CN103608175B - 具有隔氧性能的涂覆聚合物箔 - Google Patents
具有隔氧性能的涂覆聚合物箔 Download PDFInfo
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- CN103608175B CN103608175B CN201280030186.4A CN201280030186A CN103608175B CN 103608175 B CN103608175 B CN 103608175B CN 201280030186 A CN201280030186 A CN 201280030186A CN 103608175 B CN103608175 B CN 103608175B
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
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- C—CHEMISTRY; METALLURGY
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Paints Or Removers (AREA)
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- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
Abstract
本发明描述了一种涂覆聚合物箔,该涂覆聚合物箔可通过用水性组合物对其进行涂覆而制备,所述水性组合物包括(A)通过自由基聚合获得的并包含10至80重量%的选自烯键式不饱和酸酐和烯键式不饱和二元羧酸(其羧酸基团可形成酸酐基团)的化合物的聚合物,和(B)具有至少两个羟基的链烷醇胺。涂覆使聚合物箔具有隔氧层且尤其可用于包装材料生产。
Description
本发明涉及涂覆聚合物箔(polymerfoil),该涂覆聚合物箔可通过用水性组合物对其进行涂覆而制备,所述水性组合物包括(A)通过自由基聚合获得的并包含10至80重量%的烯键式不饱和酸酐和烯键式不饱和二元羧酸(其羧酸基团可形成酸酐基团)的聚合物,和(B)具有至少两个羟基的链烷醇胺。所述涂覆使聚合物箔具有隔氧层且尤其可用于生产包装材料。
当对易受氧化作用影响的产品或氧气敏感产品进行包装时,使用的包装材料具有隔氧性能是十分重要的,即该包装材料具有最低的氧透过性和最低的氧渗透性。作为包装材料使用的且例如由聚烯烃(如聚乙烯或定向聚丙烯)或聚酯(例如聚对苯二甲酸乙二醇酯)组成的聚合物箔在未涂覆的形式下本身通常具有相对较高的氧渗透性,因此人们已提出了各种措施来提高这些包装材料的隔氧性能。
WO03/068869描述了生产具有隔氧性能的包装方式的方法,其中用可聚合化合物涂覆基底材料,随后该化合物在基底材料上聚合。EP2014730描述了基于多元羧酸聚合物的用于形成隔气薄膜的涂料组合物,该涂料组合物借助锌化合物交联。WO07/002322描述了具有隔氧性能的涂覆聚合物薄膜。该涂料组合物是马来酸/丙烯酸共聚物的溶液和乙烯醇/乙烯胺共聚物的溶液。涂覆过程之后,涂料组合物中的两种共聚物在聚合物薄膜上交联。WO98/31719描述了用作隔离离涂料的涂料组合物。组合物包括烯键式不饱和酸单体和包含纳入的交联剂的多元胺。涂覆过程之后,发生由自由基引发的聚合过程导致的交联。具有隔氧性能或具有阻气性能的涂料也在EP890432(WO98/09813)和EP1683825(WO2005/037898)中有所描述。
迄今公开的具有隔氧性能的包装箔仍不完全令人满意。各种应用中的氧渗透性通常仍旧没有达到足够低,或具有聚合物基薄膜的隔离涂料过脆并缺乏足够的柔韧性,且破裂的危险意味着持久的隔离效果没有保障。当发生弯曲或折痕时,在折痕处隔离膜有损坏的危险,导致隔离效果不充分。当湿度较低时基于含有酸基团的不含氯的聚合物的氧气隔离层通常显示可接受的隔离效果,但湿度相对较高时(相对湿度超过80%)隔离效果通常显著下降。为了形成一些已知的隔离层,需要使用重金属盐,但为了健康的原因,通常不期望这样做,尤其针对食品饮料包装领域的应用。其它已知的涂料组合物为两组分体系,其中两种组分在应用于基底之前必须保持分离,否则它们会过早交联,作为单组分体系储存不稳定。
