CN110637059B - 乙烯-乙烯醇系共聚物组合物、粒料及多层结构体 - Google Patents
乙烯-乙烯醇系共聚物组合物、粒料及多层结构体 Download PDFInfo
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- CN110637059B CN110637059B CN201880032794.6A CN201880032794A CN110637059B CN 110637059 B CN110637059 B CN 110637059B CN 201880032794 A CN201880032794 A CN 201880032794A CN 110637059 B CN110637059 B CN 110637059B
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Abstract
作为着色得以抑制的乙烯‑乙烯醇系共聚物组合物，提供如下乙烯‑乙烯醇系共聚物组合物，其含有乙烯‑乙烯醇系共聚物(A)、聚酰胺系树脂(B)及铁化合物(C)，上述铁化合物(C)的含量相对于乙烯‑乙烯醇系共聚物组合物的单位重量以金属换算为0.01～20ppm。
Description
技术领域
本发明涉及含有乙烯-乙烯醇系共聚物(以下，称为“EVOH树脂”。)的EVOH树脂组合物、粒料及多层结构体，更详细而言，涉及着色及经时的粘度增加得以抑制的EVOH树脂组合物、由所述EVOH树脂组合物形成的粒料及具备由EVOH树脂组合物形成的层的多层结构体。
背景技术
EVOH树脂的透明性、氧气等的阻气性、保香性、耐溶剂性、耐油性、机械强度等优异，成形为薄膜、片、瓶等而广泛用作食品包装材料、医药品包装材料、工业药品包装材料、农药包装材料等各种包装材料。但是，若将包含EVOH树脂层的包装材料供于蒸煮(retort)、煮沸(boil)等热水杀菌处理，则有EVOH树脂层溶出、或EVOH树脂层的阻气性降低的倾向。对此，已知有组合使用聚酰胺系树脂的技术(例如，参照专利文献1、2)。
现有技术文献
专利文献
专利文献1：日本特开2005-178324号公报
专利文献2：日本特开2009-242591号公报
发明内容
发明要解决的问题
另一方面，包含EVOH树脂及聚酰胺系树脂的树脂组合物有在熔融混炼、熔融成形等加热后着色的倾向、经时地粘度增加的倾向，需要改善。
用于解决问题的方案
本发明人等鉴于上述实际情况进行了深入研究，结果发现，在包含EVOH树脂及聚酰胺系树脂的树脂组合物中配混微量的铁化合物时，能解决上述问题。
即，本发明第1主旨为一种EVOH树脂组合物，其含有EVOH树脂(A)、聚酰胺系树脂(B)及铁化合物(C)，上述铁化合物(C)的含量相对于EVOH树脂组合物的单位重量以金属换算为0.01～20ppm。另外，本发明第2主旨为一种粒料，其由上述EVOH树脂组合物形成，进而第3主旨为一种多层结构体，其具备由上述EVOH树脂组合物形成的层。
发明的效果
本发明的EVOH树脂组合物为含有EVOH树脂(A)、聚酰胺系树脂(B)及铁化合物(C)的EVOH树脂组合物，上述铁化合物(C)的含量相对于EVOH树脂组合物的单位重量以金属换算为0.01～20ppm，因此着色得以抑制，另外，动态粘度行为优异。
另外，上述EVOH树脂(A)相对于上述聚酰胺系树脂(B)的重量含有比率为(A)/(B)＝99/1～10/90时，可进一步抑制着色。
本发明的由EVOH树脂组合物形成的粒料抑制了着色，因此可以制成各种成形物适合用作例如食品、药品、农药等的包装材料、特别是热水杀菌用包装材料。
本发明的具备由EVOH树脂组合物形成的层的多层结构体抑制了着色，因此可以制成各种成形物适合用作例如食品、药品、农药等的包装材料、特别是热水杀菌用包装材料。
具体实施方式
以下，详细地对本发明的构成进行说明，但这些示出了理想的实施方式的一例，并不限定于这些内容。
<EVOH树脂组合物>
本发明的EVOH树脂组合物含有EVOH树脂(A)、聚酰胺系树脂(B)及铁化合物(C)。另外，本发明的EVOH树脂组合物以EVOH树脂(A)和聚酰胺系树脂(B)为主成分。即，EVOH树脂组合物中的EVOH树脂(A)和聚酰胺系树脂(B)的合计含量通常为70重量％以上，优选为80重量％以上、更优选为90重量％以上、特别优选为95重量％以上。以下，依次对本发明的EVOH树脂组合物的各成分进行说明。
[EVOH树脂(A)]
本发明中使用的EVOH树脂(A)通常为通过使作为乙烯和乙烯基酯系单体的共聚物的乙烯-乙烯基酯系共聚物皂化而得到的树脂，为非水溶性的热塑性树脂。作为上述乙烯基酯系单体，从经济方面出发，通常使用乙酸乙烯酯。
作为乙烯和乙烯基酯系单体的聚合法，可以使用公知的任意的聚合法、例如溶液聚合、悬浮聚合、乳液聚合等进行，通常使用以甲醇为溶剂的溶液聚合。得到的乙烯-乙烯基酯系共聚物的皂化也可以通过公知的方法进行。
如此制造的EVOH树脂(A)以源自乙烯的结构单元和乙烯醇结构单元为主，包含未皂化而残存的若干量的乙烯基酯结构单元。
