CN108367535A - 包含聚乙烯醇缩丁醛的装饰性多层表面覆盖物 - Google Patents
包含聚乙烯醇缩丁醛的装饰性多层表面覆盖物 Download PDFInfo
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- CN108367535A CN108367535A CN201680071161.7A CN201680071161A CN108367535A CN 108367535 A CN108367535 A CN 108367535A CN 201680071161 A CN201680071161 A CN 201680071161A CN 108367535 A CN108367535 A CN 108367535A
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- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 title claims abstract description 76
- 239000000203 mixture Substances 0.000 claims abstract description 112
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- 239000004626 polylactic acid Substances 0.000 claims abstract description 37
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- -1 aliphatic dicarboxylic acid Ester Chemical class 0.000 claims description 48
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- 150000001336 alkenes Chemical class 0.000 claims description 40
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- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 26
- 239000011521 glass Substances 0.000 claims description 25
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 24
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 21
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
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- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 5
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 4
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- QYQADNCHXSEGJT-UHFFFAOYSA-N cyclohexane-1,1-dicarboxylate;hydron Chemical compound OC(=O)C1(C(O)=O)CCCCC1 QYQADNCHXSEGJT-UHFFFAOYSA-N 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
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- KPMFJARPXKCVHQ-UHFFFAOYSA-N methyl prop-2-enoate Chemical compound COC(=O)C=C.COC(=O)C=C KPMFJARPXKCVHQ-UHFFFAOYSA-N 0.000 claims description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 150000007860 aryl ester derivatives Chemical class 0.000 claims 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 claims 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 58
