CN110920169A - Preparation method of single-layer copolyester iron-clad film and film-clad metal plate thereof - Google Patents
Preparation method of single-layer copolyester iron-clad film and film-clad metal plate thereof Download PDFInfo
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- CN110920169A CN110920169A CN201811090608.2A CN201811090608A CN110920169A CN 110920169 A CN110920169 A CN 110920169A CN 201811090608 A CN201811090608 A CN 201811090608A CN 110920169 A CN110920169 A CN 110920169A
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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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal 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
- B32B15/09—Layered products comprising a layer of metal comprising metal 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 comprising polyesters
-
- 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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/18—Layered products comprising a layer of metal comprising iron or steel
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/40—Applications of laminates for particular packaging purposes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/199—Acids or hydroxy compounds containing cycloaliphatic rings
-
- 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
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
Abstract
The invention discloses a preparation method of a single-layer copolyester iron-clad film, which comprises the following steps: s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol; s2: in-situ polymerization method in copolymerization reactionFormula (II) addition of SiO2To obtain SiO with the mass fraction of 1200ppm2Copolyester resin with intrinsic viscosity of 0.68-0.72 dL/g; s3: obtaining copolyester chips with the intrinsic viscosity of 0.75-0.78dL/g by adopting a solid-phase tackifying mode; s4: a single-layer polyester film is produced from the copolyester chips obtained in step S3 by biaxial stretching or casting. The polyester film prepared by the method has the advantages of high food safety level, excellent heat bonding property with a metal plate, excellent deep drawing processing resistance and complex deformation processing resistance, excellent corrosion resistance and the like, and can be widely used in the food and beverage packaging container industry.
Description
Technical Field
The invention relates to the field of polyester films, in particular to a preparation method of a single-layer copolyester iron-clad film and a film-clad metal plate thereof.
Background
Coatings containing bisphenol a are widely used in the metal can industry, and in recent years, due to the fact that environmental protection, energy consumption and food safety problems are gradually and widely concerned all over the world, the industry is constantly striving to find qualified new materials to overcome the problems.
The laminated iron is formed by directly bonding a flexible polyester film and a metal plate together in a hot melting mode, and brings many advantages to downstream users: 1. the coating link of the coating is saved, and the process is environment-friendly; 2. the food safety level is obviously improved on the basis of the coating iron; 3. the comprehensive performance is greatly improved on the basis of the coating iron; 4. can realize the molding processing of continuous can/cap making.
Due to the advantages of the coated iron, as environmental protection policies become stricter and the attention of people on food safety is promoted, the attention of the coated iron as an environment-friendly high-performance new material in the can making industry is higher and higher, and the coated iron products of a part of enterprises enter the market for application in recent years. In order to meet the different requirements of different purposes, the raw materials and the film layer structure of the polyester film need to be optimally designed so as to meet different requirements of each downstream process.
The patent application with publication number CN102463725A discloses a polyester film and a preparation method thereof, the polyester film of the patent application is of a three-layer (ABA) structure and is used in the field of electronic tags, and the polyester film is characterized in that two surface layers are made of the same resin, so that the requirements of multiple performances such as adhesion with a metal plate, contact with a mold, forming processing, contact with contents in a tank and the like are difficult to meet at the same time, the difficulty in considering the performance is easily caused, and the polyester film is not suitable for the tank making industry.
Patent No. CN 106142782B discloses an iron-clad heat-sealable polyester film and a method for preparing the same, which is characterized in that a three-layer polyester film is laminated with a metal sheet, and the properties of the film are limited by its highly crystalline lower surface layer, resulting in insufficient processing and forming properties, and thus, the film is not suitable for deep drawing and complex deformation.
CN1839036 patent application discloses a film-coated metal plate and a drawn can used therein, in which a double-layer film is laminated with a metal sheet, which is prone to generate defects such as delamination and falling off during can-making molding, and the vinyl ionomer used therein is poor in performance during filling and high-temperature sterilization.
The patent application of CN102432984A discloses a cast polyester film and a metal plate metal can used therein, wherein a single layer polyester film is combined with a metal sheet, and the modification monomer of polyester is relatively single, which is not good for improving the comprehensive performance of the polyester film, and the raw material synthesis and film preparation process in the patent are not good for improving the food safety grade of the film.
