WO2020057586A1 - 一种耐蒸煮变色覆铁膜及其覆膜金属板 - Google Patents

一种耐蒸煮变色覆铁膜及其覆膜金属板 Download PDF

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Publication number
WO2020057586A1
WO2020057586A1 PCT/CN2019/106615 CN2019106615W WO2020057586A1 WO 2020057586 A1 WO2020057586 A1 WO 2020057586A1 CN 2019106615 W CN2019106615 W CN 2019106615W WO 2020057586 A1 WO2020057586 A1 WO 2020057586A1
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WIPO (PCT)
Prior art keywords
film
blended polyester
iron
clad film
cooking
Prior art date
Application number
PCT/CN2019/106615
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English (en)
French (fr)
Inventor
谢龙
王章薇
倪骅
李秀军
陈红星
Original Assignee
宝山钢铁股份有限公司
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Filing date
Publication date
Application filed by 宝山钢铁股份有限公司 filed Critical 宝山钢铁股份有限公司
Priority to EP19863537.7A priority Critical patent/EP3854581A4/en
Priority to US17/277,479 priority patent/US20210347545A1/en
Publication of WO2020057586A1 publication Critical patent/WO2020057586A1/zh
Priority to PH12021550589A priority patent/PH12021550589A1/en

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    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the present invention relates to the field of film-coated metal plates for metal packaging, and more particularly to a cook-resistant discoloration-resistant iron-coated film and a film-coated metal plate thereof.
  • PET polyethylene terephthalate
  • a large number of well-known companies producing PET materials and PET equipment have been produced at home and abroad.
  • Film is an important branch in the field of PET materials, and is widely used in the field of food and beverage packaging.
  • metal coating technology due to the rise of metal coating technology, the combination of iron-clad film and metal plate by hot-melt lamination has overcome the harmful substance bisphenol A caused by the inside of traditional metal tanks which must be painted. (Bis-phenol), and this issue has been highly valued worldwide. With the gradual popularization of metal sheet coating technology, iron-clad film replacement coatings to improve the safety of filled food have been widely recognized.
  • the existing coated metal plates are widely used in food and beverage packaging containers, after canning and forming, the filled food and beverages need to be subjected to high-temperature sterilization for a long time by means of high-temperature cooking. After the film can is sterilized at high temperature, obvious film discoloration will occur, which seriously affects the appearance of the packaging container.
  • An object of the present invention is to provide a coated iron having excellent resistance to cooking and discoloration, and the coated iron is excellent in comprehensive properties when applied to food and beverage packaging containers.
  • the present invention adopts the following technical solutions.
  • a blended polyester iron-clad film that is resistant to cooking and discoloration.
  • the blended polyester iron-clad film includes polyethylene terephthalate (PET) and polyterephthalic acid.
  • Butylene glycol ester (PBT) the blended polyester iron-clad film includes upper, middle, and lower layers, and at least one of the upper and lower layers of the blended polyester iron-clad film includes an in-situ polymerization method.
  • the mass fraction is 1200-2000 ppm of SiO 2 .
  • a blended polyester iron-clad film that is resistant to cooking and discoloration.
  • the blended polyester iron-clad film includes polyethylene terephthalate and polybutylene terephthalate. Ester, the blended polyester iron-clad film includes upper, middle, and lower layers, and one surface layer (ie, the lower layer or the upper layer) of the blended polyester iron-clad film contains mass parts added by in-situ polymerization It was 1800 ppm of SiO 2 .
  • the blended polyester iron-clad film that is resistant to retort and discoloration is made of polyethylene terephthalate and polybutylene terephthalate.
  • a homogeneous mixture, the upper, middle and lower three layers are prepared by a three-layer coextrusion biaxial stretching method to form the blended polyester iron-clad film.
  • the blended polyester iron-clad film that is resistant to cooking and discoloration has a manufacturing temperature of 240-275 ° C.
  • the polyethylene terephthalate and polybutylene terephthalate in the blended polyester iron-coated film is in the range of 6: 4 to 4: 6.
