CN101360783B - 阻透膜 - Google Patents
阻透膜 Download PDFInfo
- Publication number
- CN101360783B CN101360783B CN2005800356104A CN200580035610A CN101360783B CN 101360783 B CN101360783 B CN 101360783B CN 2005800356104 A CN2005800356104 A CN 2005800356104A CN 200580035610 A CN200580035610 A CN 200580035610A CN 101360783 B CN101360783 B CN 101360783B
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- Prior art keywords
- film
- forming properties
- barrier polymer
- starch
- properties barrier
- Prior art date
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- 230000004888 barrier function Effects 0.000 title claims abstract description 113
- 229920002472 Starch Polymers 0.000 claims abstract description 71
- 235000019698 starch Nutrition 0.000 claims abstract description 71
- 239000008107 starch Substances 0.000 claims abstract description 70
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 66
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 41
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 35
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 35
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 33
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 229920000642 polymer Polymers 0.000 claims abstract description 32
- 239000004743 Polypropylene Substances 0.000 claims abstract description 27
- 229920001155 polypropylene Polymers 0.000 claims abstract description 25
- 235000011187 glycerol Nutrition 0.000 claims abstract description 22
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 18
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 15
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 12
- 239000004698 Polyethylene Substances 0.000 claims abstract description 11
- 229920000573 polyethylene Polymers 0.000 claims abstract description 11
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000071 blow moulding Methods 0.000 claims abstract description 9
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000811 xylitol Substances 0.000 claims abstract description 9
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims abstract description 9
- 235000010447 xylitol Nutrition 0.000 claims abstract description 9
- 229960002675 xylitol Drugs 0.000 claims abstract description 9
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 6
- 235000013361 beverage Nutrition 0.000 claims abstract description 6
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 6
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 5
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 5
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims abstract description 5
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 4
- 229930195725 Mannitol Natural products 0.000 claims abstract description 4
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims abstract description 4
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 claims abstract description 4
- 239000000944 linseed oil Substances 0.000 claims abstract description 4
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- 239000000594 mannitol Substances 0.000 claims abstract description 4
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- 239000003549 soybean oil Substances 0.000 claims abstract description 4
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 4
