CN110603292A - 树脂组合物、其制造方法和使用了其的成形体 - Google Patents
树脂组合物、其制造方法和使用了其的成形体 Download PDFInfo
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- CN110603292A CN110603292A CN201880031982.7A CN201880031982A CN110603292A CN 110603292 A CN110603292 A CN 110603292A CN 201880031982 A CN201880031982 A CN 201880031982A CN 110603292 A CN110603292 A CN 110603292A
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- resin composition
- ethylene
- nonionic surfactant
- vinyl alcohol
- alcohol copolymer
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Abstract
树脂组合物，其为含有乙烯‑乙烯醇共聚物和非离子表面活性剂的树脂组合物，上述乙烯‑乙烯醇共聚物的乙烯单元含量为15~60摩尔%、皂化度为90摩尔%以上，所述树脂组合物中含有上述乙烯‑乙烯醇共聚物作为主成分，且含有3~400ppm的上述非离子表面活性剂。此外，通过将包含非离子表面活性剂、水和上述乙烯‑乙烯醇共聚物的混合物进行熔融混炼而制造上述树脂组合物。通过使用这样得到的树脂组合物，从而使熔融成形时的喷出量增加，且能够获得外观优异的成形体。
Description
技术领域
本发明涉及包含乙烯-乙烯醇共聚物的树脂组合物、其制造方法和使用了其的成形体。
背景技术
乙烯-乙烯醇共聚物（以下有时简写为“EVOH”）是氧气等气体的阻隔性、透明性、留香性、耐油性、不带电性、机械强度等优异的高分子材料。因此，EVOH作为容器等成形品的材料而被用于广泛的用途。使用了EVOH的成形体通常利用熔融成形法来制造。因此，对于EVOH而言，要求提高熔融成形时的生产率、在熔融成形后具有优异的外观（不发生黄变等着色）等。
专利文献1提出了含有EVOH、水滑石和高级脂肪酸的金属盐的树脂组合物。据称：根据该树脂组合物，不仅熔融成形时的喷出量增加、生产效率提高，且能够获得成块、鱼眼也少的品质良好的膜等成形品。然而，将上述树脂组合物熔融成形而得到的成形品有时产生着色而出现问题。
专利文献2和专利文献3提出了使EVOH含有羧酸、磷酸等酸、碱金属盐、碱土金属盐等金属盐而成的各种树脂组合物。并且，专利文献2和专利文献3记载了这些树脂组合物的外观、熔融成形时的稳定性优异。然而，这些树脂组合物在熔融成形时的生产率有时不充分。
专利文献4记载了包含含有0.3重量%以上表面活性剂的EVOH膜的蔬菜水果用包装袋。专利文献4记载了通过将EVOH与表面活性剂组合使用而能够消除蔬菜水果包装体内的结露，但不使蔬菜水果蔫萎。然而，在制造专利文献4中记载的蔬菜水果用包装袋时，熔融成形时的生产率不充分，且进行熔融成形而得到的成形品的外观也不良。
现有技术文献
专利文献
专利文献1：日本特开平01-308440号公报
专利文献2：日本特开2001-146539号公报
专利文献3：国际公开第2011/118648号
专利文献4：日本特开2013-193759号公报。
发明内容
发明要解决的问题
本发明是为了解决上述课题而进行的，其目的在于，提供熔融成形时的喷出量多且能够获得外观优异的成形体的树脂组合物及其制造方法。此外，其目的在于，提供使用这种树脂组合物而得到的成形体和多层结构体。
用于解决问题的方法
上述课题通过提供下述树脂组合物来解决，所述树脂组合物为含有乙烯-乙烯醇共聚物和非离子表面活性剂的树脂组合物，上述乙烯-乙烯醇共聚物的乙烯单元含量为15~60摩尔%，皂化度为90摩尔%以上，所述树脂组合物中含有上述乙烯-乙烯醇共聚物作为主成分，且含有3~400ppm的上述非离子表面活性剂。
上述非离子表面活性剂优选为选自醚型、氨基醚型、酯型、酯・醚型和酰胺型中的至少一种。上述非离子表面活性剂更优选为选自聚氧亚烷基烷基醚、聚氧亚烷基烯基醚、聚氧乙烯苯乙烯化苯基醚、聚氧亚烷基烷基胺、聚氧亚烷基烯基胺、聚氧亚烷基烷基酯、聚氧亚烷基烯基酯、脱水山梨糖醇烷基酯、脱水山梨糖醇烯基酯、聚氧乙烯脱水山梨糖醇烷基酯、聚氧乙烯脱水山梨糖醇烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯和高级脂肪酸酰胺中的至少一种。
上述树脂组合物优选还含有以金属元素换算为10~500ppm的碱金属盐。
上述树脂组合物优选还含有0.005~1质量%的选自抗氧化剂、紫外线吸收剂、增塑剂、抗静电剂、润滑剂和填充剂中的至少1种添加剂。
上述树脂组合物优选的是：作为上述EVOH，含有2种乙烯单元含量不同的EVOH。