作为上述乙烯基酯系单体，从市场获得性、制造时的杂质处理效率好的方面出发，代表性的是使用乙酸乙烯酯。作为其他乙烯基酯系单体，例如可列举出甲酸乙烯酯、丙酸乙烯酯、戊酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、特戊酸乙烯酯、癸酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯、叔碳酸乙烯酯等脂肪族乙烯基酯、苯甲酸乙烯酯等芳香族乙烯基酯等，通常可以使用碳数3～20、优选碳数4～10、特别优选碳数4～7的脂肪族乙烯基酯。这些通常可以单独使用，根据需要可以同时使用多种。
EVOH树脂(A)中的乙烯结构单元的含量可以通过使乙烯基酯系单体和乙烯共聚时的乙烯的压力来控制，通常为20～60摩尔％，优选为25～50摩尔％、特别优选为25～35摩尔％。所述含量过低的情况下，有高湿下的阻气性、拉伸性降低的倾向，相反过高的情况下，有阻气性降低的倾向。需要说明的是，所述乙烯结构单元的含量可以基于ISO14663来测定。
EVOH树脂(A)中的乙烯基酯成分的皂化度可以通过使乙烯-乙烯基酯系共聚物皂化时的皂化催化剂(通常使用氢氧化钠等碱性催化剂)的量、温度、时间等来控制，通常为90～100摩尔％，优选为95～100摩尔％、特别优选为98～100摩尔％。所述皂化度过低的情况下，有阻气性、热稳定性、耐湿性等降低的倾向。所述EVOH树脂的皂化度可以基于JIS K6726(其中，EVOH树脂以均匀地溶解于水/甲醇溶剂而成的溶液的形式使用)进行测定。
另外，EVOH树脂(A)的熔体流动速率(MFR)(210℃、载荷2160g)通常为0.5～100g/10分钟，优选为1～50g/10分钟、特别优选为3～35g/10分钟。所述MFR过大的情况下，有损害制膜时的稳定性的倾向，过小的情况下，有粘度过高从而熔融挤出变困难的倾向。所述MFR为EVOH树脂的聚合度的指标，可以通过使乙烯和乙烯基酯系单体共聚时的聚合引发剂的量、溶剂的量来调整。
本发明中所用的EVOH树脂(A)中可以在不阻碍本发明效果的范围(例如，EVOH树脂(A)的20摩尔％以下)内进而包含源自以下所示的共聚单体的结构单元。
作为上述共聚单体，可列举出丙烯、1-丁烯、异丁烯等烯烃类、3-丁烯-1-醇、3-丁烯-1,2-二醇、4-戊烯-1-醇、5-己烯-1,2-二醇等含羟基的α-烯烃类、其酯化物、酰基化物等衍生物；2-亚甲基丙烷-1,3-二醇、3-亚甲基戊烷-1,5-二醇等羟基烷基亚乙烯基化合物(hydroxyalkyl vinylidene)类；1,3-二乙酰氧基-2-亚甲基丙烷、1,3-二丙酰氧基-2-亚甲基丙烷、1,3-二丁酰氧基-2-亚甲基丙烷等羟基烷基亚乙烯基二乙酸酯类；丙烯酸、甲基丙烯酸、巴豆酸、苯二甲酸(酐)、马来酸(酐)、衣康酸(酐)等不饱和酸类或其盐或烷基的碳数为1～18的这些不饱和酸的单或二烷基酯类；丙烯酰胺、烷基的碳数为1～18的N-烷基丙烯酰胺、N,N-二甲基丙烯酰胺、2-丙烯酰胺丙磺酸或其盐、丙烯酰胺丙基二甲基胺或其酸盐或其季盐等丙烯酰胺类；甲基丙烯酰胺、烷基的碳数为1～18的N-烷基甲基丙烯酰胺、N,N-二甲基甲基丙烯酰胺、2-甲基丙烯酰胺丙磺酸或其盐、甲基丙烯酰胺丙基二甲基胺或其酸盐或其季盐等甲基丙烯酰胺类；N-乙烯基吡咯烷酮、N-乙烯基甲酰胺、N-乙烯基乙酰胺等N-乙烯基酰胺类；丙烯腈、甲基丙烯腈等氰化乙烯基类；烷基乙烯基醚、羟基烷基乙烯基醚、烷氧基烷基乙烯基醚等烷基的碳数为1～18的乙烯基醚类；氯乙烯、偏氯乙烯、氟乙烯、偏氟乙烯、溴乙烯等卤化乙烯基化合物类；三甲氧基乙烯基硅烷等乙烯基硅烷类；乙酸烯丙酯；烯丙基氯等卤化烯丙基化合物类；烯丙基醇、二甲氧基烯丙基醇等烯丙基醇类；三甲基-(3-丙烯酰胺-3-二甲基丙基)-氯化铵、丙烯酰胺-2-甲基丙磺酸等共聚单体。这些可以单独使用或组合使用2种以上。
特别是侧链具有伯羟基的EVOH树脂因保持阻气性并且二次成形性良好这点而优选，其中，优选使含羟基的α-烯烃类共聚而成的EVOH树脂，特别优选侧链具有1,2-二醇结构的EVOH树脂。特别是侧链具有伯羟基的情况下，其含量通常为EVOH树脂的0.1～20摩尔％，进而为0.5～15摩尔％，特别优选1～10摩尔％。
另外，作为本发明中使用的EVOH树脂(A)，可以为进行了氨基甲酸酯化、缩醛化、氰基乙基化、氧亚烷基化等“后改性”者。
进而，本发明中使用的EVOH树脂(A)可以为与不同的其他EVOH树脂的混合物，作为所述其他EVOH树脂，可列举出乙烯结构单元的含量不同者、皂化度不同者、聚合度不同者、共聚成分不同者等。其中，从保持阻气性并且二次成形性良好的观点出发，优选使用乙烯结构单元的含量不同的2种以上的EVOH树脂。
[聚酰胺系树脂(B)]
本发明中使用的聚酰胺系树脂(B)为公知的树脂，为非水溶性的热塑性树脂。