- WEAPVABOECTMGR-UHFFFAOYSA-N triethyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCOC(=O)CC(C(=O)OCC)(OC(C)=O)CC(=O)OCC WEAPVABOECTMGR-UHFFFAOYSA-N 0.000 claims abstract description 4
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims abstract description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229920001577 copolymer Polymers 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 25
- 239000004902 Softening Agent Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 19
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 19
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
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- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 230000035699 permeability Effects 0.000 claims description 14
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 11
- 239000000080 wetting agent Substances 0.000 claims description 9
- 235000011089 carbon dioxide Nutrition 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 240000007594 Oryza sativa Species 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 6
- 230000002255 enzymatic effect Effects 0.000 claims description 6
- 235000009566 rice Nutrition 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 235000010418 carrageenan Nutrition 0.000 claims description 5
- 229920001525 carrageenan Polymers 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 150000008064 anhydrides Chemical class 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 4
- 244000215068 Acacia senegal Species 0.000 claims description 3
- 235000006491 Acacia senegal Nutrition 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- 229920002907 Guar gum Polymers 0.000 claims description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 239000000665 guar gum Substances 0.000 claims description 3
- 235000010417 guar gum Nutrition 0.000 claims description 3
- 229960002154 guar gum Drugs 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 229940117972 triolein Drugs 0.000 claims description 3
- 239000000230 xanthan gum Substances 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- 235000010493 xanthan gum Nutrition 0.000 claims description 3
- 229940082509 xanthan gum Drugs 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- BJVWCKXHSNBHGB-UHFFFAOYSA-L disodium;chloride;hydroxide Chemical compound [OH-].[Na+].[Na+].[Cl-] BJVWCKXHSNBHGB-UHFFFAOYSA-L 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 49
- 238000001125 extrusion Methods 0.000 abstract description 7
- 238000002347 injection Methods 0.000 abstract description 7
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- 238000003475 lamination Methods 0.000 abstract description 3
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- 239000010409 thin film Substances 0.000 abstract description 3
- 239000004626 polylactic acid Substances 0.000 abstract 2
- KESQFSZFUCZCEI-UHFFFAOYSA-N 2-(5-nitropyridin-2-yl)oxyethanol Chemical compound OCCOC1=CC=C([N+]([O-])=O)C=N1 KESQFSZFUCZCEI-UHFFFAOYSA-N 0.000 abstract 1
- 239000005977 Ethylene Substances 0.000 abstract 1
- 240000006240 Linum usitatissimum Species 0.000 abstract 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 abstract 1
- 239000004368 Modified starch Substances 0.000 abstract 1
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- 229920002988 biodegradable polymer Polymers 0.000 abstract 1
