CN114889289A - 可生物降解膜 - Google Patents
可生物降解膜 Download PDFInfo
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- CN114889289A CN114889289A CN202210644353.XA CN202210644353A CN114889289A CN 114889289 A CN114889289 A CN 114889289A CN 202210644353 A CN202210644353 A CN 202210644353A CN 114889289 A CN114889289 A CN 114889289A
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- acid
- relative
- dicarboxylic acid
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- 125000000524 functional group Chemical group 0.000 claims description 14
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 4
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- 238000009264 composting Methods 0.000 description 4
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 4
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- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 3
- 239000004971 Cross linker Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
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- 125000002947 alkylene group Chemical group 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 3
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 3
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- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
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Abstract
本发明涉及可生物降解膜,其尤其适合于制造包装并还特征在于高水平的机械性能。
Description
本发明专利申请是申请号201780036719.2、申请日2017年6月13日、发明名称“可生物降解膜”的发明专利申请的分案申请。
描述
本发明涉及可生物降解膜,其尤其适合用于制造各种包装,尤其是携带商品的袋子和食品包装袋,其特征在于高水平机械性能,尤其是高抗撕裂性。包装,尤其是携带商品的袋子的生产要求使用具有良好机械性能的膜。
在可生物降解包装领域,除了机械性能之外,还需要使用一旦已经完成其主要用途就能够降解的材料,从而不会在环境中产生废物积累。开发组合了这些不同性能的可生物降解膜事实上是一个挑战,这种挑战要求通常彼此非常不协调的不同需求得到平衡。
本发明解决这一问题并提供能够合适地平衡这些不同要求的解决方案。特别地,本发明涉及通过包含以下组分的组合物制得的膜:
i)相对于组分i.-v.的总量,30-95重量%,优选50-85重量%的至少一种聚酯,其包含:
a)二羧酸组分,相对于总二羧酸组分包含:
a1)35-70摩尔%,优选40-60摩尔%,更优选45-60摩尔%衍生自至少一种芳族二羧酸的单元;
a2)65-30摩尔%,优选60-40摩尔%,更优选55-40摩尔%衍生自至少一种饱和脂族二羧酸的单元;
a3)0-5摩尔%衍生自至少一种不饱和脂族二羧酸的单元;