作为聚酰胺系树脂(B)，例如，可列举出聚己内酰胺(尼龙6)、聚-ω-氨基庚酸(尼龙7)、聚-ω-氨基壬酸(尼龙9)、聚十一酰胺(尼龙11)、聚月桂内酰胺(尼龙12)等均聚物。另外，作为共聚聚酰胺树脂，可列举出聚己二酰乙二胺(尼龙26)、聚己二酰丁二胺(尼龙46)、聚己二酰己二胺(尼龙66)、聚六亚甲基癸二酰胺(尼龙610)、聚十二烷二酰己二胺(尼龙612)、聚己二酰辛二胺(尼龙86)、聚十亚甲基己二酰二胺(尼龙108)、己内酰胺/月桂内酰胺共聚物(尼龙6/12)、己内酰胺/ω-氨基壬酸共聚物(尼龙6/9)、己内酰胺/六亚甲基己二酸二铵共聚物(尼龙6/66)、月桂内酰胺/六亚甲基己二酸二铵共聚物(尼龙12/66)、己二酰乙二胺/六亚甲基己二酸二铵共聚物(尼龙26/66)、己内酰胺/六亚甲基己二酸二铵/六亚甲基癸二酸二铵共聚物(尼龙66/610)、亚乙基己二酸铵/六亚甲基己二酸二铵/六亚甲基癸二酸二铵共聚物(尼龙6/66/610)等脂肪族聚酰胺、聚六亚甲基间苯二甲酰胺、聚六亚甲基对苯二甲酰胺、聚间苯二甲基己二酰二胺、六亚甲基间苯二甲酰胺/对苯二甲酰胺共聚物、聚对亚苯基对苯二甲酰胺、聚对亚苯基-3,4’二苯基醚对苯二甲酰胺等芳香族聚酰胺、非晶性聚酰胺、将这些聚酰胺树脂用亚甲基苄基胺、间苯二甲胺等芳香族胺进行改性而成者、间苯二甲基己二酸二铵等。或者可以为它们的末端改性聚酰胺树脂，优选为末端改性聚酰胺树脂。这些聚酰胺系树脂(B)可以使用1种或组合使用2种以上。
聚酰胺系树脂(B)有与EVOH树脂等含有极性基团的树脂的结合力变高的倾向。
对于构成上述聚酰胺系树脂(B)的酰胺单体单元中的酰胺键的比率，以分子量的比例对酰胺单体单元(例如，尼龙6的情况下，[-C6H5-CONH-]中的酰胺键(-CONH-))进行计算的情况下，优选20～60％、更优选为30～50％、特别优选为35～45％。所述酰胺键的比率过低的情况下，有与EVOH树脂(A)等极性树脂的界面的结合力容易降低的倾向，相反过高的情况下，有在熔融成形时与EVOH树脂(A)等极性树脂的反应性过强，从而共挤出时引起由粘接界面粗糙导致的外观不良的倾向。
另外，聚酰胺系树脂(B)的熔点优选为160～270℃、更优选为175～250℃、特别优选为190～230℃。所述聚酰胺系树脂(B)的熔点过低的情况下，有使用EVOH树脂组合物制造的多层结构体的耐热性降低的倾向。另一方面，若聚酰胺系树脂(B)的熔点过高，则包含其他树脂层的多层结构体的情况下，有如下的倾向：其他层中使用的树脂与EVOH树脂组合物的熔点差变大，将其他树脂和EVOH树脂组合物共挤出成形时，在合流时产生层错乱从而导致多层结构体的外观降低。进而，有将EVOH树脂(A)和聚酰胺系树脂(B)共挤出成形时模头温度过高从而促进由EVOH树脂(A)的热劣化导致的多层结构体的着色的担心。
从以上的观点出发，作为优选的聚酰胺系树脂(B)，为熔点为160～270℃、更优选为175～250℃、特别优选为190～230℃、并且酰胺键的比率为20～60％、更优选为30～50％、特别优选为35～45％的聚酰胺。具体而言，例如，优选尼龙6(熔点：约220℃、酰胺键的比率：38％)、尼龙6/66(熔点：约200℃、酰胺键的比率：38％)。
聚酰胺系树脂(B)的聚合度可以将依据JIS K6810测定的相对粘度作为指标，通常优选为1.5～6、更优选为2.0～6、进一步优选为2.5～5。相对粘度过小的情况下，可看到成形时挤出机成为高扭矩状态、挤出加工变困难的倾向，过大的情况下，可看到得到的薄膜、片的厚度精度降低的倾向。需要说明的是，上述相对粘度可以依据JIS K6810，将聚酰胺系树脂(B)1g完全溶解于96％浓硫酸100mL中，在25℃下使用毛细管粘度计进行测定。
聚酰胺系树脂(B)的末端羧基含量通常为10～40μeq/g，优选为15～30μeq/g、特别优选为15～25μeq/g。末端羧基含量在上述范围外的情况下，有热稳定性差的倾向。需要说明的是，上述末端羧基含量可以如下地进行测定。
<末端羧基含量>
将聚酰胺系树脂(B)0.2g加入到邻甲酚15mL中，加热至110℃使其溶解。冷却至室温(23℃)附近后，加入苯甲醇10mL、邻甲酚50mL和甲醛50μL。将0.05mol/L的醇性氢氧化钾作为滴定液，用电位差滴定装置测定末端羧基含量([COOH]，单位：μeq/g)。
本发明的EVOH树脂组合物中，EVOH树脂(A)相对于聚酰胺系树脂(B)的重量含有比率((A)/(B))通常为99/1～10/90，优选为95/5～40/60、特别优选为90/10～60/40。若所述聚酰胺系树脂(B)的重量含有比率过小，则有聚酰胺系树脂的配混效果(例如耐热水杀菌处理性能)降低的倾向，相反若过大则有阻气性降低的倾向。
[铁化合物(C)]
本发明的EVOH树脂组合物的特征在于，除了上述EVOH树脂(A)、上述聚酰胺系树脂(B)以外，还含有铁化合物(C)，并且该铁化合物(C)的配混量为特定微量。本发明的EVOH树脂组合物具有如上所述的构成，因此能够抑制着色，另外，动态粘度行为也优异。
对于含有EVOH树脂(A)和聚酰胺系树脂(B)的EVOH树脂组合物产生的着色，认为是因为，由于热，EVOH树脂(A)所具有的羟基、聚合末端的羧基、及聚酰胺系树脂(B)所具有的酰胺键、氨基、羧基等反应性高的部位发生缩合、分解等反应。