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- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
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- 239000000463 material Substances 0.000 description 85
- 239000007789 gas Substances 0.000 description 73
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 54
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Abstract
本发明提供一种阻透组合物,该组合物可注射成型,并能够制备成透明膜或加入(通过共挤出和/或层合)多层膜产品中。以干重计,所述组合物包含:a)以重量计45%至90%的淀粉和/或改性淀粉,所述改性淀粉选自通过与羟烷基、乙酸盐或二羧酸酐或接枝聚合物反应而改性的淀粉;b)以重量计4%至12%的水溶性聚合物,所述水溶性聚合物选自聚乙烯醇、聚乙酸乙烯酯以及乙烯与乙烯醇的共聚物,所述水溶性共聚物的熔点与淀粉组分的熔融状态相容;c)以重量计5%至45%的非结晶性混合物,所述混合物由山梨醇与至少一种其它增塑剂组成,所述增塑剂选自丙三醇、麦芽糖醇、木糖醇、甘露醇、三油酸甘油酯、环氧化亚麻子油或环氧化大豆油、柠檬酸三丁酯、乙酰柠檬酸三乙酯、三乙酸甘油酯、2,2,4-三甲基-1,3-戊二醇二异丁酸酯、聚环氧乙烷或聚乙二醇;d)以重量计0.3%至2.5%的C12-22脂肪酸或盐;和e)以重量计0.25%至3%的乳化剂体系,所述乳化剂体系具有2~10的亲水亲油平衡值。该阻透组合物可以与PET或PLA共挤出成型,并吹塑成型为饮料瓶;或者可与PE、PP或可生物降解的聚合物成型为高阻气性的容器或封口;或者可与PE、PP或PLA一起用于薄膜包装用途或用于吹塑成型的容器。
Description
技术领域
本发明涉及用于包装的阻透膜,该阻透膜用以防止二氧化碳、氧气和氮气等气相出入尤其是固体和液体食品等被包装的产品。
背景技术
在包装业中,食品和饮料的保鲜是一个巨大的挑战。大多数普通包装材料在阻止气体出入包装食品方面具有很大不足。过去三十年,提供阻透膜层的行业得到了发展。这些膜用于阻止水蒸汽、O2、CO2和N2等气体出入食品或饮料。塑料用作包装材料已有六十多年,随着市场需求的增长和技术的进步,这种塑料还在继续发展。对许多塑料包装的一个重要要求是保持食品和饮料新鲜。食品和饮料变质最主要的原因是氧气透入而导致氧化。
例如聚对苯二甲酸乙二醇酯(PET)、聚丙烯(PP)、聚氯乙烯(PVC)和聚乙烯(PE)等商品塑料均对O2和H2O有一定阻透性。这种阻透性与阻透层的厚度成正比。对于高阻透性塑料的需求来自以下三个因素:首先,由于玻璃和锡/铝的重量、成本和易碎性,所以需要替代玻璃和锡/铝;其次,减少塑料材料的厚度以使其更加经济;第三,由于越来越多的食品被包装为越来越小的使用规格,所以需要具有长的保质期。在这些因素的驱使下,已经出现了一些显著提高普通消费品塑料包装的阻透性的材料。
第一种成功的高性能阻透材料是聚偏二氯乙烯(PVDC)。它是聚氯乙烯(PVC)的衍生物,因此被认为具有类似的不利于环境的特性。
现今,在市面上供应的其它普通阻透材料有乙烯-乙烯醇共聚物(EVOH)、尼龙(例如MXD6)以及腈类。它们均被当作阻透层用于由商品塑料形成的结构层。
赛璐玢是唯一一种已经商品化的可以用作阻透材料的天然聚合物,在 塑料工业起步之初,赛璐玢已经发展成熟。与现今的阻透树脂相比,它对氧的阻透特性不高,并且其成本较高。
PET(聚对苯二甲酸乙二醇酯)饮料瓶壁的阻透结构一般是多层结构,所述多层结构由含有昂贵的阻透材料的一个或多个芯层和包围芯层的PET结构层构成。
美国专利5498662、562102、65897960和6143384公开了聚甲基丙烯酸聚合物和多糖在阻透层中的用途。
WO 00/49072公开了一种阻透涂层,该涂层基于诸如蒙脱土等粘土,通过喷涂而被覆到吹塑成型的PET瓶上。
美国申请2004/0087696公开了用于PET容器的水性涂料,其中,将粘土材料与三聚氰胺、甲醛和硼酸粘合剂以及诸如多糖和纤维素材料等有机水溶性粘合剂相混合。
阻透材料用在许多不同的塑料结构和操作中,这些结构和操作都能实现各自的功能性要求。阻透结构最常用于糖果和焙烤食品等食品的包装薄膜,以及过去五年来市场上出现的大量袋子的薄膜。其中一些薄膜可以具有12层,然而其厚度小于50μm。这些薄膜通常通过共挤出来制备。
WO 90/14938公开了适合用在阻氧层合体中的高直链改性淀粉。
美国专利6569539和6692801公开了纸和/或塑料层合体,该层合体具有由分散液涂布而形成的淀粉或改性淀粉的内部阻透涂层。
WO 04/052646公开了使用淀粉层和可生物降解的聚酯层的多层阻透膜。
美国申请2002/0187340公开了聚乙烯醇和淀粉的气体阻透涂层,其中,主要材料是淀粉,并且该材料由分散液涂布。
在果汁瓶、某些碳酸饮料瓶和诸如水果和蔬菜蜜饯等各种热填充食品瓶中也采用阻透层。瓶子通常通过共注射拉伸吹塑成型而形成。这需要将材料注射成型为预型体,然后将其再次熔化并吹塑成瓶子形状。有的容器可以由共挤出吹塑成型,其中,在共挤出过程中,吹塑型坯使其紧贴模具壁,从而连续得到所期望的形状。
某些容器还需要由注射成型所形成的高阻气性封口。
使用阻透材料的其它重要领域还有诸如肉盘等硬包装,对于大多数用途而言,硬塑料包装可提供足够的阻透性,而且仅需要改善上部的薄膜的性能。
被认为制约阻透技术用途一个问题是它们对塑料再生性的影响——对包装瓶市场而言尤其如此。现在,许多PET瓶具有层合结构,在这种结构中,新料位于外部,而再生PET和阻透层处于内部。如果阻透树脂与再生体系不相容,那么采用这种技术就存在很大阻力。
最后,基于可持续、可再生资源的新材料和/或可生物降解的新材料正在进入市场。由玉米合成的聚乳酸(PLA)是这种材料的一个实例,它可以注射拉伸吹塑成型为瓶子或成型为包装用薄膜。聚乳酸的气体阻透差,而且其水蒸汽阻透性也相对较差。为了保持可生物降解性和可持续性,基于可再生资源的可生物降解阻透材料将会使这种情形有所改善。
发明内容
本发明的目的在于提供一种阻透膜,该阻透膜比现有技术的材料便宜,并易于与现有包装材料进行层合,由此可以解决上述问题。
为了实现所述目的,本发明提供了一种成膜性阻透聚合物,所述成膜性阻透聚合物具有以干重计的如下组成的组合物:
a)以重量计45%至90%的淀粉和/或改性淀粉,所述改性淀粉选自通过与羟烷基、乙酸盐或二羧酸酐或接枝聚合物反应而改性的淀粉;
b)以重量计4%至12%的水溶性聚合物,所述水溶性聚合物选自聚乙烯醇、聚乙酸乙烯酯以及乙烯与乙烯醇的共聚物,所述水溶性共聚物的熔点与淀粉组分的熔融状态相容;
c)以重量计5%至45%的非结晶性混合物,所述混合物由山梨醇与至少一种其它增塑剂组成,所述增塑剂选自丙三醇、麦芽糖醇、木糖醇、甘露醇、三油酸甘油酯、环氧化亚麻子油或环氧化大豆油、柠檬酸三丁酯、乙酰柠檬酸三乙酯、三乙酸甘油酯、2,2,4-三甲基-1,3-戊二醇二异丁酸酯、聚环氧乙烷或聚乙二醇;
d)以重量计0.3%至2.5%的C12-22脂肪酸或盐;和
e)以重量计0.25%至3%的乳化剂体系,所述乳化剂体系具有2~10的亲水亲油平衡值。
该制剂中可以包含少量的结合水,但水的量仅为水在选定工艺的处理条件下不会蒸发的程度。