b)二醇组分,相对于总二醇组分包含:
b1)95-100摩尔%衍生自至少一种饱和脂族二醇的单元;
b2)0-5摩尔%衍生自至少一种不饱和脂族二醇的单元;
ii)相对于组分i.-v.的总量,0.1-50重量%,优选5-40重量%的至少一种天然来源的聚合物;
iii)相对于组分i.-v.的总量,1-40重量%,优选2-30重量%的至少一种聚羟基烷酸酯;
iv)相对于组分i.-v.的总量,0-15重量%的至少一种无机填料;
v)相对于组分i.-v.的总量,0-5重量%,优选0-0.5重量%至少一种包含至少一种具有两个和/或更多官能团的化合物的交联剂和/或扩链剂,所述官能团包括异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、唑啉、环氧化物、酸酐或二乙烯基醚基和它们的混合物。
已经令人惊奇地发现,具有这种组分组合的膜具有出奇好的机械性能和生物降解性能,从而使得它适合于制备各种包装。
尤其地,本发明涉及以下技术方案:
第1项.由包含以下组分的组合物制造的膜:
i)相对于组分i.-v.的总量,30-95重量%的至少一种聚酯,其包含:
a)二羧酸组分,相对于总二羧酸组分含有:
a1)35-70摩尔%衍生自至少一种芳族二羧酸的单元;
a2)65-30摩尔%衍生自至少一种饱和脂族二羧酸的单元;
a3)0-5摩尔%衍生自至少一种不饱和脂族二羧酸的单元;
b)二醇组分,相对于总二醇组分包含:
b1)95-100摩尔%衍生自至少一种饱和脂族二醇的单元;
b2)0-5摩尔%衍生自至少一种不饱和脂族二醇的单元;
ii)相对于组分i.-v.的总量,0.1-50重量%的至少一种天然来源的聚合物,
iii)相对于组分i.-v.的总量,1-40重量%的至少一种聚羟基烷酸酯;
iv)相对于组分i.-v.的总量,0-15重量%的至少一种无机填料;
v)相对于组分i.-v.的总量,0-5重量%的至少一种包含至少一种具有两个和/或多个官能团的化合物的交联剂和/或扩链剂,所述官能团包括异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、唑啉、环氧化物、酸酐、二乙烯基醚基和它们的混合物,
其中所述膜的特征在于根据ASTM D1922测定(在23℃和55%相对湿度下)的>100N/mm的纵向抗撕裂性。
第2项.根据第1项的膜,其中聚酯i.的组分a1中的芳族二羧酸选自苯二甲酸型芳族二羧酸,和杂环形二羧酸芳族化合物,它们的酯、盐和混合物。
第3项.根据第1-2项中任一项的膜,其中聚酯i.的组分a2的饱和脂族二羧酸包含混合物,所述混合物包含至少50摩尔%至少一种选自琥珀酸、己二酸、壬二酸、癸二酸、巴西基酸、它们的C1-C24,优选C1-C4酯和它们的混合物的酸。
第4项.根据第1-3项中任一项的膜,其中所述组分a2中的饱和脂族二羧酸选自己二酸和壬二酸或它们的混合物。
第5项.根据第1-4项中任一项的膜,其中聚酯i.的组分b1中的脂族二醇包含至少50摩尔%的一种或多种选自1,2-乙二醇、1,3-丙二醇、1,4-丁二醇的二醇。
第6项.根据第1-5项中任一项的膜,其中天然来源的聚合物ii.是淀粉。
第7项.根据第1-6项中任一项的膜,根据标准EN 13432是可生物降解的。
第8项.包含根据第1-7项中任一项的膜的包装。
第9项.根据第8项的包装,选自携带商品的袋子和食品包装袋。
第10项.根据第9项的携带商品的袋子。
第11项.用于水果和蔬菜的袋,包含根据第1-7项中任一项的膜。
特别地,根据本发明的膜结构上包含连续相和分散相,从而使所述膜在工业堆肥化处理条件下,更优选在家庭堆肥化处理中根据标准UNI11355是可快速生物降解的。所述膜还具有高水平的机械性能,尤其是根据ASTM D1922测定(在23℃和55%相对湿度下)的>100N/mm的纵向抗撕裂性。
至于聚酯i.,组分a1中的芳族二羧酸优选选自苯二甲酸型芳族二羧酸,优选对苯二甲酸或间苯二甲酸,更优选对苯二甲酸,和杂环形二羧酸芳族化合物,优选2,5-呋喃二羧酸、2,4-呋喃二羧酸、2,3-呋喃二羧酸、3,4-呋喃二羧酸,更优选2,5-呋喃二羧酸,它们的酯、盐和混合物。在一个优选的实施方案中,所述芳族二羧酸包含:
-1-99摩尔%,优选5-95摩尔%,更优选10-80摩尔%对苯二甲酸、其酯或盐;
-99-1摩尔%,优选95-5摩尔%,更优选90-20摩尔%2,5-呋喃二羧酸、其酯或盐。