另外，认为含有铁化合物(C)的EVOH树脂组合物会因铁离子而使制品着色，因此本领域技术人员通常会避免使用其。但是，本发明出乎意料地发现，通过使EVOH树脂组合物含有微量的铁化合物(C)，可得到加热后的着色得以抑制的EVOH树脂组合物。
作为得到如上所述的效果的理由，推测为，铁作为3价离子是稳定的，因此即使为微量，也会与如上所述的羟基、羧基、酰胺键、氨基等多个官能团形成离子键、螯合物而稳定化，由此能抑制上述缩合、分解，抑制着色。
上述铁化合物(C)在EVOH树脂组合物中除了以例如氧化物、氢氧化物、氯化物、铁盐的形成存在的情况以外，还可以以经离子化的状态、或与树脂、其他配体相互作用而成的络合物的状态存在。作为上述氧化物，例如，可列举出氧化铁、四氧化三铁、氧化亚铁(ferrous oxide)等。作为上述氯化物，例如，可列举出氯化亚铁、氯化铁等。作为上述氢氧化物，例如，可列举出氢氧化亚铁、氢氧化铁等。作为上述铁盐，例如，可列举出磷酸铁、硫酸铁等无机盐、羧酸(乙酸、丁酸、硬脂酸等)铁等有机盐。这些可以单独使用或组合使用2种以上。
从在EVOH树脂组合物中的分散性的方面出发，铁化合物(C)优选为水溶性。另外，从分散性和生产率的观点出发，其分子量通常为100～10000，优选为100～1000、特别优选为100～500。
本发明的EVOH树脂组合物中，铁化合物(C)的含量相对于EVOH树脂组合物的单位重量以金属换算为0.01～20ppm。所述铁化合物的含量优选为0.03～8ppm、特别优选为0.05～3ppm，特别优选为0.05～0.8ppm。若铁化合物(C)的含量过少，则着色抑制效果变得不充分，相反若过多，则经时的粘度增加倾向变显著。
此处，对于铁化合物(C)的含量，可以将EVOH树脂组合物0.5g在红外线加热炉中进行灰化处理(氧气气流中、650℃、1小时)后，将残留的灰分进行酸溶解，用纯水进行定容，将所得溶液作为试样溶液，用ICP-MS(Agilent Technologies公司制、7500ce型；标准添加法)进行测定，由此求出。
[其他热塑性树脂]
本发明的EVOH树脂组合物中可以在不阻碍本发明效果的范围(例如，EVOH树脂组合物的通常30重量％以下、优选20重量％以下、特别优选10重量％以下)内含有除EVOH树脂(A)及聚酰胺系树脂(B)以外的热塑性树脂。
作为其他热塑性树脂，可以使用公知的热塑性树脂。例如，具体而言，可列举出聚烯烃系树脂、聚酯系树脂、聚苯乙烯系树脂、聚氯乙烯系树脂、聚碳酸酯系树脂、聚丙烯酸系树脂、离子交联聚合物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物、乙烯-甲基丙烯酸共聚物、乙烯-甲基丙烯酸酯共聚物、聚偏氯乙烯、乙烯基酯系树脂、聚酯弹性体、聚氨酯弹性体、氯化聚乙烯、氯化聚丙烯等。这些可以单独使用或组合使用2种以上。
〔其他配混剂〕
另外，本发明的EVOH树脂组合物中可以在不阻碍本发明效果的范围内含有通常配混在EVOH树脂中的配混剂。例如，可以配混无机复盐(例如，水滑石等)、增塑剂(例如，乙二醇、甘油、己二醇等脂肪族多元醇等)、氧吸收剂[例如，铝粉、亚硫酸钾、光催化剂钛氧化物等无机系氧吸收剂；抗坏血酸、进而其脂肪酸酯、金属盐等、氢醌、没食子酸、含羟基的酚醛树脂等多元酚类、双水杨醛亚胺钴、四亚乙基五胺钴、钴-希夫碱络合物、卟啉类、大环状聚胺络合物、聚乙烯亚胺-钴络合物等含氮化合物与铁以外的过渡金属的配位结合体、萜烯化合物、氨基酸类与含羟基的还原性物质的反应产物、三苯基甲基化合物等有机化合物系氧吸收剂；含氮树脂与铁以外的过渡金属的配位结合体(例如，间苯二甲胺(MXD)尼龙与钴的组合)、含叔氢的树脂与铁以外的过渡金属的共混物(例如，聚丙烯与钴的组合)、含碳-碳不饱和键的树脂与铁以外的过渡金属的共混物(例如，聚丁二烯与钴的组合)、光氧化降解性树脂(例如，聚酮)、蒽醌聚合物(例如，聚乙烯基蒽醌)等、进而在这些配混物中添加有光引发剂(二苯甲酮等)、过氧化物捕捉剂(市售的抗氧化剂等)、除臭剂(活性炭等)而成者等高分子系氧吸收剂]、热稳定剂、光稳定剂、紫外线吸收剂、着色剂、抗静电剂、表面活性剂(其中，作为润滑剂使用者除外)、抗菌剂、抗粘连剂、填充材料(例如，无机填料等)等。其中，从抑制着色的观点出发，优选氧吸收剂，特别优选使用萜烯化合物。这些化合物可以单独使用或组合使用2种以上。
[EVOH树脂组合物的制造方法]
作为使用上述各成分制造本发明的EVOH树脂组合物的方法，例如，可列举出干混法、熔融混合法、溶液混合法、浸渗法等公知的方法，也可以将它们任意组合。
作为上述干混法，例如可列举出(i)用滚筒等将含有EVOH树脂(A)及聚酰胺系树脂(B)的粒料和铁化合物(C)干混的方法等。
作为上述熔融混合法，例如可列举出：(ii)将含有EVOH树脂(A)及聚酰胺系树脂(B)的粒料与铁化合物(C)的干混物熔融混炼，得到粒料、成形物的方法；(iii)在熔融状态的EVOH树脂(A)及聚酰胺系树脂(B)的混合物中添加铁化合物(C)进行熔融混炼，得到粒料、成形物的方法等。
