CN101160339B - 用于被覆金属板的聚酯树脂、被覆聚酯树脂形成的被覆了树脂的金属板、以及金属罐和盖 - Google Patents
用于被覆金属板的聚酯树脂、被覆聚酯树脂形成的被覆了树脂的金属板、以及金属罐和盖 Download PDFInfo
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- CN101160339B CN101160339B CN2006800125621A CN200680012562A CN101160339B CN 101160339 B CN101160339 B CN 101160339B CN 2006800125621 A CN2006800125621 A CN 2006800125621A CN 200680012562 A CN200680012562 A CN 200680012562A CN 101160339 B CN101160339 B CN 101160339B
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Classifications
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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- C08G63/16—Dicarboxylic acids and dihydroxy compounds
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- 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
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Abstract
本发明提供用于被覆金属板的聚酯树脂,在本发明的用于被覆金属板的聚酯树脂中,含有2~10mol%二聚酸作为二羧酸成分,重均分子量(Mw)在70,000~160,000的范围,具有优异的成膜性和耐腐蚀性,同时具有优异的抗冲击性,本发明还可提供耐腐蚀性、抗冲击性(抗凹性)、加工性、贴合性、风格等各特性优异的被覆树脂的金属板和由该被覆树脂的金属板形成的金属罐和罐盖。
Description
技术领域
本发明涉及用于覆盖金属板的聚酯树脂,更具体地说,涉及具有优异的成膜性、抗冲击性的聚酯树脂、以及被覆该聚酯树脂而成的被覆树脂的金属板、和含有该被覆树脂的金属板的金属罐和盖。
背景技术
以往,作为使金属材料具有耐腐蚀性的方法,广泛采用将金属表面用树脂层被覆等方法,已知所述技术中使用的被覆方法有:将环氧树脂、酚醛树脂等热固化性树脂分散于溶剂中,将其涂布在金属表面上的方法;将预先形成的薄膜例如聚酯系、聚烯烃系、聚酰胺系薄膜经由异氰酸酯系、环氧系、酚系等底漆与金属基体贴合的方法等,这些方法中,是在所使用的热固化性树脂和底漆中含有双酚A,其可能溶出,同时,从溶剂的使用导致的喷涂操作性或成本的角度考虑,人们希望有取代它们的方法。
也广泛已知例如利用将热塑性树脂的热融合性,将金属基体与热塑性树脂贴合,该方法中,已知有将热塑性聚酯树脂等的预先形成的薄膜通过热粘合与金属板贴合的方法;或者将挤出的热塑性聚酯树脂等的熔融薄膜贴合在金属板上的方法。
后者的通过挤出层合法与金属板贴合的方法可以非常高速地进行处理,同时可得到可减少制膜的操作以及由此带来的成本,但是,使用通常的聚酯时,会发生膜摆动、脉动等问题,难以稳定地在金属板上贴合性良好地形成均匀膜厚的被覆层。