含有上述树脂组合物的成形体是本发明的优选实施方式。具有包含上述树脂组合物的层和包含除上述EVOH之外的热塑性树脂的层的多层结构体也是本发明的优选实施方式。
上述课题也可通过提供将包含上述非离子表面活性剂、水和上述EVOH的混合物进行熔融混炼的上述树脂组合物制造方法来解决。此时，上述混合物中的水的含量相对于上述EVOH100质量份优选为0.1~50质量份。优选将包含上述非离子表面活性剂的水溶液或水分散体添加至上述EVOH而得到上述混合物。
发明的效果
本发明的树脂组合物的外观优异。需要说明的是，通过使用该树脂组合物，熔融成形时的喷出量增加。尤其是，即使在低温下也能够确保一定的喷出量。通过使用这种树脂组合物，能够以良好的生产率制造外观优异的成形体、多层结构体。此外，根据本发明的制造方法，能够简便地制造上述树脂组合物。
具体实施方式
以下，针对本发明的树脂组合物、成形体和多层结构体进行详述。
[树脂组合物]
本发明的树脂组合物含有乙烯-乙烯醇共聚物和非离子表面活性剂，上述乙烯-乙烯醇共聚物的乙烯单元含量为15~60摩尔%，皂化度为90摩尔%以上，所述树脂组合物中含有上述乙烯-乙烯醇共聚物作为主成分，且含有3~400ppm的上述非离子表面活性剂。
（EVOH）
本发明的树脂组合物所含有的EVOH是含有乙烯单元和乙烯醇单元的共聚物。上述EVOH可按照公知的方法来制造。例如，在使乙烯与乙烯基酯共聚而得到乙烯-乙烯基酯共聚物后，通过使用碱催化剂等将该共聚物进行皂化而得到上述EVOH。作为上述乙烯基酯，可列举出乙酸乙烯酯、丙酸乙烯酯、特戊酸乙烯酯等脂肪酸乙烯酯，优选为乙酸乙烯酯。只要在不损害本发明效果的范围内，则上述EVOH可以含有除乙烯和乙烯醇之外的共聚成分。作为这样的其它共聚成分，可列举出例如源自乙烯基硅烷化合物的单元。此处，作为源自乙烯基硅烷化合物的单元，可列举出例如源自乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三（β-甲氧基-乙氧基）硅烷或γ-甲基丙烯酰氧基丙基甲氧基硅烷的单元。这些之中，优选为源自乙烯基三甲氧基硅烷或乙烯基三乙氧基硅烷的单元。进而，上述EVOH中可以含有源自丙烯、丁烯等α-烯烃；（甲基）丙烯酸、（甲基）丙烯酸甲酯等不饱和羧酸或其酯；以及N-乙烯基吡咯烷酮等乙烯基吡咯烷酮的单元来作为其它共聚成分。上述EVOH中的除乙烯单元和乙烯醇单元之外的共聚成分的含量优选为10摩尔%以下，更优选为5摩尔%以下，进一步优选为1摩尔%以下。
上述EVOH的乙烯单元含量必须为15~60摩尔%。由此，能够获得兼顾优异的熔融成形性和气体阻隔性的树脂组合物。在上述乙烯含有率小于15摩尔%的情况下，将树脂组合物进行熔融成形时的长期运转性降低，且所得成形体的耐水性、耐热水性和高湿度下的气体阻隔性也降低。上述乙烯含有率优选为20摩尔%以上，更优选超过20摩尔%，进一步优选为22摩尔%以上。另一方面，在上述乙烯含有率超过60摩尔%的情况下，所得成形体的气体阻隔性降低。上述乙烯含有率优选为50摩尔%以下。
上述EVOH的皂化度必须为90摩尔%以上。由此，能够获得具有优异气体阻隔性的树脂组合物。在上述皂化度小于90摩尔%的情况下，所得成形体的气体阻隔性降低，且外观恶化。上述皂化度优选为95摩尔%以上、更优选为99摩尔%以上。上述EVOH的乙烯单元含量和皂化度可通过在溶剂中使用DMSO-d6的1H-NMR测定来求出。
上述EVOH的熔体流动速率（温度为210℃、载荷为2160g，以下将熔体流动速率简写为MFR）优选为0.1~200g/10分钟。在上述EVOH的MFR为这种范围的情况下，上述树脂组合物的成形性、加工性、所得成形体的外观变得良好。上述EVOH的MFR更优选为0.5g/10分钟以上、进一步优选为1g/10分钟以上、特别优选为3g/10分钟以上。另一方面，上述EVOH的MFR更优选为50g/10分钟以下、进一步优选为30g/10分钟以下、特别优选为15g/10分钟以下、最优选为10g/10分钟以下。本发明中，熔体流动速率按照JIS K 7210进行测定。
上述EVOH可以包含2种以上EVOH的混合物。此时，乙烯含有率、皂化度和MFR的值设为由配合质量比算出的平均值。从生产成本、所得制品的均匀性的观点出发，本发明的树脂组合物优选含有1种EVOH。另一方面，从兼顾阻隔性和各种机械物性的观点出发，本发明的树脂组合物优选含有乙烯单元含量不同的2种EVOH。此时，2种EVOH的乙烯单元含量优选相差5摩尔%以上，更优选相差10摩尔%以上。此外，乙烯单元含量高的EVOH相对于乙烯单元含量低的EVOH的质量比优选为1/99~99/1、更优选为5/95~95/5。
本发明的树脂组合物中含有上述EVOH作为主成分。此处，主成分是指以质量基准计含量最多的成分。本发明的树脂组合物中的上述EVOH的含量优选为55质量%以上。在上述含量小于55质量%的情况下，上述树脂组合物的气体阻隔性、成形性有可能变得不充分。上述含量更优选为80质量%以上、进一步优选为90质量%以上、特别优选为95质量%以上、最优选为99质量%以上。
（非离子表面活性剂）