The laminated metal plate needs to have sufficient food safety guarantee, and meanwhile, the deep drawing processing requirement and the requirements on filling, acid and alkali salt resistance, high-temperature sterilization and the like are met. In the prior art, only one or two performance requirements can be met, however, the three characteristics are simultaneously met as high-end requirements of the food and beverage packaging industry.
Disclosure of Invention
The invention aims to provide a preparation method of a single-layer polyester film, which has high food safety characteristic, has the advantages of excellent heat bonding property with a metal plate, excellent deep drawing processing resistance and complex deformation processing property, excellent corrosion resistance and the like, and can be widely applied to the middle-high metal packaging industry.
The invention adopts the following technical scheme to realize the purpose:
according to one aspect of the present invention, there is provided a method for preparing a single-layer copolyester iron-clad film, the method comprising the steps of:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO with the mass fraction of 1200ppm2Copolyester resin with intrinsic viscosity of 0.68-0.72 dL/g;
s3: adopting a solid-phase tackifying mode to obtain copolyester chips with the intrinsic viscosity of 0.75-0.78 dL/g;
s4: a single-layer polyester film is produced from the copolyester chips obtained in step S3 by biaxial stretching or casting.
The preparation method of the single-layer copolyester iron-clad film according to one aspect of the invention further comprises the following steps:
s5: and directly laminating the single-layer polyester film on the surface of the metal plate by adopting a hot-melting laminating method to form a single-layer copolymerized polyester iron-clad film.
According to the method for preparing the single-layer copolyester iron-clad film in one aspect of the invention, the manufacturing temperature of the single-layer polyester film in the step S3 is 250-280 ℃.
According to the preparation method of the single-layer copolyester iron-clad film in one aspect of the invention, the melting point of the copolyester film is between 200 ℃ and 240 ℃.
Preferably, the melting point of the copolyester film is between 210 ℃ and 230 ℃.
According to another aspect of the present invention, there is provided a coated metal sheet comprising a metal substrate and a single layer iron copolyester film as described above directly coated on the metal substrate by a hot-melt method.
According to another aspect of the coated metal sheet of the present invention, the metal substrate is selected from the group consisting of a chromium-plated steel sheet, a tin-plated steel sheet, a low-tin steel sheet, a zinc-plated steel sheet, a cold-rolled steel sheet, a stainless steel sheet, and an aluminum sheet.
According to still another aspect of the present invention, there is provided a metal container for packaging medium-high-end food and beverage, the metal container being made of the film-coated metal plate as described above.
Compared with the prior art, the invention has the following beneficial technical effects: the single-layer copolyester film prepared by the method simultaneously has the following three characteristics: the polyester film has high food safety characteristic, excellent heat bonding performance with metal plates, deep drawing processing resistance and complex deformation processing performance, and excellent corrosion resistance, and can be widely used in the middle and high-end metal packaging industry.
SiO2 is added into the polymer through in-situ polymerization, so that the crystallization performance of the polyester film is uniformly improved on the whole; and avoids the addition of high melting point resin into the film by improving the traditional way of adding SiO2 in the form of master batch. The two points obviously improve the comprehensive performance of the polyester film, and the complex processing resistance, the corrosion resistance and the like of the coated iron containing the film are obviously improved.
Detailed Description
The objects, features, and advantages of the present invention will become more apparent from the following detailed description of non-limiting examples thereof. The content is sufficient to enable a person skilled in the art to understand and implement the invention.
Example 1
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO with the mass fraction of 1200ppm2Copolyester resin with the intrinsic viscosity of 0.72 dL/g;
s3: obtaining specific copolyester with the intrinsic viscosity of 0.78dL/g by adopting a solid-phase tackifying mode, wherein the melting point of the copolyester is 220 ℃;
s4: the single-layer polyester film is prepared from the copolyester chip obtained in the step S3 by a biaxial stretching method or a casting method, and the manufacturing temperature of the polyester film is 260 ℃ to 270 ℃.
The specific copolyester chip: adopting m-phthalic acid, 1, 4-cyclohexane dimethanol and neopentyl glycol to carry out copolymerization reaction, and adding SiO in the copolymerization reaction by adopting an in-situ polymerization mode2To obtain SiO containing 1200pp2And a copolyester resin having an intrinsic viscosity of 0.72dL/g, and further a specific copolyester having an intrinsic viscosity of 0.78dL/g and a melting point of 220 ℃ is obtained by a solid-phase tackifying method.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a biaxial stretching method, and the preparation temperature is 260-270 ℃.
