CN1950202A - 包含液体吸收剂内层、抗微生物材料和不渗透外层的膜 - Google Patents
包含液体吸收剂内层、抗微生物材料和不渗透外层的膜 Download PDFInfo
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- CN1950202A CN1950202A CNA2005800149208A CN200580014920A CN1950202A CN 1950202 A CN1950202 A CN 1950202A CN A2005800149208 A CNA2005800149208 A CN A2005800149208A CN 200580014920 A CN200580014920 A CN 200580014920A CN 1950202 A CN1950202 A CN 1950202A
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- food
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Abstract
提供包含吸收了抗微生物材料的液体吸收层和不渗透层的膜。该膜能适用于制造管状套和收缩袋,如食品的套管。还公开了在包含抗微生物材料的管状套内加工的食品。
Description
技术领域
本发明涉及能用于包装和/或封装食品的膜,例如,能用来在膜内加进抗微生物添加剂以制成用来容纳食品的套管、热成型小口袋和收缩袋的膜。
背景技术
随近些年食物传染病原体对鲜肉和即食肉污染的数起普遍爆发,肉类产品的食物安全性已成为人们越来越关注的话题。在1999年的调研中,美国疾病控制中心估计,在美国每年食物传染病造成约7,600万人生病,325,000人住院和5,000人死亡。1999年FDA在文献综述中指出,每年为动物产品中7种病原体所造成的食物传染病花费65亿~350亿美元。许多国家的报导***已有资料证明,在1975至1998年,因污染、微生物存活和微生物生长所造成的食物传染病的发病率大幅度上升。
在加工即食肉和家禽食品如熟肉、香肠和热狗的情况下,烹煮和其它加工(熟成、发酵、干燥等)后,可能因进一步处理、去皮、切片和再包装等而发生再污染。其中特别令人关注的是单增李斯特氏菌的控制,这是一种耐高温、耐盐且能在冷冻条件下繁殖的病原体。其它病原体包括沙门菌、大肠杆菌和金黄色葡萄球菌。
食品工业已多方采取了措施:辐照、巴氏杀菌、高压处理和使用抗微生物剂。见,例如,US6451365B1、US5573797、US6,172,040B1、US专利申请2004/0043922A1和US专利申请2003/009 1612。一般地说,如果膜表面不经化学处理或电晕处理,是难以在膜上有效地涂布抗微生物组合物的。纤维素膜能吸收最多35重量%的水,这是一项对传递抗微生物材料有用的性能,因为大多数对食品有意义的抗微生物体系都用含水介质涂布。虽然这类膜或套管可在其表面上吸收抗微生物溶液,但它们没有足够的阻隔性,也不能热封成食品袋。因此必须在某些点上取出食品,放进其它塑料阻隔包装,后者虽然对氧和气体有阻隔作用,却无抗微生物保护作用。
本发明要提供多层塑料包装膜的应用,所述膜有一层能把抗微生物材料传递给封装食品的吸水性聚合物内层。这种膜可以把保护作用传递过销售链的多个阶段直至零售水平;该多层包装的其它层具有包装膜的理想特性(阻隔性、耐滥用性、可成形性等)。这种膜也可以用来煮肉然后带袋运输。这种膜可用来包装加工过的和新鲜的肉和产品(如蜡肉,案例准备肉、酮体肉,附加价值肉,鱼或产品)。
发明内容
本发明包括一种膜,包含(i)内层;(ii)至少一种抗微生物材料;和(iii)外阻隔层;其中所述内层可以是适用于把抗微生物材料赋予肉的液体吸收性层;该吸收性内层能吸进溶液;以及所述外层可以是不渗透阻隔层;内层可包含或由包括嵌段共聚醚酯聚合物、嵌段共聚醚酰胺聚合物或其组合的聚合物产生;外层可以是单层膜,或包含或由至少一层聚合物层和任选地至少一层连接层产生的层合膜或多层膜;以及所述聚合物层包含或由包括聚酰胺、乙烯/乙烯醇共聚物、聚偏氨乙烯、聚烯烃或其中两种或多种组合的聚合物产生。
本发明还包括包含膜的管状套或收缩袋或热成型小口袋,所述膜包含或由以上公开的膜形成,其中内层能把抗微生物材料均匀地赋予肉。
本发明还包括能用来加工食品的方法,该方法包含下列步骤:制膜,膜可以是以上所公开的;让该膜与包含至少一种抗微生物剂的溶液接触以产生抗微生物膜;任选地,洗涤该抗微生物膜;让该抗微生物膜与食品接触,以产生与抗微生物膜接触的食品;以及任选地,加热该食品。
本发明还包括用该膜以抗微生物材料或试剂处理的食品。
具体实施方式
内层可以是除阻隔外层以外的任何层。例如,内层可以是最内层(能与放在套管内的食品直接接触的层)或吸收性内层(位于最内层与阻隔外层之间的任何层)。外层是离食品最远的层。
吸收层内所用的聚合物可以是亲水性或吸湿性的。共聚醚酯(PEPE)可以是热塑性聚合物且其粘度范围,按标准方法ISO 11443测定,可以为约20Pa·s~约3000Pa·s,约40Pa·s~约1000Pa·s,或约50Pa·s~约700Pa·s。
PEPE的熔点可高于120℃或在约120℃~约220℃范围内,如用差示扫描量热法(DSC)按标准ISO化3146测量。
