CN112646323B - Low-glossiness matte polyester film and preparation method thereof - Google Patents
Low-glossiness matte polyester film and preparation method thereof Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/001—Combinations of extrusion moulding with other shaping operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/07—Flat, e.g. panels
- B29C48/08—Flat, e.g. panels flexible, e.g. films
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/24—All layers being polymeric
- B32B2250/244—All polymers belonging to those covered by group B32B27/36
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/408—Matt, dull surface
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
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- 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
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- C08K2003/2241—Titanium dioxide
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- 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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- 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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C08K2201/003—Additives being defined by their diameter
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- C08K3/34—Silicon-containing compounds
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- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/36—Silica
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Abstract
The invention discloses a low-glossiness matte polyester film, which is mainly obtained by melting, plasticizing, sheet casting and stretching a blend consisting of glossy polyester powder and a composite additive; the composite additive comprises inorganic powder and expandable microspheres with similar sizes. Compared with the conventional matte film with the same content, the gloss of the matte film added with the composite additive can be reduced by more than 20 percent, and the gloss of the matte film is 8.3 percent; the dosage of the composite additive is only 3-5% of the weight of the gloss polyester powder, and the problem of difficult post-processing stretching of the matte polyester film can be effectively improved while the low glossiness is ensured.
Description
Technical Field
The invention relates to a polyester film and a preparation method thereof, in particular to a low-glossiness matte polyester film and a preparation method thereof.
Background
The matte film has the characteristic of low surface gloss and comfortable visual sensation, and is generally prepared by performing melt extrusion and biaxial stretching on matte polyester master batches and main materials. When parallel light rays irradiate the surface of the film, the light rays can be divided into three parts: a part is absorbed; the other part is reflected by the surface of the film, so that regular reflection light is formed when the surface is flat, and diffuse reflection is formed when the surface is not flat; the third component is the parallel rays that enter the film surface. The low gloss characteristic of matte films is a result of the combination of surface specular, diffuse, and internal scattered emissions.
In order to reduce the glossiness of the matte film, chinese patent application No. CN 201679775.7 discloses a single-sided matte polyester film, which is prepared by blending 6% -10% of polyester master batch of inorganic additive and base material into a matte film layer, co-extruding the matte film layer and the base film layer to form the matte film layer, wherein the glossiness is less than 80%, and if the content of the additive in the matte film layer is too high, the subsequent tensile property is deteriorated. In the prior art, the compound additive is prepared by compounding nano-scale, sub-nano-scale and micron-scale additives, but nano-scale, sub-nano-scale and micron-scale powder is difficult to uniformly disperse when being blended. The Chinese patent with the application number of CN01810763160.X discloses a matte two-way stretching polyester film and a preparation method thereof, wherein a three-layer co-extrusion mode is adopted to prepare the matte film, a core layer is designed to be a matte layer, and a surface layer is designed to be the matte layer, although silica with different particle sizes is selected to replace silica with single particle size, the scattering effect can be improved, and the matte film is endowed with lower glossiness, but the difference of the two particle sizes of the silica with the particle size of 0.2-0.8 mu m and the particle size of 1-6 mu m is too large, and the silica is difficult to be uniformly mixed. Chinese patent No. CN201010185433.0 discloses a high transparent thick polyester film, which is obtained by biaxially stretching copolyester with low crystallization rate, and the film contains nano-scale, sub-nano-scale and micro-scale additives, although a film meeting higher requirements for optical performance can be prepared, the film is only limited to be a thick matte film (larger than 125 μm), and it is difficult to prepare a thin high-matte film.
Disclosure of Invention
The purpose of the invention is as follows: in view of the above problems, the present invention provides a matte polyester film having an improved scattering effect, a lower gloss, and a thinner thickness. Another object of the present invention is to provide a method for preparing the matte polyester film, which is easy to stretch.
The technical scheme is as follows: the low-glossiness matte polyester film is mainly obtained by melting, plasticizing, sheet casting and stretching a blend consisting of glossy polyester powder and a composite additive; the composite additive comprises inorganic powder and expandable microspheres with similar sizes.
Preferably, the amount of the composite additive is 3-5% of the weight of the bright polyester powder. When the addition amount of the composite additive is too small, the matte effect of the film is not obvious, and when the addition amount is too large, the processing difficulty is increased, and the thickness uniformity of the film is poor.
The inorganic powder is selected from silicon dioxide, titanium dioxide, barium sulfate, kaolin, calcium carbonate, montmorillonite or talc. Silica is preferred.