本发明的树脂组合物含有3~400ppm的非离子表面活性剂。通过使上述树脂组合物含有特定量的非离子表面活性剂，能够增加进行熔融成形时的树脂喷出量。尤其是，即使在上述树脂组合物含有除上述EVOH之外的其它成分的情况下，也不会受到这种成分的影响，能够增加树脂的喷出量，且即使在已熔融的树脂为低温的情况下，也能够确保一定的喷出量。进而，令人惊讶的是，通过使上述树脂组合物含有特定量的非离子表面活性剂，能够抑制熔融成形时的该树脂组合物的着色。详情尚不明确，但可推测如下。一般可知：在EVOH含有金属离子的情况下，因该金属离子与EVOH发生反应而促进EVOH的热劣化，导致EVOH产生黄变等着色。可推测：因非离子表面活性剂阻碍这种反应等而导致EVOH的热劣化受到抑制。
上述树脂组合物所含有的非离子表面活性剂没有特别限定，优选为选自醚型、氨基醚型、酯型、酯・醚型和酰胺型中的至少一种。这些非离子表面活性剂可以单独使用，也可以组合使用2种以上。
作为上述醚型的非离子表面活性剂，优选为聚氧亚烷基烷基醚、聚氧亚烷基烯基醚、聚氧乙烯苯乙烯化苯基醚。
作为聚氧亚烷基烷基醚和聚氧亚烷基烯基醚，优选用下述式（1）表示。
R-O-（AO）nH （1）
式中，R为碳原子数6~22的直链或支链的烷基或烯基；A各自独立地为碳原子数2~4的亚烷基；n表示聚氧亚烷基单元的缩合度，为1~30。
上述式（1）中，R的碳原子数优选为8~18。A的碳原子数优选为2或3。n优选为2~25、更优选为3~20。
作为聚氧亚烷基烷基醚，具体而言，可列举出聚氧乙烯己基醚、聚氧乙烯庚基醚、聚氧乙烯辛基醚、聚氧乙烯-2-乙基己基醚、聚氧乙烯壬基醚、聚氧乙烯癸基醚、聚氧乙烯月桂基醚、聚氧乙烯十四烷基醚、聚氧乙烯鲸蜡基醚、聚氧乙烯硬脂基醚、聚氧乙烯二十烷基醚等聚氧乙烯烷基醚；聚氧丙烯硬脂基醚等聚氧丙烯烷基醚；聚氧乙烯聚氧丙烯烷基醚等。
作为聚氧亚烷基烯基醚，具体而言，可列举出聚氧乙烯油烯基醚等聚氧乙烯烯基醚等。
作为聚氧乙烯苯乙烯化苯基醚，具体而言，可列举出聚氧乙烯单苯乙烯化苯基醚、聚氧乙烯二苯乙烯化苯基醚、聚氧乙烯三苯乙烯化苯基醚等。上述聚氧乙烯苯乙烯化苯基醚的环氧乙烷加成数优选为5~30摩尔。
作为上述氨基醚型的非离子表面活性剂，优选为聚氧亚烷基烷基胺、聚氧亚烷基烯基胺等。作为聚氧亚烷基烷基胺，优选为可可烷基胺-氧化乙烯加成物、聚氧乙烯硬脂基胺、聚氧乙烯月桂基胺、聚氧乙烯聚氧丙烯月桂基胺、聚氧乙烯硬脂基胺等。作为聚氧亚烷基烯基胺，优选为聚氧乙烯油烯基胺等。上述聚氧亚烷基烷基胺的环氧乙烷加成数优选为1~40摩尔。
作为上述酯型的非离子表面活性剂，优选为聚氧亚烷基烷基酯、聚氧亚烷基烯基酯、脱水山梨糖醇烷基酯、脱水山梨糖醇烯基酯、聚氧乙烯脱水山梨糖醇烷基酯、聚氧乙烯脱水山梨糖醇亚烷基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯等。
作为聚氧亚烷基烷基酯和聚氧亚烷基烯基酯，优选用下述式（2）表示。
R-COO（AO）nH （2）
式中，R、A和n的定义与上述式（1）相同。关于优选的范围，R的碳原子数为8~18、A的碳原子数为2或3、n为7~14。n为上述范围时，能够兼顾良好的喷出量和外观。
作为聚氧亚烷基烷基酯，具体而言，可列举出聚氧乙烯单月桂酸酯、聚氧乙烯二月桂酸酯、聚氧乙烯单棕榈酸酯、聚氧乙烯单硬脂酸酯、聚氧乙烯二硬脂酸酯等。
作为聚氧亚烷基烯基酯，具体而言，可列举出聚氧乙烯油酸酯、聚乙二醇二油酸酯等。
作为脱水山梨糖醇烷基酯，具体而言，优选为脱水山梨糖醇单己酸酯、脱水山梨糖醇单月桂酸酯、脱水山梨糖醇单棕榈酸酯、脱水山梨糖醇单硬脂酸酯、脱水山梨糖醇二硬脂酸酯、脱水山梨糖醇三硬脂酸酯、脱水山梨糖醇单月桂酸酯等。
作为脱水山梨糖醇烯基酯，具体而言，优选为脱水山梨糖醇单油酸酯、脱水山梨糖醇三油酸酯、脱水山梨糖醇倍半油酸酯等。
作为聚氧乙烯脱水山梨糖醇烷基酯，具体而言，可列举出聚氧乙烯脱水山梨糖醇单月桂酸酯、聚氧乙烯脱水山梨糖醇单棕榈酸酯、聚氧乙烯脱水山梨糖醇单硬脂酸酯、聚氧乙烯脱水山梨糖醇三硬脂酸酯、聚氧乙烯脱水山梨糖醇三异硬脂酸酯、聚氧乙烯脱水山梨糖醇单月桂酸酯等。
作为聚氧乙烯脱水山梨糖醇烯基酯，具体而言，可列举出聚氧乙烯脱水山梨糖醇单油酸酯、聚氧乙烯脱水山梨糖醇三油酸酯等。
作为甘油烷基酯，具体而言，可列举出甘油单硬脂酸酯、甘油单肉豆蔻酸酯等。
作为甘油烯基酯，具体而言，可列举出甘油单油酸酯等。
作为聚甘油烷基酯，具体而言，可列举出二甘油月桂酸酯、四甘油硬脂酸酯、聚甘油月桂酸酯、聚甘油硬脂酸酯等。
作为聚甘油烯基酯，具体而言，可列举出聚甘油油酸酯等。
作为上述酯・醚型的非离子表面活性剂，优选为聚氧乙烯脱水山梨糖醇烷基酯、聚氧乙烯脱水山梨糖醇烯基酯等。
作为上述酰胺型的非离子表面活性剂，优选为高级脂肪酸酰胺，更优选为高级脂肪酸烷醇酰胺。
作为高级脂肪酸烷醇酰胺，可列举出高级脂肪酸单或二烷醇酰胺，具体而言，可列举出己酸单或二乙醇酰胺、辛酸单或二乙醇酰胺、癸酸单或二乙醇酰胺、月桂酸单或二乙醇酰胺、棕榈酸单或二乙醇酰胺、硬脂酸单或二乙醇酰胺、油酸单或二乙醇酰胺、椰油脂肪酸单或二乙醇酰胺、将构成它们的乙醇酰胺替换成丙醇酰胺或丁醇酰胺而得的产物等。