共聚醚酯已描述在US专利4,725,481中。优选PEPE含许多通过头-尾酯键无规连接起来的重复长链酯单元和短链酯单元。
重复长链酯单元可以用式(I)([A-O-G-OC(O)-R-C(O)-A])表示,以及重复短链酯单元可以是式(II)([A-O-D-OC(O)-R-C(O)-A]),其中“A”代表共聚醚酯聚合物中尚未规定的部分;G是分子量为约400~约3500,优选约1000~约2500的聚醚二醇除去端羟基后剩下的二价基团;R是分子量小于约300的二羧酸除去两个羧酸基后剩下的二价基团;以及D是分子量小于约250的二元醇除去羟基后剩下的二价基团。短链酯单元(II)可以是由二元醇和二羧酸之间的酯化反应所获得的反应产物。
酯单元,如果不是末端酯单元,两端都能与长链酯单元键接,或两端都与短链酯单元键接,或一端键接长链酯单元而另一端键接短链酯单元;如果酯单元是末端单元,则式I或式II中的未规定部分之一是长链酯单元或短链酯单元以外的取代基。术语“末端(酯单元)”是指具有聚合物领域内传统意义的酯单元,即是指在聚合物链的末端的酯单元。
PEPE的湿气透过速率可以至少为约1200(或约1200~约20000)g·25μm/m2·24h,如按ASTM D6701-01所测定。
用来制备共聚醚酯的聚亚烷基醚二醇可以是聚亚丙基醚二醇和/或聚亚乙基醚二醇。PEPE中可加入环氧乙烷基。长链二醇(即分子量大于400的二醇)可以包括足够多的环氧乙烷,以使共聚酯醚含有相对于共聚酯醚总重量约5~约68重量%,15~约68重量%,或约20~约55重量%的环氧乙烷单元。加进共聚醚酯中的环氧乙烷基团描述的是长链酯单元中的(-CH2-CH2-O-)基在共聚醚酯总重量中的重量%。
用来计算聚合物中环氧乙烷基含量的PEPE中的环氧乙烷基是衍生自聚亚烷基醚二醇的那些,而不是由低分子量二元醇引进共聚醚酯的环氧乙烷基。
长链二醇可包括聚环氧乙烷二醇、环氧乙烷封端的聚环氧丙烷二醇、聚环氧乙烷二醇与其它二醇如环氧乙烷封端的聚环氧丙烷二醇和/或聚四氢呋喃二醇的混合物,使PEPE含,例如,至少约5重量%环氧乙烷基。优选由分子量为约600~2500的聚环氧乙烷二醇制成的PEPE。特别优选的是由分子量为约2150的环氧乙烷封端的聚环氧丙烷二醇所制成的PEPE。
低分子量二醇可包括无环、脂环和芳族二醇,如含2~15个碳原子的二醇,包括,但不限于,乙二醇、丙二醇、异丁二醇、丁二醇、1,4-戊二醇、2,2-二甲基三亚甲基二醇和癸二醇、二羟基环己烷、环己烷二甲醇、间苯二酚、氢醌、1,5-二羟基萘、类似的二醇,和其中两种或多种的组合。优选的二醇可包括含2~8个碳原子的脂族二醇,如1,4-丁二醇。双酚包括双(对-羟基)联苯、双(对-羟基苯基)甲烷、双(对-羟基苯基)丙烷和其中两种或多种的组合。也可以用等代物二醇的酯-形成衍生物,包括环氧乙烷或碳酸亚乙酯。低分子量与二醇相关,而不与其衍生物相关。
二羧酸可以是脂族、环脂族或芳族二羧酸及其功能等代物,包括酯和酯-形成衍生物,如酰基卤和酸酐。公开的分子量与酸形式相关,而不与等代物酯或酯-形成衍生物相关。
脂族二羧酸是含有2个分别连接在饱和碳原子上的羧基的羧酸。如果与羧基相连的碳原于是饱和的而且是一个环,则这种酸是环脂酸。含共轭不饱和键的脂族或环脂族酸通常不能用,因为有均聚作用。某些不饱和酸如马来酸可以用。
芳族二羧酸是满足下列条件的羧酸:含有2个羧基,连接在碳环芳环结构的碳原子上,但这2个官能羧基并不都连接在同一芳环上(如果存在不止一个环),且能靠脂族或芳族二价基团或-O-或-SO2-之类的二价基连接。
二羧酸可包括癸二酸、1,3-环己烷二羧酸、1,4-环己烷二羧酸、己二酸、戊二酸、4-环己烷-1,2-二羧酸、2-乙基辛二酸、环戊烷二羧酸、十氢-1,5-萘二羧酸、4,4’-二环己基二羧酸、十氢2,6-萘二羧酸、4,4’-亚甲基双(环己基)羧酸、3,4-呋喃二羧酸、邻苯二甲酸、对苯二甲酸、间苯二甲酸、二苯甲酸、含2个苯核的取代二羧基化合物(例如,双(对-羧基苯基)甲烷)、对-氧-1,5-萘二羧酸、2,6-萘二羧酸、2,7-萘二羧酸、4,4’-磺酰基二苯甲酸,或它们的一个或多个C1-C12烷基或环取代基衍生物(例如,卤、烷氧基和芳基衍生物)。如果还存在芳族二羧酸,则也可以用羟基酸,如对-(β-羟基乙氧基)苯甲酸。在脂族酸中常用环己烷二羧酸和己二酸,在芳族酸中,常用含8~16个碳原子的那些,如对苯二甲酸本身或它与邻苯二甲酸和/或间苯二甲酸的混合物。
共聚醚酯可含约25重量%~约80重量%对应于上式(II)的短链酯单元,其余是对应于上式(I)的长链酯单元。希望不受理论的限制,(如果)PEPE含少于约25重量%的短链酯单元,则结晶速率会变慢,且PEPE处理起来会发粘,虽然还可用,另一方面,如果含约80%以上短链酯单元,则PEPE会变得太刚,虽然还可用。优选PEPE含约30~约60重量%,或约40~约60重量%短链酯单元,其余是长链酯单元。增加短链酯单元会提高拉伸强度和模量,但会减小水蒸汽渗透率。还优选至少约70%由上式(I)和式(II)中R所代表的基团是1,4-亚苯基,至少约70%由上式(II)中D所代表的基团是1,4-亚丁基,而不是1,4-亚苯基的R基与不是,1,4-亚丁基的D基之和不超过30%。如果用第二羧酸来制造PEPE,则选择间苯二甲酸;如果用第二低分子量二元醇,则1,4-丁二醇或己二醇是所选的二元醇。
可以用不同PEPE的共混物。