聚酯i.的组分a2中的饱和脂族二羧酸优选选自饱和C2-C24,优选C4-C13,更优选C4-C11二羧酸,它们的C1-C24,优选C1-C4烷基酯,它们的盐和它们的混合物。优选地,饱和脂族二羧酸选自琥珀酸、2-乙基琥珀酸、戊二酸、2-甲基戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一烷二酸、十二烷二酸、巴西基酸、十六烷二酸、十八烷二酸和它们的C1-24烷基酯。在本发明的一个优选的实施方案中,饱和脂族二羧酸包含混合物,所述混合物包含至少50摩尔%,优选超过60摩尔%,更优选超过65摩尔%琥珀酸、己二酸、壬二酸、癸二酸、巴西基酸、它们的C1-C24,优选C1-C4酯和它们的混合物。在一个尤其优选的实施方案中,所述混合物包含己二酸和壬二酸或由己二酸和壬二酸组成并按5-40摩尔%,更优选10-35摩尔%的量含有壬二酸,相对于己二酸和壬二酸的总量。
聚酯i.的组分a3中的不饱和脂族二羧酸优选选自衣康酸、富马酸、4-亚甲基庚二酸、3,4-双(亚甲基)壬二酸、5-亚甲基壬二酸,它们的C1-C24,优选C1-C4烷基酯,它们的盐和它们的混合物。在本发明的一个优选的实施方案中,不饱和脂族二羧酸包含混合物,所述混合物含至少50摩尔%,优选超过60摩尔%,更优选超过65摩尔%衣康酸和其C1-C24,优选C1-C4酯。更优选,不饱和脂族二羧酸包含衣康酸。
至于聚酯i.的组分b1中的饱和脂族二醇,它们优选选自1,2-乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、1,7-庚二醇、1,8-辛二醇、1,9-壬二醇、1,10-癸二醇、1,11-十一烷二醇、1,12-十二烷二醇、1,13-十三烷二醇、1,4-环己烷二甲醇、新戊二醇、2-甲基-1,3-丙二醇、双脱水山梨糖醇、双脱水甘露糖醇、双脱水艾杜糖醇、环己烷二醇、环己烷甲烷二醇、二亚烷基二醇和具有100-4000的分子量的聚亚烷基二醇,例如聚乙二醇、聚丙二醇和它们的混合物。优选地,二醇组分包含至少50摩尔%的一种或多种选自1,2-乙二醇、1,3-丙二醇、1,4-丁二醇的二醇。更优选,所述二醇组分包含1,4-丁二醇或由1,4-丁二醇组成。
至于聚酯i.的组分b2中的不饱和脂族二醇,它们优选选自顺式2-丁烯-1,4-二醇、反式2-丁烯-1,4-二醇、2-丁炔-1,4-二醇、顺式2-戊烯-1,5-二醇、反式2-戊烯-1,5-二醇、2-戊炔-1,5-二醇、顺式2-己烯-1,6-二醇、反式2-己烯-1,6-二醇、2-己炔-1,6-二醇、顺式3-己烯-1,6-二醇、反式3-己烯-1,6-二醇、3-己炔-1,6-二醇。
优选地,聚酯i.包含至少10摩尔%,更优选至少20摩尔%,甚至更优选至少30摩尔%芳族二羧酸和/或脂族二羧酸和/或可再生来源的二醇。根据本发明,可以认为具有可再生来源的产物是从这样的来源获得的,即该来源根据它们的性质是可再生的并且基于人类生命的时间标定是用不完的,并且它们的使用因此不会负面影响后代对自然资源的可获得性。可再生来源的单体的实例是癸二酸、琥珀酸、2,5-呋喃二羧酸、壬二酸、1,4-丁二醇。
所述聚酯i.的Mn分子量优选≥20000,更优选≥40000。至于分子量的多分散指数Mw/Mn,其改为优选在1.5-10,更优选1.6-5,甚至更优选1.8-2.7。
可以使用凝胶渗透色谱(GPC)测量Mn和Mw分子量。这种测定可以用保持在40℃的色谱系统,使用一组两个串联柱(颗粒直径5μm和3μm,具有混合孔隙度),折光指数检测器,作为洗脱剂(流量0.5ml/min)的氯仿并使用聚苯乙烯作为参考标准进行。
所述聚酯i.的末端酸基含量优选小于100meq/kg,优选小于60meq/kg,甚至更优选小于40meq/kg。
末端酸基含量可以如下测量:将1.5-3g聚酯连同60ml氯仿一起置于100ml烧瓶中。在所述聚酯已经完全溶解后,添加25ml 2-丙醇,然后添加1ml去离子水,然后立即分析。针对NaOH在乙醇中的预先标准化的溶液滴定所获得的溶液。合适的指示器用来测定滴定的终点,例如在非水溶剂中的用于酸碱滴定的玻璃电极。使用以下方程式基于乙醇中的NaOH溶液的消耗量计算末端酸基含量:
其中:Veq=在样品滴定终点时乙醇中的NaOH的ml
Vb=在空白滴定中达到pH值9.5所要求的NaOH在乙醇中的溶液的ml;
T=所述乙醇中的NaOH溶液的浓度,表示为摩尔/升;
P=样品的重量,克。