  • the blended polyester iron-resistant film with resistance to cooking and discoloration has a mass fraction ratio of the polyethylene terephthalate and the polybutylene terephthalate of 6: 4. , 5: 5, or 4: 6.
  • the blended polyester iron-clad film that is resistant to cooking and discoloration has a thickness of 12-35um.
  • a coated metal plate including a metal substrate and a blended polyester iron-clad film resistant to cooking and discoloration as described above.
  • the retort-resistant discoloration-resistant blended polyester iron-clad film is hot melted at a pressure of 2 to 10 Kg and a temperature of 180 to 260 ° C.
  • the surface layer of the blended polyester iron-clad film containing SiO 2 in an amount of 1200-2000 ppm by mass added in-situ is not in contact with the metal substrate Bonding or direct contact.
  • the melting point of the polyethylene terephthalate is 250-265 ° C
  • the melting point of the polybutylene terephthalate is 220-235 ° C.
  • the metal substrate is selected from the group consisting of a chrome-plated steel sheet, a tin-plated steel sheet, a low-tin steel sheet (amount of tin plating ⁇ 1.1 g / m 2 ), a galvanized steel sheet, a cold-rolled steel sheet, Stainless steel plate, aluminum plate.
  • a coated metal can for use in the packaging of high-end food and beverages.
  • the coated metal can is made of a coated metal plate as described above.
  • the present invention has the following beneficial effects:
  • a specific polyethylene terephthalate and a polybutylene terephthalate are blended uniformly in a specific ratio, and then a film is formed by a three-layer coextrusion method.
  • One of the surface layers of the film contains The SiO 2 of 1200-2000 ppm, preferably 1800 ppm, makes the coated metal plate prepared from the blended polyester film have excellent resistance to cooking and discoloration, and is applied to metal containers for food and beverage packaging that require high-temperature sterilization.
  • Adding SiO 2 to the polymer through in situ polymerization uniformly improves the crystallization properties of the polyester film as a whole; and by improving the traditional method of adding SiO 2 in the form of master batches, high-melting resin is avoided from being added to the film.
  • the two points mentioned above significantly improve the overall performance of the polyester film, and significantly improve the complex processability and corrosion resistance of the coated iron including the film of the present invention.
  • a blended polyester iron-clad film that is resistant to cooking and discoloration.
  • the blended polyester iron-clad film includes polyethylene terephthalate and polybutylene terephthalate. Ester, the blended polyester iron-clad film includes upper, middle, and lower layers, and at least one surface layer of the blended polyester iron-clad film includes 1200-2000 ppm by mass of the in-situ polymerization method, preferably 1500-2000ppm, more preferably 1800ppm of SiO 2.
  • the SiO 2 is added to a mixture of monomers for preparing the polyethylene terephthalate or polybutylene terephthalate, thereby being prepared by in-situ polymerization.
  • the blended polyester iron-coated film contains an in-situ polymerization method. SiO 2 .
  • the blended polyester iron-clad film includes polybutylene terephthalate and polyethylene terephthalate containing SiO 2 added in situ polymerization.
  • the mass fraction ratio of polyethylene terephthalate and polybutylene terephthalate is usually in the range of 6: 4 to 4: 6.
  • the mass proportion of polyethylene terephthalate and polybutylene terephthalate in each layer of the blended polyester iron-clad film may be the same or different, as long as the poly-p-phenylene is in three layers
  • the ratio of the sum of the total mass parts of ethylene dicarboxylate to the total mass of polybutylene terephthalate is in the range of 6: 4 to 4: 6 described above, and at least one surface layer contains the text.
  • the above mass parts of SiO 2 may be sufficient.
  • the portion ratio of the polyethylene terephthalate and polybutylene terephthalate is 6: 4, 5: 5, or 4: 6.
  • Polyethylene terephthalate and polybutylene terephthalate suitable for use in the present invention may be various commercially available polyethylene terephthalate and polybutylene terephthalate ester.