作为除高级脂肪酸烷醇酰胺之外的高级脂肪酸酰胺，可列举出己酸酰胺、辛酸酰胺、癸酸酰胺、月桂酸酰胺、棕榈酸酰胺、硬脂酸酰胺、油酸酰胺等。
作为非离子表面活性剂，更优选为选自聚氧亚烷基烷基醚、聚氧亚烷基烯基醚、聚氧乙烯苯乙烯化苯基醚、聚氧亚烷基烷基胺、聚氧亚烷基烯基胺、聚氧亚烷基烷基酯、聚氧亚烷基烯基酯、脱水山梨糖醇烷基酯、脱水山梨糖醇烯基酯、聚氧乙烯脱水山梨糖醇烷基酯、聚氧乙烯脱水山梨糖醇烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯和高级脂肪酸酰胺中的至少一种。
从能够获得具有特别优异的外观的成形体的观点出发，作为非离子表面活性剂，优选为醚型或酯型，其中，从着色的观点出发，更优选为选自聚氧亚烷基烷基醚、聚氧亚烷基烯基醚、聚氧亚烷基烷基酯、聚氧亚烷基烯基酯、甘油烷基酯、聚甘油烷基酯和聚甘油烯基酯中的至少一种。它们可以单独使用，也可以组合多种。
本发明的树脂组合物中的非离子表面活性剂的含量为3~400ppm。在该含量小于3ppm的情况下，无法充分获得增加上述树脂组合物的喷出量的效果，也无法充分获得抑制着色的效果。上述含量优选为10ppm以上，更优选为50ppm以上。另一方面，在上述含量超过400ppm的情况下，存在如下倾向：在经济上不利，且因树脂打滑而导致树脂向挤出机的供给变得不充分，上述树脂组合物的喷出量也降低，并且在挤出机内的上述树脂组合物的滞留时间变长、树脂黄变。上述含量优选为300ppm以下，更优选为150ppm以下。
（碱金属盐）
上述树脂组合物优选还包含碱金属盐。通过这样地制成含有碱金属盐的树脂组合物，对于其它树脂的粘接性变得良好。尤其是，具有包含上述树脂组合物的层和包含除上述乙烯-乙烯醇共聚物之外的热塑性树脂的层的多层结构体中的层间粘接性提高。而且，令人惊讶的是：通过使用特定量的非离子表面活性剂，能够抑制由碱金属盐导致的EVOH的热劣化，且提高粘接性。
作为形成上述碱金属盐的碱金属，可列举出锂、钠、钾等，优选为钠和钾。作为上述碱金属盐，可列举出例如锂、钠、钾等脂肪族羧酸盐、芳香族羧酸盐、碳酸盐、盐酸盐、硝酸盐、硫酸盐、磷酸盐、金属络合物等。这些之中，从容易获取的观点等出发，更优选乙酸钠、乙酸钾、碳酸钠、碳酸钾、磷酸钠和磷酸钾。
本发明的树脂组合物优选含有以金属元素换算为10~500ppm的碱金属盐。碱金属盐的含量更优选为30ppm以上，进一步优选为100ppm以上。此外，上述含量更优选为400ppm以下，进一步优选为300ppm以下。通过使碱金属盐的含量为上述下限以上，在将上述树脂组合物用作构成多层结构体的层的材料时，能够提高层间的粘接性。另一方面，通过使金属盐的含量为上述上限以下，能够抑制上述树脂组合物的着色。
（其它成分）
只要在不损害本发明效果的范围内，则上述树脂组合物可以含有除上述EVOH和非离子表面活性剂之外的其它成分。上述树脂组合物中的其它成分的含量优选为0.005~45质量%。该含量更优选为20质量%以下，进一步优选为10质量%以下，特别优选为5质量%以下，最优选为1质量%以下。此处，在使用2种以上成分的情况下，只要合计含量为上述范围即可。
上述树脂组合物优选含有选自抗氧化剂、紫外线吸收剂、增塑剂、抗静电剂、润滑剂和填充剂中的至少1种添加剂。上述树脂组合物中的该添加剂的含量优选为0.005~50质量%。该含量更优选为20质量%以下，进一步优选为10质量%以下，特别优选为5质量%以下，最优选为1质量%以下。
作为上述抗氧化剂，可列举出N,N’-己烷-1,6-二基双〔3-（3,5-二叔丁基-4-羟基苯基）丙酰胺〕、N,N’-1,6-己烷二基双｛N-(2,2,6,6-四甲基-4-哌啶基)-甲酰胺｝、2,5-二叔丁基对苯二酚、2,6-二-2,2’-亚甲基-双-（4-甲基-6-叔丁基苯酚）、3-（3’,5’-二叔丁基-4’-羟基苯基）丙酸十八烷基酯、4,4’-硫代双-（6-叔丁基苯酚）等。
作为上述紫外线吸收剂，可列举出亚乙基-2-氰基-3,3’-二苯基丙烯酸酯、2-（2’-羟基-5’-甲基苯基）苯并三唑、2-（2’-羟基-5’-甲基苯基）苯并三唑、2-（2’-羟基-5’-甲基苯基）苯并三唑、2-（2’-羟基-3’-叔丁基-5’-甲基苯基）-5-氯苯并三唑、2-羟基-4-甲氧基二苯甲酮、2,2’-二羟基-4-甲氧基二苯甲酮、2-羟基-4-辛氧基二苯甲酮等。
作为上述增塑剂，可列举出邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二辛酯、蜡、液体石蜡、磷酸酯等。
作为上述抗静电剂，可列举出季戊四醇单硬脂酸酯、脱水山梨糖醇单棕榈酸酯、硫酸化聚烯烃类、聚环氧乙烷、聚乙二醇（商品名：CARBOWAX）等。
作为上述润滑剂，可列举出例如乙撑双硬脂酰胺、丁基硬脂酸酯等。
作为上述填充剂，可列举出玻璃纤维、硅灰石、硅酸钙、滑石、蒙脱石等。
