CN114716796B - PET/LCP hybrid polyester film and preparation method thereof - Google Patents
PET/LCP hybrid polyester film and preparation method 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
- 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
- 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
- C08J2400/00—Characterised by the use of unspecified polymers
- C08J2400/12—Polymers characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5397—Phosphine oxides
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Abstract
The application relates to the technical field of polyester films, and particularly discloses a PET/LCP hybrid polyester film and a preparation method thereof. The PET/LCP hybrid polyester film comprises the following raw materials in percentage by weight: 80-98% of modified PET, 1-15% of LCP and 0.5-8% of antioxidant master batch; the preparation method comprises the following steps: mixing the modified PET, LCP and antioxidant master batch, uniformly stirring, heating for crystallization, and drying to obtain a mixture; and (3) melting the mixture, cooling the cast sheet, sequentially stretching the cast sheet longitudinally and transversely, shaping, and cooling to obtain the PET/LCP hybrid polyester film. The PET/LCP hybrid polyester film has the advantage of improving the heat resistance of the polyester film through the synergistic effect between the raw materials.
Description
Technical Field
The application relates to the technical field of polyester films, in particular to a PET/LCP hybrid polyester film and a preparation method thereof.
Background
The polyester film, also called PET, is a film material prepared by using polyethylene terephthalate as a raw material and adopting an extrusion method to prepare a thick sheet and stretching the thick sheet, and is widely applied to the glass fiber reinforced plastic industry, the building material industry, the printing industry and the medical and health. The polyester film has excellent comprehensive performance, high strength, good temperature resistance, high barrier property, chemical resistance and the like, is convenient to process and form, and can be widely applied to the fields of packaging, insulation, photoelectrons and the like, and only the productivity of China reaches 500 ten thousand tons/year.
However, the performance of the polyester film in some special fields needs to be further improved, for example, the polyester film can only be used as an E-class material as a motor insulating material, and the heat resistance of the polyester film required by B, F class is higher, so that the current polyester film cannot meet the requirements of B, F and other higher classes.
Disclosure of Invention
In order to improve the heat resistance of the polyester film, the application provides a PET/LCP hybrid polyester film and a preparation method thereof.
In a first aspect, the present application provides a PET/LCP hybrid polyester film, using the following technical scheme:
the PET/LCP hybrid polyester film comprises the following raw materials in percentage by weight: 80-98% of modified PET, 1-15% of LCP and 0.5-8% of antioxidant master batch, wherein the modified PET is prepared by modifying PET by adopting 2, 5-dihydroxyphenyl phosphine oxide.
By adopting the technical scheme, the PET/LCP hybrid polyester film not only can keep excellent mechanical properties of the polyester film, but also can improve the heat resistance of the polyester film through the synergistic effect of the raw materials, wherein the stiffness is 1.97-3.67mN.m, the heat deformation temperature is 122-184 ℃, the longitudinal tensile strength is 288-371MPa, and the transverse tensile strength is 281-342MPa.
PET is a base material of a polyester film, and has excellent mechanical properties, high rigidity, hardness and toughness, but poor high temperature resistance. The 2, 5-dihydroxyphenyl phosphine oxide has a flame retardant effect, and the high temperature resistance of PET can be enhanced by modifying PET with the 2, 5-dihydroxyphenyl phosphine oxide. Specifically, when the modified PET is subjected to high temperature or combustion, the 2, 5-dihydroxyphenyl phosphine oxide can generate a phosphoric acid or polyphosphoric acid adhesive layer film, and the phosphoric acid or polyphosphoric acid adhesive layer film is attached to the surface of the PET, so that the effect of isolating oxygen is achieved, the PET is prevented from being heated and decomposed, the PET is protected, and the heat resistance of the PET is further enhanced.
LCP is a generic name of liquid crystal polymer materials, and the molecules of the materials contain aromatic structures, so that the materials have good rigidity, high orientation degree, high strength and good heat resistance, and can be applied to raw materials of polyester films, so that the polyester films have good mechanical properties and can also enhance the heat resistance of the polyester films. The antioxidant master batch is applied to the raw materials of the polyester film, can play a role in resisting oxidation, and reduces surrounding oxygen when the polyester film is subjected to high temperature, and prevents the progress of combustion reaction, so that the heat resistance of the polyester film is improved.