  • the melting point of polyethylene terephthalate is 250-265 ° C
  • the melting point of polybutylene terephthalate is 220-235 ° C.
  • the blended polyester iron-clad film that is resistant to retort and discoloration is made of polyethylene terephthalate and polybutylene terephthalate.
  • a homogeneous mixture, the upper, middle and lower three layers are prepared by a three-layer coextrusion biaxial stretching method to form the blended polyester iron-clad film.
  • the blended polyester iron-clad film that is resistant to cooking and discoloration has a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film that is resistant to cooking and discoloration has a thickness of 12-35um.
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 5 parts of polyethylene terephthalate and 5 parts of polybutylene terephthalate.
  • the melting point of the polyethylene terephthalate is 250 ° C.
  • the melting point of butylene terephthalate is 220 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method.
  • the film thickness is 15um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 4 parts of polymer pairs.
  • the melting point of polyethylene terephthalate and 6 parts of polybutylene terephthalate is 255 ° C, and the melting point of polybutylene terephthalate is 230 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method.
  • the film thickness is 15um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 6 parts The melting point of polyethylene terephthalate and 4 parts of polybutylene terephthalate is 260 ° C, and the melting point of polybutylene terephthalate is 225 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method.
  • the film thickness is 20um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 6 parts The melting point of polyethylene terephthalate and 4 parts of polybutylene terephthalate is 265 ° C, and the melting point of polybutylene terephthalate is 220 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 35um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 5 parts of polymer pairs.
  • the melting point of polyethylene terephthalate and 5 parts of polybutylene terephthalate is 250 ° C, and the melting point of polybutylene terephthalate is 220 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method.
  • the film thickness is 12um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 4 parts of polymer pairs. Polyethylene terephthalate and 6 parts of polybutylene terephthalate. The melting point of polyethylene terephthalate is 250 ° C, and the melting point of polybutylene terephthalate is 235 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 35um.
  • One of the surface layers of the blended polyester film contains 1800 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 4 parts of polymer pairs. Polyethylene terephthalate and 6 parts of polybutylene terephthalate. The melting point of polyethylene terephthalate is 265 ° C, and the melting point of polybutylene terephthalate is 225 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 12um.
  • One of the surface layers of the blended polyester film contains 1200 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 6 parts The melting point of polyethylene terephthalate and 4 parts of polybutylene terephthalate is 265 ° C, and the melting point of polybutylene terephthalate is 220 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 15um.
  • One of the surface layers of the blended polyester film contains 2000 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 5 parts of polymer pairs.
  • the melting point of polyethylene terephthalate and 5 parts of polybutylene terephthalate is 270 ° C, and the melting point of polybutylene terephthalate is 215 ° C.
  • the blended polyester is uniformly mixed, and the film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 15um.
  • the blended polyester film is ex-situ polymerized on one of the surface layers. 1200 ppm of SiO 2 was added.
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 6 parts The melting point of polyethylene terephthalate and 4 parts of polybutylene terephthalate is 245 ° C, and the melting point of polybutylene terephthalate is 235 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 15um.
  • One of the surface layers of the blended polyester film contains 2000 ppm of SiO 2 .
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 4 parts of polymer pairs.
  • the melting point of polyethylene terephthalate and 6 parts of polybutylene terephthalate is 270 ° C, and the melting point of polybutylene terephthalate is 235 ° C.
  • the blended polyester is uniformly mixed, and the film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 15um.
  • the blended polyester film is ex-situ polymerized on one of the surface layers. 1800 ppm of SiO 2 was added.
  • a method for producing a blended polyester iron-clad film is manufactured by a biaxial stretching method at a manufacturing temperature of 240-275 ° C.
  • the blended polyester iron-clad film includes 6 parts The melting point of polyethylene terephthalate and 4 parts of polybutylene terephthalate is 250 ° C, and the melting point of polybutylene terephthalate is 215 ° C.
  • the blended polyester is uniformly mixed, and a film is manufactured by three-layer co-extrusion biaxial stretching method with a thickness of 15um.