Preferably, the inorganic powder is submicron or micron inorganic powder, and the median of the particle size is 0.7-4.0 μm.
The shell of the expandable microsphere comprises but is not limited to thermoplastic high polymer prepared by polymerizing nitrile series, amide series or acrylate series monomers; the core layer of the expandable microsphere is an expanding agent, and the components of the expandable microsphere include, but are not limited to, aliphatic compounds.
Preferably, the median particle size of the expandable microspheres is from 2.0 to 4.0 μm.
The polyester film is a three-layer matt polyester film or a single-layer matt polyester film. Three-layer matt polyester films are preferred.
The preparation method for preparing the low-glossiness matte polyester film comprises the following steps: blending conventional matte polyester powder, glossy polyester powder and inorganic powder to obtain a matte film core layer blending material, blending the glossy polyester powder and a composite additive to obtain a matte film surface layer blending material, melting and plasticizing the matte film core layer blending material and the matte film surface layer blending material by a three-layer co-extrusion extruder, casting to obtain a three-layer matte polyester thick sheet, and performing biaxial tension process treatment on the thick sheet to obtain a three-layer matte polyester film; or blending the bright polyester powder and the composite additive, crystallizing, drying, melting, plasticizing and casting the blended material to obtain a single-layer matt polyester thick sheet, and then carrying out biaxial stretching process treatment on the thick sheet to obtain the single-layer matt polyester film. The melt extrusion and biaxial stretching process is the same as the preparation process of the conventional matte polyester film.
Compared with the prior art that the single type of additive is adopted for preparing the low-glossiness polyester film, the composite additive is adopted, and the submicron or micron-sized inorganic powder (0.7-4.0 mu m) and the expandable microspheres (2.0-4.0 mu m) have similar sizes and can be uniformly mixed. After melt extrusion, the size of the expanded expandable microspheres in the matte film surface layer is 8.0-12.0 microns, and the surface of the film is roughened by the smaller inorganic powder and the larger expandable microspheres, so that stronger diffuse reflection is generated, and the glossiness of the film can be effectively reduced. In addition, in order to obtain a polyester film with lower glossiness, the prior art generally adopts a method for increasing the addition amount of the additive, but the addition amount of the additive is too much, so that the stretching is difficult, the use amount of the composite additive is only 3-5% of the weight of the glossy polyester powder, the problem of difficult subsequent processing and stretching of the matte polyester film can be effectively improved by adding the modification component in an in-situ polymerization method, and the composite additive has potential economic and application prospects.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: compared with the conventional matte film with the same content, the gloss of the matte film added with the composite additive can be reduced by more than 20 percent, and the gloss of the matte film is 8.3 percent; the dosage of the composite additive is only 3-5% of the weight of the glossy polyester powder, and the problem of difficult subsequent processing and stretching of the matt polyester film can be effectively solved while the low glossiness is ensured.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Three-layer matt polyester film prepared by ABA three-layer co-extrusion extruder
Mixing conventional matte polyester with the silica content of 3.0% and bright polyester according to the proportion of 1.
Crushing the dried bright polyester into powder, weighing 1000g of bright polyester powder, 20g of silicon dioxide powder with the average particle size of 1.5 microns and 10g of expandable microsphere powder with the average particle size of 3.0 microns, mixing the three kinds of powder in a high-speed mixer for 20min to prepare a blended material serving as a matte film surface layer blended material, wherein the silicon dioxide powder and the expandable microspheres are used as composite additives in the surface layer, and the content of the composite additives in the surface layer is 3.0% (the composite additives account for the mass percent of the bright polyester powder). It should be noted that the outer shell of the expandable microsphere used in the present invention includes, but is not limited to, thermoplastic polymers prepared by polymerizing nitrile, amide or acrylate monomers; the core layer of the expandable microspheres is an expanding agent, and the components of the expandable microspheres include, but are not limited to, aliphatic compounds.
And respectively feeding the matte film surface layer blending material and the matte film core layer blending material by using an ABA three-layer co-extrusion extruder, and then melting, plasticizing and casting to obtain the three-layer matte polyester thick sheet with the thickness of 200 mu m. After the slab was left to stand for one day, the slab was subjected to stretching treatment in a biaxial stretcher under the conditions of a preheating temperature of 100 ℃ for 30 seconds, a stretching rate of 100% by 100% and a stretching magnification of 3.5 by 3.5 to obtain a three-layer matte polyester film having a thickness of 16.9 μm.
Example 2
A three-layer matte polyester film was prepared in the same manner as in example 1, except that 15g of both the silica powder and expandable microsphere powder were used in the surface layer, and the median particle size of the silica powder was 0.8. Mu.m.