As preferable: the material comprises the following raw materials in percentage by weight: 88-96% of modified PET, 7-12% of LCP and 1-5% of antioxidant master batch.
By adopting the technical scheme, the blending amount of the modified PET, the LCP and the antioxidant master batch is optimized, so that the polyester film can maintain excellent mechanical properties and improve the heat resistance of the polyester film.
As preferable: the modified PET is prepared by the following method: mixing 2, 5-dihydroxyphenyl phosphine oxide and PET, stirring uniformly, heating and melting, extruding, granulating and drying to obtain the modified PET.
Further, the modified PET is prepared by the following method: mixing 2, 5-dihydroxyphenyl phosphine oxide and PET, stirring for 20-30min, heating to 250-260 ℃, extruding, granulating, and drying at 50-70 ℃ for 1-2h to obtain modified PET.
By adopting the technical scheme, the preparation method is used for preparing the modified PET, so that the 2, 5-dihydroxyphenyl phosphine oxide and the PET are more uniformly mixed, the modified PET can better play a role, and the heat resistance of the polyester film can be improved.
As preferable: the addition amount of the 2, 5-dihydroxyphenyl phosphine oxide is 3-8wt% of PET.
The addition amount of the 2, 5-dihydroxyphenyl phosphine oxide is too small, so that the polyester film cannot achieve better heat resistance, the addition amount of the 2, 5-dihydroxyphenyl phosphine oxide is too large, the flame retardant effect is not very obvious, and the production cost can be greatly increased. By adopting the technical scheme, when the addition amount of the 2, 5-dihydroxyphenyl phosphine oxide is in the range, the cost is not greatly increased, and a better flame retardant effect is achieved, so that the heat resistance of the polyester film is improved.
As preferable: the antioxidant master batch is prepared by the following method: and uniformly mixing the antioxidant and PET, carrying out melt extrusion, and then bracing, granulating and drying to obtain the antioxidant master batch.
Further, the antioxidant master batch is prepared by the following method: mixing antioxidant and PET, stirring for 30-40min, melt extruding at 260-290 deg.C and vacuum degree less than 100mbar, bracing, granulating, and drying at 50-70 deg.C for 1-2 hr to obtain antioxidant master batch.
As preferable: the addition amount of the antioxidant in the antioxidant master batch is 10+/-0.1 weight percent.
By adopting the technical scheme, the antioxidant master batch is prepared by the preparation method, so that the mixing of the antioxidant and the PET is more uniform, the better play of the antioxidant master batch in the polyester film is facilitated, and the heat resistance of the polyester film is improved.
As preferable: the antioxidant is a mixture of hindered phenol antioxidants and phosphite antioxidants, and the weight ratio of the hindered phenol antioxidants to the phosphite antioxidants is 1:1.
Further, the hindered phenol antioxidant is one or more of antioxidant 1010 and antioxidant 1790, and the phosphite antioxidant is one or more of triphenyl phosphite, trinaphthalenyl phosphite and diphenyl phosphite-naphthalene.
Through adopting above-mentioned technical scheme, adopt hindered phenol antioxidant and phosphite ester antioxidant, hindered phenol oxidant can produce hydrogen peroxide and stable phenol oxygen free radical when the polyester film receives the high temperature, and the stability of phenol oxygen free radical can prevent that the antioxidant from consuming too soon because of direct oxidation, also can reduce chain transfer reaction to improve oxidation resistance. The phosphite antioxidant can decompose hydrogen peroxide, cut off chain growth reaction, further prevent oxidation reaction, and better play an antioxidant role through the synergistic effect between the hindered phenol antioxidant and the phosphite antioxidant, thereby improving the heat resistance of the polyester film.
In a second aspect, the present application provides a preparation method of a PET/LCP hybrid polyester film, which adopts the following technical scheme: the preparation method of the PET/LCP hybrid polyester film comprises the following steps:
s1: mixing the modified PET, LCP and antioxidant master batch, uniformly stirring, heating for crystallization, and drying to obtain a mixture;
s2: and (3) melting the mixture, cooling the cast sheet, sequentially stretching the cast sheet longitudinally and transversely, shaping, and cooling to obtain the PET/LCP hybrid polyester film.