  • One of the surface layers of the blended polyester film contains 1200 ppm of SiO 2 .
  • the blended polyester films prepared in Examples 1-8 were heat-laminated on the surface of a 0.16 mm-thick chrome-plated steel plate at 245 ° C under a pressure of 5 Kg to prepare coated metal plates.
  • Each blended polyester film contained The surface layer of the amount of SiO 2 is a non-metal plate contact layer.
  • a 538-pot-shaped can body was prepared from the coated metal plate by using an experimental can-making mold. The results show that there is no separation between the film and the chrome-plated steel sheet during the stamping and deformation of the can.
  • the blended polyester films of Examples 1-8 were heat-laminated on the surfaces of tin-plated steel plates, low-tin tin steel plates, galvanized steel plates, cold-rolled steel plates, stainless steel plates, and aluminum plates according to the methods described above to prepare coated metal.
  • the surface layer of each blended polyester film containing the above-mentioned amount of SiO 2 is a non-metallic plate contact layer.
  • An experimental can-making mold was used to prepare a 538-can-shaped can body from the coated metal plate. The results show that there is no separation between the film and each steel plate during the process of stamping and deformation of the can.
  • the coated metal plate prepared by the above method was evaluated by the method shown below. The results are shown in Table 1.
  • the pot was cooked at 121 ° C for 45 minutes. It is preferable to visually evaluate whether the above-mentioned can body has undergone discoloration after cooking, and until the film on the outer wall of the can body has not undergone discoloration after cooking in the final step.
  • Acid resistance performance The performance of the corrosion resistance is evaluated by evaluating the acid resistance after the coated iron is washed into a can (type 538). Fill the coated tank with a 20g / L citric acid solution, cook it at 121 ° C for 30min after capping, and take out the sample after cooling to observe the occurrence of acid spots on the surface to evaluate the resistance of coated iron Acid performance.
  • Anti-sulfur performance After the coated iron is washed into a can (type 538), the anti-sulfur performance evaluation is used to represent the corrosion resistance evaluation.