上述树脂组合物中，作为其它成分，可以含有除EVOH之外的热塑性树脂。作为热塑性树脂，可列举出聚烯烃[聚乙烯、聚丙烯、聚（1-丁烯）、聚（4-甲基-1-戊烯）、乙烯-丙烯共聚物、乙烯与碳原子数为4以上的α-烯烃的共聚物、烯烃与马来酸酐的共聚物、乙烯-乙烯基酯共聚物、乙烯-丙烯酸酯共聚物、或者将它们用不饱和羧酸或其衍生物进行了接枝改性的改性聚烯烃等]；尼龙（尼龙6、尼龙66、尼龙6/66共聚物等）；聚氯乙烯；聚偏二氯乙烯；聚酯；聚苯乙烯；聚丙烯腈；聚氨基甲酸酯；聚缩醛；改性聚乙烯醇等。上述树脂组合物中的除EVOH之外的热塑性树脂的含量优选为45质量%以下，更优选为20质量%以下，进一步优选为10质量%以下，特别优选为5质量%以下，最优选为1质量%以下。
从调整热稳定性、粘度的观点出发，上述树脂组合物中，作为其它成分，可以含有各种酸等化合物。作为该化合物，可列举出羧酸、磷酸化合物和硼化合物等，具体而言，可列举出以下那样的化合物。需要说明的是，这些化合物可以预先含于EVOH中。
羧酸：草酸、琥珀酸、苯甲酸、柠檬酸、乙酸、乳酸等
磷酸化合物：磷酸、亚磷酸等各种酸或其盐等
硼化合物：硼酸、硼酸酯、硼酸盐、氢化硼等
上述树脂组合物的MFR优选为与上述EVOH相同的范围。通过将上述树脂组合物的MFR设为这种范围而得到的效果也与EVOH的情况相同。
（树脂组合物的制造方法）
本发明的树脂组合物的制造方法没有特别限定，可列举出将包含上述EVOH、非离子表面活性剂和根据需要的其它成分的混合物进行熔融混炼的方法。
上述EVOH、非离子表面活性剂等的熔融混炼可使用Kneader-Rudder、挤出机、混炼辊、班伯里密炼机等已知的混合装置或混炼装置来进行。作为非离子表面活性剂的形式，可列举出粉末等固体、熔融物、水溶液等溶液和水分散液等分散液等。可以将这种方式的非离子表面活性剂与上述EVOH、其它成分进行混合。作为非离子表面活性剂的形式，优选为溶液和分散液。将包含上述EVOH和非离子表面活性剂等的混合物进行熔融混炼时的温度根据所使用的EVOH的熔点等进行适当调节即可，通常为120℃~300℃。
优选为通过将包含上述非离子表面活性剂、水和上述EVOH的混合物进行熔融混炼来制造上述树脂组合物的方法。上述混合物中的水的含量相对于上述EVOH 100质量份优选为0.1~50质量份、更优选为0.5~50质量份。在该含量小于0.1质量份的情况下，所得树脂组合物有可能容易着色。另一方面，在上述含量超过50质量份的情况下，上述EVOH与水发生相分离而从挤出机喷出的树脂组合物有可能容易产生发泡。上述混合物中的水含量是指单独添加的水与随同其它成分一起添加的水的合计量，还包括因吸湿等而在上述非离子表面活性剂、上述EVOH中含有的水。作为随同其它成分一起添加水的方法，可列举出作为上述非离子表面活性剂而使用水溶液或水分散液的方法、如后那样地作为上述EVOH而使用含有特定量水的EVOH的方法。
在上述制造方法中，优选将包含上述非离子表面活性剂的水溶液或水分散体添加至上述EVOH而得到上述混合物。通过以水溶液或水分散体的形式添加上述非离子表面活性剂，从而该非离子表面活性剂容易分散至上述EVOH中。
在上述制造方法中，可以向熔融前的上述EVOH中添加上述非离子表面活性剂，也可以向熔融的上述EVOH中添加上述非离子表面活性剂。从生产率的观点出发，优选为后者。
作为将包含上述非离子表面活性剂、水和上述EVOH的混合物进行熔融混炼的方法，可列举出例如将上述EVOH导入至挤出机后，对于已熔融的该EVOH，添加非离子表面活性剂和根据需要的其它成分并混炼后，进行喷出的方法。此时，可以将含水率为5~40质量%的上述EVOH导入至挤出机中。
[成形体]
含有如此得到的树脂组合物的成形体是本发明的优选实施方式。该成形体可以仅由该树脂组合物组成，也可以具有包含该树脂组合物的部分和包含除该树脂组合物之外的组合物的部分。
作为含有上述树脂组合物的成形体，可列举出粒料、膜、片、容器（袋、杯、管、托盘、瓶等）、燃料容器、管、纤维、饮料食品用包装材料、容器用填充材料、医疗用输液包材料、轮胎用管材、鞋用缓冲材料、箱中衬袋用内袋材料、有机液体贮藏用罐材、有机液体运输用管材、暖气用温水管材（地暖用温水管材等）、化妆品用包装材料、牙科护理用包装材料、药品用包装材料、包材用小部件(盖、箱中衬袋的阀部分等)、农药瓶、农业用膜（温室用膜、土壤熏蒸用膜）、谷物保管用袋、土工膜、壁纸或化妆板、氢气、氧气等的气罐等。作为上述燃料容器，可列举出汽车、摩托车、船舶、飞机、发电机、工业用机器、农业用机器等所搭载的燃料容器、用于向这些燃料容器补充燃料的便携用容器、用于保管燃料的容器等。作为燃料可列举出汽油，其中，作为代表例而列举出共混有甲醇、乙醇或MTBE等的汽油、即含氧汽油。进而，还可列举出其它的重油、轻油、灯油等。
上述成形体通常可通过将上述树脂组合物进行熔融成形来制造。这些成形体出于再使用的目的而粉碎后，也可以再次成形。此外，也可以将膜、片、纤维等进行单轴拉伸或双轴拉伸。作为熔融成形法，也可以应用例如挤出成形、吹胀挤出、吹塑成形、熔融纺丝、注射成形等公知的任意成形法。作为熔融成形时的熔融温度，优选为150~300℃，更优选为200~250℃。通过使用本发明的树脂组合物，从而抑制熔融成形后的黄变等着色、凝胶、起块、鱼眼、条纹等的发生。因此，通过将上述树脂组合物进行熔融成形而得到的成形体具有优异的外观。此外，在制造膜时，通常为了获得一定的喷出量而包含EVOH的组合物按照供给部/压缩部/计量部/模具的温度依次为例如175℃/200℃/210℃/210℃的情况设定为压缩部和计量部的温度较高的温度，但通过使用上述树脂组合物，即使在供给部和压缩部的温度比通常的温度低10℃以上的低温条件下，也能够获得一定的喷出量。