制罐中使用的被覆树脂的金属板中,必须使被覆树脂的金属板具有可耐受拉深加工或者拉深、减薄加工等严酷的加工条件的覆膜加工贴合性,同时还要求可耐受折弯机等的抗冲击性(抗凹性(dent resistance))。另外还要求可满足由于内容物的不同而可能在蒸馏灭菌等高温湿热条件下使用的情况、或者在用于热折弯机的情况的耐腐蚀性或抗冲击性。
作为具有上述特性的被覆树脂的金属板,在日本特开2001-328208 号公报中提出了一种被覆树脂的金属板,其特征在于:热塑性树脂层含有以聚对苯二甲酸乙二醇酯为主体的聚酯和乙烯系聚合物,且该树脂层含有0.5-3重量%生育酚及其衍生物。
发明内容
上述被覆树脂的金属板可以保持优异的抗冲击性和贴合性,同时具有良好的风格,通过配合离子键树脂可以获得更优异的抗冲击性,但是,在向聚酯树脂中掺混离子键树脂时,根据条件的不同,可能发生离子键树脂的凝聚导致的突起,产生了成品率无法提高的新的技术问题。
因此,本发明的目的在于提供具有优异的成膜性,同时即使不掺混离子键树脂也具有优异的抗冲击性的、用于被覆金属板的聚酯树脂。
本发明的另一目的在于提供耐腐蚀性、抗冲击性(抗凹性)、加工性、贴合性、风格(フレ一バ一性)等各特性均优异的被覆树脂的金属板、以及由该被覆树脂的金属板形成的金属罐和罐盖。
本发明可提供用于被覆金属板的聚酯树脂,其特征在于:含有2~10mol%二聚酸作为二羧酸成份,重均分子量(Mw)在70,000~160,000范围。
本发明的用于被覆金属板的聚酯树脂中,优选
1.含有1~15mol%间苯二甲酸作为二羧酸成份;
2.玻璃化转变温度在30~70℃的范围,以及185℃下的结晶速度为0.014秒-1以下。
本发明提供一种薄膜,其特征在于:该薄膜含有上述聚酯树脂。
本发明进一步提供被覆了树脂的金属板,其特征在于:该被覆了树脂的金属板具有含有上述聚酯树脂的被覆层。本发明的被覆了树脂的金属板中,优选以含有下述聚酯树脂的层作为下层,上层具有含其它聚酯树脂的层。
本发明还提供金属罐和盖,其特征在于:该金属罐和盖由上述被覆树脂的金属板形成。
本发明用于被覆金属板的树脂,含有2~10mol%二聚酸作为二羧酸成分,重均分子量(Mw)在70,000~160,000的范围,由此,即使不配合离子键树脂也可以使其具有优异的抗冲击性,可以产率良好地生产成膜性良好、具有优异的抗冲击性(抗凹性)的被覆树脂的金属板。
并且,本发明的被覆了聚酯树脂的树脂被覆金属板耐腐蚀性、加工贴合性、风格等也优异,使用该树脂被覆金属板成型得到的金属罐和盖在严酷的加工条件下也可以具有优异的加工贴合性、耐腐蚀性,并且,在进行蒸馏灭菌处理或用于热弯折机等时,抗冲击性不会降低,可体现优异的抗冲击性。
本发明聚酯树脂的重要特征是:含有2~10mol%二聚酸作为二羧酸成分,且重均分子量(Mw)在70,000~160,000的范围。
本发明的聚酯树脂的必须成分二聚酸的分子链中具有富于挠曲性的长的亚烷基链,因此,通过使所述二聚酸作为共聚成分,可以使聚酯树脂的玻璃化转变温度降低,使其具有柔软性,提高抗冲击性。结果,不会发生以往的问题,即,由于离子键树脂的凝聚而导致的成品率降低的问题,可以产率良好地制备薄膜或被覆树脂的金属板。
本发明的聚酯树脂的重均分子量(Mw)在70,000~160,000,特别是90,000~140,000的范围,这是很重要的,由此可以获得优异的成膜性,即,一般的聚酯树脂(聚对苯二甲酸乙二醇酯)熔融粘度低,如果以高速进行流延薄膜成型或在金属基体上挤出层合,则由T模头挤出的熔融树脂膜宽度方向的端部摆动,出现膜摆动现象;由T模头挤出的熔融树脂膜沿长度方向产生膜厚偏差,发生脉动现象。对此,本发明的聚酯树脂通过具有上述范围的重均分子量(Mw),可以保持聚酯树脂熔融混炼挤出时在常规条件即260℃和剪切速度243秒-1下的熔融粘度为6000泊以上,因此不会发生上述问题,具有优异的成膜性。