- 239000000463 material Substances 0.000 description 21
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 15
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- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 7
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- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 6
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Abstract
本发明涉及包含芯层的装饰性多层表面覆盖物，其中所述芯层包含聚合物共混物，所述聚合物共混物包含聚乙烯醇缩丁醛和聚乳酸。
Description
技术领域
本发明涉及包含芯层的装饰性多层表面覆盖物，所述芯层包含聚乙烯醇缩丁醇和聚乳酸和/或一种或多种包含丙烯酸酯的聚合物。本发明进一步涉及一种用于生产所述表面覆盖物的方法。
背景技术
合成地板已经获得广泛的商业接受，并且由各种地板组合物制成，这些地板组合物可以包含各种各样的树脂或树脂的混合物。
地板材料必须满足若干技术标准，例如像耐磨性和耐擦伤性，耐污性，在硬度与柔性之间的良好平衡，与附加辅助剂例如像增塑剂、填充剂、UV稳定剂、颜料和着色剂、阻燃剂和抗静电剂的相容性，其易于工业加工的可能性，以及经济上有吸引力的原料成本。
尽管诸如贴砖等地板经常被制成单层，但也可以使用表现出不同使用特性的多层施工组合物。
典型的多层地板可以含有例如从下到上看到的芯层、着色的和/或印刷的界面层、透明的耐磨层以及有可能地聚氨酯或聚(甲基)丙烯酸酯的额外的顶部耐磨层。这种地板可以任选地与形式稳定元件(例如像，玻璃纤维毡和背衬层)组合。
许多当前的合成地板组合物的主要组分是可以以各种形式施用的聚氯乙烯(PVC)，例如像增塑的PVC和PVC泡沫。事实上，PVC几乎是广泛用于地板材料中的唯一聚合物。
出于环境和其他原因，存在开发用于地板的具有大大减少的氯含量的适当的树脂组合物的持续努力。
与PVC装饰性覆盖段有关的生态关注涉及再循环能力或能量回收、挥发性有机物含量水平和重金属稳定剂的使用。
来自重金属稳定剂分解的氯化氢和重金属灰是来自与PVC基覆盖材料的制造和安装相关的废料的焚烧的不希望的结果。
因此，即使PVC在其到地板覆盖物的应用中提供了优异的机械、隔音和隔热折中，这些覆盖物的制造商一直在寻找其替代物，提供对以下三个关注点的答案：
-在燃烧时不释放有毒气体，诸如氯气、盐酸、二氧化硫或氮氧化物；
-具有与现今用PVC获得的特性相同量级的特性，尤其是机械特性和耐火性；
-能够在现有设备上加工或制造，尤其是通过挤出、压延等。
近年来，不含PVC的地板和墙壁覆盖物材料已经变得流行并且已经成为相当多专利的主题，例如像EP 0257796(B1)、EP 0742098(B1)、EP 0850272(B1)、EP1611201(B1)、US4,379,190、US 4,403,007、US 4,438,228、US 5,409,986、US 6,214,924、US 6,187,424、US2011/0305886、JP 2004168860、JP 2002276141、JPH 07125145、JPH 06128402、JP2000063732、JPH 1148416、JP 2000045187、JPH 0932258、JPS 6092342以及JPH 09302903。
鉴于日益增长的环保意识，有利的是，最大程度地替换石油化学塑料并且具有再循环的“难生物降解的”聚合物，如聚乙烯醇缩丁醛(PVB)和/或生态友好的“绿色”材料，如聚乳酸(PLA)作为用于地板应用的一种或多种原料，从而提供具有希望的物理和机械特性的地板。
PLA(聚乳酸)已经成为大多数商业上成功的生物塑料之一，并且将其引入地板和墙壁覆盖物中已经成为许多专利的主题。
US 2005/0136259涉及基于聚丙交酯的产品，并且更具体地涉及耐久的贴砖或薄片形式的地板覆盖物，这些地板覆盖物由适合于例如在延长的时间段内的国内行人交通和/或其他情形的聚合物的一个或多个层制成。
US 2010/0015420涉及一种生物层压复合组件，其包括一个或多个生物层压层、非塑料刚性基板以及与该基板和该一个或多个生物层压层接触的粘合剂层。生物层压件是指包括与任选的添加剂、着色剂、填充剂、增强剂、矿物和其他输入组合的衍生自天然或生物组分的材料如聚乳酸的一个或多个薄层。
US 2013/004751披露了一种使用聚乳酸树脂的地板材料，其包含基础层、在该基础层顶部上形成并且在其上侧上具有印刷图案的印刷层、以及在该印刷层顶部上形成的透明层，其中该基础层、该印刷层、以及该透明层中的一个或多个包括聚乳酸树脂。