聚酯i.具有大于0.3dl/g,优选0.3-2dl/g,更优选0.4-1.1dl/g的特性粘度(使用厄布洛德(Ubbelohde)粘度计对在CHCl3中浓度为0.2g/dl的溶液在25℃下测量)。
优选地,聚酯i.是可生物降解的。对于本发明意义来说,可生物降解聚合物是指根据标准EN 13432可生物降解的聚合物。
所述聚酯i.可以根据现有技术中已知的任何方法合成。特别地,它可以有利地经由缩聚反应获得。
有利地,合成方法可以在适合的催化剂存在下进行。作为适合的催化剂,可以提及例如锡的有机金属化合物,例如锡酸衍生物,钛化合物,例如钛酸正-丁酯(orthobutyltitanate),铝化合物,例如三异丙基铝,锑和锌和锆的化合物,和它们的混合物。
至于组分ii.,根据本发明的膜的组合物包含0.1-50重量%,优选5-40重量%的至少一种天然来源的聚合物,相对于组分i.-v.的总量。天然来源的聚合物(组分ii.)有利地选自淀粉,壳多糖,壳聚糖,藻酸盐,蛋白例如谷蛋白、玉米蛋白、酪蛋白,胶原,明胶,天然橡胶,松香酸和它们的衍生物。优选地,天然来源的聚合物是淀粉。
术语“淀粉”在这里是指所有类型的淀粉,即:面粉、天然淀粉、水解淀粉、变性淀粉(destructured starch)、糊化淀粉、增塑淀粉、热塑性淀粉、包含复合淀粉的生物填料或它们的混合物。根据本发明尤其适合的是淀粉例如马铃薯、玉米、木薯和豌豆淀粉。
可以容易变性并且具有高初始分子量的淀粉,例如马铃薯或玉米淀粉已经证明是尤其有利的。
淀粉可以按原样存在或呈化学改性形式,例如呈具有0.2-2.5的取代度的淀粉酯、羟基丙基化淀粉或脂肪链改性淀粉形式。
此处提到“变性淀粉”参考在专利EP-0 118 240和EP-0 327 505中包括的教导,此种淀粉是指已经被加工使得在光学显微镜下在偏振光中基本上不具有所谓的"偏光十字(Maltese crosses)"和在相差光学显微镜下基本上不具有所谓的"重影(ghosts)"。
有利地,借助挤出方法,在110-250℃,优选130-180℃的温度下,优选在0.1-7MPa,优选0.3-6MPa的压力下,使淀粉变性,从而优选在所述挤出期间提供大于0.1kWh/kg的比能。
淀粉的变性优选相对于淀粉的重量,在1-40重量%选自水和含2-22个碳原子的多元醇中的一种或多种增塑剂存在下进行。至于水,它也可以是天然存在于淀粉中的水。在多元醇当中,优选的那些是具有1-20个羟基含有2-6个碳原子的多元醇,它们的醚,硫醚和有机和无机酯。多元醇的实例是甘油、二甘油、聚甘油、季戊四醇、聚甘油乙氧基化物、乙二醇、聚乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、新戊二醇、山梨糖醇单乙酸酯、山梨糖醇二乙酸酯、山梨糖醇单乙氧基化物、山梨糖醇二乙氧基化物及其混合物。在一个优选的实施方案中,在甘油或含甘油,更优选含2-90重量%甘油的增塑剂的混合物存在下,使淀粉变性。优选地,根据本发明的变性和交联淀粉包含1-40重量%增塑剂,相对于淀粉的重量。
淀粉优选以具有圆形或椭圆形截面或者在任何情况下类似于椭圆的截面的颗粒形式存在,所述椭圆具有在使用颗粒的主轴情况下测量的小于1微米,更优选小于0.5μm的平均直径的算术平均直径。
至于组分iii.,根据本发明的膜的组合物相对于组分i.-v.的总量包含1-40重量%,优选2-30重量%的至少一种聚羟基烷酸酯(组分iii.),优选选自乳酸的聚酯、聚-ε-己内酯、聚羟基丁酸酯、聚羟基丁酸酯-戊酸酯、聚羟基丁酸酯-丙酸酯、聚羟基丁酸酯-己酸酯、聚羟基丁酸酯-癸酸酯、聚羟基丁酸酯-十二烷酸酯、聚羟基丁酸酯-十六烷酸酯、聚羟基丁酸酯-十八烷酸酯、聚-3-羟基丁酸酯-4-羟基丁酸酯。优选地,所述聚羟基烷酸酯包含至少80重量%的一种或多种乳酸聚酯。
在一个优选的实施方案中,所述乳酸聚酯选自聚-L-乳酸、聚-D-乳酸、聚-D-L-乳酸立构复合物,包含大于50摩尔%所述乳酸聚酯的共聚物,或它们的混合物。
尤其优选的是含至少95重量%衍生自L-乳酸或D-乳酸或其组合的重复单元的具有大于50000的分子量Mw和50-500Pa.s,优选100-300Pa.s(根据ASTM标准D3835在T=190℃、剪切速率=1000s-1、D=1mm、L/D=10下测量)的剪切粘度的乳酸聚酯。
在本发明的一个尤其优选的实施方案中,乳酸聚酯包含至少95重量%衍生自L-乳酸的单元,≤5%衍生自D-乳酸的重复单元,具有135-180℃的熔点、55-65℃的玻璃化转变温度(Tg)和1-50g/10min的MFR(根据标准ISO1133-1在190℃和2.16kg下测量)。具有这些性能的乳酸聚酯的商业实例是例如IngeoTMBiopolymer4043D、3251D和6202D制造的产品。