本发明的聚酯树脂中,二聚酸含量和重均分子量(Mw)具有临界性的意义,这可由后述实施例的结果了解。即,二聚酸含量和重均分子量(Mw)在上述范围内的本发明的聚酯树脂,其成膜性、抗冲击性(抗凹性)、贴合性、耐腐蚀性、风格等均优异(实施例1~6),而与此相对,二聚酸比上述范围少时,即使全部满足其它要件,抗冲击性也差(比较例1、2);另外,二聚酸比上述范围多时,树脂造粒时发生胶着,无法得到适合用于被覆金属板的树脂。另外,即使通过冷却完成造粒,其成膜性也差(比较例3)。重均分子量比70,000小时,即使全部满足其它要件,也会发生膜摆动或脉动,成膜性差(比较例4);重均分子量如果超过160,000,则固相聚合需要较长时间,并且聚合时发生凝胶化,无法获得适合用于被覆金属板的树脂。
具体实施方式
(聚酯树脂)
本发明的聚酯树脂含有2~10mol%、特别是3~7.5mol%二聚酸作为二羧酸成分,且重均分子量(Mw)在70,000~160,000、特别优选90,000~140,000的范围,除此之外均可以与公知的聚酯树脂同样地制备。
本发明的聚酯树脂中优选使用的二聚酸通常是含有不饱和脂肪酸的二聚体的二羧酸,不饱和脂肪酸优选碳原子数为10以上,特别优选碳原子数为18的油酸、亚油酸、亚麻酸等,通过将它们二聚化来制备。
二聚酸可以是将同样的不饱和脂肪酸二聚化,也可以是将不同的不饱和脂肪酸二聚化,还可以是在二聚化后进行氢化、还原。二聚酸可以部分含有芳环或环烷环(シクロ環)。
本发明中,从抗冲击性角度考虑,特别优选使用完全氢化的二聚酸,优选的二聚酸可通过购自商品名PRIPOL 1009(ュニケマ公司生产)获得。
除二聚酸以外的二羧酸成分例如可以是聚酯树脂制备中使用的以往公知的二羧酸,例如对苯二甲酸、间苯二甲酸、萘二甲酸、对-β-羟基乙氧基苯甲酸、联苯-4,4’-二甲酸、二苯氧基乙烷-4,4’-二甲酸、5-钠代磺基间苯二甲酸(5-ナトリウムスルホイソフタル酸)、六氢对苯二甲酸、己二酸、癸二酸、偏苯三酸、均苯四甲酸、连苯三酸、1,1,2,2-乙烷四甲酸、1,1,2-乙烷三甲酸、1,3,5-戊烷三甲酸、1,2,3,4-环戊烷四甲酸、联苯-3,4,3’,4’-四甲酸等,从被覆层的机械性质或热学性质考虑,优选对苯二甲酸占二羧酸成分的75%以上,特别优选含有80%以上。
本发明的聚酯树脂中,优选含有1~15mol%间苯二甲酸作为二羧酸成分。由此,185℃下的结晶速度为0.014秒-1以下,可以使其与被覆树脂的金属板的贴合性提高。
本发明的聚酯树脂中可以同时含有间苯二甲酸与二聚酸作为共聚成分,或者也可以制备以间苯二甲酸作为共聚成分的其它对苯二甲酸乙二醇酯系聚酯树脂,将其与含有上述二聚酸的聚酯树脂掺混来含有。
可在本发明的聚酯树脂中使用的二醇成分中,从被覆层的机械性质或热学性质考虑,优选二醇成分的50%以上、特别是80%以上为乙二醇,乙二醇以外的二醇成分有:1,4-丁烷二醇、丙二醇、新戊二醇、1,6-己二 醇、二甘醇、三甘醇、环己烷二甲醇、双酚A的环氧乙烷加成物、甘油、三羟甲基丙烷、季戊四醇、甘油、三羟甲基丙烷、1,2,6-己烷三醇、山梨醇、1,1,4,4-四(羟基甲基)环己烷等。
特别优选本发明的聚酯树脂中以0.1~2重量%的量含有维生素E(生育酚)。在聚酯树脂的成型工艺中,维生素E可以防止各种热历程导致的分子量降低。
除维生素E之外,还可以按照公知的配方配合本身公知的树脂用配合剂,例如非晶二氧化硅等防粘连剂、二氧化钛(钛白)等颜料、抗氧化剂、稳定剂、各种抗静电剂、润滑剂等。
本发明的聚酯树脂如前所述,含有2~10mol%二聚酸作为二羧酸成分,因此玻璃化转变温度(Tg)在30~70℃的范围,比一般的聚对苯二甲酸乙二醇酯(Tg=78℃)低,因此抗冲击性特别优异。