可以加入其它组分来优化反应过程或PEPE的性能。
嵌段PEPE及其制造法已公开在聚合物科学与工程百科全书,第12卷,76-177页(1985)(Encyclopedia of Polymer Science andEngineering,Volume 12,pages 76-177(1985))及其中所列的参考文献中。
适用嵌段共聚醚酯可包括源自公司的商品,例如,源自E.I.du Pontde Nemours and Company(杜邦)的商品Hytrel,源自Ticona的商品Ritenex,和源于DSM的商品Arnitel。
膜内的吸收层也可包含嵌段共聚醚酰胺。这类共聚醚酰胺可包含或由结晶聚酰胺和非结晶聚醚嵌段组成。聚酰胺可以是尼龙6或尼龙12。聚醚酰胺的商品系列是源自Atofina的商品“Pebax”。
不渗透外层
不渗透层可以是单层膜、包含至少一层包含聚酰胺、乙烯/乙烯醇共聚物;聚偏氯乙烯和聚烯烃之类聚合物膜的层合膜或多层膜。该层还任选地包含粘结剂层,宜用作层合外层内两层不相容层之间的连接层。粘结剂层(连接层)可包含酸酐改性的乙烯均聚物、酸酐-改性的乙烯共聚物和/或本领域技术人员所知的其它聚合物。
该层可以起不渗透阻隔结构的作用且包含数层聚合物,以提供对水份和氧的有效阻隔性以及适用于加工和/或包装食品的本体机械性能,如透明性、韧性和耐穿刺性。对于烟熏和/或烹煮工艺,收缩性可以是最需要的。多层阻隔结构的实例包括,自最外层至最内层:聚乙烯/连接层/聚酰胺;聚乙烯/连接层/聚酰胺/连接层/聚乙烯;聚丙烯/连接层/聚酰胺/EVOH/聚酰胺;聚酰胺/连接层/聚乙烯;聚酰胺/连接层/聚乙烯/连接层/聚酰胺;聚酰胺/连接层/聚酰胺/EVOH/聚酰胺。取决于不渗透结构最内层的性质,在不渗透结构与吸收层之间可***另一个内连接层以提供与吸收层的理想粘结性。
这里适用的聚酰胺包括脂族聚酰胺、无定形聚酰胺,或它们的组合。脂族聚酰胺可以指脂族聚酰胺、脂族共聚酰胺和诸如聚酰胺6、聚酰胺6.66和它们的共混物与混合物之类的共混物或混合物。聚酰胺6.66是源自BASF的商品“Ultramid C4”和“Ultramid C35”或源自UbeIndustries Ltd.的商品“Ube5033FXD27”。聚酰胺6是源自杜邦的商品Nylon 4.12。
脂族聚酰胺的粘度,用在96%H2SO4中浓度为0.5%的溶液按ISO307测定,可以在约140~约270cm3/g范围内。
该膜还可以包含其它聚酰胺,如US专利5,408,000;4,174,358;3,393,210;2,512,606;2,312,966和2,241,322所公开的那些。该膜还可以包含部分芳族聚酰胺。适用的部分芳族聚酰胺是式为[C(O)ArC(O)N(H)CH2CH2CH2CH2CH2CH2NH]n的无定形共聚酰胺6-I/6-T,其中Ar是亚芳基或亚苯基。有些部分芳族共聚酰胺是无定形尼龙树脂6-I/6-T,可以购自杜邦公司,商品名为SelarPA,或购自EMS-ChemieAG,商品名为GrivoryG21。
聚烯烃包括聚丙烯、聚乙烯的聚合物和共聚物。聚乙烯可以用很多方法制造,包括周知的Ziegler-Natta催化剂聚合(见,例如,US专利4,076,698和3,645,992)、茂金属催化剂聚合(见,例如,US专利5,198,401和5,405,922)以及自由基聚合。聚乙烯可包括线形聚乙烯,如高密度聚乙烯(HDPE)、线形低密度聚乙烯(LLDPE)、很低或超低密度聚乙烯(VLDPE或ULDPE),和支化聚乙烯,如低密度聚乙烯(LDPE)。适用于本发明的聚乙烯的密度在0.865g/cm3~0.970g/cm3范围内。在线形聚乙烯中可掺进α-烯烃共聚单体,如丁烯、己烯或辛烯,以便把密度降到该密度范围内。不渗透层可包含乙烯共聚物,如乙烯/乙烯酯、乙烯/丙烯酸烷基酯、乙烯/酸二聚物、乙烯/酸三聚物以及它们的离聚物。这类乙烯共聚物的实例是乙烯/醋酸乙烯酯、乙烯/丙烯酸甲酯和乙烯/(甲基)丙烯酸聚合物及它们的离聚物。适用于实施本发明的聚丙烯聚合物包括丙烯均聚物、冲击改性聚丙烯和丙烯与α-烯烃的共聚物以及它们的共混物。
含约20~约50mol%乙烯的聚乙烯/乙烯醇共聚物(“EVOH”)能适用,如源自Kuraray的商品Evalca或源自Nippon Goshei的商品Noltex。聚偏氯乙烯(PVDC)可获自Dow Chemicai,商品名为Saran。
在聚合物彼此间不能良好粘结时,可以用酸酐或酸-改性的乙烯和丙烯的均聚物和共聚物作为可挤出胶粘剂层(“连接”层),以增加聚合物层之间的结合力,从而提高多层结构中层与层之间的粘结性。连接层的组成可根据多层结构中所需粘结的相邻层的组成来确定。聚合物领域的技术人员能根据该结构中所用的其它材料来选择恰当的连接层。各种连接层组合物可购自杜邦公司,商品名为Bynel。
不渗透膜还可以包含一种或多种材料或试剂,如聚合物膜中常用的添加剂,包括增塑剂、稳定剂、抗氧剂、紫外线吸收剂、水解稳定剂、抗静电剂、染料或颜料、填料、阻燃剂、润滑剂、增强剂如玻璃纤维和箔、加工助剂、防粘连剂、脱模剂,和/或它们的混合物。
本文所公开的聚合物能由多种技术转换成层合膜。例如,可以用共挤出法获得多层膜如下:在挤出机内熔化各组分的粒料;使熔融聚合物通过一个或一系列口模,以形成熔融聚合物层,然后作为层流进行加工。可以使熔融聚合物冷却下来以形成层结构。共挤出聚合物膜还可以层合到一层或多层其它膜上,如取向聚酯或取向聚丙烯膜上。