至于组分iv.,根据本发明的膜的组合物相对于组分i.-v.的总量包含0-15重量%的至少一种无机填料(组分iv.),其优选选自高岭土,重晶石,粘土,滑石,钙和镁、铁和铅的碳酸盐,氢氧化铝,硅藻土,硫酸铝,硫酸钡,二氧化硅,云母,二氧化钛,硅灰石。
在本发明的一个优选的实施方案中,无机填料包括呈颗粒形式存在的滑石、碳酸钙或它们的混合物,所述颗粒具有在考虑颗粒的主轴情况下小于10微米的算术平均直径。已经事实上发现,上述类型的不以所述算术平均直径为特征的填料证明在含它们的物体的工业堆肥化处理期间显著更低的可粉碎能力(disintegratability)特性。
至于组分v.,本发明的膜的组合物相对于组分i.-v.的总量包含0-5重量%,优选0-0.5重量%的至少一种交联剂和/或扩链剂(组分v.)以便改进水解稳定性。
所述交联剂和/或扩链剂选自具有两个和/或多个官能团的化合物,所述官能团包括异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、唑啉、环氧基、酸酐或二乙烯基醚基和它们的混合物。优选地,交联剂和/或扩链剂包含至少一种具有两个和/或多个官能团的化合物,所述官能团包括异氰酸酯基。更优选,交联剂和/或扩链剂包含至少25重量%的一种或多种具有两个和/或多个官能团的化合物,所述官能团包括异氰酸酯基。尤其优选的是具有两个和/或多个包括异氰酸酯基的官能团的化合物与具有两个和/或多个包括环氧基的官能团的化合物的混合物,甚至更优选包含至少75重量%的具有两个和/或多个包括异氰酸酯基的官能团的化合物。
具有两个和多个包括异氰酸酯基的官能团的化合物优选选自对-亚苯基二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4-二苯基甲烷-二异氰酸酯、1,3-亚苯基-4-氯二异氰酸酯、1,5-萘二异氰酸酯、4,4-二亚苯基二异氰酸酯、3,3'-二甲基-4,4-二苯甲烷二异氰酸酯、3-甲基-4,4'-二苯甲烷二异氰酸酯、二苯酯二异氰酸酯、2,4-环己烷二异氰酸酯、2,3-环己烷二异氰酸酯、1-甲基2,4-环己基二异氰酸酯、1-甲基2,6-环己基二异氰酸酯、双-(异氰酸酯环己基)甲烷、2,4,6-甲苯三异氰酸酯、2,4,4-二苯醚三异氰酸酯、多亚甲基-多苯基-多异氰酸酯、亚甲基二苯基二异氰酸酯、三苯甲烷三异氰酸酯、3,3'-二甲苯-4,4-二异氰酸酯、4,4'-亚甲基双(2-甲基-苯基异氰酸酯)、六亚甲基二异氰酸酯、1,3-亚环己基二异氰酸酯、1,2-亚环己基二异氰酸酯和它们的混合物。在一个优选的实施方案中,含异氰酸酯基的化合物是4,4-二苯基甲烷二异氰酸酯。
至于具有两个和/或多个包括过氧化物基团的官能团的化合物,它们优选选自过氧化苯甲酰、过氧化月桂酰、过氧化异壬酰、二-(叔丁基过氧异丙基)苯、过氧化叔丁基、过氧化二枯基、α,α-二(叔丁基过氧)二异丙苯、2,5-二甲基-2,5-二(叔丁基过氧)己烷、过氧化叔丁基异丙苯、过氧化二-叔丁基、2,5-二甲基-2,5-二(叔丁基过氧)己-3-炔、过氧化二碳酸二(4-叔丁基环己基)酯、过氧化二碳酸二鲸蜡基酯、过氧化二碳酸二肉豆蔻酯、3,6,9-三乙基-3,6,9-三甲基-1,4,7-三过氧壬烷、过氧化二碳酸二(2-乙基己基)酯和它们的混合物。
优选用于根据本发明的组合物的具有两个和/或多个包括碳二亚胺基团的官能团的化合物选自聚(环辛烯碳二亚胺)、聚(1,4-二亚甲基环己烯碳二亚胺)、聚(环己烯碳二亚胺)、聚(乙烯碳二亚胺)、聚(丁烯碳二亚胺)、聚(异丁烯碳二亚胺)、聚(壬烯碳二亚胺)、聚(十二碳烯碳二亚胺)、聚(新戊烯碳二亚胺)、聚(1,4-二亚甲基亚苯基碳二亚胺)、聚(2,2',6,6'-四异丙基二亚苯基碳二亚胺)(D)、聚(2,4,6-三异丙基-1,3-亚苯基碳二亚胺)(P-100)、聚(2,6二异丙基-1,3-亚苯基碳二亚胺)(P)、聚(甲苯基碳二亚胺)、聚(4,4'-二苯甲烷碳二亚胺)、聚(3,3'-二甲基-4,4'-亚联苯基碳二亚胺)、聚(对亚苯基碳二亚胺)、聚(间亚苯基碳二亚胺)、聚(3,3'-二甲基-4,4'-二苯甲烷碳二亚胺)、聚(萘碳二亚胺)、聚(异佛尔酮碳二亚胺)、聚(枯烯碳二亚胺)、对亚苯基双(乙基碳二亚胺)、1,6-六亚甲基双(乙基碳二亚胺)、1,8-八亚甲基双(乙基碳二亚胺)、1,10-十亚甲基双(乙基碳二亚胺)、1,12十二亚甲基双(乙基碳二亚胺)和它们的混合物。