本发明的目的是提供可使得生产具有良好隔氧性能的包装的其他组合物和方法,尤其当湿度相对较高时并且在折痕、弯曲和角落处。该包装应具有最大抗温度变化性、柔韧性和防粘能力,并且应该具有最小量的对健康有害的任何物质,例如金属。特别需要使用不含氯、不含金属盐且储存稳定的涂料组合物单组分体系。
本发明提供了涂覆聚合物箔,其可通过用水性组合物对聚合物箔进行涂覆而制备,所述水性组合物包括
A)通过自由基聚合获得的、且包含10至80重量%的至少一种选自烯键式不饱和酸酐和烯键式不饱和二元羧酸(其羧酸基团可以形成酸酐基团)的化合物的聚合物,和
B)至少一种具有至少两个羟基的链烷醇胺。
本发明还提供了上述水性组合物的用途,其用于制备或增强聚合物箔上的隔氧层。
本发明制备的涂料具有隔氧性能。在实施例中描述的渗透性测试可用于测量隔离性能。表述“隔氧性能”意指与未涂覆的基底相比氧透过性和氧渗透性分别降低。本发明涂覆的聚合物箔的氧渗透性优选小于30%,特别小于20%或小于10%,例如未涂覆聚合物箔的值为1%至3%(在23℃且0%相对湿度下测量)。
本发明中使用的水性组合物包括聚合物A),其包含10至80重量%、优选10至50重量%、特别优选15至40重量%的烯键式不饱和酸酐或其羧酸基团可形成酸酐基团的烯键式不饱和二元羧酸(以下称为单体a))。优选的酸酐为二元羧酸酐。合适的烯键式不饱和二元羧酸通常是相邻碳原子上具有羧酸基团的那些。羧酸基团也可以其盐的形式存在。优选的单体a)为马来酸、马来酸酐、衣康酸、1,2,3,6-四氢邻苯二甲酸、1,2,3,6-四氢邻苯二甲酸酐及其碱金属盐和铵盐,或这些材料的混合物。特别优选马来酸和马来酸酐。
除了单体a),聚合物也可包含单体b)。可使用的单体b)的实例为:单烯键式不饱和C3至C10单羧酸(单体b1),例如丙烯酸、甲基丙烯酸、乙基丙烯酸、烯丙基乙酸、巴豆酸、乙烯基乙酸、马来酸半酯(如马来酸单甲酯)、上述这些单体b1的混合物和这些单体b1的碱金属盐及铵盐,线性1-烯烃、支链1-烯烃、或环烯烃(单体b2),例如乙烯、丙烯、丁烯、异丁烯、戊烯、环戊烯、己烯、环己烯、辛烯、任选与2,4,4-三甲基-2-戊烯、C8-C10-烯烃、1-十二碳烯、C12-C14-烯烃、十八烯、1-二十烯(C20)、C20-C24-烯烃混合的2,4,4-三甲基-1-戊烯;用茂金属催化剂生产的且具有末端双键的低聚烯烃,例如低聚丙烯、低聚己烯和低聚十八烯;通过阳离子聚合生产的且具有高α烯烃含量的烯烃,例如聚异丁烯,在烷基部分具有1-40个碳原子的乙烯基和烯丙基烷基醚,其中烷基部分也可带有其他的取代基,如羟基、氨基或二烷基氨基基团,或一种或多种烷氧基基团(单体b3),例如甲基乙烯基醚、乙基乙烯基醚、丙基乙烯基醚、异丁基乙烯基醚、2-乙基己基乙烯基醚、乙烯基环己基醚、乙烯基4-羟丁基醚、癸基乙烯基醚、十二烷基乙烯基醚、十八烷基乙烯基醚、2-(二乙基氨基)乙基乙烯基醚、2-(二-正丁基氨基)乙基乙烯基醚、甲基二甘醇基乙烯基醚,以及相应的烯丙基醚及其混合物。丙烯酰胺和烷基取代的丙烯酰胺(单体b4),例如丙烯酰胺、甲基丙烯酰胺、N-叔丁基丙烯酰胺、N-甲基(甲基)丙烯酰胺,含磺基的单体(单体b5),例如烯丙基磺酸、甲基烯丙基磺酸、苯乙烯磺酸盐、乙烯基磺酸、烯丙基氧代苯磺酸、2-丙烯酰胺基-2-甲基丙磺酸,其相应的碱金属盐或铵盐,及其混合物。