The thickness of the prepared thick plate is 198 μm, and the thickness of the thin film is 17.0 μm.
Example 3
A three-layer matte polyester film was produced in the same manner as in example 1, except that the amounts of silica powder and expandable microsphere powder used in the surface layer were 10g and 20g, respectively, and the median particle size of the silica powder was 3.5. Mu.m.
The thickness of the prepared thick sheet is 204 μm, and the thickness of the thin film is 17.1 μm.
Example 4
A three-layer matte polyester film was prepared in the same manner as in example 1, except that the amounts of silica powder and expandable microsphere powder used in the surface layer were 45g and 5g, respectively, and the average particle size of the expandable microspheres was 2.0 μm.
The thickness of the prepared thick plate is 202 μm, and the thickness of the thin film is 17.0 μm.
Example 5
A three-layer matte polyester film was prepared in the same manner as in example 1, except that the amounts of silica powder and expandable microsphere powder used in the surface layer were 5g and 45g, respectively, and the average particle size of the expandable microspheres was 4.0. Mu.m.
The thickness of the prepared thick plate is 205 μm, and the thickness of the thin film is 17.2 μm.
Example 6
Single-layer matte polyester film prepared by adopting single-layer extruder
Crushing the dried bright polyester into powder, weighing 1000g of bright polyester powder, 20g of silicon dioxide powder with the average particle size of 1.5 mu m and 10g of expandable microsphere powder with the average particle size of 3.0 mu m, mixing the three kinds of powder in a high-speed mixer for 20min to prepare a blended material, pre-crystallizing and drying the blended material, melting and plasticizing the cast sheet to prepare the single-layer matt polyester thick sheet with the thickness of 197 mu m. After the slab was left for one day, the slab was subjected to a stretching treatment in a biaxial stretcher under the conditions of a preheating temperature of 100 ℃ for 30 seconds, a stretching rate of 100% by 100% and a stretching ratio of 3.5 by 3.5 to obtain a single-layer matt polyester film having a thickness of 16.7 μm.
Example 7
A three-layer matte polyester film was prepared in the same manner as in example 1, except that 10g and 20g of barium sulfate powder and expandable microsphere powder were used in the surface layer, respectively, and the median particle size of the barium sulfate powder was 4.0. Mu.m.
The thickness of the prepared thick sheet is 199 μm, and the thickness of the film is 16.9 μm.
Comparative example 1
A three-layer matte polyester film was produced in the same manner as in example 1, except that 30g of silica powder was used as the additive in the surface layer.
The thickness of the prepared thick plate is 202 μm, and the thickness of the thin film is 16.8 μm.
Comparative example 2
A matte film was produced in the same manner as in example 2, except that 30g of silica powder was used as the additive in the surface layer.
The thickness of the prepared thick plate is 206 μm, and the thickness of the thin film is 17.0 μm.
Comparative example 3
A three-layer matte polyester film was prepared in the same manner as in example 1, except that the barium sulfate powder and expandable microsphere powder were used in the surface layer in an amount of 10g and 10g, respectively, and the median particle diameters of the two additives were 0.5 μm and 1.0. Mu.m, respectively.
The thickness of the prepared thick plate is 203 μm, and the thickness of the thin film is 17.1 μm.
Comparative example 4
A matte film was prepared in the same manner as in example 2, except that barium sulfate powder and expandable microsphere powder were used in the surface layers, the amounts of the barium sulfate powder and the expandable microsphere powder were 30g and 30g, respectively, and the median particle diameters of the two additives were 5.0. Mu.m.
The thickness of the prepared thick sheet is 202 mu m, the drawing success rate is lower than that of other samples due to the high content of the additive in the biaxial drawing film forming process, the thickness of the film is 16.1 mu m-18.1 mu m, and the thickness uniformity is poor.
Comparative example 5
A matte film was prepared in the same manner as in example 7, except that the added amount of barium sulfate powder used in the surface layer was 30g.
The thickness of the prepared thick sheet is 200 μm, and the thickness of the thin film is 17.0 μm.
The raw material compositions and the performance parameters of the polyester films of the examples and the comparative examples are shown in Table 1.