上述定义的组合物包括适于(共)挤出或浇铸可用于层合结构的薄膜的制剂。可以采用的其它加工方法包括:(共)注射成型,随后可以吹塑成型(注射-吹塑-成型);(共)挤出成型为包括可用于吹塑成型的管的形状(挤出-吹塑-成型);和(共)挤出和/或层合为用于后续热成型的片材。
本发明的材料对氧气及二氧化碳的阻透性能比基于淀粉的现有技术和当前普通商品阻透材料优异。在高湿度下,其阻透性能至少等于或优于当前普通商品阻透材料。
本发明的聚合物具有优异的阻氧性,在相对湿度至高为60%RH时,氧渗透系数小于0.1cm3 mm/m2 day atm(厘米3·毫米/米2·天·大气压),并且,在相对湿度至高为90%RH时,氧渗透系数小于0.7cm3 mm/m2 dayatm。
本发明的聚合物在相对湿度至高为60%RH时,其具有的二氧化碳渗透系数小于0.5cm3 mm/m2 day atm,并且,当相对湿度至高为90%RH时,其具有的二氧化碳的渗透系数小于0.9cm3 mm/m2 day atm。
可以通过共挤出、共注射成型、膜吹塑或热层合技术将所述材料与诸如PET、PE、(BO)PP、LDPE和聚乳酸等其它包装聚合物进行层合。具有PET和聚乳酸的层合体适于用作形成软性饮料的饮料瓶、啤酒瓶或调味品瓶的预型体。其它注射拉伸吹塑成型的层合产品包括用于汤汁和加工水果的热填充PET或PP容器。所述材料可以用在用于氧气和二氧化碳阻透用途的注射成型PP盖或封口中。用于食品和药品用途的挤吹成型的PE瓶也可以包含本发明的共挤出膜。
具有PE、PP、BO-PP和聚乳酸(PLA)的层合体适于用在薄膜包装用途中,例如休闲食品包装,或者诸如肉等产品的气调保鲜包装的薄膜罩。当使用诸如PET之类的极性材料时,粘附性是优异的,然而在与诸如PP等非极性材料的粘附方面,可以举出普通粘结层树脂(tie layer resin)。合 适的粘结层材料包括基于PP、EVA、LDPE或LLDPE的接枝聚合物。
因为本发明的阻透膜是可生物降解和水溶性的,所以它适于与可再生塑料一起使用。例如,它适于与PET一起使用,因为它在PET回收时所采用的碱洗过程中溶解。它适于与PLA一起使用,因为它是可生物降解的,并且其生物降解速度至少与PLA一样快。
改性的高直链淀粉
改性淀粉的含量的上限取决于其成本。该组分对于所得材料的结构改善有贡献,包括优异的成膜性能、优异的光学性能和抗凝沉性。淀粉的凝沉和结晶涉及基于淀粉的塑料的一个最重要的实际问题,因为它们有随时间变脆的倾向,这与焙烤产品的变陈过程类似。
典型的改性淀粉包括具有C2-6羟烷基的淀粉或通过与二羧酸酐反应而改性的淀粉。优选的组分是羟丙基化直链淀粉。其它的取代基可以是羟乙基或羟丁基,从而形成羟基醚取代物,可以使用乙酸盐或诸如乙酸酐、顺丁烯二酸酐、邻苯二甲酸酐或辛烯基琥珀酸酐等酸酐来制备酯衍生物。
取代度[被取代单元中羟基的平均数]优选为0.05至2。
优选的淀粉是高直链玉米淀粉。优选的组分是由Penford Australia出售的羟丙基化高直链淀粉A939。所用的羟丙基化的最小量是6.0%。典型的值为6.1%至6.9%。为了节省成本的原因和为了优化性能的原因,可以用以下物质替代一部分这种淀粉:
1)较高或较低量羟丙基化
2)较高含量的未改性淀粉。如果改性淀粉的羟丙基化的量较高,也可以使用较高含量的未改性淀粉。
3)用具有高度疏水性的辛烯基琥珀酸酐(OSA)改性的淀粉。随着取代度的增大,添加这种改性淀粉可提高耐水性。在盛放液体的包装物中加入这种淀粉聚合物作为阻透层,因为这时相对湿度可能高达90%,所以添加这种改性淀粉是有效的。OSA淀粉中的乙酰基键保证该材料在接触水和生物活性环境时保持生物降解性。
4)淀粉共聚物,优选由接枝有淀粉的苯乙烯-丁二烯共聚物组成。这种材料提高了产品的抗冲击性能。
淀粉
组合物中未改性淀粉的量受到所有其它成分的必要添加量的限制,未改性淀粉的量为补足配比量的余量。未改性淀粉可以获自小麦、玉米、马铃薯、稻米、燕麦、竹芋和豌豆等来源。未改性淀粉是来自可再生资源的廉价且可生物降解的原材料,它有益于最终产品的阻透性能,因此在该用途中颇具吸引力。但是,它的使用因发生凝沉(导致脆性的结晶化)、所制备的成型产品的透光性差、成膜性和拉伸弹性差而受到制约。高直链淀粉不易凝沉,因为已经发现,这种现象主要与熟化淀粉中的支链淀粉的结晶化有关。作为淀粉总量的一部分,未改性淀粉的优选浓度范围为0%至50%。
水溶性聚合物
所述组合物的聚合物组分b)优选与淀粉相容,具有水溶性,并且其熔点与淀粉的处理温度相容。聚乙烯醇是优选的聚合物,但是也可以使用乙烯-乙烯醇、乙烯-乙酸乙烯酯等聚合物或它们与聚乙烯醇的混合物。所选聚合物优选在室温条件下不具有水溶性。PVOH同时具有优异的成膜性、粘合特性和良好的弹性,并有助于基于淀粉的制剂的处理。PVOH由聚乙酸乙烯酯经水解而成,聚乙酸乙烯酯由乙酸乙烯酯单体聚合而成。完全水解级PVOH(如果有的话)几乎不含有残留乙酸酯基;然而部分水解级PVOH含有部分残留乙酸酯基。完全水解级溶于热水(200°F)中,并且当冷却到室温时仍保持为溶液。PVOH的优选等级包括DuPont Elvanol 71-30和Elvanol 70-62。它们的特性列于表I中。
表I:在本发明中使用的各等级PVOH的特性
等级 71-30 70-62
重均分子量MWt 93,700 107,000-112,000
特性粘度(mPa·s) 27-33 58.0-68.0
水解(%) 99.0-99.8 99.4-99.8
高分子量的等级可以提高抗冲击性和降低水敏性。其最大含量主要取决于成本。提高PVOH的含量会显著地提高断裂伸长率和减小杨氏模量。当低于6%时,成膜变得困难。因此,在薄膜阻透材料中的优选的浓度范围为7%至12%,并且,对于应用在注射吹塑成型的瓶子中的阻透材料, 优选的浓度范围为4%至12%。
多元醇增塑剂
可将多种增塑剂和湿润剂用在该制剂中,以便有助于加工,并且控制和稳定阻透材料的机械性能,尤其是降低对水分含量和相对湿度(RH)的依赖性。所需的增塑剂的含量主要取决于(共)挤出或(共)注射成型过程中和后续的吹塑或拉伸过程中所需的加工性能,并取决于最终产品所需的机械性能。
在选择适当的增塑剂方面,成本和与食品的接触是需要考虑的重要问题。优选的增塑剂是多元醇(尤其是山梨醇)和一种或多种其它多元醇(尤其是丙三醇、麦芽糖醇、甘露醇和木糖醇)的混合物,但赤藻糖醇、乙二醇和二甘醇也是合适的。增塑剂具有三重作用:
1.它为挤出混炼工序和层合工序提供合适的流变性;
2.它对产品的机械性能有积极影响;以及
3.它可以作为抗凝沉剂或抗结晶剂。
根据特定用途和共挤出或层合工艺,优选的增塑剂含量为10%~40%。
山梨醇、丙三醇和麦芽糖醇混合物特别适于改变制剂的机械性能,木糖醇以及木糖醇与山梨醇和丙三醇的混合物也是如此。OH基的数量越多,增塑剂在降低结晶化方面越有效。山梨醇、麦芽糖醇和木糖醇是特别好的湿润剂。丙三醇有助于在加工过程中溶解PVOH。当单独使用山梨醇时,可观察到结晶化。一些多元醇(尤其是山梨醇和丙三醇)会表现为向表面迁移,在山梨醇的情况下会形成不透明的结晶膜,或者在丙三醇的情况下会形成油膜。混合各种多元醇不同程度地抑制了这种作用。当添加单硬脂酸甘油酯和硬脂酰乳酸钠作为乳化剂时,可以提高稳定性。此外,使用盐的协同作用对机械性能的影响更强。
其它增塑剂
PEG化合物可以用作乳化剂、增塑剂或湿润剂。聚环氧乙烷和聚乙二醇也可以各自或一起提高耐水性以防止溶胀,溶胀将导致多层结构(MLS)分层。
另外的增塑剂有环氧化亚麻子油或环氧化大豆油。由于这些添加剂是疏水性的,所以可提高材料的湿敏性。增塑剂(优选由乳化体系稳定化的,参看如下部分)有助于进行加工,但不会显著地进一步减小杨氏模量。可以使用在PVC工业中更普遍使用的其它增塑剂,包括柠檬酸三丁酯、2,2,4-三甲基-1,3-戊二醇二异丁酸酯和乙酰柠檬酸三乙酯。