  • the coated can was filled with 0.5% Na 2 S solution, and after being capped, it was cooked at 121 ° C. for 30 minutes. After cooling, the sample was taken out to observe the occurrence of sulfur spots on the surface to evaluate the resistance of coated iron. Sulfur properties.
  • Blended polyester iron-clad film by uniformly blending polyethylene terephthalate and polybutylene terephthalate, and then forming a film by a biaxial stretching method, good moldability and thin thickness can be obtained.
  • Blended polyester iron-clad film The blended polyester iron-clad film can be used to prepare a coated metal plate with excellent comprehensive properties.
  • the coated metal plate can be used to manufacture food and beverage packaging containers, and the coated metal plate and packaging container have excellent resistance to cooking and discoloration. .

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Abstract

一种耐蒸煮变色的共混聚酯覆铁膜，包括聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯，共混聚酯覆铁膜包括上、中、下三层，一个表层包含原位聚合方式加入的质量份数为1200-2000ppm的SiO 2。共混聚酯覆铁膜通过三层共挤双向拉伸法制备形成，制造温度为240-275℃。由共混聚酯覆铁膜制备的覆膜金属板具有优良的耐蒸煮变色性能，应用于需要高温杀菌的食品饮料包装用金属容器。

Description

一种耐蒸煮变色覆铁膜及其覆膜金属板 技术领域
本发明涉及金属包装用覆膜金属板领域，更具体地指一种耐蒸煮变色覆铁膜及其覆膜金属板。
背景技术
近年来，聚对苯二甲酸乙二醇酯(PET)工业发展十分迅速，国内外已有一大批著名的生产PET材料及PET设备的公司，1987年PET的世界产量已跃居工程塑料的第五位，薄膜是PET材料应用领域中的一个重要分支，广泛应用于食品、饮料的包装领域。近年来，由于金属覆膜技术的兴起，将覆铁膜与金属板通过热熔覆合的方式相结合，克服了传统金属罐内侧必须经过涂装加工所导致的有害物质——双酚A类(Bis-phenol A)的析出问题，而这一问题已受到全球范围的高度重视。随着金属板覆膜技术的逐步推广，覆铁膜替代涂料以提升灌装的食品安全性已得到广泛认可。
现有的覆膜金属板广泛应用于食品饮料包装容器时，在制罐成型后往往需要通过高温蒸煮的方式对灌装的食品饮料进行较长时间高温杀菌，而现有的覆膜铁/覆膜罐在高温蒸煮杀菌后会出现明显的薄膜变色现象，严重影响了包装容器的外观。
发明内容
本发明的目的是提供一种具有优异的耐蒸煮变色特性的覆膜铁，且该覆膜铁应用于食品饮料包装容器时各项综合性能优异。
为了实现上述目的，本发明采用以下技术方案。
根据本发明的一个方面，提供一种耐蒸煮变色的共混聚酯覆铁膜，所述共混聚酯覆铁膜包括聚对苯二甲酸乙二醇酯(PET)和聚对苯二甲酸丁 二醇酯(PBT)，所述共混聚酯覆铁膜包括上、中、下三层，所述共混聚酯覆铁膜上层和下层中至少一层包含以原位聚合方式加入的质量份数为1200-2000ppm的SiO 2。
根据本发明的一个方面，提供一种耐蒸煮变色的共混聚酯覆铁膜，所述共混聚酯覆铁膜包括聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯，所述共混聚酯覆铁膜包括上、中、下三层，所述共混聚酯覆铁膜中的一个表层(即下层或上层)包含以原位聚合方式加入的质量份数为1800ppm的SiO 2。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜为聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的均匀混合物，所述上、中、下三层通过三层共挤双向拉伸法制备形成所述共混聚酯覆铁膜。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜的制造温度240-275℃。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜中所述聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的质量份数比在6：4到4：6的范围内。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的质量份数比为6:4、5:5、或4:6。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜的厚度为12-35um。
根据本发明的另一个方面，提供一种覆膜金属板，所述覆膜金属板包括金属基板和如上所述的耐蒸煮变色的共混聚酯覆铁膜。
根据本发明的另一个方面的覆膜金属板中，所述耐蒸煮变色的共混聚酯覆铁膜采用热熔方式在压力2～10Kg、温度180～260℃。