作为该成形体，优选为具有包含上述树脂组合物的层和包含除EVOH之外的其它热塑性树脂的层的多层结构体。上述树脂组合物的长期运转性优异，且还抑制熔融成形后的黄变等着色、凝胶、起块、鱼眼、条纹等的发生。因此，通过使用上述树脂组合物和其它热塑性树脂来进行熔融成形，能够以良好的生产率制造具有优异外观的多层结构体。
上述多层结构体的厚度构成没有特别限定，从成形性和成本等的观点出发，上述树脂组合物层相对于所有层厚度的厚度比优选为2~20%。上述多层结构体的层构成没有特别限定，若将其它热塑性树脂层记作A、将上述树脂组合物层记作B、将粘接性树脂层记作C，则可例示出A/B、A/B/A、A/C/B、A/C/B/C/A、A/B/A/B/A、A/C/B/C/A/C/B/C/A等层构成。也可以向它们中进一步添加其它层。在设有多个其它热塑性树脂层的情况下，可以使用不同的层，也可以使用相同的层。进而，可以另行设置由成形时产生的边角等碎料形成的回收树脂的层，也可以将由回收树脂与其它热塑性树脂的共混物形成的层制成其它热塑性树脂层。
作为上述粘接性树脂，优选为羧酸改性聚烯烃。作为羧酸改性聚烯烃，可适合地使用使烯属不饱和羧酸、其酯或其酸酐化学（例如加成反应、接枝反应等）键合于烯烃系聚合物而得到的含有羧基的改性烯烃系聚合物。作为烯属不饱和羧酸、其酯或其酸酐，可列举出马来酸、富马酸、衣康酸、马来酸酐、衣康酸酐、马来酸单甲酯、马来酸单乙酯、马来酸二乙酯、富马酸单甲酯等，更优选为马来酸酐。这些粘接性树脂可以单独使用，或者，也可以混合使用两种以上。
作为上述其它热塑性树脂，可列举出直链状低密度聚乙烯、低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯共聚物、聚丙烯、丙烯-α-烯烃共聚物、聚丁烯、聚戊烯等聚烯烃；聚对苯二甲酸乙二醇酯等聚酯；聚酯弹性体；尼龙6、尼龙66等聚酰胺；聚苯乙烯；聚氯乙烯；聚偏二氯乙烯；丙烯酸系树脂；乙烯基酯系树脂；聚氨基甲酸酯弹性体；聚碳酸酯；氯化聚乙烯；氯化聚丙烯。这些之中，优选使用聚丙烯、聚乙烯、乙烯-丙烯共聚物、乙烯-乙酸乙烯酯共聚物、聚酰胺、聚苯乙烯和聚酯。
这些之中，优选使用聚烯烃层作为其它热塑性树脂层，且使用羧酸改性聚烯烃层作为粘接性树脂层。这是因为：通过设置聚烯烃层，上述多层结构体的力学特性提高，耐湿性也提高。尤其是，在上述多层结构体的两个外层设置聚烯烃层对于有效地防止树脂组合物层的吸湿而言是优选的。此时，也可以在不损害这种效果的范围内向聚烯烃中添加回收树脂。
作为制造上述多层结构体的方法，可列举出例如以下的方法。
（1）将上述树脂组合物与其它热塑性树脂进行共挤出的方法
（2）在包含上述树脂组合物的成形体上熔融挤出其它热塑性树脂的方法
（3）将上述树脂组合物与其它热塑性树脂进行共注射的方法
（4）使用粘接剂使包含上述树脂组合物的成形体与包含其它热塑性树脂的成形体进行层叠的方法。
这些方法之中，优选为（1）。本发明的树脂组合物即使在高温条件下进行熔融成形，其长期运转性也优异，且熔融成形后的着色也受到抑制。因此，即使将该树脂组合物与其它高熔点的热塑性树脂进行共挤出，着色也受到抑制，能够获得外观优异的多层结构体。作为共挤出方法，可列举出例如多歧管合流方式T模法、喂料块合流方式T模法、吹胀法等。
通过将利用上述共挤出得到的多层结构体进行二次加工，从而得到例如以下的成形体。
（1）通过将多层结构体（片、膜等）沿着单轴方向或双轴方向进行拉伸，且进行热处理而得到的多层拉伸片或多层拉伸膜
（2）通过将多层结构体（片、膜等）进行压延而得到的多层压延片或多层压延膜
（3）通过将多层结构体（片、膜等）进行热成形（真空成形、压空成形、真空压空成形等）而得到的多层托盘或多层杯状容器
（4）通过将多层结构体（管等）进行拉伸吹塑成形而得到的多层瓶、多层杯状容器等。
进行这些二次加工而得到的成形体可优选地用作例如深拉容器、杯状容器、瓶等食品容器。
实施例
以下，通过实施例更详细地说明本发明。
实施例1
（1）树脂组合物粒料的制作
准备乙烯单元含量为32摩尔%、皂化度为99.98摩尔%、MFR为3.8g/10分钟（温度为210℃、载荷为2160g）、含水率为0.2质量%、作为金属盐以钠换算含有200ppm乙酸钠的EVOH1。此外，作为非离子表面活性剂，准备分散有聚氧乙烯（7）硬脂基醚（非离子表面活性剂的化合物名中的括弧内的数字表示聚氧乙烯单元的缩合度。以下相同）的水分散液（非离子表面活性剂的含量：10.0g/L）。将100质量份的EVOH1与1质量份的上述水分散液进行共混。将所得混合物按照下述条件进行熔融混炼后，进行粒料化并进一步使其干燥，由此得到树脂组合物粒料。
装置：25mmφ双螺杆挤出机（东洋精机制作所制的“LABO PLASTOMILL 4C150”）
L/D：25
螺杆：同向完全啮合型
模孔数：2孔（3mmφ）