适用的其它技术包括吹塑薄膜挤出、流延薄膜挤出、流延片材挤出和挤出涂装。本文所公开的不渗透阻隔膜可以是用吹塑薄膜挤出法获得的吹塑薄膜。
层合膜除立即淬火或膜的流延外还可以再进行取向。该方法可包含共挤出多层熔融聚合物的层流,淬火共挤出物并在至少一个方向上取向已良好淬火的共挤出物。“良好淬火”是指挤出物已基本冷却到其熔点以下,以便获得固体膜。
该膜可以进行单轴取向,或通过在膜平面内两个互相垂直方向上的拉伸进行双轴取向,以达到力学与物理性能的满意组合。
单轴或双轴拉伸薄膜的取向和拉伸设备是本领域周知的,且本领域内的技术人员可用它们来生产本发明的膜。这类设备和工艺的实例包括,例如,下列US专利中公开的那些:3,278,663;3,337,665;3,456,044;4,590,106;4,760,116;4,769,421;4,797,235和4,886,634。
在优选实施方案中,层合膜用双膜泡挤出法进行取向,这时可同时双轴取向如下:挤出第一管,接着淬火,再加热之,然后靠内压使之膨胀以引进横向取向,同时靠速度不同的夹辊或输运辊以能引进纵向取向的速率拉伸。
获得取向吹塑薄膜的方法在本领域内称为双膜泡技术,且可以如US 3,456,044所公开的那样进行。例如,从环状口模中熔体挤出第一管。迅速冷却该挤出的第一管,以尽量减少结晶。然后把它加热到其取向温度(如用水浴)。在薄膜制造单元的取向区内,通过吹胀形成第二管,使膜在横向上径向膨胀并在机器方向上受拉,从而在两个方向上发生膨胀,可能是同时进行的;管在膨胀的同时会在受拉点发生厚度的突然锐减。然后使管状膜通过夹辊再变平。该膜可以再次吹胀并通过退火步骤(热定型),在该步骤期间,膜被再次加热以调节收缩性能。为制成食品套管(如香肠套管、收缩口袋)最好使膜保持管状。为制造平膜,可以沿管的长度方向裁开并摊成平片,平片可卷起来和/或进一步加工。
在另一个实施方案中,可以把膜制成口袋,如真空袋、收缩袋和小口袋。这类口袋可以从管状膜形成如下:密封然后横向切割该膜。或者,也可以把管状膜剖成平膜,然后上、下横向密封,以形成口袋。或者不论用管状膜或流延膜生产的平膜都可以制成口袋如下:折叠该膜,然后密封并沿两个暴露长度切开。制造大、小口袋的其它方法是周知的且都可采用。
抗微生物剂
膜、管状套、收缩袋等要进一步处理如下:在套管吸收层内吸附至少一种溶液中的抗微生物剂。然后通过让食品与膜表面接触和在,例如,加热、熟成、烟熏或烹煮之类的食品加工期间,把抗微生物材料基本转移到食品上。抗微生物组合物保持与食品接触直到食品被取用,因为本文所公开的层合膜可用来包装食品。
适用的抗微生物材料包括细菌多肽和酒花浸膏的组合;杀菌化合物与β-酒花酸或β-酒花酸衍生物或同时两者的组合;包含游霉素、二碳酸二烷基酯和山梨酸酯保存剂的组合;包含乳酸钙和螯合剂的组合(包括但不限于柠檬酸、酒石酸、马来酸、草酸、抗坏血酸、异抗坏血酸、磷酸、苯甲酸、山梨酸,它们的盐和它们的混合物);热处理过的乳酸和/或乙醇酸、抗菌素、溶菌酶、由一株戊糖片球菌产生的乳酸菌细菌素、具有广谱抗菌特性的乳酸菌细菌素、活化乳铁蛋白、脱乙酰几丁质和其中两种或多种的组合。本文公开的脱乙酰几丁质也包括脱乙酰几丁质的盐或衍生物。也可以加入乙酸钠或乙酸钾来增强抗微生物组合。乳酸铁蛋白可以靠乳铁蛋白的N-terminus区被固定在天然存在的基材上。杀菌化合物是乳链菌肤、由一株戊糖片球菌产生的乳酸菌细菌素、具有广谱抗菌特性的乳酸菌细菌素类杆菌素、溶解酶,或其中两种或多种的组合。
这些抗微生物剂能用来有效地控制很多有害微生物,包括如单增李斯特氏菌、伊氏利斯特菌、沙门氏菌在BS平板上的菌落等、蜡质芽孢杆菌、枯草芽孢杆菌、酿酒酵母菌、S.cerevisiae var.paradoxes、卡尔斯伯酵母、荧光假单胞杆菌、梭状芽孢杆菌、肉制品发酵剂清酒乳杆菌、热杀索丝菌、微量溶菌酶、小肠结肠炎耶尔生氏菌、产气肠杆菌、拜耳接合酵母,或其中的两种或多种的组合。
本专利还公开能用来加工食品的方法,其中可以让以上公开的膜与包含至少一种前面公开的抗微生物剂的溶液接触。溶液可以是水本身或水和约0.1~约95重量%或体积%的溶剂如醇,以促进试剂的溶解。溶剂之一是乙醇,因为它常用于食品。其它溶剂可包括丙酮、乙酸、丙酸、丁酸,或其中两种或多种的组合。溶液可包含约0.01~约50重量%,或约0.1~约20重量%,或约0.2~约10重量%,或约0.2~约8重量%的抗微生物剂。
包含抗微生物剂的溶液可以被吸进或浸进膜,从而产生包含抗微生物剂的抗微生物膜。吸收和浸渍可用本领域内已知的任何方法进行,例如让膜浸渗溶液。
抗微生物膜可以用水、溶剂或含约0.1~约50重量%碱或酸,如金属氢氧化物或矿物酸或低烷基脂肪酸,的溶液进行洗涤。洗涤可以在任何环境温度或高达100℃的温度下进行约1min~约5h。抗微生物膜,不论是否经过洗涤,都可制成以上公开的制品。制品可包括小口袋、大口袋、盒、泡形罩、箱、热成形膜、真空袋膜或其它容器。制品可以与几乎所有已知的食品接触,包括易腐食品在内,以产生含抗微生物剂的食品。这类食品可以任选地在高温下,如在约30℃~约250℃下,加热约1min~约5h。