丙烯酸、甲基丙烯酸或马来酸的C1至C8烷基酯或C1至C4羟基烷基酯,或经2至50mol的环氧乙烷、环氧丙烷、环氧丁烷或其混合物烷氧化的C1至C18醇与丙烯酸、甲基丙烯酸或马来酸的酯(单体b6),例如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸己酯、(甲基)丙烯酸2-乙基己基酯、(甲基)丙烯酸羟乙酯、(甲基)丙烯酸羟丙酯、单丙烯酸1,4-丁二醇酯、马来酸二丁酯、丙烯酸乙基二甘醇基酯、丙烯酸甲基多甘醇基酯(11EO)、与3、5、7、10或30mol的环氧乙烷反应的C13/C15-氧代醇的(甲基)丙烯酸酯及其混合物,(甲基)丙烯酸烷基氨基烷基酯或烷基氨基烷基(甲基)丙烯酰胺或其碱化产物(单体b7),例如2-(N,N-二甲基氨基)乙基(甲基)丙烯酸酯、3-(N,N-二甲基氨基)丙基(甲基)丙烯酸酯、2-(N,N,N-三甲基氯化铵)乙基(甲基)丙烯酸酯、2-二甲基氨基乙基(甲基)丙烯酰胺、3-二甲基氨基丙基(甲基)丙烯酰胺、3-三甲基氯化铵丙基(甲基)丙烯酰胺,C1至C30单羧酸的乙烯基和烯丙基酯(单体b8),例如甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、戊酸乙烯酯、2-乙基己酸乙烯酯、壬酸乙烯酯、癸酸乙烯酯、新戊酸乙烯酯、棕榈酸乙烯酯、硬脂酸乙烯酯、月桂酸乙烯酯。其他可被提到的单体b9为:N-乙烯基甲酰胺、N-乙烯基-N-甲基甲酰胺、苯乙烯、[α]甲基苯乙烯、3-甲基苯乙烯、丁二烯、N-乙烯基吡咯烷酮、N-乙烯基咪唑、1-乙烯基-2-甲基咪唑、1-乙烯基-2-甲基咪唑啉、N-乙烯基己内酰胺、丙烯腈、甲基丙烯腈、烯丙醇、2-乙烯基吡啶、4-乙烯基吡啶、二烯丙基二甲基氯化铵、氯亚乙烯、氯乙烯、丙烯醛、异丁烯醛和乙烯基咔唑及其混合物。
除了单体a),聚合物还可包含20至90重量%的单体b。除了单体a),优选聚合物还包含50至90重量%、特别地60至85重量%的单体b。优选的单体b为丙烯酸、甲基丙烯酸、乙烯、丙烯、丁烯、异丁烯、环戊烯、甲基乙烯基醚、乙基乙烯基醚、丙烯酰胺、2-丙烯酰胺基-2-甲基丙磺酸、乙酸乙烯酯、苯乙烯、丁二烯、丙烯腈或其混合物。特别优选丙烯酸、甲基丙烯酸、乙烯、丙烯酰胺、苯乙烯和丙烯腈或其混合物。极特别优选丙烯酸、甲基丙烯酸,和丙烯酰胺,或其混合物。
在本发明的一个具体实施方案中,聚合物包含10至80重量%的马来酸或马来酸酐。在本发明的一个实施方案中,聚合物A包含20至40重量%的马来酸或马来酸酐,和60至80重量%的丙烯酸和/或甲基丙烯酸,且交联过程每100重量份聚合物A使用20至40重量份的链烷醇胺B。
聚合物可通过传统的聚合方法生产,例如通过本体聚合、乳液聚合、悬浮聚合、分散聚合、沉淀聚合或溶液聚合。合适的聚合方法在WO97/31036中有所描述。特定的聚合方法优选用在除去氧气的条件下进行,优选在氮气流中进行。所有的聚合方法都使用传统的设备,例如搅拌槽、多级搅拌槽、高压釜、管式反应器和捏合机。优选使用溶液聚合、乳液聚合、沉淀聚合或悬浮聚合的操作方法。特别优选下列方法:溶液聚合和乳液聚合。聚合过程可在溶剂或稀释剂中进行,例如甲苯、邻二甲苯、对二甲苯、异丙基苯、氯苯、乙苯、烷基芳香烃的工业混合物、环己烷、工业脂肪族混合物、丙酮、环己酮、四氢呋喃、二氧六环、二醇类和乙二醇衍生物、聚(亚烷基)二醇及其衍生物、乙醚、叔丁基甲基醚、乙酸甲酯,异丙醇、乙醇、水或其混合物,例如异丙醇/水混合物。优选使用的溶剂或稀释剂包含任选地含有最高达60重量%的醇或二醇类的水。特别优选使用水。聚合过程可在20-300℃、优选60-200℃温度下进行。重均分子量取决于聚合条件的选择,并可设为例如800至5000000,特别为1000至1000000。优选重均分子量Mw为5000以上。特别优选的重均分子量为5000至500000或10000至200000。Mw通过凝胶渗透色谱测定。
聚合过程优选在形成自由基的化合物(引发剂)的存在下进行。所述化合物需要的量最高达30重量%,优选0.05至15重量%,特别优选0.2至8重量%,基于聚合过程中使用的单体计。在多组分引发剂体系(例如氧化还原引发剂体系)的情况下,上述重量数据基于全部组分。合适的聚合引发剂实例为过氧化物、氢过氧化物、过二硫酸盐、过碳酸盐、过氧酯、过氧化氢和偶氮化合物。可以是水溶性的或非水溶性的引发剂实例为过氧化氢、过氧化二苯甲酰、二环己基过氧二碳酸盐、过氧化二月桂酰、过氧化甲乙酮、二叔丁基过氧化物、过氧化乙酰丙酮、叔丁基过氧化氢、异丙基苯过氧化氢、过新癸酸叔丁基酯、过新戊酸叔戊基酯、过新戊酸叔丁基酯、过新己酸叔丁基酯、2-乙基过己酸叔丁基酯、过苯甲酸叔丁基酯、过二硫酸锂、过二硫酸钠、过二硫酸钾和过二硫酸铵,偶氮二异丁腈、2,2’-偶氮双(2-脒基丙烷)二氢氯化物、2-(氨基甲酰偶氮)异丁腈和4,4-偶氮双(4-氰基戊酸)。