Further, the preparation method of the PET/LCP hybrid polyester film comprises the following steps:
s1: mixing modified PET, LCP and antioxidant master batch, stirring for 1-2h, crystallizing at 165-175 deg.C for 15-25min, drying at 170-190 deg.C for 2-4h until water content is below 20ppm to obtain a mixture;
s2: heating the mixture to 290-320 ℃, carrying out melt extrusion, cooling to 20-30 ℃ for casting, then placing the casting at 100-120 ℃ for longitudinal stretching, heating to 130-150 ℃ for transverse stretching, shaping at 230-240 ℃ for 10-20s, and cooling at 50-70 ℃ for 1-2h to obtain the PET/LCP hybrid polyester film.
As preferable: the stretching ratio of the longitudinal stretching of the cast sheet in the step S2 is 2-3 times, and the stretching ratio of the transverse stretching of the cast sheet is 2.5-3 times.
Through adopting above-mentioned technical scheme, at first evenly mix modified PET, LCP, antioxidant master batch, then through melting, extrusion, cast piece, tensile, design, cooling, make hybrid polyester film, can make more even that mixes between each raw materials, help each raw materials better performance, be convenient for make polyester film keep good mechanical properties while still improve polyester film's heat resistance.
In summary, the present application includes at least one of the following beneficial technical effects:
1. as the 2, 5-dihydroxyphenyl phosphine oxide is adopted to modify PET, the 2, 5-dihydroxyphenyl phosphine oxide has good flame retardant property, and after the PET is modified, the high temperature resistance of the PET is enhanced, so that the polyester film not only maintains good mechanical property, but also has improved heat resistance, the stiffness can reach 3.67mN.m, the thermal deformation temperature reaches 184 ℃, the longitudinal tensile strength reaches 371MPa, and the transverse tensile strength reaches 342MPa.
2. The antioxidant master batch is preferably selected, has good antioxidant effect, and can be applied to raw materials of the polyester film to enhance the antioxidant performance of the polyester film, so that the heat resistance of the polyester film is improved.
Detailed Description
The present application is described in further detail below in conjunction with the detailed description.
Raw materials
PET has a viscosity of 0.65-0.5dL/g and a product number of 720805258; LCP model NC-301-B with melting point of 240-300 ℃;2, 5-dihydroxyphenyl phosphine oxide CAS number 13291-46-8, boiling point 537 ℃, density 1.34g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Antioxidant 1790 has molecular weight of 699, CAS number of 40601-76-1, melting point of 163-165 deg.C, boiling point of 793 deg.C; triphenyl phosphite CAS number 101-02-0, molecular weight 310, density 1.184g/mL, boiling point 360 ℃, melting point 22-24 ℃.
Preparation example
Preparation example 1
A modified PET prepared by the following method:
mixing 2, 5-dihydroxyphenyl phosphine oxide and PET, stirring for 25min, heating to 255 ℃, extruding, granulating, and drying at 60 ℃ for 1.5h to obtain modified PET; wherein the addition amount of the 2, 5-dihydroxyphenyl phosphine oxide is 3wt% of PET.
Preparation example 2
A modified PET was different from that of preparation example 1 in the amount of 2, 5-dihydroxyphenyl phosphine oxide added, and in preparation example 2, the amount of 2, 5-dihydroxyphenyl phosphine oxide added was 5% by weight based on PET.
Preparation example 3
A modified PET was different from preparation example 1 in the amount of 2, 5-dihydroxyphenyl phosphine oxide added, and in preparation example 3, the amount of 2, 5-dihydroxyphenyl phosphine oxide added was 8% by weight based on PET.
Preparation example 4
An antioxidant masterbatch is prepared by the following method:
mixing antioxidant and PET, stirring for 35min, melt-extruding at 275 deg.C under the condition of vacuum degree of 50mbar, bracing, granulating, and drying at 60 deg.C for 1.5 hr to obtain antioxidant master batch; wherein, the weight ratio of the antioxidant to the PET is 1:9, the antioxidant is the mixture of the antioxidant 1010 and triphenyl phosphite, and the weight ratio of the antioxidant 1010 to the triphenyl phosphite is 1:1.
examples
Example 1
The raw material ratio of the PET/LCP hybrid polyester film is shown in table 1.
