
step two, granulating, homogenizing and packaging: putting the mixed material obtained in the step one into a discharging barrel of an extruder, starting feeding the mixed material, and extruding and granulating; after obtaining the granules, opening a homogenizing stirring barrel for homogenizing for 10min before sampling or packaging; and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
Wherein the extrusion granulation process parameters are as follows: the temperatures in the extruder zones were: the temperature of the first zone is 50 +/-10 ℃, the temperature of the second zone is 210 +/-10 ℃, the temperature of the third zone is 250 +/-10 ℃, the temperature of the fourth zone is 260 +/-10 ℃, the temperature of the fifth zone to the sixth zone is 270 +/-10 ℃, the temperature of the seventh zone is 265 +/-10 ℃, the temperature of the eighth zone to the ninth zone is 260 +/-10 ℃, the temperature of the tenth zone is 250 +/-10 ℃, the temperature of the eleventh zone is 255 +/-10 ℃ and the temperature of the head is 270 +/-10 ℃; the rotating speed of the screw is 350 +/-15 revolutions per minute, the feeding rotating speed is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before entering water is 15-20mm, the length of the material strip before entering water is 3-6m, and the temperature of the water front tank is 40 +/-10 ℃.
Wherein, the granulation process requirements of the granules are as follows: the cut of the granular material is flat, the length is 2-3mm, and the granular material has no sticking knife, diamond-shaped granular material, impurity grains and color change.
The application of the high-transparency toughening master batch for the polyester sheets of the embodiments 1 to 4 is to add the high-transparency toughening master batch for the polyester sheets of the embodiments 1 to 4 according to the weight percentage of 5 percent of the PET raw material and extrude the mixture to obtain the PET polyester sheets.
Comparative examples 1 to 3
The formulation of the master batch of comparative examples 1 to 3, the preparation method and the use thereof were substantially the same as in example 3, with the following differences as shown in table 2 below:
TABLE 2
| Raw materials | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| PET resin | 70.8 portions | 70.8 portions | 70.8 portions |
| TPEE material | —— | 18 portions of | 18 portions of |
| Epoxidized soybean oil | 5 portions of | 5 portions of | 5 portions of |
| Nano calcium carbonate | 3 portions of | —— | 3 portions of |
| MBS resin | 2 portions of | 2 portions of | —— |
| Antioxidant agent | 0.2 part | 0.2 part | 0.2 part |
Performance testing
The master batches of examples 1-4 and comparative examples 1-3 were subjected to performance tests with reference to the standards GB T2410-2008, GB/1040-. Specifically, the master batches of examples 1 to 4 and comparative examples 1 to 3 were added in an amount of 5 wt% based on the PET raw material and extruded to prepare PET polyester sheets 300um thick, and the PET polyester sheets were subjected to an optical test and a ball drop test of 300g/1 m; adding the master batches of the examples 1-4 and the comparative examples 1-3 according to 5 weight percent of the PET raw material, respectively injecting sample strips, and carrying out performance test on the impact strength and the elongation at break of the sample strips; the test results are shown in tables 3-4 below.
TABLE 3
| Detecting items | Standard value | Example 1 | Example 2 | Example 3 | Example 4 |
| Light transmittance | ≥85％ | Conform to | Conform to | Conform to | Conform to |
| Haze degree | ≤2％ | Conform to | Conform to | Conform to | Conform to |
| Definition of | ≥98％ | Conform to | Conform to | Conform to | Conform to |
| Impact strength | ≥9KJ/M2 | Conform to | Conform to | Conform to | Conform to |
| Elongation at break | ≥200％ | Conform to | Conform to | Conform to | Conform to |
| Ball drop test | 300g/1m does not crack | Conform to | Conform to | Conform to | Conform to |
TABLE 4
| Detecting items | Comparative example 1 | Comparative example 2 | Comparative example 3 | Example 3 |
| Light transmittance | 87.8％ | 87.6％ | 87.6％ | 87.6％ |
| Haze degree | 1.2％ | 1.3％ | 1.3％ | 1.3％ |
| Definition of | 99％ | 99％ | 99％ | 99％ |
| Impact strength | 6.6％ | 8.5％ | 10.2％ | 10.8％ |
| Elongation at break | 405％ | 387％ | 377％ | 384％ |
| 300g/1m non-cracking in ball drop test | NG | NG | OK | OK |
As can be seen from tables 3-4, compared with comparative examples 1-3, after the high-transparency toughening master batch for the polyester sheet is added into a PET material and is produced by an extrusion process to obtain the PET polyester sheet, the toughness of the PET polyester sheet products can be greatly improved, the influence of the high-transparency toughening master batch for the polyester sheet on the transparency of the products is very small (the influence of the light transmittance is less than or equal to 1 percent), the application requirements of the market on the high-transparency high-toughness PET polyester sheet can be met, and the application range of the PET polyester sheet can be further expanded.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the embodiments of the invention.