EP 1361039B1披露了聚合物材料以及由这些聚合物材料制备的产物，这些聚合物材料包括与增塑剂和增容剂组合的聚乳酸基聚合物，并且任选地包括填充剂。该聚合物材料可以包括在约30至约50重量百分比之间的聚氯乙烯、聚乙二醇、聚乙交酯、乙烯-乙酸乙烯酯、聚碳酸酯、聚己酸内酯、聚羟基链烷酸酯和用极性基团改性的聚烯烃如离聚物。该增塑剂典型地是环氧化的植物油或者酯化的并且环氧化的植物油，并且典型地以按重量计在约10％与约50％之间的量存在。包含用一个或多个极性官能团改性的聚烯烃的增容剂典型地以按重量计在约5％与约10％之间的量存在。该材料可以在装饰性表面覆盖物如地板覆盖物中使用，特别是当它呈聚合物薄片的形式时。
WO 2007/089451和WO 2009/045564涉及一种或多种可生物降解聚合物与按重量计从0.1％至15％的量的一种或多种丙烯酸共聚物的共混物，为了改进所述一种或多种可生物降解聚合物的良好的金属释放特性以及其他改进的特性如熔体强度的目的。例如聚丙交酯的一个问题是其差的熔体强度，导致在随后熔融加工中的困难。
WO 92/04412涉及多羟基酸聚合物(如聚乳酸)以及特征为具有足够数量和分布的亲水基团的其他相容的热塑性聚合物(如共聚醚酯、包含乙烯乙烯醇的共聚物和聚烯烃)的共混物的膜，以及这些膜通过熔融加工的生产。
聚乙烯醇缩丁醛(PVB)薄片在用于机动车辆、飞机、建筑、安全和类似应用的层压安全玻璃窗中被广泛用作清晰透明的冲击吸收夹层。
来自这些安全玻璃的玻璃可以通过常规技术来回收，如研磨、破碎、以及碾磨废玻璃以便将碎玻璃回收给玻璃制造商，而PVB在填埋场或焚化炉中被处置掉。
考虑到可获得丰富的量的消费后的PVB，已经检查了合适的再循环可能性如其在成形物品如表面覆盖物的生产中的使用。
EP 1084188B1披露了一种包含以下各项的组合物：a)5至95重量份的聚氯乙烯以及b)95至5重量份的未经利用的或再循环的/回收的聚乙烯醇缩丁醛/100重量份的组合的所述聚氯乙烯和所述聚乙烯醇缩丁醛；以及c)1至50重量份的高分子量固体含乙烯的增塑剂/100重量份的组合的所述聚氯乙烯、所述聚乙烯醇缩丁醛和所述含乙烯的增塑剂。
US 2,552,600披露了由包括粘合剂的柔性的耐碱的装饰性耐磨层构成的地板和墙壁覆盖物，该粘合剂包含增塑的聚乙烯醇缩丁醛和热固性酚醛树脂。
EP 0471658B1披露了一种地板组合物，其在包含按重量计95％至25％的回收的增塑的PVB和按重量计5％至75％的另一种相容的树脂的树脂混合物中包含从层压的安全玻璃回收的增塑的聚乙烯醇缩丁醛树脂，该层压的安全玻璃含有按重量计最高达10％的量的微小玻璃颗粒，该相容的树脂包括均聚物和共聚物，例如像聚乙烯醇缩丁醛、聚氯乙烯、聚乙酸乙烯酯、聚乙基乙酸乙烯酯、聚乙烯醇缩甲醛、丁腈橡胶等。
EP 0419438B1披露了由聚合物共混物形成的薄片，该聚合物共混物包含基于重量的a)30％至90％的含有约11％至30％的羟基的聚乙烯醇缩丁醛以及b)70％至10％的热塑性聚氨酯。
EP 0853097披露了一种适合于弹性地板的聚合物组合物，该聚合物组合物包含聚乙烯醇缩丁醛以及含有极性部分的聚合物，该极性部分对于与该聚乙烯醇缩丁醛形成氢键是有效的，其中该具有极性部分的聚合物以基于组合的该聚乙烯醇缩丁醛和该具有极性部分的聚合物的重量按重量计从约3％至约25％范围内的量存在，其中进一步地该组合物是充分不黏附的，以至于它可以被挤出并且压延而没有大量粘附到热金属零件上。该具有极性部分的聚合物选自下组，该组由以下各项组成：聚乙烯甲基丙烯酸、聚乙烯甲基丙烯酸的部分金属盐、聚乙烯丙烯酸、聚乙烯乙酸乙烯酯、聚酰胺、聚胺、热塑性聚氨酯、聚乙烯醇、聚乙烯一氧化碳及其混合物。
用“绿色”和/或再循环的替代物代替PVC通常需要接受关于衍生的装饰性表面覆盖物的技术性能的折中。
例如，聚乳酸受制于水解不稳定性、不足的耐醇性和耐污性，并且此外其特征为用于无故障压延的过低的熔体粘度。
聚乙烯醇缩丁醛受制于不足的耐醇性和足够的刚性。此外，再循环的聚乙烯醇缩丁醛总体上包含大量的增塑剂，该增塑剂限制其在非玻璃表面上的粘附，在多层装饰性表面覆盖物中情况是这样，并且总体上导致某些希望的层压体特性的退化。
此外，包含聚乙烯醇缩丁醛的组合物趋于黏附到热金属零件上，并且引起加工中的问题如聚合物在金属上的开裂和积累，或者易于黏附到金属上以使得此类材料根本不能被加工。
发明目的.
本发明的一个方面目的在于提供装饰性地板和墙壁覆盖物，其包含生物基的和/或再循环的聚合物，这些装饰性地板和墙壁覆盖物没有呈现出现有技术的包含绿色和/或再循环的聚合物的装饰性表面覆盖物的缺陷。
本发明的一个方面目的在于提供一种多层装饰性表面覆盖物，其包含由包含再循环的和/或生物基的聚合物的聚合物共混物制备的芯层，该芯层的特征为出色的到与其接触的层上的粘附，这些层中的至少一个包含生物基的和/或再循环的聚合物；该多层装饰性表面覆盖物通过常规方法制备。
此外，本发明的一个方面目的在于提供一种包含芯层的多层装饰性表面覆盖物，该芯层包含生物基增塑剂。
本发明的另一方面目的在于提供使用常规加工设备和加工条件的多层装饰性表面覆盖物，这些表面覆盖物符合与现有PVC替代物相似的技术标准。
发明内容.