引发剂可单独使用或彼此混合使用,实例为过氧化氢和过二硫酸钠的混合物。对于在水相中的聚合过程,优选使用水溶性引发剂。已知的氧化还原引发体系也可用作聚合引发剂。这些氧化还原引发体系包含至少一种含过氧化物的化合物和氧化还原共引发剂的组合,例如具有还原效果的硫化合物,如碱金属的重亚硫酸盐、亚硫酸盐、硫代硫酸盐、连二亚硫酸盐,和连四硫酸盐及铵基化合物。因此,可能使用碱金属氢亚硫酸盐或氢亚硫酸铵与过二硫酸盐的结合物。含过氧化物的化合物的量与氧化还原共引发剂的量之比为30:1至0.05:1。
为了制备具有低平均分子量的聚合物,在调节剂的存在下进行共聚合过程通常是有利的。针对该目的可以使用传统调节剂,实例为包含SH基团的有机化合物,例如2-巯基乙醇、2-巯基丙醇、巯基乙酸、叔丁基硫醇、正辛基硫醇、正十二烷硫醇和叔十二烷硫醇,C1至C4醛,例如甲醛、乙醛、丙醛,羟铵盐,例如硫酸羟铵,甲酸,亚硫酸氢钠或异丙醇。聚合调节剂的用量通常为基于单体计,0.1至10重量%。也可用合适溶剂的选择来影响平均分子量。例如,在含有苄基氢原子的稀释剂的存在下的聚合,平均分子量通过链转移而下降。
为了制备相对较高分子量的共聚物,在交联剂的存在下进行聚合反应通常是有利的。这些交联剂为具有两个或多个烯键式不饱和基团的化合物,例如至少二元饱和醇的二丙烯酸酯或二甲基丙烯酸酯,例如二丙烯酸乙二醇酯、二甲基丙烯酸乙二醇酯、1,2-二丙烯酸丙二醇酯、1,2-二甲基丙烯酸丙二醇酯、二丙烯酸1,4-丁二醇酯、二甲基丙烯酸1,4-丁二醇酯、二丙烯酸己二醇酯、二甲基丙烯酸己二醇酯、二丙烯酸新戊二醇酯、二甲基丙烯酸新戊二醇酯、二丙烯酸3-甲基戊二醇酯和二甲基丙烯酸3-甲基戊二醇酯。使用的交联剂还可包含具有超过2个OH基团的醇的丙烯酸酯和甲基丙烯酸酯,例如三羟甲基丙烷三丙烯酸酯或三羟甲基丙烷三甲基丙烯酸酯。另一类的交联剂为每种情况分子量具有200至9000的聚乙二醇或聚丙二醇的二丙烯酸酯或二甲基丙烯酸酯。用于生产二丙烯酸酯或二甲基丙烯酸酯的聚乙二醇或聚丙二醇的分子量优选每种情况下为400至2000。除了环氧乙烷或环氧丙烷的均聚物,可以使用的材料还有环氧乙烷和环氧丙烷的嵌段共聚物和包含环氧乙烷单元与环氧丙烷单元无规分布的环氧乙烷和环氧丙烷共聚物。适合生产交联剂的其它材料为环氧乙烷或环氧丙烷的低聚物,例如二丙烯酸二乙二醇酯、二甲基丙烯酸二乙二醇酯、二丙烯酸三乙二醇酯、二甲基丙烯酸三乙二醇酯、二丙烯酸四乙二醇酯和/或二甲基丙烯酸四乙二醇酯。其它合适的交联剂为丙烯酸乙烯酯、甲基丙烯酸乙烯基酯、衣康酸乙烯基酯、己二酸二乙烯基酯、丁二醇二乙烯基醚、三羟甲基丙烷三乙烯基酯、丙烯酸烯丙酯、甲基丙烯酸烯丙酯、季戊四醇三烯丙基醚、三烯丙基蔗糖、五烯丙基蔗糖、亚甲基双(甲基)丙烯酰胺、二乙烯基亚乙基脲、二乙烯基亚丙基脲、二乙烯基苯、二乙烯基二氧六环、三聚氰酸三烯丙酯、四烯丙基硅烷、四乙烯基硅烷和双或聚丙烯酸硅氧烷(例如,来自Th.GoldschmidtAG的Tegomer产品)。交联剂优选用量为10ppm至重量5%,基于待聚合的单体计。
如果操作使用乳液聚合、沉淀聚合、悬浮聚合或分散聚合方法,则通过使用表面活性剂助剂来稳定聚合物液滴或聚合物颗粒是有利的。为此,通常使用乳化剂或保护性胶体。可能使用阴离子、非离子、阳离子和两性乳化剂。阴离子乳化剂的实例为烷基苯磺酸、磺化脂肪酸、磺基琥珀酸酯、脂肪醇硫酸酯、烷基苯酚硫酸酯和脂肪醇醚硫酸酯。可使用的非离子乳化剂的实例为烷基苯酚乙氧基化物、伯醇乙氧基化物、脂肪酸乙氧基化物、烷醇酰胺乙氧基化物、脂肪胺乙氧基化物、EO/PO嵌段共聚物和烷基多聚葡萄糖苷。使用的阳离子或两性乳化剂的实例为:季胺烷氧化物、烷基甜菜碱、烷基氨基甜菜碱和磺基甜菜碱。典型的保护性胶体的实例为纤维素衍生物、聚乙二醇、聚丙二醇、乙二醇和丙二醇的共聚物、聚乙酸乙烯酯、聚乙烯醇、聚乙烯基醚、淀粉和淀粉衍生物、葡聚糖、聚乙烯基吡咯烷酮、聚乙烯基吡啶、聚乙烯亚胺、聚乙烯基咪唑、聚乙烯基琥珀酰亚胺、聚乙烯基-2-甲基琥珀酰亚胺、聚乙烯基-1,3-氧氮杂环戊烷-2-酮、聚乙烯基-2-甲基咪唑啉和包含马来酸或包含马来酸酐的共聚物,例如在DE2501123中描述的。乳化剂或保护性胶体通常使用的浓度为0.05至20重量%,基于单体计。