本发明的聚酯树脂按照后述实施例所示方法测定的特性粘度[η]优选在0.8~1.2的范围。
(薄膜)
本发明的聚酯薄膜优选为通过T-模头法、吹塑制膜法等挤出成型方法成型的流延薄膜,特别优选将挤出的薄膜骤冷的流延成型法得到的未拉伸的薄膜。
薄膜的厚度根据所使用的用途而不同,通常为1~500μm,特别优选3~100μm的范围。如后所述,制罐用的被覆树脂的金属板的被覆层优选制成3~40μm、特别是5~35μm的厚度。
(被覆树脂的金属板)
本发明的被覆树脂的金属板中使用的金属板可以使用各种表面处理钢板或铝等轻金属板。表面处理钢板可以使用下述钢板:将冷轧压延钢板进行退火,然后进行二次冷轧压延,进行镀锌、镀锡、镀镍、电解铬酸处理、铬酸处理等表面处理中的一种或两种以上所得。还可以使用实施了镀铝、铝压延等的被覆铝的钢板。
轻金属板除了所谓的纯铝板之外,还可使用铝合金板。
金属板的原板厚度根据金属的种类、容器的用途或尺寸而不同,通常可具有0.10-0.50mm的厚度,其中,为表面处理钢板时,可具有0.10-0.30mm的厚度,为轻金属板时,可具有0.15-0.40mm的厚度。
本发明的被覆树脂的金属板中,可通过将上述含有聚酯树脂的聚酯 薄膜热粘合在金属板上来制备,也可以通过挤出涂布法,将上述聚酯树脂直接挤出到金属板上,形成薄膜,由此可以形成含有本发明的聚酯树脂的被覆层。
采用挤出涂布法时,使用与树脂层的种类对应的挤出机,通过模头挤出聚酯,同时将其以熔融状态挤出涂布在金属基体上,热粘合。聚酯树脂与金属基体的热粘合可通过熔融树脂组合物层所具有的热量和金属板所具有的热量进行。金属板的加热温度通常为90-290℃,特别是100-280℃的温度较为恰当。
本发明的被覆树脂的金属板中,无需在树脂被覆层和金属材料之间设置底漆层,可以将树脂被覆层直接与金属材料粘合,当然,设置底漆层不是不可以,可以根据需要设置底漆层。
本发明的被覆树脂的金属板优选在金属板表面、特别是作为容器内面的金属表面上设置上述含有聚酯树脂的被覆层,该被覆层的厚度优选为3-40μm,特别优选以5-35μm的厚度,优选在金属表面上形成。
本发明的被覆树脂的金属板中,以被覆树脂的金属板作为容器时,在内面一侧至少设置一层含有本发明的聚酯树脂的被覆层,优选将含有本发明的聚酯树脂的层作为下层(金属板一侧),再形成含有风格优异的其它聚酯树脂的上层。
特别优选形成双层结构,其中,以含有共聚聚对苯二甲酸乙二醇酯的层作为上层,其中所述共聚聚对苯二甲酸乙二醇酯含有间苯二甲酸作为共聚成分。间苯二甲酸的含量优选为1~10mol%。
在金属板上形成上述两层时,在使用另外制备的流延薄膜时没有问题,但是在共挤出层合时,下层的聚酯树脂与上层的聚酯树脂以熔融张力比1.1∶1-5∶1共挤出,这从高速挤出层合中脉动的发生或挤出性考虑是优选的。
含有本发明的聚酯树脂的下层和含有其它聚酯树脂的上层的厚度比为1∶15-15∶1的范围,进行高速挤出,这样,可以同时平衡良好地兼具层合性和风格两者。
(罐和盖)
本发明的罐可通过以往公知的成型方法将上述被覆树脂的金属板制罐,使含有本发明的聚酯树脂的被覆层为罐内面,特别优选侧面没有接缝的无缝罐,可通过拉深加工、拉深-深度拉深加工、拉深-减薄加工、 拉深-弯曲拉伸加工-减薄加工等方法制备。其侧壁部优选通过被覆树脂的金属板的拉深-再拉深加工的弯曲拉伸或进一步减薄加工实现薄壁化,形成被覆树脂的金属板原来厚度的20-95%、特别是30-85%的厚度。
本发明的盖也可通过将上述被覆树脂的金属板成型,使含有本发明的聚酯树脂的被覆层为盖内面来制造。此外,还可以通过以往公知的盖的制备方法成型。
关于盖的形状,可以制成用于形成内容物注入倒出开口的、设有划痕和开罐用的拉环的易开盖等以往公知的罐盖,或者是通过将上述被覆树脂的金属板进行拉深加工等方法成型的、含有顶板部和裙部的盖。