可以使用0%至20%的湿润剂或水结合剂或胶凝剂,它们可以用作(共)增塑剂,如角叉胶、黄原胶、阿拉伯树胶、瓜尔胶或白明胶。可以使用其它湿润剂,如蔗糖或葡萄糖。例如角叉胶等生物聚合物适于调整机械性能,角叉胶通常在食品中作为增稠剂,它部分溶于冷水中,而完全溶于热水中。通过结合水,这些组分可以具有显著的增塑功能。可以添加白明胶,以提高机械性能和降低湿敏性。黄原胶具有较高的持水能力,并且还用作乳化剂,并在淀粉组合物中具有抗凝沉作用。阿拉伯树胶还可以用作织构化助剂和成膜剂,亲水性碳水化合物和疏水性蛋白质能够为之提供水胶体乳化和稳定性能。瓜尔胶在淀粉组合物中具有类似的抗结晶化作用。另一种合适的湿润剂是三乙酸甘油酯。
盐类
可以用诸如氯化钠和氢氧化钠之类的盐来获得或提高增塑和增湿作用。钾盐、乙酸钾、氧化钙和碘化钠也是适合的。钙盐提高挤出淀粉材料的硬度和尺寸稳定性,并还可以与角叉胶组合使用,从而有助于凝胶化。
脂肪酸和脂肪酸盐
将硬脂酸用作润滑剂,因为与例如蜡相比,硬脂酸与淀粉的相容性较优。硬脂酸是疏水性的,因此可以提高基于淀粉的材料的湿敏性。除了硬脂酸外,还可以使用诸如硬脂酸钙之类的盐。硬脂酸迁移到基于淀粉的聚合物的表面。据认为,淀粉可以与脂肪酸形成复合物。淀粉吡喃葡糖苷(葡萄糖)是“椅式”构象的六元环。环的周边是亲水性的,而各个面是疏水性的。淀粉链形成螺旋状,每转具有约六个残基。结果成为具有亲水性的外表面和疏水性的内表面的中空圆柱体。内部空间的直径大约为4.5 ,像硬脂酸那样的直链烷基分子可以在其中匹配。这样,诸如单硬脂酸甘油酯(GMS)之类的乳化剂的脂肪酸部分可以与胶凝淀粉形成复合物,以阻碍 淀粉结晶化,从而减缓变陈过程。与直链淀粉(淀粉中的直链部分)和支链淀粉(淀粉中的支化部分)复合的单酸甘油酯的量取决于乳化剂的脂肪酸部分的饱和度。不饱和的脂肪酸具有由脂肪酸链中的双键产生的弯曲,这限制了脂肪酸形成复合物的能力。
硬脂酸特别可用作加工助剂,但是在聚环氧乙烷(PEO)或聚乙二醇(PEG)的存在下,硬脂酸不是必需的。硬脂酸的优选含量为0.5%至1.5%。也可以使用硬脂酸的钠盐和钾盐。另外,在选择该组分时,成本也可以是一个考虑因素,但是,月桂酸、肉豆蔻酸、棕榈酸、亚油酸和山嵛酸均是合适的。对于多层结构中的抗分层能力的要求极大地限制了对适当的加工助剂的选择。
热稳定剂
亚硫酸盐化剂(二氧化硫、亚硫酸钠、亚硫酸氢钠和亚硫酸氢钾以及偏亚硫酸氢盐)被添加到许多食品中,以防止酶促褐变和非酶促褐变,并作为抗氧化剂或还原剂。亚硫酸盐通过与碳酰基中间体反应来抑制非酶促褐变,由此防止其进一步反应而形成褐色素。通常与抗坏血酸或亚硫酸氢钠结合使用的柠檬酸作为酶促褐变的化学抑制剂已有很长时间。在不希望褐变的用途中,亚硫酸氢钾的优选浓度最高达2%,它也可以与最高达2%的抗坏血酸结合。事实证明,柠檬酸在高于1%的水平时并无益处。
乳化剂
乳化剂优选是食品级乳化剂,并有助于保持脂类和亲水性组分均匀分散在组合物中。通常,根据HLB(亲水亲油平衡值)值进行选择。优选的乳化剂选自HLB值为2~10的食品级乳化剂,这类乳化剂包括单硬脂酸丙二醇酯、单油酸甘油酯、三油酸甘油酯、单硬脂酸甘油酯、乙酰化单酸甘油酯(硬脂酸酯)、单油酸失水山梨醇酯、单月桂酸丙二醇酯、失水山梨醇单硬脂酸酯、硬脂酰基-2-乳酸钙、单月桂酸甘油酯、失水山梨醇单棕榈酸酯、大豆卵磷脂、双乙酰化酒石酸甘油单酯、硬脂酰乳酸钠、失水山梨醇单月桂酸酯。硬脂酰乳酸钠和单硬脂酸甘油酯通常用在淀粉体系中。
表II-一些乳化剂的疏水/亲水平衡(HLB)值
乳化剂 HLB值
硬脂酰乳酸钠(SSL) 21.0
Polysorbate 80(失水山梨醇单油酸酯) 15.4
Polysorbate 60(失水山梨醇单硬脂酸酯) 14.4
蔗糖单硬脂酸酯 12.0
Polysorbate 65(失水山梨醇三硬脂酸酯) 10.5
双乙酰酒石酸甘油单酯(DATEM) 9.2
蔗糖二硬脂酸酯 8.9
三聚甘油单硬脂酸酯 7.2
失水山梨醇单硬脂酸酯 5.9
琥珀酸单甘油酯(SMG) 5.3
单硬脂酸甘油酯(GMS) 3.7
丙二醇单酯(PGME) 1.8
单硬脂酸甘油酯是亲脂性的非离子表面活性剂,它特别适用于这种用途,因为它在淀粉组合物中具有消泡作用和抗凝沉作用。添加量的范围为1%~1.5%的单硬脂酸甘油酯用作乳化剂,以稳定机械性能并提高混合物的均匀性。可以将0.25%至1.5%的硬脂酰乳酸钠添加到增塑剂体系中,以稳定机械性能并提高混合物的均匀性。硬脂酰乳酸盐(作为钠盐或钙盐)也通常用作面团增筋剂,并因此而作为抗凝沉剂。结合使用单硬脂酸甘油酯和硬脂酰乳酸钠导致性能较快稳定。HLB值遵循添加剂规则,并且对于适当的SSL和GMS的混合物而言,其值约为4至10。
水
添加水的目的是为了使淀粉“胶凝”(也称为解构或熔化)成聚合物凝胶结构。在最终产品中,水也可以像增塑剂一样发挥作用,因为它可以软化材料或减小模量。阻透材料的湿含量可以在水分活度或相对湿度(RH)低于30%或高于75%时改变。在许多阻透膜和阻透瓶用途中,阻透材料接触的局部RH可以达到最高90%的值。为了获得稳定的机械性能、层合性能和阻透性能,并且为了便于在所有温度下进行加工,非挥发性的增塑剂 是优选的。因此,在混料阶段的期间或之后,和/或在后续注射成型或成膜的进料阶段,可以干燥掉一部分或全部水分。这可以通过对挤出机机筒进行排气和/或对粒料在生产线上进行干燥(on-line drying)来实现。应当使用湿润剂适当地结合任何残余的水分,以避免在加工期间形成泡沫,或避免在使用中机械性能发生显著改变。未经增塑的制剂的挤出加工可以具有低至10%的游离水浓度,可以在注射成型之前将含有多元醇类增塑剂的制剂干燥至0%游离水。优选的游离湿含量是,根据脱湿实验测定,该制剂在最终产品所应用的RH范围内的平衡湿含量。这依赖于制剂的具体组成,但是在0%~3%的范围内。
附图说明
图1:本发明的所选制剂与瓶级PET和膜级PP相比较的粘度的剪切速率依赖性;
图2:本发明的阻透材料与EVOH和MXD6相比较的氧气渗透率的相对湿度依赖性;
图3:本发明的阻透材料与专利公开WO 90/14938的淀粉膜相比较的氧气渗透率的相对湿度依赖性;
图4:本发明的阻透材料与EVOH和MXD6相比较的二氧化碳渗透率的相对湿度依赖性。
具体实施方式
本发明的阻透材料(用于薄膜或用于共注射成型)优选由表1所示的配方的淀粉聚合物组合物形成。
表1-以干重计的优选组成,可以包含0%~3%的水分
羟丙基化高 直链淀粉 | 山梨醇 | PVOH | 其它增塑剂 | 硬脂酸 | GMS | 硬脂酰 乳酸钠 |
48.3% | 27.4% | 9.6% | 12.8% | 0.6% | 1% | 0.25% |
实施例1
一种制剂,其组成为48.3%的羟丙基化高直链玉米淀粉、27.4%的山 梨醇、9.6%的聚乙烯醇、7.7%的麦芽糖醇、5.1%的丙三醇、1%的GMS、0.6%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例2
一种制剂,其组成为64.1%的羟丙基化高直链玉米淀粉、12.8%的聚乙烯醇、11.7%的山梨醇、5%的丙三醇、3.3%的麦芽糖醇、1%的GMS、0.8%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例3
一种制剂,其组成为52.0%的羟丙基化高直链玉米淀粉、35.1%的丙三醇、11.0%的聚乙烯醇、1%的GMS、0.7%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例4
一种制剂,其组成为53.0%的羟丙基化高直链玉米淀粉、34%的木糖醇、11.2%的聚乙烯醇、1%的GMS、0.7%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例5