可以在根据本发明的组合物中有利使用的具有两个和多个包括环氧基的官能团的化合物的实例是所有得自环氧基化油和/或苯乙烯-缩水甘油醚-甲基丙烯酸甲酯、或缩水甘油醚甲基丙烯酸甲酯,包括1000-10000的分子量并具有1-30,优选5-25的环氧值/分子的所有聚环氧化物,所选的环氧化物在包括以下物质的组中:二乙二醇二缩水甘油醚、聚乙二醇二缩水甘油醚、甘油聚缩水甘油醚、双甘油聚缩水甘油醚、1,2-环氧丁烷、聚甘油聚缩水甘油醚、异戊二烯二环氧化物和脂环族二环氧化物、1,4-环己烷二甲醇二缩水甘油醚、缩水甘油基2-甲基苯基醚、甘油丙氧基合三缩水甘油醚、1,4-丁二醇二缩水甘油醚、山梨糖醇聚缩水甘油醚、甘油二缩水甘油醚、间二甲苯二胺的四缩水甘油醚和双酚A的二缩水甘油醚和它们的混合物。
催化剂也可以与具有两个和多个包括异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、唑啉、环氧基、酸酐和二乙烯基醚基的官能团的化合物例如上述那些一起用于提高反应性基团的反应性。在聚环氧化物情况下,优选可以使用脂肪酸盐,甚至更优选硬脂酸钙和锌。
在本发明的一个尤其优选的实施方案中,组合物的交联剂和/或扩链剂包含包括异氰酸酯基的化合物,优选4,4-二苯基甲烷二异氰酸酯,和/或含碳二亚胺基的化合物,和/或含环氧基的化合物,优选苯乙烯-缩水甘油醚-甲基丙烯酸甲酯型化合物。
除了上述的组分i.-v.之外,还可以有利地存在一种或多种其它组分。根据本发明的膜包含组合物,所述组合物包含组分i.-v.和优选一种或多种不与组分i.、ii.和iii.相同的可以可生物降解或可以非生物降解的合成或天然来源的聚合物,连同可能的一种或多种其它组分。
至于所述不与组分i.、ii.和iii.相同的可以可生物降解或可以非生物降解的合成或天然来源的聚合物,它们有利地选自包括以下物质的组:乙烯基聚合物、与聚酯i.不相同的二酸二醇聚酯、聚酰胺、聚氨酯、聚醚、聚脲、聚碳酸酯和它们的混合物。
乙烯基聚合物中,优选的那些是:聚乙烯、聚丙烯、它们的共聚物、聚乙烯醇、聚乙酸乙烯酯、聚乙酸乙基乙烯酯和聚乙烯乙烯基醇、聚苯乙烯、氯化乙烯基聚合物、聚丙烯酸酯。
氯化乙烯基聚合物当中,据理解应包括在这里的那些是,除了聚氯乙烯之外,聚偏二氯乙烯、聚氯化乙烯、聚(氯乙烯-乙酸乙烯酯)、聚(氯乙烯-乙烯)、聚(氯乙烯-丙烯)、聚(氯乙烯-苯乙烯)、聚(氯乙烯-异丁烯)和其中聚氯乙烯占超过50摩尔%的共聚物。所述聚合物可以是无规、嵌段或交替共聚物。
至于根据本发明的组合物中的聚酰胺,它们优选选自包括以下物质的组:聚酰胺6和6,6,聚酰胺9和9,9,聚酰胺10和10,10,聚酰胺11和11,11,聚酰胺12和12,12和它们的所述6/9、6/10、6/11、6/12型的组合,它们的混合物和无规和嵌段共聚物。
优选地,根据本发明的组合物中的聚碳酸酯选自包括以下物质的组:聚碳酸亚烷基酯,更优选聚碳酸亚乙基酯、聚碳酸亚丙基酯、聚碳酸亚丁基酯、它们的混合物和无规和嵌段共聚物。
聚醚当中,优选的那些是选自具有70000-500000的分子量的聚乙二醇、聚丙二醇、聚丁二醇、它们的共聚物和它们的混合物的那些。
至于与聚酯i.不相同的二酸二醇聚酯,它们优选包含:
c)二羧酸组分,相对于总二羧酸组分包含:
c1)20-100摩尔%衍生自至少一种芳族二羧酸的单元,
c2)0-80摩尔%衍生自至少一种饱和脂族二羧酸的单元,
c3)0-5摩尔%衍生自至少一种不饱和脂族二羧酸的单元;
d)二醇组分,相对于总二醇组分包含:
d1)95-100摩尔%衍生自至少一种饱和脂族二醇的单元;
d2)0-5摩尔%衍生自至少一种不饱和脂族二醇的单元。
优选地,所述聚酯的芳族二羧酸c1、饱和脂族二羧酸c2、不饱和脂族二羧酸c3、饱和脂族二醇d1和不饱和脂族二醇d2选自上面对根据本发明的聚酯i描述的那些。
除了上述组分以外,根据本发明的组合物优选还包含选自以下物质中的至少一种其它组分:增塑剂、UV稳定剂、润滑剂、成核剂、表面活性剂、抗静电剂、颜料、阻燃剂、增容剂、木质素、有机酸、抗氧化剂、防霉剂、蜡、加工助剂和优选选自乙烯基聚合物、不是上述脂族-芳族聚酯的二酸二醇聚酯、聚酰胺、聚氨酯、聚醚、聚脲或聚碳酸酯的聚合物组分。
至于增塑剂,除了优选用于制备上述变性淀粉的增塑剂以外,还存在一种或多种选自苯二甲酸酯,例如邻苯二甲酸二异壬酯,偏苯三酸酯,例如偏苯三酸与C4-C20一元醇(其优选选自正辛醇和正癸醇)的酯,和具有下述结构的脂族酯中的增塑剂:
R1-O-C(O)-R4-C(O)-[-O-R2-O-C(O)-R5-C(O)-]m-O-R3
其中:
R1选自如下的一种或多种基团:H,C1-C24类型的线性和支化饱和和不饱和烷基残基,用C1-C24一元羧酸酯化的多元醇残基;
R2包含-CH2-C(CH3)2-CH2-和C2-C8亚烷基,并包含至少50摩尔%的所述-CH2-C(CH3)2-CH2-基团;
R3选自如下的一种或多种基团:H,C1-C24类型的线性和支化饱和和不饱和烷基残基,用C1-C24一元羧酸酯化的多元醇残基;
R4和R5是相同或不同的,包含一个或多个C2-C22,优选C2-C11,更优选C4-C9亚烷基,并包含至少50摩尔%的C7亚烷基。
m是1-20,优选2-10,更优选3-7的数值。优选地,在所述酯中,基团R1和/或R3中的至少一个包含用至少一种C1-C24一元羧酸酯化的多元醇残基,相对于R1和/或R3基团的总量,优选按≥10摩尔%,更优选≥20摩尔%,甚至更优选≥25摩尔%的量,所述一元羧酸选自硬脂酸、棕榈酸、9-酮基硬脂酸、10-酮基硬脂酸及其混合物。这种类型的脂族酯的实例描述在意大利专利申请MI2014A000030和PCT申请PCT/EP2015/050336、PCT/EP2015/050338中。
当存在时,所选的增塑剂优选存在至多10重量%,相对于根据本发明的膜的组合物的总重量。
润滑剂优选选自脂肪酸的酯和金属盐例如硬脂酸锌、硬脂酸钙、硬脂酸铝和乙酰基硬脂酸酯。优选地,根据本发明的膜的组合物包含至多1重量%的润滑剂,更优选至多0.5重量%,相对于根据本发明的膜的组合物的总重量。
成核剂的实例包括糖精的钠盐,硅酸钙,苯甲酸钠,钛酸钙,氮化硼,全同立构聚丙烯,或低分子量PLA。这些添加剂优选按至多10重量%,更优选2-6重量%的量添加,相对于该组合物的总重量。
如果有必要的话,也可添加颜料,例如二氧化钛,粘土,酞菁铜,硅酸盐、铁氧化物和氢氧化物,炭黑和氧化镁。这些添加剂优选至多添加10重量%。
根据本发明的膜有利地具有小于40μm,优选小于30μm的厚度。
根据本发明的膜的特征在于根据ASTM D1922测定(在23℃和55%相对湿度下)的>100N/mm的纵向抗撕裂性。
优选地,根据本发明的膜的特征在于根据ASTM D1922测定(在23℃和55%相对湿度下)的>150N/mm的沿横向的抗撕裂性。
优选地,根据本发明的膜的特征在于根据标准ASTM D882(拉伸性能,在23℃和55%相对湿度和Vo=50mm/min下)测定的>15MPa的断裂负荷、>200%的断裂伸长率、>200MPa的弹性模量、>2000MPa的断裂能。
优选地,根据本发明的膜的特征在于>100N/mm的纵向抗撕裂性、>150N/mm的横向抗撕裂性(根据ASTM D1922在23℃和55%相对湿度下测定)、>15MPa的断裂负荷、>200%的断裂伸长率、>200MPa的弹性模量、>2000MPa的断裂能(根据标准ASTM D882测定,拉伸性能,在23℃和55%相对湿度和Vo=50mm/min下)。根据本发明的膜根据标准EN 13432是可生物降解的。优选地,根据本发明的膜在根据标准UNI11355的家庭堆肥化处理中是可生物降解的。
根据本发明的膜尤其适合于制备广泛范围的制品,例如各种包装,尤其是携带商品的袋子和食品包装袋例如用于水果和蔬菜的袋。优选地,所述包含本发明膜的用于水果和蔬菜的袋的特征在于小于20μm,更优选小于17μm,甚至更优选小于15μm的厚度。
根据本发明的膜可以有利地作为单个层使用或用于多层膜。所述多层膜可以根据本领域中已知的那些方法中的任一种,经由例如共挤出、涂覆/铺展或层压方法制备。
现将基于许多不希望用来进行限制的实施例说明本发明。
实施例
i-1.含49摩尔%对苯二甲酸1,4-丁二醇酯单元和30摩尔%壬二酸单元的聚(己二酸1,4-丁二醇酯-共聚-壬二酸1,4-丁二醇酯-共聚-对苯二甲酸1,4-丁二醇酯),相对于壬二酸和己二酸单元的总量。MFR6.7/10min(在190℃,2.16kg)和33meq/kg量末端酸基。
i-2.含48.5摩尔%对苯二甲酸1,4-丁二醇酯单元和20摩尔%壬二酸单元的聚(己二酸1,4-丁二醇酯-共聚-壬二酸1,4-丁二醇酯-共聚-对苯二甲酸1,4-丁二醇酯),相对于壬二酸和己二酸单元的总量。MFR 6.6/10min(在190℃,2.16kg)和35meq/kg量末端酸基。