实施例
通过以下例子说明本发明。将各实施例和比较例中使用的树脂与下述(1)-(4)的树脂特性值一并示于表1中。使用表1的树脂制备的薄膜的(2)-(5)所示的特性值和被覆树脂的金属板的(6)-(9)所示的评价结果如表2所示。
(1)树脂特性粘度
将200mg表1所示的树脂在110℃下溶解于苯酚/1,1,2,2-四氯乙烷混合溶液(重量比1∶1)中,使用乌氏粘度计测定30℃下的比粘度。特性粘度[η](dl/g)可通过下式求出。
[η]=[(-1+(1+4K’ηsp)1/2)/2K’C]
K’:赫金常数(=0.33)
C:浓度(g/100ml)
ηsp:比粘度[=(溶液的滴落时间-溶剂的滴落时间)/溶剂的滴落时间]
(2)分子量测定
将树脂溶解于HFIP/氯仿=3/40(V/V)的溶剂中,通过GPC测定。此时,流动相是氯仿,柱温40℃、检测使用UV(254nm)进行。以聚苯乙烯作为基准物质测定,得到重均分子量(Mw)。
(3)熔融粘度
使用东洋精机制作所制造的キヤピロゲラフ测定树脂的熔融粘度,得 到树脂温度260℃、剪切速度243秒-1时的熔融粘度。
(4)玻璃化转变温度
将5mg树脂用差示扫描量热分析装置(DSC)、在氮气环境下以10℃/分钟由0℃升温至300℃,在300℃下保持1分钟,然后骤冷至0℃,再以10℃/分钟升温至300℃进行测定。通过第二次的升温测定读取的玻璃化转变温度如表1所示。
(5)结晶速度
用差示扫描量热分析装置(DSC)对10mg流延薄膜进行测定。测定首先是以30℃/分钟的升温速度由室温加热至300℃,保持5分钟,然后骤冷至185℃,开始保持。等温保持开始后,观测结晶产生的发热峰。该峰顶时间的倒数作为结晶速度(秒-1)进行评价。此时,测定在氮气环境中进行。
(6)平板抗凹ERV试验
将被覆树脂的金属板在225℃下热处理3分钟、在205℃下热处理2分钟,然后在125℃进行30分钟的蒸馏处理,将该被覆树脂的金属板在保持37℃的水中保存一个月。然后,在5℃、湿润下,使待评价的被覆面与厚度3mm、硬度50°的硅橡胶接触,在夹持金属板的另一侧放置直径5/8英寸的钢球,将1kg的重锤由40mm处落下,进行冲击顶出加工。
然后,通过对加工部施加6.30V电压时的电流值来评价冲击加工部的树脂被覆层的破裂程度。
评价结果如下所示:
○:平均电流值≤0.1mA
×:平均电流值>0.1mA
(7)罐抗凹试验
在95℃下,向罐中填充蒸馏水,在125℃进行30分钟的蒸馏处理,在37℃的保温箱内放置一个月,在5℃气氛下,沿着15°的斜面、从高50cm处垂直落下,冲击罐底。冲击后除去蒸馏水,通过对冲击加工部施加6.30V电压时的电流值来评价罐底加工部的树脂被覆层的破裂程度。
评价结果如下所示:
○:平均电流值≤3mA
×:平均电流值>3mA。
(8)压延加工后贴合性
使用与薄膜的贴合性较低的铬酸磷酸处理的铝合金(5021材)作为基材,制作一个面被表2所示树脂被覆的树脂被覆金属板,通过压延机进行压延,等效应变为80%。接着,在1英寸的方块树脂被覆面上划10×10的小格,在划格面上贴合工业用强力胶带,通过顺势剥离胶带时金属板上的薄膜残留率(%)评价贴合性。
评价结果如下所示:
○:平均薄膜残留率≥50%
×:平均薄膜残留率<50%。
(9)蒸馏耐腐蚀性
在95℃下向罐中填充蒸馏水,在125℃进行30分钟的蒸馏处理,再恢复至室温,除去蒸馏水,为金属罐时观察罐内面、为盖时观察盖内面的腐蚀状态进行评价。
评价结果如下所示:
○:完全未见腐蚀。
×:可见腐蚀等异常。
(实施例1)
使用两台挤出机和双层T模头,将表1中的树脂A供给下层,将表1中的树脂J供给表层,熔融混炼,挤出,使下层为12μm,表层为4μm,将其用冷却辊冷却,卷取所得薄膜,制成流延薄膜。