根据本发明的另一个方面的覆膜金属板中，所述共混聚酯覆铁膜中所述包含以原位聚合方式加入的质量份数为1200-2000ppm的SiO 2的表层不与金属基板粘接或直接接触。
根据本发明的另一个方面的覆膜金属板中，所述聚对苯二甲酸乙二醇酯的熔点为250-265℃，聚对苯二甲酸丁二醇酯的熔点为220-235℃。
根据本发明的另一个方面的覆膜金属板中，所述金属基板选自镀铬钢板、镀锡钢板、低锡钢板(镀锡量≤1.1g/m 2)、镀锌钢板、冷轧钢板、不锈钢板、铝板。
根据本发明的再一个方面，提供一种应用于中高端食品饮料包装的覆膜金属罐，所述覆膜金属罐采用如权上所述的覆膜金属板制成。
与现有技术相比，本发明具有如下有益效果：
本发明通过将特指的聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯按照特指的比例共混均匀后，通过三层共挤法制膜，薄膜的其中一个表层含有1200-2000ppm、优选1800ppm的SiO 2，使得由所述共混聚酯薄膜制备的覆膜金属板具有优良耐蒸煮变色性能，应用于需要高温杀菌的食品饮料包装用金属容器。
聚合物中通过原位聚合加入SiO 2，从整体上均匀地改善聚酯薄膜的结晶性能；并且通过改善传统以母粒形式加入SiO 2的方式，避免了高熔点树脂加入薄膜中。上述两点使聚酯薄膜的综合性能得到明显提升，包含本发明薄膜的覆膜铁的耐复杂加工性、覆膜铁的耐腐蚀性能等得到显著提高。
具体实施方式
以下在具体实施方式中通过对非限制性实施例所作的详细描述，本发明的目的、特征、和优点将变得更清楚明显，其内容足以使本领域技术人员了解和实施本发明。
根据本发明的一个方面，提供一种耐蒸煮变色的共混聚酯覆铁膜，所述共混聚酯覆铁膜包括聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯，所述共混聚酯覆铁膜包括上、中、下三层，所述共混聚酯覆铁膜中的至少一个表层包含原位聚合方式加入的质量份数为1200-2000ppm、优选1500-2000ppm、更优选1800ppm的SiO 2。优选地，所述SiO 2是在制备所述聚对苯二甲酸乙二醇酯或聚对苯二甲酸丁二醇酯时加入到其制备单体的混合物中，从而通过原位聚合的方式制备得到含有SiO 2的聚对苯二甲酸 乙二醇酯或含有SiO 2的聚对苯二甲酸丁二醇酯。本发明中，用于制备所述共混聚酯覆铁膜的聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯中至少有一种聚合物含有通过原位聚合方式加入的SiO 2。在一些优选的实施方案中，所述共混聚酯覆铁膜包括聚对苯二甲酸丁二醇酯和含有以原位聚合方式加入的SiO 2的聚对苯二甲酸乙二醇酯。
本发明的共混聚酯覆铁膜中，聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的质量份数比通常在6：4到4：6的范围内。该共混聚酯覆铁膜中的每一层的聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的质量份配比可相同或不同，只要三层中聚对苯二甲酸乙二醇酯的总质量份数之和与聚对苯二甲酸丁二醇酯的总质量份数之比在上述6：4到4：6的范围内，且使得至少一个表层含有本文上述质量份数的SiO 2即可。在一些实施方案中，所述聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的份数比为6:4、5:5、或4:6。
适用于本发明的聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯可以是各种市售来源的聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯。通常，聚对苯二甲酸乙二醇酯的熔点为250-265℃，聚对苯二甲酸丁二醇酯的熔点为220-235℃。选择此类聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯，按本发明所述的用量配比制备得到的本发明薄膜具有优异的耐蒸煮变色性能，在水、酸、含硫水溶液等溶液中长时间高温蒸煮，薄膜的表面无蒸煮变色现象，且薄膜表面不起皱、不与金属板之间剥离。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜为聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的均匀混合物，所述上、中、下三层通过三层共挤双向拉伸法制备形成所述共混聚酯覆铁膜。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜的制造温度240-275℃。
根据本发明的一个方面的耐蒸煮变色的共混聚酯覆铁膜中，所述共混聚酯覆铁膜的厚度为12-35um。
实施例1
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃。所述共混聚酯覆铁膜包括5份聚对苯二甲酸乙二醇酯和5份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为250℃，聚对苯二甲酸丁二醇酯的熔点为220℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例2
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括4份聚对苯二甲酸乙二醇酯和6份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为255℃，聚对苯二甲酸丁二醇酯的熔点为230℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例3