i-3.含48摩尔%对苯二甲酸1,4-丁二醇酯单元和13摩尔%壬二酸单元的聚(己二酸1,4-丁二醇酯-共聚-壬二酸1,4-丁二醇酯-共聚-对苯二甲酸1,4-丁二醇酯),相对于壬二酸和己二酸单元的总量。MFR6.2/10min(在190℃,2.16kg)和48meq/kg量末端酸基。
i-4.含48摩尔%对苯二甲酸1,4-丁二醇酯单元和6摩尔%壬二酸单元的聚(己二酸1,4-丁二醇酯-共聚-壬二酸1,4-丁二醇酯-共聚-对苯二甲酸1,4-丁二醇酯),相对于壬二酸和己二酸单元的总量。MFR5.5/10min(在190℃,2.16kg)和49meq/kg量末端酸基。
i-5.含47摩尔%对苯二甲酸1,4-丁二醇酯单元的聚(己二酸1,4-丁二醇酯-共聚-对苯二甲酸1,4-丁二醇酯)。MFR 6.9/10min(在190℃,2.16kg)和42meq/kg量末端酸基。
iii.Ingeo 4043D聚乳酸(“PLA”)。MFR 3.0/10min(在190℃,2.16kg)。
ii.热塑性玉米淀粉。
iv.碳酸钙Cacitec M/2,得自Mineraria Sacilese。
v-1.得自Anderson Development Company的苯乙烯-缩水甘油醚-甲基丙烯酸甲酯共聚物Almatex PD4440。
v-2.得自Nisshinbo Chemical Inc.的HMV-15CA Carbodilite。
表1
将表1指示的组合物供给具有L/D=40和直径30mm配备有15个加热区的同向旋转双螺杆挤出机(APV2030)。挤出参数如下:
-rpm:250
-流速:9Kg/h
-热分布:30-90-160-200×10-165×3℃
-脱气,以L/D=30
在40mm Ghioldi上(模口间隙=0.9mm,流动速率24kg/h和吹胀比=3.2)将表1的组合物成膜而获得具有25μm(牵伸比=11.4)、20μm(牵伸比=14.3)和14μm(牵伸比=20.4)厚度的膜。
根据标准ASTM D882(在23℃和55%相对湿度,Vo=50mm/min下牵引)以及根据ASTM D1922(抗撕裂,在23℃和55%相对湿度下)对所述膜进行机械表征。
结果提供在下表2中。
表2
Claims (9)
1.包含膜的多层膜,所述膜由包含以下组分的组合物制造:
i)相对于组分i.-v.的总量,30-95重量%的至少一种聚酯,其包含:
a)二羧酸组分,相对于总二羧酸组分含有:
a1)35-70摩尔%衍生自至少一种芳族二羧酸的单元;
a2)65-30摩尔%衍生自至少一种饱和脂族二羧酸的单元;
a3)0-5摩尔%衍生自至少一种不饱和脂族二羧酸的单元;
b)二醇组分,相对于总二醇组分包含:
b1)95-100摩尔%衍生自至少一种饱和脂族二醇的单元;
b2)0-5摩尔%衍生自至少一种不饱和脂族二醇的单元;
ii)相对于组分i.-v.的总量,0.1-50重量%的至少一种天然来源的聚合物,
iii)相对于组分i.-v.的总量,1-40重量%的至少一种聚羟基烷酸酯;
iv)相对于组分i.-v.的总量,0-15重量%的至少一种无机填料;
v)相对于组分i.-v.的总量,0-5重量%的至少一种包含至少一种具有两个和/或多个官能团的化合物的交联剂和/或扩链剂,所述官能团包括异氰酸酯、过氧化物、碳二亚胺、异氰脲酸酯、唑啉、环氧化物、酸酐、二乙烯基醚基和它们的混合物,
其中所述膜的特征在于根据ASTM D1922测定(在23℃和55%相对湿度下)的>100N/mm的纵向抗撕裂性。
2.根据权利要求1的多层膜,其中聚酯i.的组分a1中的芳族二羧酸选自苯二甲酸型芳族二羧酸,和杂环形二羧酸芳族化合物,它们的酯、盐和混合物。
3.根据权利要求1-2中任一项的多层膜,其中组分a2中的饱和脂族二羧酸选自己二酸和壬二酸或它们的混合物。
4.根据权利要求1-3中任一项的多层膜,其中聚酯i.的组分b1中的脂族二醇包含至少50摩尔%的一种或多种选自1,2-乙二醇、1,3-丙二醇、1,4-丁二醇的二醇。
5.根据权利要求1-4中任一项的多层膜,其中天然来源的聚合物ii.是淀粉。
6.包含根据权利要求1-5中任一项的多层膜的包装。
7.根据权利要求6的包装,选自携带商品的袋子和食品包装袋。
8.根据权利要求7的携带商品的袋子。
9.用于水果和蔬菜的袋,包含根据权利要求1-5中任一项的多层膜。
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