接着,将该流延薄膜在铝合板(板厚0.28mm、A3004材料、铬酸/磷酸表面处理)的一个面上、将含有树脂K的流延薄膜在另一个面上同时热层合,立即进行水冷,得到被覆树脂的金属板。此时,层合前金属板的温度设定为比聚酯树脂的熔点高15℃。层合辊的温度为150℃,过板速度为40m/分钟。
进一步向该被覆树脂的金属板上涂布蜡系润滑剂,冲压出直径152mm的圆盘,进行拉深加工,使下层为树脂A、表层为树脂J的树脂被覆面作为内面一侧,得到浅拉深的杯子。接着,将该浅拉深的杯子进行减薄加工,得到无缝杯。
该无缝杯的各特性如下所示。
杯直径:66mm
杯高度:127mm
侧壁相对于原板的厚度:45%
将该无缝杯按照常规方法进行隆起成型,在聚酯树脂的Tm-10℃下进行3分钟的热处理,将杯放置冷却后,将开口边缘部进行修剪加工,进行曲面印刷,烧结干燥、缩幅加工、凸缘加工等后工序,得到350ml无缝罐。
(实施例2)
使用两台挤出机和双层T模头,将表1中的树脂B供给下层,将表1中的树脂J供给表层,熔融混炼,挤出,使下层为24μm,表层为4μm,将其用冷却辊冷却,卷取所得薄膜,制成流延薄膜。
接着,将该流延薄膜在TFS钢板(板厚0.18mm、金属铬量为120mg/m2、铬氢氧化物(クロム水和酸化物)量为15mg/m2)的一个面上、将配合了20重量%作为颜料的二氧化钛的含有聚酯树脂的流延薄膜在另一个面上同时热层合,立即进行水冷,得到被覆树脂的金属板。此时,层合前金属板的温度设定为比聚酯树脂的熔点高15℃。层合辊的温度为150℃,过板速度为40m/分钟。
进一步向该被覆树脂的金属板上涂布蜡系润滑剂,冲压出直径166mm的圆盘,进行拉深加工,下层为树脂B、表层为树脂J的树脂被覆面作为内面一侧,得到浅拉深的杯子。接着,将该浅拉深的杯子进行再拉深、减薄加工,得到无缝杯。
该无缝杯的各特性如下所示。
杯直径:66mm
杯高度:128mm
侧壁相对于原板的厚度:50%
将该无缝杯按照常规方法进行杯底成型,在聚酯树脂的Tm-10℃下进行3分钟的热处理,将杯放置冷却后,将开口边缘部进行修剪加工,进行外面印刷,烧结干燥、缩幅加工,得到350ml无缝罐。
(实施例3)
将表1中的树脂C供给到具有挤出涂布设备的挤出机中,在板厚0.235mm的铝合金(A5182材)的一个面上挤出层合,得到树脂厚度为20μm的被覆树脂的金属板。
此时,层合前铝合金板的温度设定为比树脂的熔点低30℃。层合辊的温度为90℃,过板速度为40m/分钟。
接着,将该被覆树脂的金属板冲压成直径68.7mm的盖,使树脂被覆面作为盖的内面一侧,接着在盖的外面一侧进行部分开口型的划痕加工(宽22mm,划痕后的剩余厚度110μm、划痕宽度20μm)、铆钉加工以及开罐用的拉环的安装,制作SOT盖(拉环保留在盖上)。
(实施例4)
使用两台挤出机和双层T模头,将表1中的树脂D供给下层,将表1中的树脂J供给表层,熔融混炼,挤出,使下层为16μm,表层为4μm,将其用冷却辊冷却,卷取所得薄膜,制成流延薄膜。
接着,将该流延薄膜在TFS钢板(板厚0.24mm、金属铬量为120mg/m2、铬氢氧化物量为15mg/m2)的一个面上、将配合了20重量%作为颜料的二氧化钛的含有聚酯树脂的流延薄膜在另一个面上同时热层合,立即进行水冷,得到被覆树脂的金属板。此时,层合前金属板的温度设定为比聚酯树脂的熔点高15℃。层合辊的温度为150℃,过板速度为40m/分钟。
进一步向该被覆树脂的金属板上涂布蜡系润滑剂,冲压出直径158mm的圆盘,进行拉深加工,下层为树脂D、表层为树脂J的树脂被覆面作为内面一侧,得到浅拉深的杯子。接着,将该浅拉深的杯子进行再拉深、减薄加工,按照常规方法进行瓶成型,得到深度拉深、减薄的杯。