本发明披露了一种包含芯层的装饰性多层表面覆盖物，所述芯层包含聚合物共混物，所述聚合物共混物包含：
-按重量计从20％至95％、优选按重量计30％至95％、更优选按重量计40％至95％的PVB(i)；以及
-按重量计从5％至80％、优选按重量计从5％至70％、更优选按重量计从5％至60％的PLA(ii)或PLA和一种或多种包含链烷酸乙烯酯的聚合物(iv)和/或一种或多种包含(甲基)丙烯酸烷基酯的聚合物(iii)和/或一种或多种热塑性聚氨酯(v)的混合物，其中所述混合物包含按重量计至少5％的聚乳酸；
该聚合物共混物中的聚合物的总量代表按重量计100％。如在此使用的，术语“芯层”表示该多层表面覆盖物的主要结构层，典型地在背衬层与一个或多个顶层之间。
本发明的优选实施例披露了以下特征中的一项或多项：
-该聚乙烯醇缩丁醛是再循环的聚乙烯醇缩丁醛；
-该聚乙烯醇缩丁醛是包含按重量计从约5％至约50％的一种或多种选自下组的增塑剂的再循环的聚乙烯醇缩丁醛，该组由以下各项组成：聚乙二醇的烷基酯，脂肪族二羧酸的二烷基酯，脂肪族二羧酸的烷基芳基酯，芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯，芳香族二羧酸、三羧酸或四羧酸的烷基芳基酯，磷酸酯和蓖麻油酸酯；
-该一种或多种包含(甲基)丙烯酸烷基酯的聚合物(iii)选自以下各项的组：
-(iii.a)包含按重量计至少60％、优选按重量计至少70％、更优选至少80重量份的(甲基)丙烯酸甲酯的(甲基)丙烯酸烷基酯均聚物或无规(共)聚合物；
-(iii.b)该(甲基)丙烯酸烷基酯共聚物是嵌段共聚物，该嵌段共聚物包含甲基丙烯酸酯单元的一个或多个嵌段和丙烯酸酯单元的一个或多个嵌段；
-(iii.c)包含按重量计从50％至95％的一种或多种烯烃以及按重量计从5％至50％的一种或多种(甲基)丙烯酸C1-C8烷基酯的烯烃/(甲基)丙烯酸烷基酯共聚物；
-(iii.d)包含按重量计从40％至80％的一种或多种烯烃和按重量计从5％至60％的一种或多种(甲基)丙烯酸C1-C8烷基酯以及按重量计3％至30％的一氧化碳的烯烃/(甲基)丙烯酸烷基酯/一氧化碳共聚物；以及
-(iii.a)、(iii.b)、(iii.c)和(iii.d)的混合物；
-该一种或多种包含链烷酸乙烯酯的聚合物(iv)选自下组，该组由以下各项组成：
-(iv.a)包含按重量计60％或更多、优选70％或更多、更优选80％或更多、最优选90％或更多的乙酸乙烯酯的链烷酸乙烯酯均聚物或共聚物；
-(iv.b)包含按重量计60％或更多、优选70％或更多、更优选80％或更多、最优选85％或更多的链烷酸乙烯酯的烯烃/链烷酸乙烯酯共聚物；
-(iv.c)包含按重量计40％至80％的一种或多种烯烃、按重量计5％至60％的一种或多种链烷酸乙烯酯以及按重量计3％至30％的一氧化碳的烯烃/链烷酸乙烯酯/一氧化碳共聚物；以及
-(iv.a)、(iv.b)和(iv.c)的混合物；
-该芯层包含对于100重量份的聚合物共混物从2至100重量份、优选从3至70重量份、更优选从4至55重量份并且最优选从5至40重量份的一种或多种选自下组的增塑剂，该组由以下各项组成：环己烷二羧酸的二烷基酯；脂肪族二羧酸的二烷基酯；芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯；磷酸低级烷基酯；磷酸低级烷基芳基酯；磺酸烷基酯和生物增塑剂；
-该芯层包含一种或多种选自下组的生物增塑剂，该组由乙酰化的甘油单酯、柠檬酸C1-C8烷基酯、乙酰柠檬酸C1-C8烷基酯和环氧化的植物油组成；
-该芯层包含对于100重量份的聚合物共混物从50至500重量份、优选从75至350重量份、更优选从100至300重量份的一种或多种选自下组的填充剂，该组由滑石、云母、碳酸钙、碳酸镁、白云石、重晶石、铝土矿、氢氧化镁、高岭土、二氧化硅和玻璃组成；
-该芯层不含聚氯乙烯；