能用本发明的膜加工和包装的食品包括牛肉、猪肉、家禽肉(如鸡和火鸡)、海产品(如鱼和软体动物)和奶酪。肉类产品包括,但不限于,香肠、午餐肉、火腿、火鸡、热狗和基尔巴萨香肠。肉类产品可以是整块瘦肉,也可以配制成各种肉浆、成形肉或研磨肉。成形肉或研磨肉可任选地是衍生自不止一种材料的混合物。食品可以在放进本发明的膜之前进行加工,然后在包装膜内再进一步加工。
抗微生物膜可制成小口袋、大口袋、套管或热成形膜的形式。也能把该膜层合到其它基材上后再热成形。然后可用这类膜来包装未烹煮的生肉或酮体肉(例如牛肉、猪肉、家禽肉或海产品)或加工过的肉,如热狗、香肠、即食熟肉(如火腿、家禽肉、波洛尼亚香肠等)。
下面的实施例仅是说明性的而无意限制本发明的范围。在表内,“w%”是指重量%。表1公开实施例(1~3针对共聚醚酯和4~5针对共聚醚酰胺)和对比实施例(1是尼龙,2是尼龙6.66,3是杜邦的商品共聚酯SelarPT 8307以及4~5是不含环氧乙烷单元的共聚醚酯)的组成,用来进行表2所公开的吸收层试验。
表1
实施例 | MP(℃) | 描述 |
12345 | 200170155156195 | 45w%对苯二甲酸1,4-丁二酯,55w%对苯二甲酸环氧乙烷/环氧丙烷共聚醚酯.计算的环氧乙烷含量为33%.42w%对苯二甲酸1,4-丁二酯,12w%间苯二甲酸1,4-丁二酯,36w%对苯二甲酸环氧乙烷/环氧丙烷共聚醚酯,10重量%间苯二甲酸环氧乙烷/环氧丙烷共聚醚酯.计算的环氧乙烷含量为13%.32w%对苯二甲酸1,4-丁二酯,9w%间苯二甲酸1,4-丁二酯,46w%对苯二甲酸环氧乙烷/环氧丙烷共聚醚对苯二甲酸酯,13w%间苯二甲酸环氧乙烷/环氧丙烷共聚醚酯.计算的环氧乙烷含量为17%PebaxMV 1074PebaxMH 1657 |
对比1对比2对比3对比4对比5 | 219211203 | CapronB 135ZPUltramidC135SelarPT 830770w%对苯二甲酸1,4-丁二酯,30w%聚对苯二甲酸四氢呋喃酯.计算的环氧乙烷含量为0%.60w%对苯二甲酸1,4-丁二酯,40w%聚对苯二甲酸四氢呋喃酯.计算的环氧乙烷含量为0%. |
在3-层吹塑薄膜生产线上把表1的聚合物与其它非粘结性聚合物共挤出,以产生膜内吸收层很易除去的3-层膜。在所有情况下,HDPE或尼龙6都是紧挨表1聚合物共挤出的其它层。在很多情况下,也可以如以下情况所述加进杜邦公司销售的防粘连提浓物ConpolAC B。吹胀比为2∶1,剥离膜层的各种厚度范围为25~64μm。
为确定24h后的吸水率,把共挤出膜切成15.24cm×15.24cm(6英寸×6英寸)正方形,然后剥层。然后把吸收层放在23℃和20%相对湿度的条件下调节处理至少24小时,然后称重,然后把它放进水容器内。24h后,取出该膜,用纸巾干燥之,使其表面上无可见游离水,然后立即称重。对于表2中的各实施例,取3个样品的平均值并报告为吸水重量%。同时,对已在23℃和20%相对湿度的条件下调节处理过至少24小时的膜,还要测定其在38℃和100%相对湿度下的水蒸汽渗透率(MVTR)。对于水渗透率高的样品,MVTR试验在MoconPermatran-W101k上按ASTM D6701-01测定。对于其它样品,MVTR试验在Mocon Permatran-W700上测定(ASTM F 1249-01)。
表2
实施例 | 聚合物类型 | 膜厚(μ) | 24h吸水率(w%) | MVTR |
1112345对比1对比2对比3对比4对比5 | 共聚醚酯1共聚醚酯1共聚醚酯1共聚醚酯2共聚醚酯3共聚酯酰胺1共聚酯酰胺2尼龙6尼龙6.66共聚酯共聚醚酯4共聚醚酯5 | 305364484143432022254646 | 23.924.024.1215.929.860.67.68.21.10.70.1 | 144631663514109226151151069813106651809169762822 |
注:实施例1,2和3及对比实施例4和5还含2重量%防粘连剂ConpolAC B.MVTR单位为g·25μm/m2·24h。
表2显示了高吸水性和高渗水性,而对比实施例则表现出低吸水性和低渗水性或高吸水性和低渗水性。
同时也记录了24h内的吸水量随时间的变化。对膜的处理与对表2的描述相同。每次浸水后,取出膜,用纸巾轻轻拍干,使膜表面无可见游离水,然后立即称重。然后扔掉这些膜,用另一组不同的膜测定不同浸水时间的吸水率。对于表3中的每个实施例,测定3个样品的平均值并记录为吸水重量%。
表3
23℃的吸水率(重量%增重)随时间的变化
实施例 | 膜厚(μ) | 0h | 0.5h | 1h | 3h | 5h | 7h | 24h |
1a1b2a3a对比5a对比2 | 535348644322 | 000000 | 18.2±6.016.0±152.4±0.27.4±40.6±0.810.1±0.1 | 23.6±5.023.2±162.6±0.33.8±4.31.4±1.68.6±1.8 | 22.7±0.521.8±0.82.1±0.36.9±1.00.4±0.27.9±0.7 | 21.1±0.819.9±1.42.4±0.14.2±0.42.7±3.48.6±0.8 | 24.2±0.423.0±1.22.7±0.25.41±1.60.2±0.17.0±0.8 | 24.0±1.423.8±0.52.07±0.25.9±0.40.1±0.18.2±1.0 |
a实施例1,2,3和对比实施例5还含2重量%防粘连剂ConpolAC.