如果聚合过程在水性溶液或稀释液中进行,则在聚合过程之前或之中单体可完全或在一定程度上用碱中和。可使用的碱的实例为碱金属化合物或碱土金属化合物,例如氢氧化钠、氢氧化钾、氢氧化钙、氧化镁、碳酸钠;氨;伯胺、仲胺和叔胺,例如乙胺、丙胺、单异丙胺、单丁胺、己胺、乙醇胺、二甲胺、二乙胺、二正丙胺、三丁胺、三乙醇胺、二甲氧基乙基胺、2-乙氧基乙基胺、3-乙氧基丙基胺、二甲基乙醇胺、二异丙醇胺或吗啉。针对中和过程也可使用多元胺,例如乙二胺、2-二乙基氨基乙胺、2,3-二氨基丙烷、1,2-丙二胺、二甲氨基丙胺、新戊烷二胺、六亚甲基二胺、4,9-二氧杂十二烷-1,12-二胺、聚乙烯亚胺和聚乙烯胺。聚合过程之前或之中针对烯键式不饱和羧酸的部分或完全中和而优选使用的化合物为氨、三乙醇胺和二乙醇胺。特别优选在聚合过程之前和之中不对烯键式不饱和羧酸进行中和。还优选除了链烷醇胺B)外,在聚合过程后不加入中和剂。
聚合过程可通过各种不同方法连续或间歇进行。在通常方法中,部分单体任选地在合适的稀释剂或溶剂中且任选地在乳化剂、保护性胶体或其它助剂的存在下用作起始进料,体系经惰性化处理,并升高温度直到达到所需的聚合温度。然而,还可仅使用一种合适的稀释剂作为起始投料。在确定的时间内,任选地稀释剂中,自由基引发剂、其他的单体和其它助剂,例如调节剂或交联剂,计量加入混合物中。选择的进料时间可以不相同。例如,选作引发剂进料的进料时间可以比单体进料的时间长。如果聚合物是通过在水中的溶液聚合获得的,则通常没有必要除去溶剂。然而,例如,如果目的是分离聚合物,则可进行喷雾干燥过程。如果在蒸汽挥发性溶剂或溶剂混合物中使用溶液聚合、沉淀聚合或悬浮聚合方法来生产聚合物,则溶剂可通过引入蒸汽除去,目的是获得水性溶液或分散液。从有机稀释剂中除去聚合物的另一方法使用了干燥过程。
优选聚合物A)采取具有固体含量优选10至80重量%、特别优选40至65重量%的水性分散液或溶液的形式。
聚合物A)也可通过马来酸或马来酸酐、或包含马来酸或马来酸酐的单体混合物向接枝底物的接枝而获得。合适的接枝底物实例为单糖、寡糖、改性多糖和烷基聚乙二醇醚。这些接枝聚合物在例如DE4003172和EP116930中有所描述。
具有至少两个OH基团的链烷醇胺用作组分B)。优选下式的链烷醇胺
NR1R2R3(I)
其中R1为H原子、C1-C10烷基基团或C1-C10羟烷基基团,且R2和R3为C1-C10羟烷基基团。特别优选R2和R3相互独立地为C2-C5羟烷基基团,且R1为H原子、C1-C5烷基基团或C2-C5羟烷基基团。可被提到的式I的化合物的实例为二乙醇胺、三乙醇胺、二异丙醇胺、三异丙醇胺、甲基二乙醇胺、丁基二乙醇胺和甲基二异丙醇胺。特别优选三乙醇胺。
为了制备本发明中使用的水性组合物,优选聚合物A)和链烷醇胺B)彼此之间以如此比例使用,组分A)的羧基基团和组分B)的羟基基团的摩尔比为20:1至1:1,优选8:1至5:1,且特别优选5:1至1.7:1(其中酸酐基团算作两个羧基基团)。在本发明中使用的水性组合物的制备的一个简单实例中,将链烷醇胺加入到聚合物A)的水性分散液或溶液中。
本发明中使用的水性组合物优选包含小于1.0重量%、特别地小于0.5重量%、且极特别地小于0.3重量%,特别是小于0.1重量%的含磷的反应促进剂,基于A)+B)总量计。含磷的反应促进剂在US651088和US583086中详细描述。这些含磷的反应促进剂特别包含碱金属次磷酸盐、碱金属亚磷酸盐、碱金属多磷酸盐、碱金属二氢磷酸盐、多磷酸、连二磷酸、磷酸、烷基次膦酸,或所述盐和酸各自的低聚物或聚合物。本发明中使用的水性组合物优选不包括含磷的反应促进剂或对反应促进有效的含磷化合物。本发明中使用的水性组合物可包含酯化作用催化剂,例如硫酸或对甲苯磺酸。
本发明中使用的水性组合物可包含在水中作为仅有成分的聚合物A)和链烷醇胺B)。然而,水性组合物还可包含适于各自预期用途的其他的添加剂。可使用的实例为浸润剂、染料、颜料、杀菌剂、增塑剂、用于流变调整的增稠剂、助粘剂、还原剂和酯交换催化剂。