挤出温度：C1＝200℃、C2~C5＝220℃、模具＝220℃
干燥：真空干燥90℃/20hr。
（2）非离子表面活性剂的定量
将树脂组合物粒料10g溶解于1,1,1,3,3,3-六氟-2-丙醇后，将该溶液滴加至甲醇。将该液体用过滤器过滤而去除析出物后，进行浓缩。将所得浓缩液用Waters公司的“UPLC H-Class”进行测定，由此算出EVOH粒料中的非离子表面活性剂的含量。需要说明的是，进行定量时，采用了使用各非离子表面活性剂而制作的标准曲线。树脂组合物粒料中的聚氧乙烯（7）硬脂基醚的含量为100ppm。
（3）喷出量的评价
使用东洋精机制作所制的20mm挤出机“D2020”（D＝20mm、L/D＝20、压缩比＝2.0、螺杆：全平行），按照下述条件，由树脂组合物粒料得到厚度20μm的单层膜。将此时的每1小时的单层膜的生产量作为树脂组合物的喷出量来进行评价。如果喷出量为0.5kg/hr以上则能够实用。测定的结果，树脂组合物的喷出量为1.6kg/hr。
单层膜制作条件
挤出温度：供给部/压缩部/计量部/模具
＝160/180/210/210℃
螺杆转速：40rpm
牵引辊温度：80℃。
（4）单层膜的外观
将通过上述方法而制作的单层膜卷取于纸管，用肉眼按照下述基准来评价膜端面的着色。其结果，确认不到膜端面的着色。
A：确认不到着色
B：略微黄变
C：发生了黄变，但处于能够实用的程度
D：剧烈黄变，无法实用。
（5）多层结构体的粘接性
使用树脂组合物粒料、直链状低密度聚乙烯（LLDPE：三井化学公司制的ULTZEX 2022L）和粘接性树脂（SUMICA.ATOCHEM Co.Ltd制的Bondine TX8030、以下有时简写为Ad），如下所示地获得3种5层的多层膜（LLDPE/Ad/树脂组合物/Ad/LLDPE＝50μm/10μm/10μm/10μm/50μm）。将所得多层膜在刚刚进行多层制膜后沿着MD方向切出150mm，且沿着TD方向切出10mm后，立即利用AUTOGRAPH（岛津制作所社制的DCS-50M）以T型剥离模式测定树脂组合物层/Ad层间的剥离强度，并按照下述基准进行评价。其结果，粘接强度为550g/15cm。
〈多层制膜条件〉
挤出机：
EVOH用：20mmφ挤出机 试验机ME型CO-EXT（东洋精机公司制）
Ad用：25mmφ挤出机 P25-18AC（大阪精机公司制）
LLDPE用：32mmφ挤出机 GF-32-A（塑料工学研究所公司制）
EVOH挤出温度 供给部/压缩部/计量部/模具
＝175/210/220/220℃
Ad挤出温度 供给部/压缩部/计量部/模具
100/160/220/220℃
LLDPE挤出温度 供给部/压缩部/计量部/模具
150/200/210/220℃
模具 300mm宽的衣架模（塑料工学研究所公司制）。
〈粘接性的判定基准〉
A：600g/15cm以上
B：450g/15cm以上且小于600g/15cm
C：300g/15cm以上且小于450g/15cm
D：小于300g/15cm。
实施例2~33和比较例1~6
除了如表1和表2所示地变更EVOH的种类、非离子表面活性剂的种类和含量之外，与实施例1同样地制作树脂组合物的粒料、单层膜和多层结构体后，进行它们的分析和评价。将结果示于表2。
1）日油株式会社制“UNILUB MS-70K”、2）日油株式会社制“NONION HT-510”、3）第一工业制造公司制“NOIGEN EA-157”、4）日油株式会社制“NOIGEN S-210”、5）日油株式会社制“NOIGEN L-703”、6）日油株式会社制“NONION L-4”、7）日油株式会社制“NONION S-4”、8）日油株式会社制“NONION L-2”、9）日油株式会社制“NONION DO-6”、10）第一工业制造公司制“SOLGEN TW-60”、11）第一工业制造公司制“SOLGEN 110”。
实施例34
与实施例1同样地准备EVOH1和非离子表面活性剂的水分散液。将100质量份EVOH1、1质量份上述水分散液和作为抗氧化剂的0.5质量份N,N’-己烷-1,6-二基双〔3-（3,5-二叔丁基-4-羟基苯基）丙酰胺〕进行共混。使用这样得到的混合物，除此之外，与实施例1同样地制作树脂组合物粒料、单层膜和多层结构体后，进行它们的分析和评价。将结果示于表3。
实施例35~48
除了如表3所示那样地变更非离子表面活性剂量以及添加剂的种类和添加量之外，与实施例34同样地制作树脂组合物粒料、单层膜和多层结构体后，进行它们的分析和评价。将结果示于表3。
实施例49、50
使用85质量份EVOH1和15质量份EVOH3（乙烯含量为48摩尔%、皂化度为99.98摩尔%、MFR为15g/10分钟（温度为210℃、载荷为2160g）、含水率为0.2质量%）来代替100质量份EVOH1，且使非离子表面活性剂的含量如表3所示，除此之外，与实施例1同样地制作树脂组合物的粒料、单层膜和多层结构体后，进行它们的分析和评价。将结果示于表3。
1）质量份
2）1抗氧化剂A：N,N’-己烷-1,6-二基双〔3-（3,5-二叔丁基-4-羟基苯基）丙酰胺〕