b实施例1还含15重量%防粘连剂ConpolAC B.
该表说明实施例和对比实施例都迅速吸水。在0.5h以内,实施例已接近于23℃下的平衡吸水率。
还记录了膜的脱水率随时间的变化和温度.在这些实验中,将膜在23℃和20%相对湿度下调节处理至少24h,称重,记录其“干”重,然后在23℃水中浸泡至少24h(在有些情况下浸2~3天),取出膜,用纸巾轻轻拍干,使膜表面无可见游离水,立即称取其吸水重量。称重后立即把膜悬挂在90℃的辐射热烘箱内。任何时刻,烘箱内的膜不超过3片,使各片膜不会彼此接触或接触烘箱壁。然后在5、10和60min取出膜称重。在下表4内报告的是5~8片膜试样的平均值。
表4
90℃下的脱水失重a%随时间的变化
在23℃吸水24h或更长时间后的吸水率w% | 5min | 10min | 60min | |
实施例1b实施例3b实施例4实施例5对比实施例5b | 29.4±3.75.4±0.645±1129±90.8±1.0 | -1.0±1.2-0.8±0.2-0.6±0.48.9±5.6-0.2±0.2 | -0.8±1.1-0.9±0.2-0.8±0.3-8.1±0.6-0.05±0.2 | -0.8±1.2-0.8±0.2-0.9±0.3-8.3±0.3-0.1±0.2 |
a膜相对于“干”重的脱水失重%,如文中所述.
b含2重量%防粘连剂ConpolAC B的实施例
表4的结果说明吸水膜在90℃下于5min内就迅速脱去其含水量。在很多情况下,膜的重掉到其起始“干”重之下,可能是因为起始“干”重是在20%相对湿度下称取的,而经过热处理的膜处在更低的相对湿度下。
还试验了实施例膜上各种抗微生物溶液的有效性,如下文所述。
用手把含有厚53μ的实施例1的膜放在含0.5重量%乙酸和1重量%获自Primex,Iceland的商品脱乙酰几丁质(2-氨基-脱氧-β-D-吡喃型葡萄糖)Chitoclear PM588的去离子水溶液中浸泡1min,然后使之干燥。相同的第二片膜留下不处理。然后对这两片膜都作如下所述的振荡烧瓶试验。
在无菌烧瓶内把来自大肠杆菌ATTCC#25922琼脂基片培养液的单一分立菌落培养成15~25ml的胰化酪蛋白大豆培养液(TSB)。然后使该烧瓶边振荡边在37℃下培养至少16h。然后把该培养液稀释进无菌pH7.0的磷酸盐缓冲液中,以获得约105cfu/ml(每毫升菌落形成单位)。为获得起始接种数,在胰酪胨大豆琼脂(TSA)基片上同样制备一式2份10-4和10-3的最后稀溶液(在磷酸缓冲液中制备),然后在37℃下培养过夜。把已培养的磷酸缓冲液(50ml)转移进3个无菌烧瓶。烧瓶1中没有试验膜材料。烧瓶2含0.5g用1重量%脱乙酰几丁质处理过的实施例1的膜。烧瓶3含0.5g未经处理的实施例1的膜。在另一个无菌烧瓶(烧瓶4)内还制备了50ml未培养磷酸缓冲液的对比缓冲液。
把所有的烧瓶都放在摆式振荡器内并在剧烈振荡中在室温(约25℃)下培养。所有烧瓶都在0、1、4和8h取样,并在一式2份的TSA基片上涂覆足量的稀溶液。把这些基片都在37℃下培养至少16h,并以每ml菌落形成单位(cfu/ml)计数菌落,如表5所报告。
表5E.Coli AT CC#2592(cfu/ml)
小时 | 对比缓冲液 | 培养缓冲液 | 对比膜,重量/实施例1 | 实施例1的膜,重量/1%脱乙酰几丁质常浸泡 |
0 | 1.00E+00 | 1.11E+05 | 1.11E+05 | 1.11E+05 |
1 | 1.00E+00 | 1.33E+05 | 7.75E+04 | 1.36E+03 |
4 | 1.00E+00 | 1.24E+05 | 1.26E+05 | 2.50E+01 |
8 | 1.00E+00 | 1.56E+05 | 1.52E+05 | 1.00E+00 |
把厚150μ的实施例1和实施例2的膜切成15mm×15mm样品,放在铝箔上,并在层流罩内的UV光下暴露4~7min。然后把样品从箔上转移到表6所示的各种溶液中,使它们在室温下吸收12~24h。
对于抗微生物溶液的每一浓度,首先在琼脂基片上进行菌苔上斑点试验,以评价溶液对菌落控制的有效性。在该方法中,用SpiralBiotech的Autoplate 4000型仪器,以10E+08cfu/ml的单增李斯特氏菌15313培养TSA琼脂基片。然后用体积吸移泵在试验基片的适当区域内放上3滴10μl的抗微生物斑点。对于抗微生物溶液的每一浓度,制备3片这样的琼脂基片。斑点滴好后,让基片在层流罩内不受干扰地放置10~30min,然后在37℃培养至少24h。用度盘式卡尺(Brown andSharpe,精度0.02mm)测量所得的抑制区,每个区在90°轴上测2次。对每片基片上的3个斑点都这样测量,每个条件下总共产生18个这样的测量值。这组测量值的平均值示于表6。对于所有对比斑点,未观察到抑制区。在菌苔上膜试验中,把15mm×15mm实施例1和实施例2的膜放在新配制的溶液中于室温下浸12~24h,然后用一对经火焰消毒过的眼科细解剖镊子取出样品,让样品滴干,然后在Petri-皿上放置60s,然后放在琼脂基片上进行菌苔上膜试验。TSA琼脂基片已用SpiralBiotech的Autoplate 4000型以10E+08cfu/ml单增李斯特氏菌制成。把2片这样的膜放在制好的TSA琼脂基片上。把第三片15mm×15mm膜在相同条件下浸在对比溶液(该溶液不含抗微生物剂)中吸收并放在基片的第三区内。对抗微生物剂的每一浓度,都以这种方式制备3片这样的基片。膜放好后,让基片在层流罩内不受干扰地静置10~30min,然后在37℃下培养至少24小时。用度盘式卡尺(Brown andSharpe,精度0.02mm)测量抑制区,每个区都在90°轴上测2次。对每个基片都测定2片这样的膜(抗微生物剂处理过的膜),3个基片在每一条件下产生12个这样的测量值。这组测量值的平均值报告在表6中。对比膜不存在抑制区。