作为上述溶液混合法，例如可列举出：(iv)使用市售的含有EVOH树脂(A)及聚酰胺系树脂(B)的粒料制备溶液，向其中配混铁化合物(C)，进行凝固成形而粒料化，进行固液分离并进行干燥的方法；(v)在EVOH树脂(A)的制造过程中，使EVOH树脂的均匀溶液(水/醇溶液等)含有聚酰胺系树脂(B)的溶液和铁化合物(C)后，进行凝固成形而粒料化，进行固液分离并进行干燥的方法等。
作为上述浸渗法，例如，可列举出：(vi)使含有EVOH树脂(A)及聚酰胺系树脂(B)的粒料与含有铁化合物(C)的水溶液接触，使上述粒料中含有铁化合物(C)后进行干燥的方法等。
本发明中，可以组合上述不同的方法。其中，从得到生产率、本发明的效果更显著的树脂组合物的方面出发，优选熔融混合法，特别优选(ii)的方法。
需要说明的是，通过上述各方法得到的EVOH树脂组合物粒料、各方法中所用的含有EVOH树脂(A)及聚酰胺系树脂(B)的粒料的形状是任意的。例如有球形、椭圆形、圆柱形、立方体形、长方体形等，通常为椭圆形、或圆柱形，对于其大小，从以后用作成形材料时的便利性的观点出发，椭圆形的情况下，短径通常为1～10mm、优选为2～6mm、进一步优选为2.5～5.5mm，长径通常为1.5～30mm、优选为3～20mm、进一步优选为3.5～10mm。另外，圆柱形的情况下，底面的直径通常为1～6mm、优选为2～5mm，长度通常为1～6mm、优选为2～5mm。
另外，作为上述各方法中所用的铁化合物(C)，如前所述，优选使用水溶性的铁化合物，例如，可列举出氧化铁、四氧化三铁、氧化亚铁等氧化物、氯化亚铁、氯化铁等氯化物、氢氧化亚铁、氢氧化铁等氢氧化物、磷酸铁、硫酸铁等无机盐、羧酸(乙酸、丁酸、硬脂酸等)铁等有机盐等铁盐。需要说明的是，所述铁化合物(C)如前所述除了在EVOH树脂组合物中以上述盐的形式存在的情况以外，还可以以经离子化的状态、或与树脂、其他配体相互作用而成的络合物的状态存在。
另外，作为上述(vi)的方法中所用的含有铁化合物(C)的水溶液，可以使用通过将上述铁化合物的水溶液、钢铁材料浸渍在包含各种化学试剂的水中而使铁离子溶出的水溶液。需要说明的是，该情况下，EVOH树脂组合物中的铁化合物(C)的含量(金属换算)可以通过浸渍粒料的水溶液中的铁化合物(C)的浓度、浸渍温度、浸渍时间等来控制。作为上述浸渍温度、浸渍时间，通常为0.5～48小时，优选为1～36小时，浸渍温度通常为10～40℃，优选为20～35℃。浸渍后的粒料通过公知的方法进行固液分离并通过公知的干燥方法进行干燥。作为所述干燥方法，可以采用各种干燥方法，可以为静置干燥、流动干燥中的任意者。另外，也可以将它们组合来进行。
本发明的EVOH树脂组合物粒料的含水率通常为0.01～0.5重量％，优选为0.05～0.35重量％，特别优选为0.1～0.3重量％。
需要说明的是，本发明中的EVOH树脂组合物粒料的含水率可以通过以下的方法来测定·算出。
用电子天平称量EVOH树脂组合物粒料的干燥前重量(W1)，在150℃的热风干燥机中进行5小时干燥，称量在干燥器中放冷30分钟后的重量(W2)，通过下述式算出。
含水率(重量％)＝[(W1-W2)/W1]×100
如此得到的EVOH树脂组合物的粒料可以直接供于熔融成形，从使熔融成形时的供料性稳定的方面出发，还优选使公知的润滑剂附着于粒料的表面。作为润滑剂的种类，例如，可列举出碳数12以上的高级脂肪酸(例如，月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山嵛酸、油酸等)、高级脂肪酸酯(例如，高级脂肪酸的甲酯、异丙酯、丁酯、辛酯等)、高级脂肪酸酰胺(例如，月桂酸酰胺、肉豆蔻酸酰胺、棕榈酸酰胺、硬脂酸酰胺、山嵛酸酰胺等饱和高级脂肪酸酰胺；油酸酰胺、芥酸酰胺等不饱和高级脂肪酸酰胺、乙烯基双硬脂酸酰胺、乙烯基双油酸酰胺、乙烯基双芥酸酰胺、乙烯基双月桂酸酰胺等双高级脂肪酸酰胺等)、低分子量聚烯烃(例如，分子量500～10,000左右的低分子量聚乙烯、或低分子量聚丙烯等、或其酸改性品)、碳数6以上的高级醇、酯低聚物、氟乙烯树脂等。这些化合物可以单独使用或组合使用2种以上。另外，所述润滑剂的含量为EVOH树脂组合物的通常5重量％以下，优选为1重量％以下。
本发明的EVOH树脂组合物被制备成粒料、或粉末状、液体状等各种形态的EVOH树脂组合物，作为各种成形物的成形材料而提供。特别是本发明中作为熔融成形用的材料而提供的情况下，有更有效地得到本发明的效果的倾向，是优选的。需要说明的是，本发明的EVOH树脂组合物还包括将本发明的EVOH树脂组合物中使用的EVOH树脂(A)及聚酰胺系树脂(B)以外的树脂混合而得到的树脂组合物。
而且，作为所述成形物，以使用本发明的EVOH树脂组合物成形的单层薄膜为首，可以以具有使用本发明的EVOH树脂组合物成形而成的层的多层结构体的形式供于实用。
[多层结构体]
本发明的多层结构体具备由上述本发明的EVOH树脂组合物形成的层。由本发明的EVOH树脂组合物形成的层(以下，称为“EVOH树脂组合物层”。)可以通过与以本发明的EVOH树脂组合物以外的热塑性树脂为主成分的其他基材(以下，称为“基材树脂”。)层叠，进而赋予强度、或保护EVOH树脂组合物层免受水分等的影响，赋予其他功能。