-包含这些聚合物、一种或多种增塑剂和一种或多种填充剂的共混物的特征为在200℃下并且在100/s的剪切速率下的包括在500与10000Pa.s之间、优选在800与7000Pa.s之间并且更优选在1000与2500Pa.s之间的动态粘度(在此指出的动态粘度的任何值是如根据标准ISO11443:2014测量的)；
-该装饰性表面覆盖物包含：
-与该芯层的底部表面接触的背衬层，
-与该芯层的顶部表面接触的印刷层，
-与该印刷层的顶部表面接触的耐磨层，
其中所述背衬层、印刷层和耐磨层中的至少一个包含聚乳酸和/或聚乙烯醇缩丁醛和/或包含(甲基)丙烯酸酯的聚合物和/或包含链烷酸乙烯酯的聚合物；
-该背衬层、该印刷层和该耐磨层中的至少一个不含聚氯乙烯。
-该芯层包含载体，其中所述载体包含特征为大于3000l/m2.s、优选包括在3000与15000l/m2.s之间、并且优选包括在3500与10000l/m2.s之间的透气度的玻璃纤维毡和/或非织物。在此指出的任何透气度值根据标准DIN EN ISO 9237:1995进行测量。
本发明进一步披露了一种用于制备该装饰性多层表面覆盖物的方法，该方法包括以下步骤：
a)在包括在150℃与240℃之间的温度下熔融混合这些芯层成分以形成芯糊料；
b)在包括在120℃与200℃之间的温度下使用压延法将步骤a)的该芯糊料转化成该芯层；
c)将步骤b)的该芯层与一种或多种糊料接触并且粘接，其中所述糊料中的至少一种包含聚乳酸和/或聚乙烯醇缩丁醛，所述接触和粘接通过压延法在包括在130℃与220℃之间的温度下进行，以形成装饰性多层堆叠体。
该用于制备所述多层装饰性表面覆盖物的方法的优选实施例披露了以下特征中的一项或多项：
-该聚乙烯醇缩丁醛至少部分地从再循环过程获得；
-在步骤b)的压延中用步骤a)的该芯糊料浸渍非织物或玻璃纤维毡。
具体实施方式.
本发明提供了一种装饰性多层表面覆盖物，其包含背衬层、在该背衬层顶部上形成的芯层、在该芯层顶部上形成的印刷层以及在该印刷层顶部上形成的透明耐磨层，其中该芯层包含聚合物共混物，该聚合物共混物包含PVB和PLA并且任选地包含一种或多种包含(甲基)丙烯酸酯的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物和/或一种或多种热塑性聚氨酯，并且其中该背衬层、该印刷层和该耐磨层中的至少一个包含PLA和/或PVB和/或一种或多种包含(甲基)丙烯酸酯的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物。
诸位发明人已经出人意料地发现，将一种或多种包含(甲基)丙烯酸酯的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物与PVB或与PVB和PLA的混合物组合导致所述混合物的熔体强度的增加，而不引入不合适的特性。
有利地，该聚合物共混物包含PVB、PLA和一种或多种包含(甲基)丙烯酸酯的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物，其中该一种或多种包含(甲基)丙烯酸酯和/或链烷酸乙烯酯的聚合物使所述共混物的熔体强度增加，同时该PLA降低所述共混物的动态粘度，因此降低PVB降解风险。
该地板材料可以进一步包括在该透明耐磨层顶部上形成的表面处理层。
本发明的装饰性多层表面覆盖物的特征进一步在于，接触该芯层的这些层中的至少一个包含PVB和/或PLA和/或一种或多种包含(甲基)丙烯酸的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物。
优选地，该芯层不含聚氯乙烯。
优选地，该背衬层、该印刷层和该耐磨层中的至少一个不含聚氯乙烯；更优选地，该装饰性多层表面覆盖物不含聚氯乙烯。
用于本发明的组合物中的聚乙烯醇缩丁醛(i)(PVB)可以是未经利用的乙烯醇缩丁醛，这是之前未使用的PVB，但是优选是回收的或再循环的，提供较低成本但同样高品质的原料。回收的或再循环的PVB的种类不是关键的。已经发现，不同种类以及来自不同制造来源的回收的或再循环的PVB以及不同种类的PVB的混合物适合根据本发明使用。回收的或再循环的PVB可以含有常用的添加剂和污染物，如增塑剂、砂、以及细小玻璃颗粒，同时对于用于本发明的装饰性基材中仍是可接受的。