一种制剂,其组成为52.0%的羟丙基化高直链玉米淀粉、35.0%的山梨醇、11.0%的聚乙烯醇、1%的GMS、0.7%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例6
一种制剂,其组成为52.0%的羟丙基化高直链玉米淀粉、35.0%的赤藻糖醇、11.0%的聚乙烯醇、1%的GMS、0.7%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例7
一种制剂,其组成为51.9%的羟丙基化高直链玉米淀粉、20.2%的丙三醇、10.8%的聚乙烯醇、10.1%的麦芽糖醇、5.0%的山梨醇、1%的GMS、0.7%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例8
一种制剂,其组成为53.3%的羟丙基化高直链玉米淀粉、18.4%的丙三醇、12.5%的聚乙烯醇、8.1%的麦芽糖醇、5.4%的山梨醇、1.1%的GMS、 0.8%的硬脂酸和0.3%的硬脂酰乳酸钠。
实施例9
一种制剂,其组成为54.9%的羟丙基化高直链玉米淀粉、18.7%的丙三醇、10.0%的聚乙烯醇、8.3%的麦芽糖醇、5.5%的山梨醇、0.9%的GMS、0.5%的硬脂酸和0.23%的硬脂酰乳酸钠。
实施例10
一种制剂,其组成为66.5%的羟丙基化高直链玉米淀粉、13.1%的丙三醇、7.6%的聚乙烯醇、5.8%的麦芽糖醇、3.9%的山梨醇、1.7%的GMS、1.1%的PEO和0.5%的硬脂酸。
实施例11
一种制剂,其组成为66.5%的羟丙基化高直链玉米淀粉、11.0%的丙三醇、7.6%的聚乙烯醇、9.2%的山梨醇、2.6%的麦芽糖醇、1.7%的GMS、1.1%的PEO和0.5%的硬脂酸。
实施例12
一种制剂,其组成为50%的羟丙基化高直链玉米淀粉、20%的丙三醇、10.3%的聚乙烯醇、10%的麦芽糖醇、5%的山梨醇、1%的GMS、0.26%的硬脂酰乳酸钠、1.1%的亚硫酸氢钾、1.1%的抗坏血酸、0.7%的硬脂酸和0.5%的柠檬酸。
实施例13
一种制剂,其组成为47.2%的羟丙基化高直链玉米淀粉、20%的丙三醇、10%的聚乙烯醇、10%的麦芽糖醇、5%的山梨醇、5%的柠檬酸、0.9%的GMS、0.23%的硬脂酰乳酸钠、1%的亚硫酸氢钾、0.1%的抗坏血酸和0.6%的硬脂酸。
实施例14
一种制剂,其组成为50.9%的羟丙基化高直链玉米淀粉、20.5%的丙三醇、10.8%的聚乙烯醇、10.3%的麦芽糖醇、5.1%的山梨醇、1%的GMS、0.7%的硬脂酸、0.5%的柠檬酸、0.24%的硬脂酰乳酸钠、0.1%的抗坏血酸和0.01%的亚硫酸氢钾。
实施例15
一种制剂,其组成为47.2%的羟丙基化高直链玉米淀粉、20.2%的丙三醇、9.7%的聚乙烯醇、10.1%的麦芽糖醇、5%的山梨醇、4.96%的柠檬酸、1%的抗坏血酸、0.9%的GMS、0.6%的硬脂酸、0.22%的硬脂酰乳酸钠和0.01%的亚硫酸氢钾。
阻透性能
表2
本发明的所选制剂在20℃~25℃时的氧气渗透率与市售聚合物和阻透材料的文献数据的比较
材料等级名称 | RH(%) | 渗透率(cm3 mm/m2 day atm) 平均(stdev) | 来源 |
PET | 0%~90% | 1.2~2.4 | [1] |
PET | 0% | 2.2~3.8 | [2] |
PP | 0~100% | 53~100 | [1] |
PP | 0~100% | 58~99 | [2] |
EVOH Eval-E | 0% | 0.02 | [1] |
EVOH Eval-E | 100% | 0.477 | [1] |
EVOH Eval-F | 0% | 0.01 | [1] |
EVOH Eval-F | 100% | 0.776 | [1] |
EVOH Eval-L | 0% | 0.0024~0.005 | [1] |
EVOH Eval-L | 100% | 1.036 | [1] |
尼龙MXD6 | 0% | 0.06~0.07 | [1] |
尼龙MXD6 | 90% | 0.32 | [1] |
尼龙MXD6 | 100% | 1.055 | [1] |
WO 90/14938配方1-4 | 11% | 0.657 | [3] |
WO 90/14938配方1-4 | 52% | 1.96~7.22 | [3] |
WO 90/14938配方1-4 | 75% | 131~460 | [3] |
本发明 | 30%~35% | 0.013~0.042 | [4] |
本发明 | 50% | 0.0085~0.039 | [4] |
本发明 | 60% | 0.037~0.079 | [4] |
本发明 | 85% | 0.0273(0.0044) | [4] |
“Permeability and other film propperties of plastics and elastomers(塑料和弹性体的渗透性及其他膜性质),”Plastics Design Library,1995
“Plastics Packaging(塑料包装)”,Hernandez Selke and Culter编,Hanser Verlag
WO 90/14938(以ml(STP)cm×1010/cm2s cmHg报道的渗透率)
由Independent Laboratories实施的Mocon Ox-Tran 2/21试验
本发明所选制剂的氧气渗透率列于表2中,与普通包装材料和用于包装用途的阻透材料进行比较。
在图2中示出了本发明所选制剂的相对湿度依赖性。本发明的制剂与EVOH等效,而在高湿度下优于EVOH和MXD6。这特别适用于饮料用途,饮料瓶壁以内的局部湿度约为80%~90%。
对本发明的阻透性能有贡献的主要成分是淀粉和PVOH,所述淀粉尤其是化学改性的高直链淀粉。多元醇增塑剂也对阻透性能有贡献。
表2和表3显示,本发明的制剂显著优于在WO 90/14938中描述的高直链淀粉膜所获得的阻氧性。各组分以及在挤出加工中可能由这些组分形成的任何复合物的协同作用可能有助于显著提高本发明的聚合物材料的阻氧性。
表3
本发明的所选制剂在20℃~25℃时的二氧化碳渗透率与市售聚合物和阻透材料的文献数据的比较
材料等级名称 | RH(%) | 渗透率(cm3 mm/m2 day atm) 平均(stdev) | 来源 |
PET | 0% | 4.7~9.8 | [1] |
PET | 8~20 | [2] | |
PP | 0% | 208 | [1] |
PP | 213 | [2] | |
EVOH Eval-E | 0% | 0.251 | [1] |
EVOH Eval-E | 90% | 0.886 | [1] |
EVOH Eval-E | 100% | 3.117 | [1] |
EVOH Eval-F | 0% | 0.026 | [1] |
EVOH Eval-F | 90% | 1.432 | [1] |
EVOH Eval-F | 100% | 8.230 | [1] |
尼龙MXD6 | 0% | 0.61 | [3] |
本发明 | 35% | 0.297(0.054) | [4] |
本发明 | 50% | 0.134(0.047) | [4] |
本发明 | 85% | 0.547(0.119) | [4] |
本发明 | 90% | 0.823(0.194) | [4] |
“Permeability and other film properties of plastics and elastomers,”Plastics Design Library,1995
“Plastics Packaging”,Hernandez Selke and Culter编,Hanser Verlag