作为上述基材树脂，例如，可列举出直链状低密度聚乙烯、低密度聚乙烯、超低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、乙烯-丙烯(嵌段及无规)共聚物、乙烯-α-烯烃(碳数4～20的α-烯烃)共聚物等聚乙烯系树脂、聚丙烯、丙烯-α-烯烃(碳数4～20的α-烯烃)共聚物等聚丙烯系树脂、聚丁烯、聚戊烯、聚环状烯烃系树脂(在主链及侧链中的至少一者中具有环状烯烃结构的聚合物)等(未改性)聚烯烃系树脂、包含将这些聚烯烃类用不饱和羧酸或其酯接枝改性而成的不饱和羧酸改性聚烯烃系树脂等改性烯烃系树脂在内的广义的聚烯烃系树脂、离子交联聚合物、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物、聚酯系树脂、聚酰胺系树脂(也包含共聚聚酰胺)、聚氯乙烯、聚偏氯乙烯、丙烯酸系树脂、聚苯乙烯系树脂、乙烯基酯系树脂、聚酯系弹性体、聚氨酯系弹性体、聚苯乙烯系弹性体、氯化聚乙烯、氯化聚丙烯等卤素化聚烯烃、芳香族或脂肪族聚酮类等。
这些之中，优选作为疏水性树脂的、聚酰胺系树脂、聚烯烃系树脂、聚酯系树脂、聚苯乙烯系树脂，更优选为聚乙烯系树脂、聚丙烯系树脂、聚环状烯烃系树脂及这些不饱和羧酸改性聚烯烃系树脂等聚烯烃系树脂。
对于多层结构体的层构成，将本发明的EVOH树脂组合物层设为a(a1、a2、…)、基材树脂层设为b(b1、b2、…)时，可以为a/b、b/a/b、a/b/a、a1/a2/b、a/b1/b2、b2/b1/a/b1/b2、b2/b1/a/b1/a/b1/b2等任意的组合。另外，使在制造该多层结构体的过程中产生的端部、次品等再熔融成形而得到的、包含本发明的EVOH树脂组合物与基材树脂的混合物的再循环层设为R时，也可以采用b/R/a、b/R/a/b、b/R/a/R/b、b/a/R/a/b、b/R/a/R/a/R/b等。多层结构体的层的数量以总数计通常为2～15、优选为3～10。上述的层构成中，可以根据需要在各个层间插入含粘接性树脂的粘接性树脂层。
作为上述粘接性树脂，可以使用公知的树脂，可根据基材树脂层“b”中使用的热塑性树脂的种类适宜选择即可。代表性地可列举出通过加成反应、接枝反应等使不饱和羧酸或其酐化学键合于聚烯烃系树脂而得到的含羧基的改性聚烯烃系聚合物。作为上述含羧基的改性聚烯烃系聚合物，例如，可列举出马来酸酐接枝改性聚乙烯、马来酸酐接枝改性聚丙烯、马来酸酐接枝改性乙烯-丙烯(嵌段及无规)共聚物、马来酸酐接枝改性乙烯-丙烯酸乙酯共聚物、马来酸酐接枝改性乙烯-乙酸乙烯酯共聚物、马来酸酐改性聚环状烯烃系树脂、马来酸酐接枝改性聚烯烃系树脂等。而且，可以使用选自这些中的1种或2种以上的混合物。
多层结构体中，在本发明的EVOH树脂组合物层与基材树脂层之间使用粘接性树脂层的情况下，粘接性树脂层位于EVOH树脂组合物层的两侧，因此优选使用疏水性优异的粘接性树脂。
上述基材树脂、粘接性树脂可以在不阻碍本发明的主旨的范围(例如，相对于树脂整体为30重量％以下、优选为10重量％以下)内包含以往已知的增塑剂、填料、粘土(蒙脱石等)、着色剂、抗氧化剂、抗静电剂、润滑剂、成核剂、抗粘连剂、蜡等。这些可以单独使用或组合使用2种以上。
本发明的EVOH树脂组合物与上述基材树脂的层叠(包括插入粘接性树脂层的情况)可以通过公知的方法进行。例如可列举出：在本发明的EVOH树脂组合物的薄膜、片等上将基材树脂熔融挤出层压的方法；在基材树脂层上将本发明的EVOH树脂组合物熔融挤出层压的方法；将EVOH树脂组合物和基材树脂共挤出的方法；将EVOH树脂组合物层和基材树脂层使用有机钛化合物、异氰酸酯化合物、聚酯系化合物、聚氨酯化合物等公知的粘接剂进行干式层压的方法；在基材树脂上涂布EVOH树脂组合物的溶液后去除溶剂的方法等。这些中，从成本、环境的观点考虑，优选共挤出的方法。
如上所述，多层结构体接着根据需要实施(加热)拉伸处理。拉伸处理可以为单轴拉伸、双轴拉伸中的任意者，双轴拉伸的情况下，可以为同时拉伸也可以为逐次拉伸。另外，作为拉伸方法，辊拉伸法、拉幅机拉伸法、管拉伸法、拉伸吹塑法、真空压空成形等中拉伸倍率高者也可以采用。对于拉伸温度，以多层结构体的熔点附近的温度计，选自通常40～170℃、优选60～160℃左右的范围。拉伸温度过低的情况下，有拉伸性变不良的倾向，过高的情况下，有难以维持稳定的拉伸状态的倾向。
需要说明的是，拉伸后出于赋予尺寸稳定性的目的，可以接着进行热固定。热固定可以通过周知的方法来实施，例如可以边将上述拉伸薄膜保持为紧张状态边在通常80～180℃、优选100～165℃下进行通常2～600秒钟左右的热处理。另外，将由本发明的EVOH树脂组合物得到的多层拉伸薄膜用作收缩用薄膜的情况下，为了赋予热收缩性，不进行上述热固定，而进行例如对拉伸后的薄膜吹冷风而进行冷却固定等的处理即可。