Preparing a film-coated metal plate: and thermally laminating the prepared biaxially oriented polyester film on the surface of a 0.10-0.50 mm thin metal plate under the pressure of 2-10 Kg and the temperature of 180-260 ℃ to obtain the film-coated metal plate.
Example 2
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO containing 1200pp2A copolyester resin having an intrinsic viscosity of 0.68 dL/g;
s3: obtaining the specific copolyester with the intrinsic viscosity of 0.75dL/g by a solid-phase tackifying mode, wherein the melting point is 200 ℃;
s4: a single-layer polyester film is prepared from the specific copolyester chip by a biaxial stretching method, and the manufacturing temperature of the polyester film is 250-270 ℃.
The specific copolyester chip: adopting m-phthalic acid, 1, 4-cyclohexane dimethanol and neopentyl glycol to carry out copolymerization reaction, and adding SiO in the copolymerization reaction by adopting an in-situ polymerization mode2To obtain SiO containing 1200pp2And a copolyester resin having an intrinsic viscosity of 0.68dL/g, and further a specific copolyester having an intrinsic viscosity of 0.75dL/g and a melting point of 200 ℃ is obtained by a solid-phase thickening method.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a biaxial stretching method, and the preparation temperature is 250-270 ℃.
Example 3
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO containing 1200pp2Copolyester resin with the intrinsic viscosity of 0.72 dL/g;
s3: obtaining the specific copolyester with the intrinsic viscosity of 0.78dL/g by a solid-phase tackifying mode, wherein the melting point is 230 ℃;
s4: a single-layer polyester film is prepared from the specific copolyester chip by a biaxial stretching method, and the manufacturing temperature of the polyester film is 260-280 ℃.
The specific copolyester chip: isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol are adopted for copolymerization, SiO2 is added in an in-situ polymerization manner in the copolymerization to obtain a copolyester resin containing SiO2 of 1200pp and with the intrinsic viscosity of 0.72dL/g, and the specific copolyester with the intrinsic viscosity of 0.78dL/g is obtained in a solid-phase tackifying manner, wherein the melting point is 230 ℃.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a biaxial stretching method, and the preparation temperature is 260-280 ℃.
Example 4
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO containing 1200pp2Copolyester resin with the intrinsic viscosity of 0.72 dL/g;
s3: obtaining the specific copolyester with the intrinsic viscosity of 0.78dL/g by a solid-phase tackifying mode, wherein the melting point is 230 ℃;
s4: a single-layer polyester film was prepared from the specific copolyester chips by a casting method, and the manufacturing temperature of the polyester film was 260-280 ℃.
The specific copolyester chip: isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol are adopted for copolymerization, SiO2 is added in an in-situ polymerization manner in the copolymerization to obtain a copolyester resin containing SiO2 of 1200pp and with the intrinsic viscosity of 0.72dL/g, and the specific copolyester with the intrinsic viscosity of 0.78dL/g is obtained in a solid-phase tackifying manner, wherein the melting point is 230 ℃.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a tape casting method, and the preparation temperature is 260-280 ℃.
Example 5
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO containing 1200pp2A copolyester resin having an intrinsic viscosity of 0.68 dL/g;
s3: obtaining the specific copolyester with the intrinsic viscosity of 0.75dL/g by a solid-phase tackifying mode, wherein the melting point is 200 ℃;
s4: a single-layer polyester film was prepared from the specific copolyester chips by a casting method, and the manufacturing temperature of the polyester film was 250-270 ℃.
The specific copolyester chip: isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol are adopted for copolymerization, SiO2 is added in an in-situ polymerization manner in the copolymerization to obtain a copolyester resin containing SiO2 of 1200pp and having an intrinsic viscosity of 0.68dL/g, and the specific copolyester having the intrinsic viscosity of 0.75dL/g is obtained in a solid-phase tackifying manner, wherein the melting point of the copolyester is 200 ℃.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a tape casting method, and the preparation temperature is 250-270 ℃.
Example 6
A method for preparing a single-layer copolyester iron-clad film adopts specific copolyester chips to prepare a polyester film.
The method comprises the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO with the mass fraction of 1200ppm2Copolyester resin with intrinsic viscosity of 0.72 dL/g;
s3: obtaining copolyester chips with the intrinsic viscosity of 0.78dL/g by adopting a solid-phase tackifying mode, wherein the melting point of the copolyester is 240 ℃;
s4: a single-layer polyester film was prepared from the copolyester chips obtained in step S3 by a casting method.