根据供应厂(Rhodia)所提供的信息,表6内的乳链菌肽估计有455IU/mg的Novaguard CB1。抗微生物组分和溶液组分的总量为100重量%。
表6
抗微生物剂(S)0 | 抑制区平均值1(mm) | ||||
组分1 | 组分2 | 溶液2 | 菌苔上斑点检定 | 菌苔上膜检定实施例1 | 菌苔上膜检定实施例2 |
苯甲酸(0.75) | - | 乙醇/水(36/63.25) | 7.31±0.91 | 21.55±.77 | 23.49±1.47 |
苯甲酸(1.5) | 乙醇/水(36/62.5) | 7.70±0.61 | 25.92±1.02 | 27.85±0.96 | |
苯甲酸(3.0) | 乙醇/水(36/61) | 8.64±0.76 | 25.76±0.41 | 27.6±2.03 | |
柠檬酸(5) | 水(95) | - | Slight3 | 0 | |
柠檬酸(7.5) | 水(92.5) | - | 19.21±0.25 | 0 | |
柠檬酸(10) | 水(90) | - | 21.00±0.63 | 0 | |
苯甲酸(2.9) | 乳链菌肽4(7500) | 乙醇/水(60/35) | - | 30.26±1.04 | 28.56±1.22 |
苯甲酸(2.9) | 乳链菌肽4(10000) | 乙醇/水(60/35) | - | 30.06±0.49 | 28.33±0.74 |
0括号中的数字是重量%.
1所有对比斑点和对比膜都未出现抑制区.
2溶液是乙醇在水中以及括号中的数字是95%乙醇在水中的重量%
3存在抑制区,但不能得到定量测定,因为整个区未包围膜.
4获自Rhodia的乳链菌肽Novaguard CB1,一种据报告含455IU乳链菌肽/mg的溶菌酶乳链菌肽级;括号中数字的单位是IU/ml;IU/ml表示每ml溶液的国际单位。
Claims (10)
1.一种层压膜,包含(i)内层;(ii)至少一种抗微生物剂;和(iii)外层;其中内层包含包括嵌段共聚醚酯聚合物、嵌段共聚醚酰胺聚合物或其组合的聚合物或由所述聚合物生成;内层任选地在其中已吸收一种抗微生物剂的溶液;外层是单层膜,或包含至少一层聚合物层和任选地至少一层连接层的层合膜或多层膜或由所述至少一层聚合物层和任选地至少一层连接层生成的层合膜或多层膜;以及所述聚合物层包含包括聚酰胺、乙烯/乙烯醇共聚物、聚偏氯乙烯、聚烯烃或其中两种或多种的组合的聚合物,或由包括聚酰胺、乙烯/乙烯醇共聚物、聚偏氯乙烯、聚烯烃或其中两种或多种的组合的聚合物生成。
2.权利要求1的膜,其中内层包含共聚醚酯或共聚醚酰胺聚合物,其水蒸汽透过率(MVTR)至少为约1200g·25μm/m2·24h,或约1200~约20000g·25μm/m2·24h。
3.权利要求1或2的膜,其中内层是共聚醚酯,包含衍生自分子量约2150的环氧乙烷/环氧丙烷共聚醚二醇的长链酯。
4.权利要求1,2或3的膜,其中所述膜是吹胀膜或流延膜以及该膜任选地经过双轴取向。
5.权利要求4的膜,其中所述膜是双轴取向的。
6.权利要求1,2,3或4的膜,其中内层已吸收了抗微生物剂的溶液;所述抗微生物剂是一种或多种细菌多肽和一种或多种酒花浸膏的组合;杀菌化合物和β-酒花酸或β-酒花酸衍生物或两者的组合;包含游霉素、二碳酸二烷基酯和山梨酸酯保存剂的组合;包含乳酸钙和螯合剂的组合;热处理过的乳酸、热处理过的乙醇酸、抗菌素、溶菌酶、由一株戊糖片球菌产生的乳酸菌细菌素、具有广谱抗菌特性的乳酸菌细菌素、固定乳铁蛋白、脱乙酰几丁质、苯甲酸、山梨酸或其中两种或多种的组合;所述螯合剂包括柠檬酸、酒石酸、马来酸、草酸、抗坏血酸、异抗坏血酸、磷酸、它们的盐,或其中两种或多种的组合;以及所述杀菌化合物是乳链菌肤、由一株戊糖片球菌产生的乳酸菌细菌素、具有广谱抗菌特性的乳酸菌细菌素类杆菌素、溶解酶或其中两种或多种的组合。
7.权利要求6的膜,其中抗微生物剂是脱乙酰几丁质、苯甲酸、柠檬酸或其中两种或多种的组合。
8.包含层合膜的制品,其中所述膜如权利要求1,2,3,4,5,6或7所述,以及所述制品是食品套管、热成型膜、真空袋表层膜、盒、泡形罩、小口袋或大口袋。
9.包含下列步骤的方法:使膜与包含至少一种抗微生物剂的溶液接触以产生抗微生物膜;任选地,由该抗微生物膜制成制品;让抗微生物膜或制品与食品接触,以产生含抗微生物剂的食品;以及任选地加热该食品,其中所述膜如权利要求1,2,3,4,5,6或7所述。
10.权利要求9的方法,其中所述方法包含制造制品,其中所述制品如权利要求8所述以及食品是鲜肉、酮体肉、即食肉、热狗或香肠。
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US7081139B2 (en) * | 2001-05-11 | 2006-07-25 | E. I. Du Pont De Nemours And Company | Antimicrobial polyester-containing articles and process for their preparation |