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括6份聚对苯二甲酸乙二醇酯和4份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为260℃，聚对苯二甲酸丁二醇酯的熔点为225℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为20um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例4
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括6份聚对苯二甲酸乙二醇酯和4份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为265℃，聚对苯二甲酸丁二醇酯的熔点为220℃。将所述的共混聚酯 均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为35um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例5
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括5份聚对苯二甲酸乙二醇酯和5份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为250℃，聚对苯二甲酸丁二醇酯的熔点为220℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为12um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例6
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括4份聚对苯二甲酸乙二醇酯和6份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为250℃，聚对苯二甲酸丁二醇酯的熔点为235℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为35um，所述共混聚酯薄膜的其中一个表层中含有1800ppm的SiO 2。
实施例7
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括4份聚对苯二甲酸乙二醇酯和6份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为265℃，聚对苯二甲酸丁二醇酯的熔点为225℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为12um，所述共混聚酯薄膜的其中一个表层中含有1200ppm的SiO 2。
实施例8
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸 方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括6份聚对苯二甲酸乙二醇酯和4份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为265℃，聚对苯二甲酸丁二醇酯的熔点为220℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜的其中一个表层中含有2000ppm的SiO 2。
比较例1
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括5份聚对苯二甲酸乙二醇酯和5份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为270℃，聚对苯二甲酸丁二醇酯的熔点为215℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜采用非原位聚合方式在其中一个表层加入1200ppm的SiO 2。
比较例2
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括6份聚对苯二甲酸乙二醇酯和4份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为245℃，聚对苯二甲酸丁二醇酯的熔点为235℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜的其中一个表层中含有2000ppm的SiO 2。
比较例3
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括4份聚对苯二甲酸乙二醇酯和6份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为270℃，聚对苯二甲酸丁二醇酯的熔点为235℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为 15um，所述共混聚酯薄膜采用非原位聚合方式在其中一个表层加入1800ppm的SiO 2。
比较例4
一种共混聚酯覆铁膜的生产方法，所述共混聚酯覆铁膜采用双向拉伸方法制造，制造温度240-275℃，所述共混聚酯覆铁膜包括6份聚对苯二甲酸乙二醇酯和4份聚对苯二甲酸丁二醇酯，聚对苯二甲酸乙二醇酯的熔点为250℃，聚对苯二甲酸丁二醇酯的熔点为215℃。将所述的共混聚酯均匀混合，采用上、中、下三层共挤双向拉伸方法制造薄膜，薄膜厚度为15um，所述共混聚酯薄膜的其中一个表层中含有1200ppm的SiO 2。