在本发明的一个实施方案中,在本发明中使用的水性组合物包含层状颜料的量优选为2至40重量%。层状颜料的实例为层状硅酸盐,尤其为滑石粉、粘土或云母。优选滑石粉。优选的形状因子(长度:厚度比例)为大于10。
本发明进一步提供了在衬底基板上制备或增强氧气隔离效果的方法。该衬底基板包括聚合物箔,其中衬底基板用上面详细描述的水性组合物直接或间接涂覆。用水性组合物涂覆后,对聚合物箔进行干燥处理并加热到至少100℃,优选至少130℃,例如140-180℃,从而引发交联反应。加热时间优选3秒至60分钟,特别为3秒至10分钟。
交联之后,本发明的聚合物箔具有一层涂层,在该涂层中聚合物通过聚合物A的酸基团与链烷醇胺B的羟基基团之间的酯键交联。
在干燥(50℃,72小时)得到厚度为0.3至1mm的薄膜后,接着在130℃空气中处理15分钟,本发明中使用的水性组合物的凝胶含量优选50重量%以上,特别优选60重量%以上,非常特别优选70重量%以上,且特别是75重量%以上。本文确定凝胶含量的方法是在固化过程结束后固化薄膜在23℃的水中储存48小时。本文可溶性含量在水中保持。随后将薄膜在50℃干燥至恒重,并称重。重量对应于凝胶含量,以重量%计,基于除去可溶性内容物之前的重量计。当超过3小时的失重小于0.5重量%时,已经达到恒重。
适合用作基材的聚合物箔的箔实例为由聚酯制备的箔,例如聚对苯二甲酸乙二醇酯,和由聚烯烃、聚酰胺、聚苯乙烯或聚氯乙烯制备的箔。优选的聚合物箔为由聚对苯二甲酸乙二醇酯、定向聚丙烯或聚乙烯制备的箔,或由生物可降解脂肪族-芳香族共聚酯制备的那些,其中聚乙烯可由乙烯通过高压聚合方法或通过低压聚合方法制备。特别优选由聚对苯二甲酸乙二醇酯制备的箔。生物可降解箔的实例为由生物可降解脂肪族-芳香族共聚酯和/或聚乳酸制备的箔,例如箔或箔。合适的共聚酯的实例为由烷二醇形成的那些,尤其是C2至C8烷二醇,例如1,4-丁二醇,由脂肪族二元羧酸形成的那些,尤其是C2-C8二元羧酸,例如己二酸,和由芳香族二元羧酸形成的那些,例如对苯二甲酸。
衬底箔的厚度通常在10至200μm范围,在箔由聚酰胺制成的情况下为30至50μm,在箔由聚对苯二甲酸乙二醇酯制成的情况下为10至40μm,在箔由聚氯乙烯制成的情况下为约100μm,且在箔由聚苯乙烯制成的情况下为约30至75μm。
涂布机中的应用方法的实例是将涂覆组合物施用在由塑料制成的衬底箔上。就网状形式的材料的使用而言,水性组合物可由槽中通过涂布辊施用并借助气刷使之平整。涂覆箔的优选施用方法包括刮片系统、绕线刮胶刀、气刷、反辊施用方法、反向凹面涂覆、帘膜式淋涂或冲模或模头。
通过热过程引发的交联可在涂覆过程之后直接发生,或在稍晚的时间发生,例如在网状形式的材料经涂覆、干燥和卷轴之后的卷轴状态中发生。
在聚合物中纳入产生自由基的UV引发剂或将这些作为添加剂加入到水性组合物中可以导致另外的交联,其中聚合物箔在涂覆过程之后用UV光照射。
衬底箔先前的电晕处理和/或用底漆涂覆可用来进一步改善在箔上的粘附。施用到聚合物箔的材料量的实例优选0.25至10g(聚合物,固体)/m2,优选0.5至7g/m2。在水性组合物向该基材施用之后,将溶剂蒸发。为此,可以例如在连续操作的情况下使材料通过烘道,该烘道已配有红外辐射装置。随后将已涂覆和干燥的材料在冷却辊上操作并最终进行卷轴。干燥涂层的厚度优选至少0.5μm,例如0.5至50μm,特别优选0.5至20μm。
涂覆的聚合物箔对氧气显示出优良的隔离效果,特别是当相对湿度较高时,例如大于或等于80%,或大于或等于85%。涂覆的聚合物箔自身可用作包装材料或包装材料的一部分,例如食品或饮料的包装材料。涂层具有非常好的机械性能,并显示出例如良好的隔离性能,并且大体上显示无裂痕。
为了获得特定表面性能或特定涂覆性能的包装方法,例如良好的印刷性能、进一步改善的密封性能和进一步改善的隔离性能,和良好的耐水性,使用另外提供这些所需性能的外层对这些涂覆基底进行涂覆可能是有利的。涂覆箔可通过重复上述方法进行涂覆,或者可以不使用箔的中间卷轴过程和回卷过程以连续过程进行重复涂覆。因此,隔氧层的位置在体系的内部,而表面性能由外层决定。本发明还提供了涂覆聚合物箔,其中聚合物箔不仅用本发明的隔离层涂覆,还用至少一种粘合层或至少一种密封层涂覆。也可以使用涂覆箔生产由多层箔构成的层压制品。在这一点上,隔氧层的位置也优选在系统的内部。