DE10124581A1 (de) * | 2001-05-21 | 2002-11-28 | Wolff Walsrode Ag | Verfahren zur Herstellung von rauchimprägnierten Schlauchhüllen |
CN1604945A (zh) * | 2001-11-06 | 2005-04-06 | 纳幕尔杜邦公司 | 抗微生物聚烯烃制品和其制备方法 |
US20030118704A1 (en) * | 2001-12-11 | 2003-06-26 | Purac Biochem B.V. | Process for preserving food products |
TW200306373A (en) | 2002-05-10 | 2003-11-16 | Du Pont | Antimicrobial polyeter-containing articles and process for their preparation |
-
2005
- 2005-05-11 AU AU2005245407A patent/AU2005245407B9/en not_active Ceased
- 2005-05-11 JP JP2007513345A patent/JP2007537073A/ja active Pending
- 2005-05-11 US US11/126,652 patent/US8858985B2/en active Active
- 2005-05-11 CN CNA2005800149208A patent/CN1950202A/zh active Pending
- 2005-05-11 BR BRPI0510204-9A patent/BRPI0510204A/pt not_active IP Right Cessation
- 2005-05-11 WO PCT/US2005/016588 patent/WO2005113236A2/en active Application Filing
- 2005-05-11 EP EP05779980A patent/EP1753615A2/en not_active Withdrawn
- 2005-05-12 AR ARP050101950A patent/AR048843A1/es active IP Right Grant
Cited By (9)
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CN102066087B (zh) * | 2008-06-11 | 2014-05-14 | 杜邦帝人薄膜美国有限公司 | 抗微生物聚合物膜和所述膜的制造方法 |
CN102316747A (zh) * | 2009-02-17 | 2012-01-11 | 帝斯曼知识产权资产管理有限公司 | 用于乳酪的箔熟化的方法 |
CN102316747B (zh) * | 2009-02-17 | 2013-11-20 | 帝斯曼知识产权资产管理有限公司 | 用于乳酪的箔熟化的方法 |
CN102469799A (zh) * | 2009-07-24 | 2012-05-23 | 乔迪·波阿迪斯·赫尔南德兹-索斯卡 | 从食品中除水的方法 |
CN105813954A (zh) * | 2013-12-18 | 2016-07-27 | 帝斯曼知识产权资产管理有限公司 | 包在膜中的新鲜食品 |
CN106457795A (zh) * | 2014-06-27 | 2017-02-22 | 帝斯曼知识产权资产管理有限公司 | 包含新鲜食物产品的包装件 |
CN106457796A (zh) * | 2014-06-27 | 2017-02-22 | 帝斯曼知识产权资产管理有限公司 | 包含新鲜食物产品的包装件 |
CN114246201A (zh) * | 2021-12-09 | 2022-03-29 | 宜宾市娥天歌食品有限公司 | 一种延长肉制品保存期的肠衣及其制作方法和香肠制品 |
CN114246201B (zh) * | 2021-12-09 | 2022-08-09 | 宜宾市娥天歌食品有限公司 | 一种延长肉制品保存期的肠衣及其制作方法和香肠制品 |
Also Published As
Publication number | Publication date |
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EP1753615A2 (en) | 2007-02-21 |
AU2005245407A1 (en) | 2005-12-01 |
JP2007537073A (ja) | 2007-12-20 |
WO2005113236A2 (en) | 2005-12-01 |
AR048843A1 (es) | 2006-05-31 |
BRPI0510204A (pt) | 2007-10-16 |
WO2005113236A3 (en) | 2006-05-04 |
US20050266056A1 (en) | 2005-12-01 |
AU2005245407B2 (en) | 2010-06-17 |
US8858985B2 (en) | 2014-10-14 |
AU2005245407B9 (en) | 2010-10-14 |
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