The preparation method of the PET/LCP hybrid polyester film comprises the following steps:
s1: mixing the modified PET and LCP prepared in preparation example 1 and the antioxidant master batch prepared in preparation example 4, stirring for 1.5h, crystallizing at 170 ℃ for 20min, and drying at 180 ℃ for 3h until the water content is below 20ppm to obtain a mixture;
s2: heating the mixture to 315 ℃, carrying out melt extrusion, cooling to 25 ℃ for sheet casting, carrying out longitudinal stretching on the sheet casting at 115 ℃, heating to 140 ℃ for transverse stretching at 3 times, shaping at 240 ℃ for 15s, and cooling at 50 ℃ for 1.5h to obtain the PET/LCP hybrid polyester film.
Examples 2 to 6
A PET/LCP hybrid polyester film is different from example 1 in that the raw material ratios of the polyester films are shown in Table 1.
TABLE 1 examples 1-6 polyester films weight of raw materials (unit: kg)
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Modified PET | 80 | 88 | 96 | 98 | 80 | 88 |
| LCP | 12 | 11 | 1 | 1.5 | 15 | 7 |
| Antioxidant master batch | 8 | 1 | 3 | 0.5 | 5 | 5 |
Example 7
A PET/LCP hybrid polyester film is distinguished from example 5 in that the modified PET in example 7 is obtained using preparation example 2, and the source of the modified PET is different.
Example 8
A PET/LCP hybrid polyester film is distinguished from example 5 in that the modified PET in example 7 is obtained using preparation example 3, and the source of the modified PET is different.
Comparative example
Comparative example 1
A PET/LCP hybrid polyester film differs from example 1 in that the raw material of the polyester film is replaced with an equivalent amount of modified PET.
Comparative example 2
A PET/LCP hybrid polyester film is different from example 1 in that no antioxidant master batch is added to the raw materials of the polyester film.
Comparative example 3
A PET/LCP hybrid polyester film differs from example 1 in that triphenyl phosphite is replaced with an equivalent amount of antioxidant 1010 in the antioxidant masterbatch.
Comparative example 4
A PET/LCP hybrid polyester film differs from example 1 in that antioxidant 1010 is replaced in the antioxidant masterbatch with an equal amount of triphenyl phosphite.
Comparative example 5
A polyester film is prepared by the following steps:
crystallizing PET at 165 ℃, drying at 155 ℃ for 3 hours, heating to 250 ℃, carrying out melt extrusion, cooling to 22 ℃ for casting, then placing the casting at 85 ℃ for longitudinal stretching, wherein the stretching ratio is 3.5 times, heating to 120 ℃, carrying out transverse stretching, wherein the stretching ratio is 4.0 times, shaping at 235 ℃ for 15 seconds, and cooling at 75 ℃ for 1.5 hours to obtain the polyester film.
Performance test
The polyester films of examples 1 to 8 and comparative examples 1 to 5 were cut into a rectangle of 70mm X38 mm and 100 μm in thickness, and the following performance tests were conducted:
stiffness of: the stiffness of the polyester film was measured according to GB/T22364-2018 paper and paperboard bending stiffness measurement, and the detection results are shown in Table 2.
Heat distortion temperature: the heat distortion temperature of the polyester film was measured by DSC method, and the temperature rise rate was 5℃per minute, and the measurement results are shown in the table.
Tensile strength: the tensile strength of the polyester film was measured according to GB/T13022-1991 Plastic bag tensile Property test method, and the test results are shown in Table 2.
TABLE 2 detection results
As can be seen from Table 2, the PET/LCP hybrid polyester film of the present application can not only maintain excellent mechanical properties but also improve heat resistance of the polyester film by the synergistic effect between the raw materials, wherein the stiffness is 1.97-3.67mN.m, the heat deformation temperature is 122-184 ℃, the longitudinal tensile strength is 288-371MPa, and the transverse tensile strength is 281-342MPa.
As can be seen from the combination of example 1 and comparative example 1, the stiffness in example 1 is 1.97mN.m, the heat distortion temperature is 122 ℃, the longitudinal tensile strength is 288MPa, the transverse tensile strength is 281MPa, and the polyester film is superior to comparative example 1, and the modified PET is more suitable for the raw material of the polyester film, so that the heat resistance of the polyester film can be enhanced.
As can be seen from the combination of example 1 and comparative examples 2 to 4, the stiffness in example 1 was 1.97mN.m, the heat distortion temperature was 122 ℃, the longitudinal tensile strength was 288MPa, the transverse tensile strength was 281MPa, and the polyester film was superior to comparative examples 2 to 4, and it was shown that the use of a mixture of antioxidant 1010 and triphenyl phosphite as the raw material of the antioxidant master batch in the polyester film was more suitable, and the heat resistance of the polyester film was more improved by the synergistic effect between antioxidant 1010 and triphenyl phosphite.