The specific copolyester chip: isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol are adopted for copolymerization, SiO2 is added in an in-situ polymerization manner in the copolymerization to obtain a copolyester resin containing SiO2 of 1200pp and with the intrinsic viscosity of 0.72dL/g, and the specific copolyester with the intrinsic viscosity of 0.78dL/g is obtained in a solid-phase tackifying manner, wherein the melting point is 240 ℃.
The single-layer polyester film is prepared by adopting the specific copolyester chip through a tape casting method, and the preparation temperature is 260-270 ℃.
In the six embodiments, the single-layer polyester film prepared by using the specific copolyester chip has good formability in casting film making and biaxial stretching film making, and can prepare the polyester iron-clad film with a small thickness. The polyester film has high food safety, has the advantages of excellent heat bonding property with metal plates, excellent deep drawing processing and complex deformation processing resistance, excellent corrosion resistance and the like, and can be widely used in the middle and high-end metal packaging industry.
SiO2 is added into the polymer through in-situ polymerization, so that the crystallization performance of the polyester film is uniformly improved on the whole; and avoids the addition of high melting point resin into the film by improving the traditional way of adding SiO2 in the form of master batch. The two points obviously improve the comprehensive performance of the polyester film, and the complex processing resistance, the corrosion resistance and the like of the coated iron containing the film are obviously improved.
Finally, it should be noted that while the present invention has been described with reference to the specific embodiments thereof, it should be understood by those skilled in the art that the above embodiments are only for illustrating the present invention and are not to be construed as limiting the present invention, and various equivalent changes and substitutions may be made therein without departing from the spirit of the present invention, and therefore, it is intended that all changes and modifications to the above embodiments within the spirit and scope of the present invention be covered by the appended claims.
Claims (9)
1. A preparation method of a single-layer copolyester iron-clad film is characterized by comprising the following steps:
s1: carrying out copolymerization reaction on isophthalic acid, 1, 4-cyclohexanedimethanol and neopentyl glycol;
s2: in the copolymerization reaction, SiO is added in an in-situ polymerization mode2To obtain SiO with the mass fraction of 1200ppm2Copolyester resin with intrinsic viscosity of 0.68-0.72 dL/g;
s3: adopting a solid-phase tackifying mode to obtain copolyester chips with the intrinsic viscosity of 0.75-0.78 dL/g;
s4: a single-layer polyester film is produced from the copolyester chips obtained in step S3 by biaxial stretching or casting.
2. The method of claim 1, further comprising the steps of:
s5: and directly laminating the single-layer polyester film on the surface of the metal plate by adopting a hot-melting laminating method to form a single-layer copolymerized polyester iron-clad film.
3. The method of preparing a single layer copolyester iron-clad film according to claim 1 or 2, wherein:
the manufacturing temperature of the single-layer polyester film in the step S3 is 250-280 ℃.
4. The method of preparing a single layer copolyester iron-clad film according to claim 1 or 2, wherein:
the melting point of the copolyester film is between 200 ℃ and 240 ℃.
5. The method of claim 4, wherein the iron-clad film is prepared by the following steps:
the melting point of the copolyester film is between 210 ℃ and 230 ℃.
6. A film-coated metal sheet comprising a metal substrate and the single-layer copolyester iron-clad film according to any one of claims 1 to 6 directly coated on the metal substrate by a hot-melt method.
7. The coated metal sheet defined in claim 6, wherein: the single-layer copolyester iron-clad film is thermally bonded on the surface of the metal substrate under the pressure of 2-10 Kg and the temperature of 180-260 ℃.
8. The coated metal sheet defined in claim 6, wherein: the thickness of the metal substrate is 0.10-0.50 mm, and the metal substrate is selected from a chromium-plated steel plate, a tin-plated steel plate, a low-tin steel plate, a galvanized steel plate, a cold-rolled steel plate, a stainless steel plate and an aluminum plate.
9. A metal container for middle and high-end food and beverage packaging applications, wherein the metal container is made of the film-coated metal sheet according to any one of claims 7 to 9.
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| CN112048252A (en) * | 2020-08-26 | 2020-12-08 | 江苏鼎胜新能源材料股份有限公司 | Cold roofing that PET modified film prepared |
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