另外，根据情况，也可以使用本发明的多层结构体而得到杯、托盘状的多层容器。该情况下，通常采用深拉成形法，具体而言，可列举出真空成形法、压空成形法、真空压空成形法、柱塞辅助式真空压空成形法(plug-assisted vacuum pressure forming)等。进而由多层型坯(吹塑前的中空管状的预备成形物)得到管、瓶状的多层容器(层叠体结构)的情况下，采用吹塑成形法。具体而言，可列举出挤出吹塑成形法(双头式、模具移动式、型坯移位式、旋转式、蓄能器式、水平型坯式等)、冷型坯式吹塑成形法、注射吹塑成形法、双轴拉伸吹塑成形法(挤出式冷型坯双轴拉伸吹塑成形法、注射式冷型坯双轴拉伸吹塑成形法、注射成形直列式双轴拉伸吹塑成形法(injection inline type biaxial stretching blowmolding method)等)等。得到的层叠体根据需要可以进行热处理、冷却处理、轧制处理、印刷处理、干式层压处理、溶液或熔融涂布处理、制袋加工、深拉加工、箱加工、管加工、狭缝加工等。
多层结构体(包含进行了拉伸者)的厚度、进而构成多层结构体的EVOH树脂组合物层、基材树脂层及粘接性树脂层的厚度根据层构成、基材树脂的种类、粘接性树脂的种类、用途、包装方式、要求的物性等而异，不能一概而论，多层结构体(包含进行了拉伸者)的厚度通常为10～5000μm、优选为30～3000μm、特别优选为50～2000μm。EVOH树脂组合物层通常为1～500μm，优选为3～300μm、特别优选为5～200μm，基材树脂层通常为5～3000μm，优选为10～2000μm，特别优选为20～1000μm，粘接性树脂层通常为0.5～250μm，优选为1～150μm，特别优选为3～100μm。
进而，对于多层结构体中的EVOH树脂组合物层相对于基材树脂层的厚度的比(EVOH树脂组合物层/基材树脂层)，各层为多个的情况下，厚度最后的层彼此的比通常为1/99～50/50，优选为5/95～45/55，特别优选为10/90～40/60。另外，对于多层结构体中的EVOH树脂组合物层相对于粘接性树脂层的厚度比(EVOH树脂组合物层/粘接性树脂层)，各层为多个的情况下，厚度最厚的层彼此的比通常为10/90～99/1，优选为20/80～95/5，特别优选为50/50～90/10。
包含由如上所述得到的薄膜、片、拉伸薄膜形成的袋及杯、托盘、管、瓶等的容器、盖材料作为通常的食品、以及蛋黄酱、色拉调料等调味料、味噌等发酵食品、色拉油等油脂食品、饮料、化妆品、医药品等各种的包装材料容器有用。特别是由本发明的EVOH树脂组合物形成的层抑制了着色，因此作为食品、药品、农药等热水杀菌处理用包装材料特别有用。
实施例
以下，举出实施例具体地对本发明进行说明，本发明在不超过其主旨的范围内不限定于实施例的记载。
需要说明的是，例中的“份”在没有特别说明下是指重量基准。
在实施例之前，准备以下的EVOH树脂(A)及聚酰胺系树脂(B)的粒料，进行该EVOH树脂(A)及聚酰胺系树脂(B)中所含的铁化合物(C)的含量的测定。
·EVOH树脂(A)：乙烯结构单元的含量29摩尔％、皂化度99.6摩尔％、MFR3.9g/10分钟(210℃、载荷2160g)的乙烯-乙烯醇共聚物
·聚酰胺系树脂(B)：熔点220℃、末端羧基含量20μeq/聚合物1g(相对于聚合物1g的摩尔当量)的尼龙6(Mitsubishi Engineering-Plastics Corporation制“Novamid1028EN”)
[铁化合物(C)的含量的测定]
将上述EVOH树脂(A)的粒料冷冻粉碎作为测定用试样。将该测定用试样0.5g在红外线加热炉中进行灰化处理(氧气气流中650℃、1小时)后，将灰分进行酸溶解，用纯水进行定容，将所得溶液作为试样溶液。用下述的ICP-MS(Agilent Technologies公司制ICP质谱装置7500ce型)以标准添加法对该溶液进行测定。其结果，铁化合物(C)的含量以金属换算为0ppm。
另外，上述聚酰胺系树脂(B)也与上述EVOH树脂(A)同样地测定。其结果，铁化合物(C)的含量以金属换算为0.15ppm。
<实施例1>
将上述EVOH树脂(A)的粒料80份、上述聚酰胺系树脂(B)的粒料20份、及作为铁化合物(C)的磷酸铁(III)n水合物(和光纯药工业株式会社制、230℃干燥减重为20.9重量％)0.000034份(相对于EVOH树脂组合物的单位重量以金属换算为0.1ppm)以塑性计(Brabender Corporation制)在250℃下进行5分钟预热后进行5分钟熔融混炼，得到实施例1的EVOH树脂组合物。将得到的EVOH树脂组合物用粉碎机(Sometani Sangyo Co.,Ltd.制、SKR16-240)以650rpm粉碎，得到粉碎物。所述粉碎物为1～5mm见方的小片。
<实施例2>
将实施例1中磷酸铁(III)n水合物的配混量变更为0.00034份(相对于EVOH树脂组合物的单位重量以金属换算为1ppm)，除此以外，与实施例1同样地操作，得到实施例2的EVOH树脂组合物及其粉碎物。
<实施例3>
将实施例1中磷酸铁(III)n水合物的配混量变更为0.0034份(相对于EVOH树脂组合物的单位重量以金属换算为10ppm)，除此以外，与实施例1同样地操作，得到实施例3的EVOH树脂组合物及其粉碎物。
<比较例1>
不配混实施例1中的磷酸铁(III)n水合物，除此以外，与实施例1同样地操作，得到比较例1的EVOH树脂组合物及其粉碎物。