As can be seen from the combination of example 1 and comparative example 5, the stiffness in example 1 is 1.97mN.m, the heat distortion temperature is 122 ℃, the longitudinal tensile strength is 288MPa, the transverse tensile strength is 281MPa, and the polyester film is more suitable to be obtained by hybridization of modified PET and LCP, so that the polyester film has excellent mechanical properties, excellent stiffness, excellent longitudinal tensile strength and excellent transverse tensile strength, and enhanced heat resistance.
As can be seen from examples 1 to 6, the stiffness of example 5 was 3.52mN.m, the heat distortion temperature was 170℃and the longitudinal tensile strength was 350MPa, and the transverse tensile strength was 320MPa, which is superior to other examples, indicating that the polyester film of example 5 was more suitable in the addition of the respective raw materials, and not only was the polyester film maintained excellent mechanical properties, but also the heat resistance of the polyester film was improved.
As can be seen from the combination of examples 5 and examples 7 to 8, the stiffness in example 7 is 3.67mN.m, the heat distortion temperature is 184 ℃, the longitudinal tensile strength is 371MPa, and the transverse tensile strength is 342MPa, which is superior to other examples, and shows that the modified PET is more suitable to be prepared by adopting the preparation example 2, so that the polyester film can keep excellent mechanical properties, and the heat resistance of the polyester film can be improved.
The foregoing embodiments are all preferred examples of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (4)
1. A PET/LCP hybrid polyester film characterized by: the material comprises the following raw materials in percentage by weight: 80-98% of modified PET, 1-15% of LCP and 0.5-8% of antioxidant master batch, wherein the modified PET is prepared by the following method: mixing diphenyl anthraquinone phosphine oxide and PET, uniformly stirring, heating and melting, extruding, granulating and drying to obtain modified PET; the addition amount of the diphenyl anthraquinone phosphine oxide is 3-8wt% of PET; the antioxidant master batch is prepared by the following method: uniformly mixing an antioxidant and PET, carrying out melt extrusion, and then bracing, granulating and drying to obtain an antioxidant master batch; the addition amount of the antioxidant in the antioxidant master batch is 10+/-0.1 wt%; the antioxidant is a mixture of hindered phenol antioxidants and phosphite antioxidants, and the weight ratio of the hindered phenol antioxidants to the phosphite antioxidants is 1:1.
2. A PET/LCP hybrid polyester film according to claim 1, wherein: the material comprises the following raw materials in percentage by weight: 88-96% of modified PET, 7-12% of LCP and 1-5% of antioxidant master batch, wherein the sum of the weight percentages of the raw materials of the PET/LCP hybrid polyester film is 100%.
3. A process for the preparation of a PET/LCP hybrid polyester film according to any one of claims 1 to 2, comprising the steps of:
s1: mixing the modified PET, LCP and antioxidant master batch, uniformly stirring, heating for crystallization, and drying to obtain a mixture;
s2: and (3) melting the mixture, cooling the cast sheet, sequentially stretching the cast sheet longitudinally and transversely, shaping, and cooling to obtain the PET/LCP hybrid polyester film.
4. The method for preparing the PET/LCP hybrid polyester film according to claim 3, which is characterized in that: the stretching ratio of the longitudinal stretching of the cast sheet in the step S2 is 2-3 times, and the stretching ratio of the transverse stretching of the cast sheet is 2.5-3 times.
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| CN106317792A (en) * | 2015-06-19 | 2017-01-11 | 江苏裕兴薄膜科技股份有限公司 | 190 DEG C-grade PET (Polyethylene Terephthalate) insulating film and preparation method thereof |
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| TWI790460B (en) * | 2020-07-15 | 2023-01-21 | 南亞塑膠工業股份有限公司 | Flame retardant polyester film and method for manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106317792A (en) * | 2015-06-19 | 2017-01-11 | 江苏裕兴薄膜科技股份有限公司 | 190 DEG C-grade PET (Polyethylene Terephthalate) insulating film and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 新型含磷阻燃剂阻燃PET热稳定性研究;王忠卫等;山东科技大学学报(自然科学版);第35卷(第2期);86-93 * |
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