该深度拉深、减薄的杯的各特性如下所示。
杯直径:52mm
杯高度:141.5mm
侧壁相对于原板的厚度:37%
凸缘相对于原板的厚度:69%
将该深度拉深、减薄的杯按照常规方法进行杯底成型,在聚酯树脂的Tm-10℃下进行3分钟的热处理,将杯放置冷却后,进行开口边缘部的修剪加工、外面印刷,烧结干燥。将该杯再次进行缩幅加工、卷边加工、螺纹加工、弯曲加工,制作口径30mm的可再封罐。
(实施例5)
在下层使用表1的树脂E和树脂K的共混树脂,制成流延薄膜在内面使用,除此之外与实施例1同样地得到被覆树脂的金属板、无缝罐。
(实施例6)
在下层使用表1的树脂F和维生素E,制成流延薄膜在内面使用,除 此之外与实施例1同样地得到被覆树脂的金属板、无缝罐。
(比较例1)
在下层使用表1的树脂J和,制成流延薄膜在内面使用,除此之外与实施例1同样地得到被覆树脂的金属板、无缝罐。
(比较例2)
在下层使用表1的树脂G,制成流延薄膜在内面使用,除此之外与实施例1同样地得到被覆树脂的金属板、无缝罐。
(比较例3)
在下层使用表1中的树脂H,除此之外与实施例1同样地得到流延薄膜。
(比较例4)
在下层使用表1中的树脂I,除此之外与实施例1同样地得到流延薄膜。
如表2所示,实施例1~6中成膜性良好,将其被覆得到的被覆树脂的金属板在平板抗凹性ERV试验中的抗凹性、压延加工后的树脂贴合性优异,并且将该被覆树脂的金属板成型得到的无缝罐、罐盖的抗凹性、耐腐蚀性优异。另外,实施例1~6中,由被覆树脂的金属板制作的罐和盖的风格良好。
比较例1、2成膜性良好,但是将其被覆得到的被覆树脂的金属板或罐抗凹性、耐腐蚀性差。比较例3、4中,成膜性显著变差,之后的评价无法进行。
表1
二聚酸量 mol% | 间苯二甲酸量 mol% | 特性粘度 cc/g | 分子量 Mw | 熔融粘度 泊 | 玻璃化转变温度 ℃ | |
树脂A | 2.0 | 10.0 | 0.93 | 90,000 | 8,500 | 64 |
树脂B | 4.0 | 5.0 | 1.06 | 98,000 | 10,750 | 54 |
树脂C | 4.0 | 15.0 | 1.18 | 141,000 | 12,400 | 53 |
树脂D | 5.0 | 10.0 | 1.12 | 131,000 | 10,280 | 50 |
树脂E | 7.5 | 0.0 | 1.17 | 123,000 | 10,790 | 41 |
树脂F | 7.5 | 10.0 | 1.18 | 138,000 | 11,180 | 40 |
树脂G | 1.0 | 5.0 | 1.09 | 117,000 | 11,080 | 68 |
树脂H | 12.0 | 5.0 | 0.77 | 87,000 | 1,280 | 24 |
树脂I | 5.0 | 5.0 | 0.83 | 68,000 | 4,710 | 49 |
树脂J | 0.0 | 5.0 | 0.90 | 79,000 | 10,090 | 77 |
树脂K | 0.0 | 15.0 | 0.90 | 82,000 | 2,000 | 74 |
[0140] 表2
下层成分 | 二聚酸量 (mol%) | 间苯二甲酸量 (mol%) | 成膜性 | 分子量 Mw | 玻璃化转变温度 (℃) | 结晶速度 (秒-1) | 基材 | 成型 | 抗凹性 (平板) | 抗凹性 (罐) | 贴合性 | 耐腐 蚀性 | |
实施例1 | 树脂A:100% | 2.0 | 10.0 | 良好 | 71,000 | 64 | 0.001以下 | 铝 | 350ml罐 | ○ | ○ | ○ | ○ |