实施例
水性涂料组合物可以按WO97/31036中描述的生产。
氧隔离效果的测量:
氧透过率和氧渗透率分别在各自规定的相对湿度下在聚合物箔的涂层上测定。该方法由测量氧透过率开始,随后基于1μm层厚对此进行重新计算,并规定其为氧渗透性,单位为(cm3x1μm)/(m2xdx巴),其中d为以天计算的时间。测定方法基于ASTMD3985。
实施例B1(对比,无链烷醇胺)
聚合物箔:聚对苯二甲酸乙二醇酯,厚度36μm。
水性涂料组合物:
由75重量份的丙烯酸和25重量份的马来酸制成的聚合物
重均摩尔质量:80000g/mol
固体含量:水中50重量%
实施例B2
聚合物箔:聚对苯二甲酸乙二醇酯,厚度36μm
水性涂料组合物:
由75重量份的丙烯酸和25重量份的马来酸制成的聚合物
重均分子质量:80000g/mol
对于每100重量份的聚合物,30重量份的三乙醇胺
固体含量:水中50重量%
聚合物箔用水性涂料组合物涂覆,使用6μm(实施例1)或10μm(实施例2)的层厚(干燥后)。交联通过在160℃加热30分钟实现。
每种情况的氧隔离效果在0%和85%的相对湿度下测量。表1为整理的测量结果。
表1:氧隔离测量结果
Claims (14)
1.水性组合物用于制备或增强聚合物箔上的隔氧层的用途,其中用水性组合物对聚合物箔进行涂覆,所述水性组合物包括:
A)通过自由基聚合获得的且包含10至80重量%的至少一种选自烯键式不饱和酸酐和烯键式不饱和二元羧酸的化合物的聚合物,其中所述二元羧酸的羧酸基团可以形成酸酐基团,和
B)至少一种具有至少两个羟基的链烷醇胺。
2.根据权利要求1的用途,其中,在涂覆过程之后,将具有水性组合物的涂覆聚合物箔干燥并加热到至少100℃。
3.根据权利要求2的用途,其中聚合物箔具有涂层,所述涂层中聚合物借助聚合物A的酸基团与链烷醇胺B的羟基基团之间的酯键交联。
4.根据权利要求1的用途,其中聚合物包括10至80重量%的马来酸或马来酸酐。
5.根据权利要求1的用途,其中链烷醇胺包括化合物NR1R2R3,其中R1为H原子、C1-C10烷基基团或C1-C10羟烷基基团,且R2和R3为C1-C10羟烷基基团。
6.根据权利要求5的用途,其中链烷醇胺包括三乙醇胺。
7.根据权利要求1的用途,其中A)的羧基基团和酸酐基团与B)的羟基基团的摩尔比为20:1至1:1,其中所述酸酐基团算作两个羧基基团。
8.根据权利要求1的用途,其中在干燥和15分钟的130℃固化之后,水性组合物的凝胶含量超过50重量%。
9.根据权利要求2的用途,其中涂层的厚度至少为0.5μm。
10.根据权利要求1的用途,其中聚合物薄膜的基材选自聚对苯二甲酸乙二醇酯、定向聚丙烯、聚乙烯、或生物可降解的脂肪族-芳香族共聚酯。
11.根据权利要求1的用途,其中聚合物箔为包装材料或包装材料的一部分。
12.根据权利要求1的用途,其中聚合物箔还用至少一种粘合层或至少一种密封层涂覆。
13.根据权利要求1的用途,其中聚合物A包括20至40重量%的马来酸或马来酸酐和60至80重量%的丙烯酸和/或甲基丙烯酸,并对于每100重量份的聚合物A使用20至40重量份的链烷醇胺B。
14.一种制备或增强选自聚合物箔的衬底基板上的隔氧效果的方法,其中衬底基板用包括下列组分的水性组合物直接或间接涂覆:
A)通过自由基聚合获得的且包含10至80重量%的至少一种选自烯键式不饱和酸酐和烯键式不饱和二元羧酸的化合物的聚合物,其中所述二元羧酸的羧酸基团可以形成酸酐基团,和
B)至少一种具有至少两个羟基的链烷醇胺,
其中,在涂覆过程之后,将具有水性组合物的涂覆聚合物箔干燥并加热到至少130℃。
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DE102017204525A1 (de) | 2016-03-23 | 2017-09-28 | Basf Se | Verbundfolienlaminate für flexible Verpackungen |