2抗氧化剂B：N,N’-1,6-己烷二基双｛N-(2,2,6,6-四甲基-4-哌啶基)-甲酰胺｝
3紫外线吸收剂：亚乙基-2-氰基-3,3’-二苯基丙烯酸酯
4增塑剂：邻苯二甲酸二甲酯
5抗静电剂：季戊四醇单硬脂酸酯
6润滑剂：乙撑双硬脂酰胺
7填充剂：滑石。
实施例51
使用实施例1中得到的树脂组合物粒料，使用3种5层共挤出机，制作聚丙烯层（200μm）/粘接性树脂层（25μm）/树脂组合物层（50μm）/粘接性树脂层（25μm）/聚丙烯层（200μm）的5层构成的多层膜。此处，作为粘接性树脂，使用了马来酸酐改性聚丙烯。与实施例1同样地评价所得多层膜的外观，结果未确认到膜端面的着色。
比较例7
除了使用比较例1中得到的树脂组合物粒料之外，与实施例51同样地进行多层膜的制作和外观的评价。膜端面剧烈黄变，无法实用。
Claims (11)
1.树脂组合物，其为含有乙烯-乙烯醇共聚物和非离子表面活性剂的树脂组合物，
所述乙烯-乙烯醇共聚物的乙烯单元含量为15~60摩尔%，皂化度为90摩尔%以上，
所述树脂组合物中含有所述乙烯-乙烯醇共聚物作为主成分，
且含有3~400ppm的所述非离子表面活性剂。
2.根据权利要求1所述的树脂组合物，其中，所述非离子表面活性剂为选自醚型、氨基醚型、酯型、酯・醚型和酰胺型中的至少一种。
3.根据权利要求2所述的树脂组合物，其中，所述非离子表面活性剂为选自聚氧亚烷基烷基醚、聚氧亚烷基烯基醚、聚氧乙烯苯乙烯化苯基醚、聚氧亚烷基烷基胺、聚氧亚烷基烯基胺、聚氧亚烷基烷基酯、聚氧亚烷基烯基酯、脱水山梨糖醇烷基酯、脱水山梨糖醇烯基酯、聚氧乙烯脱水山梨糖醇烷基酯、聚氧乙烯脱水山梨糖醇烯基酯、甘油烷基酯、甘油烯基酯、聚甘油烷基酯、聚甘油烯基酯和高级脂肪酸酰胺中的至少一种。
4.根据权利要求1~3中任一项所述的树脂组合物，其还含有以金属元素换算为10~500ppm的碱金属盐。
5.根据权利要求1~4中任一项所述的树脂组合物，其还含有0.005~1质量%的选自抗氧化剂、紫外线吸收剂、增塑剂、抗静电剂、润滑剂和填充剂中的至少1种添加剂。
6.根据权利要求1~5中任一项所述的树脂组合物，其中，作为所述乙烯-乙烯醇共聚物，含有2种乙烯单元含量不同的乙烯-乙烯醇共聚物。
7.成形体，其含有权利要求1~6中任一项所述的树脂组合物。
8. 多层结构体，其具有：
包含权利要求1~6中任一项所述的树脂组合物的层；以及
包含除所述乙烯-乙烯醇共聚物之外的热塑性树脂的层。
9.根据权利要求1~6中任一项所述的树脂组合物的制造方法，其中，将包含所述非离子表面活性剂、水和所述乙烯-乙烯醇共聚物的混合物进行熔融混炼。
10.根据权利要求9所述的制造方法，其中，所述混合物中的水的含量相对于所述乙烯-乙烯醇共聚物100质量份为0.1~50质量份。
11.根据权利要求9或10所述的制造方法，其中，将包含所述非离子表面活性剂的水溶液或水分散体添加至所述乙烯-乙烯醇共聚物而得到所述混合物。
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| CN113784836A (zh) * | 2019-03-11 | 2021-12-10 | 株式会社可乐丽 | 多层结构体和使用了其的蒸煮用包装材料 |
| CN113784836B (zh) * | 2019-03-11 | 2024-05-07 | 株式会社可乐丽 | 多层结构体和使用了其的蒸煮用包装材料 |
| CN114829490A (zh) * | 2019-12-27 | 2022-07-29 | 株式会社可乐丽 | 树脂组合物以及包含其的成形品和多层结构体 |
| CN115135724A (zh) * | 2020-02-21 | 2022-09-30 | 松下知识产权经营株式会社 | 树脂组合物 |
| CN115135724B (zh) * | 2020-02-21 | 2024-01-09 | 松下知识产权经营株式会社 | 树脂组合物 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3597701A1 (en) | 2020-01-22 |
| US20200385546A1 (en) | 2020-12-10 |
| WO2018168903A1 (ja) | 2018-09-20 |
| TWI761470B (zh) | 2022-04-21 |
| EP3597701A4 (en) | 2020-12-02 |
| US11560464B2 (en) | 2023-01-24 |
| JP6411705B1 (ja) | 2018-10-24 |
| JPWO2018168903A1 (ja) | 2019-03-22 |
| TW201842031A (zh) | 2018-12-01 |
| CN110603292B (zh) | 2022-04-19 |
| EP3597701B1 (en) | 2022-03-02 |
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