Hu等,Polymer 46(2005)2685-2698
由Independent Laboratories实施的Mocon Oxtran试验
表3示出了本发明的制剂的二氧化碳阻透性,图4示出了该性能的湿度依赖性。该阻透性能等效于在商业包装用途中通常使用的EVOH等级。
光学性质
本发明的阻透层是透明的,并且理想地适用于可看到产品的多层包装物品中。
对250微米的片材测量本发明的阻透材料的光学性质,结果是:8%~10%的混浊度(ASTM D1003-00),85%~95%的透光率(ASTMD1746-92),和84.7%的60°镜面光泽(ASTM D2457-97)。因为所测的膜的厚度是所用阻透层厚度的10倍,所以,对于在PET软饮料瓶中的20~40微米厚度的阻透层,这种阻透材料获得了所需的光学性质,即透光率高于90%,混浊度低于3%,以及由lab b*读数表征的黄变小于2。层厚度为15微米的EVOH-F具有1.5%的混浊度,12~14微米的PET具有2.5%~3.9%的混浊度。20~22微米的PP具有2.2%~3.5%的混浊度。
制备方法
使用同向或异向旋转双螺杆挤出机或选定设计的单螺杆挤出机,通过挤出混炼来制备所述材料。优选的加工方法是双螺杆同向旋转混炼,所用的挤出压力至少为10巴(Bar),并且螺杆转速至少为100转/分钟(RPM)。可以根据其它增塑剂的含量和性质在该过程中添加水(通过与增塑剂一同进行液体注射)。对于挤出线材,可以通过对流干燥、接触加热、红外线(IR)加热或微波干燥来脱水,对于粒料,可以通过离心分离及流化床来脱水,或者可以通过机筒排气或者这些方法的组合而将水分去除。可以通过水中造粒、模面切割或线材冷却及切割来获得粒料。
单层或多层转化过程中的加工性
多层用途中的流变学相容性
在图1中示出了本发明的几种制剂与薄膜级聚丙烯和瓶级PET在其 各自的处理温度下相比较的粘度对剪切速率的依赖性。可以通过改变增塑剂的类型和含量而调整粘度曲线,从而实现与共挤出工艺中的其它聚合物的相容性。实施例10和11的粘度曲线之间的差异说明了这一点。这两个实施例的粘度曲线很不相同,尽管其配方的差别仅是山梨醇和麦芽糖醇的比例。此外,如图1所示,实施例10在130℃的机筒温度与200℃的机筒温度相比,不同的机筒温度将有助于粘度调节。实施例11的粘度曲线与PP的粘度曲线尤其相容,从而使其适合于使用进料块的膜共挤出。
与PET的共注射拉伸吹塑成型
热稳定性
通过DSC研究干燥制剂的耐热性,并且采用对流烘箱实验评价制剂的起泡性和/或褐变。表4示出了本发明的一系列制剂的观测到的热稳定性。研究发现,具有较高含量的山梨醇或木糖醇的制剂的热稳定性最高,其次是具有高含量的丙三醇的制剂。具有高含量的麦芽糖醇的制剂的热稳定性较差。同时添加亚硫酸氢钾和抗坏血酸可显著抑制热降解,然而添加柠檬酸和抗坏血酸甚至在室温条件下都会导致随时间而发生褐变。在亚硫酸氢钾存在时,与不含有柠檬酸和亚硫酸氢钾的制剂相比,柠檬酸在较低的温度下都会导致褐变,但与抗坏血酸存在时相比,其褐变较慢或较不严重。对于这些未干燥的制剂而言,使用保湿增塑剂有助于抑制水分蒸发。因此,甚至在PET共注射成型中使用较高喷嘴温度的情况下,用保湿增塑剂增塑的部分干燥的制剂也不会发生任何起泡现象。
表4
制剂 | 降解温度 DSC[1](℃) | 降解温度 DSC[2](℃) | 褐变温度 (℃)[3] | 起泡 200℃[4] |
实施例7 | 245~295 | 270~310 | 170 | 有 |
实施例4 | 275~325 | 300~340 | 180 | 很少 |
实施例5 | 280~305 | 300~350 | 185 | 没有 |
实施例3 | 280 | 180 | 很少 | |
实施例8 | 270 | |||
实施例12 | 290 | 185 | 有 |
带有中间冷却器的TA Instruments Q100(-70℃~400℃的温度范围),由QAdvantage v 2.1.0.240(Release 4.1.0)软件进行控制。后处理使用Universal Analysis2000v 4.2E Build 4.2.0.38。升温速率20℃/分钟。
Perkin-Elmer DSC-7(以10℃/分钟从50℃加热到350℃)。
短时间(升温1分钟,保持20秒)暴露于对流的热和空气,处于Perkin ElmerHB43湿度平衡;未干燥的制剂。
长时间暴露于对流的热和空气,处于Perkin Elmer HB43湿度平衡。
共注射
可以使用热或冷流道系统,通过传统的螺杆传动或注射传动方法将材料进行注射成型。本发明的制剂被设计为与PET相容,用于在高温下进行共注射成型。在Husky IN-90预成型机(preform index machine)上使用99吨的夹紧力将本发明的一系列制剂成功地共注成型,该机器具有可制造28g预型体的4-腔模具。螺杆“A”是标准的45mm RS PET螺杆;螺杆“B”是18mm RS螺杆,并带有截流式喷嘴,用于本发明的阻透材料。预型体模具的冷半模为标准设计。热半模是特殊设计。两种材料在分开的支管中进行传送,并在喷嘴处合并,从而形成环形流动模式。对各个支管进行单独的温度控制,保持其隔热良好。喷嘴是支管系统中两种物流必定处于相同的温度的唯一部件。为了适应PET的要求,该温度通常约为250℃~280℃。根据需要在常规工业除湿干燥机中将材料进行干燥。与PET一起进行共注射时,具有高含量的山梨醇、低含量的麦芽糖醇或者具有亚硫酸氢钾的制剂具有足够的热稳定性。表5示出了用于实施例1、7、8和9的共注射工艺的典型加工条件。
表5-用于0.5L瓶的典型28g预型体的处理条件
吹塑制瓶
可以在传统的拉伸吹塑成型生产线上将本发明的制剂容易地吹成瓶 子。在具有红外加热灯和机械拉伸杆的市售PET拉伸吹塑成型机上,将具有由实施例1和实施例9制备的阻透层的预型体吹成瓶子。预型体的温度处于100℃至120℃的范围,并且使用35巴至45巴的吹塑成型压力。产出速率为每个模腔每小时1000个瓶子。
粘合
研究发现,与PET的粘附优异,且显著优于MXD6和EVOH,原因是表面张力大于50达因/厘米的这种阻透材料具有极性,并且不存在涉及结晶的收缩。
机械性能
阻透层通常大约占多层结构的总层厚的5%~20%。因此其机械性能对最终产品的机械性能有一定贡献。当阻透材料的机械性能较差时,需要通过稍微增加容器的壁厚来进行一定补偿,但增加的厚度不需要大于阻透层厚度,因此至多增加10%,利用其在低于传统阻透材料的成本的条件下具有优异的阻透性能的优势来进行补偿。伸长性能也是很重要的,在吹塑制瓶加工中,轴向伸长率约为1.5倍至3.5倍,并且环向伸长率约为3.5倍至5倍。这种伸长在加热状态下发生,并且阻透层由基材支撑。
在表6中,将该阻透材料的机械性能与用于注射拉伸吹塑成型的市售材料作了对比。
表6
性能 | ASTM | 本发明 | PET | PLA | MXD6 |
弹性模量(MPa) | D638 | 20~450 | 3400~3800 | 3000~3400 | 3500~4700 |
拉伸强度(MPa) | D638 | 7~30 | 160~190 | 90~120 | 220 |
断裂伸长率(%) | D638 | 30~340 | 100~120 | 150~170 | 2~3 |
流延膜挤出
最后,这种阻透材料还可以用作单层产品,其上可以根据需要进行印刷和涂饰。所产生的膜可以是用于糖果包装纸或小袋的薄膜,或是用于热成型用途的厚膜,因为这种材料还理想地适用于热成型加工。