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ES2931335T3 (es) * | 2018-04-20 | 2022-12-28 | Basf Se | Composición adhesiva con contenido de gel a base de reticulación mediante grupos ceto o aldehído |
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- 2012-06-18 ES ES12730870.8T patent/ES2538854T3/es active Active
- 2012-06-18 BR BR112013032551A patent/BR112013032551A2/pt not_active Application Discontinuation
- 2012-06-18 EP EP12730870.8A patent/EP2723565B1/de active Active
- 2012-06-18 CN CN201280030186.4A patent/CN103608175B/zh active Active
- 2012-06-18 WO PCT/EP2012/061547 patent/WO2012175433A1/de unknown
- 2012-06-18 DK DK12730870.8T patent/DK2723565T3/en active
- 2012-06-18 PL PL12730870T patent/PL2723565T3/pl unknown
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WO2003104327A1 (en) * | 2002-06-07 | 2003-12-18 | Dsm Ip Assets B.V. | Polyesteramide barrier film layer and its use |
EP2014730A1 (en) * | 2006-04-26 | 2009-01-14 | Kureha Corporation | Coating liquid, gas barrier film, gas barrier laminate and gas barrier multilayer film each using the coating liquid, and their production methods |
WO2007147560A1 (en) * | 2006-06-19 | 2007-12-27 | Dsm Ip Assets B.V. | Polyesteramides and compositions comprising them |
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Also Published As
Publication number | Publication date |
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WO2012175433A1 (de) | 2012-12-27 |
EP2723565A1 (de) | 2014-04-30 |
CN103608175A (zh) | 2014-02-26 |
DK2723565T3 (en) | 2015-06-01 |
EP2723565B1 (de) | 2015-03-11 |
BR112013032551A2 (pt) | 2017-01-17 |
ES2538854T3 (es) | 2015-06-24 |
PL2723565T3 (pl) | 2015-08-31 |
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