测试例1
将实施例1-8所制备出的共混聚酯薄膜在5Kg压力下，在245℃热覆合于0.16mm厚度镀铬钢板表面上，制备出覆膜金属板，各共混聚酯薄膜中含所述量SiO 2的表层为非金属板接触层。用实验制罐模具将所述覆膜金属板制备出538罐型的罐体。结果显示，制罐的冲压、变形过程中薄膜与镀铬钢板之间无分离。
类似地，将实施例1-8共混聚酯薄膜按上述方法热覆合到镀锡钢板、低锡钢板、镀锌钢板、冷轧钢板、不锈钢板、铝板等表面上，制备出覆膜金属板，各共混聚酯薄膜中含所述量SiO 2的表层为非金属板接触层。用实验制罐模具由所述覆膜金属板制备出538罐型的罐体。结果显示，制罐的冲压、变形过程中薄膜与各钢板之间无分离。
测试例2
采用以下所示方法评价上述方法所制备的覆膜金属板。其结果见表1。
(1)耐蒸煮变色性能
将该罐体在121℃条件下蒸煮45min。用肉眼评价上述罐体是否发生蒸煮后变色的现象，直到最终工序罐体外壁的薄膜尚未出现蒸煮后变色的状态为优。
(2)抗酸性能：将覆膜铁冲罐(罐型538)后以抗酸性能评价来代表耐蚀性能评价。将覆膜罐灌装20g/L的柠檬酸溶液，封盖后在121℃温度条件下蒸煮30min，待冷却后将试样取出观察表面产生酸化斑的情况，以此来评价覆膜铁的抗酸性能。
(3)抗硫性能：将覆膜铁冲罐(罐型538)后以抗硫性能评价来代表耐蚀性能评价。将覆膜罐灌装0.5％的Na 2S溶液，封盖后在121℃温度条件下蒸煮30min，待冷却后将试样取出观察表面产生硫化斑的情况，以此来评价覆膜铁的抗硫性能。
表1：耐蒸煮变色性、耐腐蚀性评价结果
Figure PCTCN2019106615-appb-000001
注：表1中╳表示较差；△表示一般；○表示较好；◎表示很好。
综上所述，本发明通过将聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯均匀共混后，由双向拉伸法制膜，可制备得到成型性良好、厚度较薄的共混聚酯覆铁膜。采用该共混聚酯覆铁膜可制备得到综合性能优异的覆膜金属板，该覆膜金属板可用于制造食品饮料包装容器，且该覆膜金属板 及包装容器具有优异的耐蒸煮变色性能。
最后，需要指出的是，虽然本发明已参照当前的具体实施例来描述，但是本技术领域中的普通技术人员应当认识到，以上的实施例仅是用来说明本发明，而并非用作为对本发明的限定，在不脱离本发明构思的前提下还可以作出各种等效的变化或替换，因此，只要在本发明的实质精神范围内对上述实施例的变化、变型都将落在本发明的权利要求书范围内。

Claims (15)

  1. 一种耐蒸煮变色的共混聚酯覆铁膜，其特征在于：所述共混聚酯覆铁膜包括聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯，所述共混聚酯覆铁膜包括上、中、下三层，其中，所述上层或下层包含以原位聚合方式加入的质量份数为1200-2000ppm的SiO 2。
  2. 如权利要求1所述的共混聚酯覆铁膜，其特征在于，所述上层或下层包含原位聚合方式加入的质量份数为1800ppm的SiO 2。
  3. 如权利要求1所述的耐蒸煮变色的共混聚酯覆铁膜，其特征在于：所述聚对苯二甲酸乙二醇酯的熔点为250-265℃；所述聚对苯二甲酸丁二醇酯的熔点为220-235℃。
  4. 如权利要求1所述的耐蒸煮变色的共混聚酯覆铁膜，其特征在于：所述共混聚酯覆铁膜中所述聚对苯二甲酸乙二醇酯和所述聚对苯二甲酸丁二醇酯的质量份数比在6：4到4：6的范围内。
  5. 如权利要求1所述的耐蒸煮变色的共混聚酯覆铁膜，其特征在于：所述聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的份数比为6:4、5:5、或4:6。
  6. 如权利要求1所述的耐蒸煮变色的共混聚酯覆铁膜，其特征在于：所述共混聚酯覆铁膜的厚度为12-35um。
  7. 权利要求1所述的耐蒸煮变色的共混聚酯覆铁膜的制造方法，其特征在于：所述方法包括由聚对苯二甲酸乙二醇酯和聚对苯二甲酸丁二醇酯的均匀混合物通过三层共挤双向拉伸法制备形成所述共混聚酯覆铁膜。
  8. 如权利要求7所述的耐蒸煮变色的共混聚酯覆铁膜的制造方法，其特征在于：所述共混聚酯覆铁膜的制造温度240-275℃。
  9. 一种覆膜金属板，其特征在于：所述覆膜金属板包括金属基板和如权利要求1-6中任一项所述的耐蒸煮变色的共混聚酯覆铁膜。
  10. 如权利要求9所述的覆膜金属板，其特征在于：所述金属基板选自镀铬钢板、镀锡钢板、低锡钢板、镀锌钢板、冷轧钢板、不锈钢板和铝板。
  11. 如权利要求9所述的覆膜金属板，其特征在于，所述共混聚酯覆铁膜含以原位聚合方式加入的质量份数为1200-2000ppm的SiO 2的表层为非金属基板接触层。
  12. 权利要求9所述的覆膜金属板的制造方法，其特征在于：所述方法包括采用热熔方式在压力2～10Kg、温度180～260℃下将所述耐蒸煮变色的共混聚酯覆铁膜热覆合到金属基板表面上。
  13. 一种应用于中高端食品饮料包装的覆膜金属罐，其特征在于，所述覆膜金属罐采用如权利要求9所述的覆膜金属板制成。
  14. 如权利要求13所述的覆膜金属罐，其特征在于，所述覆膜金属板的金属基板选自镀铬钢板、镀锡钢板、低锡钢板、镀锌钢板、冷轧钢板、不锈钢板和铝板。
  15. 如权利要求13所述的覆膜金属罐，其特征在于，所述覆膜金属板中，所述共混聚酯覆铁膜含以原位聚合方式加入的质量份数为1200-2000ppm的SiO 2的表层为非金属基板接触层。
PCT/CN2019/106615 2018-09-19 2019-09-19 一种耐蒸煮变色覆铁膜及其覆膜金属板 WO2020057586A1 (zh)

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