TABLE 1 composition of raw materials and performance parameters of polyester film for examples and comparative examples
As shown in Table 1, the composite additive is added into the raw materials for preparing the matte polyester film, the inorganic powder and the expandable microspheres have similar sizes, so that the materials can be uniformly mixed in the blending process, the expandable microspheres are heated after the blending materials are melted and extruded to reach the glass transition temperature of the thermoplastic high polymer material forming the shell, the shell is softened and has plasticity, the shell of the microsphere is expanded due to the pressure generated by heating the low-boiling-point core layer in the microsphere, and the expandable microspheres are expanded to be 8.0-12.0 μm in size from the original 2.0-4.0 μm. The inorganic powder with smaller size of 0.7-4.0 μm and the expandable microspheres with large size of 8.0-12.0 μm cause the surface of the film to be rough, generate stronger diffuse reflection, and obtain the matte polyester film with lower glossiness (8.3-10.2%).
The content of the composite additive in the film of comparative example 3 is 2 percent and is less than the content limited by the invention by 3 to 5 percent, the median particle diameters of the barium sulfate powder and the expandable microspheres are respectively 0.5 mu m and 1.0 mu m and are also lower than the particle diameter size limit values of the invention (inorganic powder is 0.7 to 4.0 mu m and the expandable microspheres are 2.0 to 4.0 mu m), the glossiness of the prepared film is up to 20.7 percent, the content of the visible composite additive is too little, the particle diameter is too small, and the matte effect of the film is not obvious. Analysis of comparative example 4, the content of the composite additive in the film was 6% which is higher than the limit value of the present invention, although a good matte effect was obtained, the gloss was 8.1%, but since the content of the composite additive was too large, it was equivalent to that a large amount of impurity components having a large particle size difference existed in the inside of the film substrate, which resulted in an increase in the difficulty of stretching during the processing and a deterioration in the thickness uniformity of the film (16.1 to 18.0 μm).
Comparing example 3 with example 7, when barium sulfate is selected as the inorganic powder, the matte effect is inferior to that of silica, and therefore, silica is preferable as the inorganic powder of the present invention.
Compared with the thick matte film with the thickness of more than 125 mu m prepared by the prior art, the polyester film prepared by the invention has the thickness of 16.7-17.2 mu m and is a thin high-matte film.
Under the premise of the same other formulas and process conditions and the same additive adding amount, the comparative examples 1 and 2 only add inorganic powder into the preparation raw materials, the glossiness of the film is 12.5-13.6%, which is obviously higher than that of the polyester film (8.3-10.2%) added with the composite additive in the examples 1-6; when barium sulfate is selected as the inorganic powder, the glossiness of the film of the comparative example 5 is up to 25.0 percent and is obviously higher than that of the polyester film added with the composite additive in the example 7 by 15.8 percent. It can be seen that, when the same inorganic powder is used, the gloss of the matte film containing the expandable microspheres is reduced by more than 20% compared with the matte film containing only the inorganic powder and the same additive.
Claims (4)
1. The low-glossiness matte polyester film is characterized in that the polyester film is mainly obtained by melting, plasticizing, sheet casting and stretching a blend consisting of glossy polyester powder and a composite additive; the composite additive comprises inorganic powder and expandable microspheres with similar sizes;
the using amount of the composite additive is 3-5% of the mass of the glossy polyester powder;
the inorganic powder is submicron or micron inorganic powder, and the median of the particle size is 0.7 to 4.0 mu m;
the shell of the expandable microsphere is a thermoplastic polymer prepared by polymerizing nitrile series, amide or acrylate monomers; the core layer of the expandable microsphere is an expanding agent, and the component of the expandable microsphere is an aliphatic compound;
the median of the particle size of the expandable microspheres is 2.0-4.0 mu m.
2. The low gloss matte polyester film according to claim 1, wherein the inorganic powder is selected from silica, titanium dioxide, barium sulfate, kaolin, calcium carbonate, montmorillonite or talc.
3. The low gloss matte polyester film according to claim 1, wherein the polyester film is a three-layer matte polyester film or a single-layer matte polyester film.
4. A method for preparing the low-gloss matte polyester film as claimed in any one of claims 1 to 3, which comprises the following steps: blending conventional matte polyester powder, glossy polyester powder and inorganic powder to obtain a matte film core layer blending material, blending the glossy polyester powder and a composite additive to obtain a matte film surface layer blending material, melting and plasticizing the matte film core layer blending material and the matte film surface layer blending material by a three-layer co-extrusion extruder, casting to obtain a three-layer matte polyester thick sheet, and performing biaxial tension process treatment on the thick sheet to obtain a three-layer matte polyester film; or blending the bright polyester powder and the composite additive, crystallizing, drying, melting, plasticizing and casting the blended material to obtain a single-layer matt polyester thick sheet, and then carrying out biaxial stretching process treatment on the thick sheet to obtain the single-layer matt polyester film.
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