The technical solutions provided by the present invention are described in detail above, and the principle and the implementation of the present invention are explained in this document by applying specific examples, and the descriptions of the above examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. The high-transparency toughening master batch for the polyester sheet is characterized by comprising the following raw materials in parts by weight:
45-78 parts of PET resin
5-20 parts of TPEE material
3-12 parts of epoxidized soybean oil
1-5 parts of nano calcium carbonate
1-5 parts of MBS resin
0.1-0.5 part of antioxidant.
2. The highly transparent toughening master batch for the polyester sheet according to claim 1, wherein the PET resin is a film-grade or bottle-grade special PET resin with a viscosity of 0.6-0.85.
3. The high-transparency toughening master batch for the polyester sheet according to claim 2, wherein the TPEE material is a thermoplastic polyester elastomer with Shore hardness of D45-D60.
4. The highly transparent toughening master batch for the polyester sheet according to claim 1, wherein the particle size of the nano calcium carbonate is 50-150 nm.
5. The high-transparency toughening master batch for the polyester sheet according to claim 1, wherein the antioxidant is a compound of a hindered phenol antioxidant and a phosphite antioxidant.
6. The preparation method of the high-transparency toughening master batch for the polyester sheet according to any one of claims 1 to 5, which is characterized by comprising the following preparation steps:
step S1, adding the PET resin, the TPEE material and the epoxidized soybean oil into a stirring barrel, and uniformly stirring at a low speed;
step S2, adding the nano calcium carbonate, the MBS resin and the antioxidant into the stirring barrel, and uniformly stirring at a low speed to obtain a mixed material;
and step S3, putting the mixed material into a discharging barrel of an extruder, starting feeding the mixed material, extruding, granulating, homogenizing and packaging to obtain the high-transparency toughening master batch for the polyester sheet.
7. The method for preparing the highly transparent toughening master batch for the polyester sheet according to claim 6, wherein in the step S1, the low-speed stirring speed is 300 revolutions per minute, and the stirring time is 5 minutes;
in step S2, the low-speed stirring speed is 300 rpm, and the stirring time is 10 minutes.
8. The method for preparing the highly transparent toughening master batch for the polyester sheet according to claim 6, wherein in the step S3, the extrusion granulation process parameters are as follows: the temperatures in the extruder zones were: the temperature of the first zone is 50 +/-10 ℃, the temperature of the second zone is 210 +/-10 ℃, the temperature of the third zone is 250 +/-10 ℃, the temperature of the fourth zone is 260 +/-10 ℃, the temperature of the fifth zone to the sixth zone is 270 +/-10 ℃, the temperature of the seventh zone is 265 +/-10 ℃, the temperature of the eighth zone to the ninth zone is 260 +/-10 ℃, the temperature of the tenth zone is 250 +/-10 ℃, the temperature of the eleventh zone is 255 +/-10 ℃ and the temperature of the head is 270 +/-10 ℃; the rotating speed of the screw is 350 +/-15 revolutions per minute, the feeding rotating speed is 100-120 revolutions per minute, the rotating speed of the granulator is 25-40 revolutions per minute, the vacuum degree is less than or equal to 1Mpa, the length of the material strip before entering water is 15-20mm, the length of the material strip before entering water is 3-6m, and the temperature of the water front tank is 40 +/-10 ℃.
9. The use of the highly transparent toughening master batch for the polyester sheet according to any one of claims 1 to 5, wherein the highly transparent toughening master batch for the polyester sheet is used for preparing a PET polyester sheet.
10. The use of the highly transparent toughening master batch for the polyester sheet according to claim 9, wherein the highly transparent toughening master batch for the polyester sheet is added in a weight percentage of 5% to prepare the PET polyester sheet.
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