通过下述所示的方法进行实施例1～3及比较例1的着色评价及动态粘度行为的测定。将结果示于后述表1。
[着色评价]
将上述的EVOH树脂组合物的粉碎物作为样品，用日本电色工业株式会社制分光色差计SE6000测定加热前的YI值。此时，在将样品在填充至内径32mm、高度30mm的圆筒中并刮平的状态下供于测定。另外，将所述样品在空气气氛下的烘箱内以150℃进行5小时加热处理后，同样地测定加热后的YI值。算出加热后的YI值相对于所述加热前的YI值的比。所述值越大，意味着EVOH树脂组合物在加热后着色为黄色。
[动态粘度行为]
将上述的EVOH树脂组合物的粉碎物以塑性计(Brabender Corporation制)在250℃、50rpm的条件下进行5分钟预热后进行30分钟混炼。用混炼结束时(第30分钟)时刻的扭矩除以混炼开始时(第0分钟)的扭矩所得的数值进行评价。所述值越低，经时的粘度上升越得以抑制，意味着动态粘度行为优异。
[表1]
如上述表1所示，含有铁化合物(C)的实施例1～3中得到的EVOH树脂组合物与不具有铁化合物(C)的比较例1相比，YI值低，抑制了着色。另外，对于将所述EVOH树脂组合物加热后的着色性，与比较例1相比，实施例1～3的YI值也低，抑制了着色。
进而可知，含有铁化合物(C)的实施例1～3中得到的EVOH树脂组合物与不具有铁化合物(C)的比较例1相比，粘度增加得以抑制，动态粘度行为优异。特别是，实施例1的加热时的YI值增加率最少，动态粘度行为显示出最良好的值，可知得到了优异的EVOH树脂组合物。
上述实施例中，示出了本发明中的具体的方式，但上述实施例仅仅是例示，并不作限定性的解释。对于本领域技术人员显而易见的各种变形被认为在本发明的范围内。
产业上的可利用性
本发明的EVOH树脂组合物抑制了由热劣化导致的着色，因此除了各种食品以外，作为蛋黄酱、色拉调料等调味料、味噌等发酵食品、色拉油等油脂食品、饮料、化妆品、医药品等的各种包装材料、特别是热水杀菌处理用包装材料也特别有用。
Claims (4)
1.一种乙烯-乙烯醇系共聚物组合物，其特征在于，含有乙烯-乙烯醇系共聚物(A)、聚酰胺系树脂(B)及铁化合物(C)，所述铁化合物(C)的含量相对于乙烯-乙烯醇系共聚物组合物的单位重量以金属换算为0.01～20ppm。
2.根据权利要求1所述的乙烯-乙烯醇系共聚物组合物，其特征在于，所述乙烯-乙烯醇系共聚物(A)相对于所述聚酰胺系树脂(B)的重量含有比率为(A)/(B)＝99/1～10/90。
3.一种粒料，其特征在于，由权利要求1或2所述的乙烯-乙烯醇系共聚物组合物形成。
4.一种多层结构体，其特征在于，具备由权利要求1或2所述的乙烯-乙烯醇系共聚物组合物形成的层。
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| CN115298263A (zh) * | 2020-03-26 | 2022-11-04 | 三菱化学株式会社 | 树脂组合物、成形物、聚酰胺系树脂用改性剂和聚酰胺系树脂的改性方法 |
| US11124642B1 (en) | 2021-03-18 | 2021-09-21 | Chang Chun Petrochemical Co., Ltd. | Ethylene-vinyl alcohol copolymer composition with improved oxygen barrier properties |
| US11746170B2 (en) | 2021-06-16 | 2023-09-05 | Chang Chun Petrochemical Co., Ltd. | Ethylene-vinyl alcohol copolymer resin composition, ethylene-vinyl alcohol copolymer film formed therefrom, and multilayer structure containing the same |
| TWI761235B (zh) * | 2021-06-16 | 2022-04-11 | 長春石油化學股份有限公司 | 乙烯-乙烯醇共聚物樹脂組合物、由其形成之乙烯-乙烯醇共聚物膜及包含其之多層結構 |
| JP7303276B2 (ja) | 2021-06-16 | 2023-07-04 | 長春石油化學股▲分▼有限公司 | エチレン－ビニルアルコール共重合体樹脂組成物 |
| TWI765750B (zh) * | 2021-06-16 | 2022-05-21 | 長春石油化學股份有限公司 | 乙烯-乙烯醇共聚物樹脂組合物、由其形成之乙烯-乙烯醇共聚物膜及包含其之多層結構 |
| CN113881221A (zh) * | 2021-11-12 | 2022-01-04 | 惠州市晋裕塑料科技有限公司 | 一种高阻隔尼龙共混材料 |
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