本发明的制剂适用于薄膜的挤出流延。本领域的技术人员将能够选择合适的增塑剂含量,以获得所需的熔体强度和用于所需用途的机械强度。 使用90mm的单螺杆挤出机,以90℃~200℃的机筒温度范围,以70kg/h~200kg/h的生产速率通过1050mm宽的膜形口模,从而将本发明所选的制剂流延成单层薄膜。在辊速范围为10米/分钟~50米/分钟的情况下,使用约10~30的拉伸比(haul off ratio),以导致从一定程度的单轴取向性到强的单轴取向性。
在表7中列出了这种材料的单层薄膜的机械性能。
表7:本发明的30微米的薄膜的机械性能
在本发明中使用的优选的组合物可以冷密封,也可以热密封。
双轴取向的薄膜挤出
可以将这种阻透材料共挤出为层合体,或者在单独的层合步骤中将其与传统的膜聚合物(例如双轴取向的PP)组合。其它的材料可以是任何合适的包装用聚合物,例如聚丙烯(PP)、聚乙烯(PE)或低密度聚乙烯(LDPE),或者是可生物降解的聚合物,例如聚乳酸(PLA)或其它聚酯。如果认为需要额外的粘结层和保护性涂层,则本发明的阻透材料优选作为三层层合体或五至七层的产品的中间层。
此外,如果仅在一个面上要求具有耐水性,或者如果所包装的产品不要求具有水蒸汽阻透性的话,它也可以是两层式包装的内层或外层。
本领域的技术人员能够通过选择适合的增塑剂含量来获得所需的粘度相容性,以便于实现所希望的聚合物组合。在大多数情况下,进料块足以实现各种材料层的控制,在另外一些情况下,多支管口模可能更为合适。
多层相容性
它与诸如PET之类的极性材料的粘附性是优异的,然而对于与诸如 BO-PP等非极性材料的粘附性,则需要普通粘结层树脂。合适的粘结层材料包括基于PP、EVA、LDPE或LLDPE的接枝聚合物。对于与PP的粘合,来自Atofina的Orevac PPC适合于透明用途,而Orevac 18729或18910适合于不透明的用途。其它合适的粘结层包括EVA共聚物、丙烯酸共聚物及三元共聚物、离聚物、茂金属PE、乙烯-丙烯酸酯三元共聚物以及乙烯-乙酸乙烯酯三元共聚物。对于本发明的干燥制剂来说,酸酐改性的聚合物也是合适的。阻透材料本身具有抗静电性,并可以使用任何常规的印刷技术对其进行印刷或涂饰。通过胶带剥离试验发现,对于溶剂型油墨而言,它与油墨和涂料的粘附性优异。抗撕裂传播性(ASTM D 1938)为200~400Nm,并且动摩擦系数(ASTM D 1434)为0.1~0.3。
吹塑成膜
基本上按照以上用于多层双轴取向薄膜挤出的原则,可以将这种阻透材料共挤出为吹塑膜,如果需要的话,可以遵照类似的粘结层原则。
在阻透材料之中,本发明的配方的独特之处在于,它以显著较低的成本提供了比最常用的材料(例如MXD6)更好的阻透性能,从层的厚度和组合物的价格来看,本发明可以节约成本。
这种阻透材料的组分的性质确保它们比油性聚合物具有价格稳定性,并且比MXD6更具价格竞争力,因为用MXD6价格的80%就可以廉价地获得这些组分。
此外,它的水溶性为与这种阻透材料相组合的基质材料提供了优异的再生性。如果将这种材料用作单层结构的阻透包装,它还是可做成堆肥和可生物降解的,并且在环境温度下将崩解及生物降解为垃圾。这些独特的性质归因于该配方中各化合物的组合。
本领域的技术人员应当认识到,在不脱离本发明的基本思想的情况下,可以用多种方式来实施本发明。
Claims (12)
1.一种成膜性阻透聚合物,所述成膜性阻透聚合物具有以干重计的如下组成的组合物:
a)以重量计45%至90%的淀粉和/或改性淀粉,所述改性淀粉选自通过与羟烷基、乙酸盐或二羧酸酐或接枝聚合物反应而改性的淀粉;
b)以重量计4%至12%的水溶性聚合物,所述水溶性聚合物选自聚乙烯醇、聚乙酸乙烯酯以及乙烯与乙烯醇的共聚物,所述水溶性共聚物的熔点与所述淀粉组分的熔融状态相容;
c)以重量计5%至45%的非结晶性混合物,所述混合物由山梨醇与至少一种其它增塑剂组成,所述增塑剂选自丙三醇、麦芽糖醇、木糖醇、甘露醇、三油酸甘油酯、环氧化亚麻子油或环氧化大豆油、柠檬酸三丁酯、乙酰柠檬酸三乙酯、三乙酸甘油酯、2,2,4-三甲基-1,3-戊二醇二异丁酸酯、聚环氧乙烷或聚乙二醇;
d)以重量计0.3%至2.5%的C12-22脂肪酸或其盐;和
e)以重量计0.25%至3%的乳化剂体系,所述乳化剂体系具有2~10的亲水亲油平衡值。
2.如权利要求1所述的成膜性阻透聚合物,其中,组分b)为聚乙烯醇。
3.如权利要求1所述的成膜性阻透聚合物,所述成膜性阻透聚合物还包含热稳定剂,以防止酶促褐变和非酶促褐变。
4.如权利要求1所述的成膜性阻透聚合物,所述成膜性阻透聚合物还包含作为水结合剂或胶凝剂的氯化钠、氢氧化钠、钾盐、氧化钙或碘化钠。
5.如权利要求1所述的成膜性阻透聚合物,所述成膜性阻透聚合物还包含以重量计0%至20%的可用作增塑剂或共增塑剂的湿润剂或水结合剂或胶凝剂。
6.如权利要求5所述的成膜性阻透聚合物,所述湿润剂或水结合剂或胶凝剂为角叉胶、黄原胶、阿拉伯树胶、瓜尔胶或白明胶。
7.如权利要求1所述的成膜性阻透聚合物,在相对湿度至高为60%RH时,所述成膜性阻透聚合物的氧渗透系数小于0.1厘米3·毫米/米2·天·大气压,并且,在相对湿度至高为90%RH时,所述成膜性阻透聚合物的氧渗透系数小于0.7厘米3·毫米/米2·天·大气压。
8.如权利要求1所述的成膜性阻透聚合物,在相对湿度至高为60%RH时,所述成膜性阻透聚合物的二氧化碳渗透系数小于0.5厘米3·毫米/米2·天·大气压,并且,在相对湿度至高为90%RH时,所述成膜性阻透聚合物的二氧化碳渗透系数小于0.9厘米3·毫米/米2·天·大气压。
9.一种共注射成型的层合体,所述共注射成型的层合体由聚对苯二甲酸乙二醇酯或聚乳酸与权利要求1所述的成膜性阻透聚合物形成。
10.一种预型体,所述预型体是权利要求9所述的共注射成型的层合体,所述预型体用于吹塑成型为饮料瓶。
11.一种共挤出层合体,所述共挤出层合体由聚乙烯、聚丙烯或聚乳酸与权利要求1所述的成膜性阻透聚合物形成。
12.如权利要求11所述的共挤出层合体,所述共挤出层合体用于薄膜包装用途。
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- 2005-10-18 CN CN2005800356104A patent/CN101360783B/zh active Active
- 2005-10-18 JP JP2007537065A patent/JP2008517108A/ja not_active Withdrawn
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WO2006042364A1 (en) | 2006-04-27 |
CA2583945A1 (en) | 2006-04-27 |
US20090110942A1 (en) | 2009-04-30 |
CN101360783A (zh) | 2009-02-04 |
EP1802698A4 (en) | 2011-08-03 |
JP2008517108A (ja) | 2008-05-22 |
ATE555160T1 (de) | 2012-05-15 |
IL182416A0 (en) | 2007-07-24 |
JP2015042745A (ja) | 2015-03-05 |
US7854994B2 (en) | 2010-12-21 |
NZ554682A (en) | 2010-04-30 |
EP1802698B1 (en) | 2012-04-25 |
EP1802698A1 (en) | 2007-07-04 |
ES2388041T3 (es) | 2012-10-05 |
JP6066970B2 (ja) | 2017-01-25 |
KR20070088638A (ko) | 2007-08-29 |
IL182416A (en) | 2013-03-24 |
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