实施例2 | 树脂B:100% | 4.0 | 5.0 | 良好 | 77,000 | 54 | 0.001 | TFS | 350ml罐 | ○ | ○ | ○ | ○ |
实施例3 | 树脂C:100% | 4.0 | 15.0 | 良好 | 78,000 | 54 | 0.001以下 | 铝 | SOT盖 | ○ | - | ○ | ○ |
实施例4 | 树脂D:100% | 5.0 | 10.0 | 良好 | 76,000 | 50 | 0.001以下 | TFS | 可再封罐 | ○ | ○ | ○ | ○ |
实施例5 | 树脂E:80% 树脂K:20% | 6.0 | 2.9 | 良好 | 72,000 | 46 | 0.005 | TFS | 350ml罐 | ○ | ○ | ○ | ○ |
实施例6 | 树脂F:99.5% 维生素E:0.5% | 7.5 | 10.0 | 良好 | 84,000 | 39 | 0.001以下 | TFS | 350ml罐 | ○ | ○ | ○ | ○ |
比较例1 | 树脂J:100% | 0.0 | 5.0 | 良好 | 67,000 | 73 | 0.001 | TFS | 350ml罐 | × | × | ○ | × |
比较例2 | 树脂G:100% | 1.0 | 5.0 | 良好 | 78,000 | 68 | 0.001 | TFS | 350ml罐 | × | × | ○ | × |
比较例3 | 树脂H:100% | 12.0 | 5.0 | 膜摆动、脉动 | - | - | - | TFS | - | - | - | - | - |
比较例4 | 树脂I:100% | 5.0 | 5.0 | 膜摆动、脉动 | - | - | - | TFS | - | - | - | - | - |
Claims (7)
1.用于被覆金属板的聚酯树脂,其特征在于:在二羧酸成分中,含有2~4mol%完全氢化的二聚酸、1~15mol%间苯二甲酸,重均分子量(Mw)在70,000~160,000的范围,玻璃化转变温度在54~70℃的范围。
2.权利要求1的聚酯树脂,其中,185℃下的结晶速度为0.014秒-1以下。
3.薄膜,其特征在于:该薄膜含有权利要求1的树脂。
4.被覆了树脂的金属板,其特征在于:该被覆了树脂的金属板具有包含权利要求1的树脂的被覆层。
5.权利要求4的被覆了树脂的金属板,该被覆了树脂的金属板上形成有下层和上层,以含有上述树脂的被覆层作为所述下层,含有聚对苯二甲酸乙二醇酯的层作为所述上层,该聚对苯二甲酸乙二醇酯含有间苯二甲酸作为共聚成分。
6.金属罐,其特征在于:该金属罐由权利要求4的被覆了树脂的金属板形成。
7.盖,其特征在于:该盖由权利要求4的被覆了树脂的金属板形成。
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CN107254034A (zh) * | 2017-04-20 | 2017-10-17 | 浙江传化天松新材料有限公司 | 一种具有良好抗石击性透明粉末涂料用聚酯树脂及其制备方法 |
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US20090011162A1 (en) | 2009-01-08 |
EP1849813A1 (en) | 2007-10-31 |
WO2006088212A1 (ja) | 2006-08-24 |
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CN101160339A (zh) | 2008-04-09 |
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