PVB是可以取决于希望的应用以关于结构特征和组成的大的变化制造的复杂树脂。
总体上，聚乙烯醇缩醛由醛和聚乙烯醇制备。
聚乙烯醇是通过聚乙酸乙烯酯的水解产生的含有各种百分比的羟基和乙酸酯基团的高分子量树脂。严格控制缩醛反应的条件和所使用的具体的醛和聚乙烯醇的浓度，以形成含有预定比例的羟基基团、乙酸酯基团和缩醛基团的聚合物。
PVB树脂由已知的水性或溶剂缩醛化方法生产，其中聚乙烯醇与丁醛在酸催化剂存在下反应以产生PVB，随后是催化剂的中和、分离、稳定化并且干燥该PVB树脂。
用于再循环PVB的方法披露于例如US 2005/0146074、US2009/0209667和US 2010/0249254中。
在不同类型的PVB之间的主要差异涉及分子量的差异，羟基、丁缩醛和残余酯基团的含量的差异，以及其他添加剂的类型和含量的差异。
用于本发明的组合物中的典型的PVB具有根据施陶丁格方程(Staudingerequation)从30,000至600,000、优选从50,000至400,000的分子量范围；按重量计从10％至30％、优选按重量计从12％至25％的范围的以聚乙烯醇计算的羟基，以及按重量计从0％至5％、优选按重量计从0％至3％的范围的以聚乙酸乙烯酯计算的残余酯基团。
优选地，用于本发明的装饰性表面中的PVB包含再循环的PVB；更优选地，用于本发明的装饰性表面中的PVB是再循环的PVB。
总体上，再循环的PVB是增塑的。PVB中的增塑剂的含量可以变化很大，例如按重量计从约5％至约50％，一般来说按重量计从约20％至约30％。
在再循环的PVB中存在的典型的增塑剂是聚乙二醇的烷基酯，如二乙二醇二-2-乙基丁酸酯、二乙二醇二正己酸酯、三乙二醇二-2,乙基丁酸酯、三乙二醇二正己酸酯、三乙二醇二-2-甲基戊酸酯、三乙二醇二-2-乙基己酸酯、三乙二醇二庚酸酯、四乙二醇二-2-乙基丁酸酯、四乙二醇二庚酸酯、四乙二醇二-2-乙基己酸酯、戊乙二醇二-2-乙基丁酸酯；脂肪族二羧酸的二烷基酯，如己二酸二丁酯、己二酸二正戊酯、己二酸二正己酯、己二酸二正庚酯和己二酸二正辛酯、癸二酸二正丁酯；混合的己二酸烷基芳基酯，如己二酸苄基癸基酯、己二酸苄基辛基酯、己二酸苄基己基酯和己二酸苄基丁基酯；芳香族二羧酸、三羧酸或四羧酸的烷基芳基酯，如邻苯二甲酸丁苄酯(BBP)；芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯，如邻苯二甲酸二异辛酯；磷酸酯，如磷酸2-乙基己基二苯基酯；以及蓖麻油酸酯，如蓖麻油酸丁酯。
用于本发明的组合物中的聚乳酸(ii)(PLA)是指衍生自2-羟基乳酸酯(乳酸)或丙交酯(环二酯)的热塑性聚酯。亚单元的式是：-[O-CH(CH3)-CO]-
单体(CH3CH(OH)CO2H)的α碳是光学活性的，所述单体通过发酵法使用从玉米、土豆等中提取的糖产生。聚乳酸典型地选自下组，该组由以下各项组成：D-聚乳酸、L-聚乳酸、D,L-聚乳酸、内消旋聚乳酸、及其任何组合。
总体上PLA被分类为结晶PLA和无定形PLA。无定形特征随外消旋含量的增加而增加。
用于本发明的芯层的聚合物共混物中的典型的PLA(ii)是有可能包括一定的结晶度并且特征为包括在15,000与300,000之间、优选在50,000与250,000之间的数均分子量的无定形树脂。
用于本发明的芯层的聚合物共混物中的丙烯酸酯聚合物(iii)选自下组，该组由以下各项组成：(甲基)丙烯酸烷基酯均聚物和无规共聚物(iii.a)；(甲基)丙烯酸烷基酯嵌段共聚物(iii.b)；烯烃/(甲基)丙烯酸烷基酯共聚物(iii.c)；烯烃/(甲基)丙烯酸烷基酯/一氧化碳共聚物(iii.d)及其混合物。
这些(甲基)丙烯酸烷基酯(共)聚物(iii.a)包含甲基丙烯酸甲酯的均聚物、和/或甲基丙烯酸甲酯和(甲基)丙烯酸C1至C8烷基酯的无规共聚物，所述(甲基)丙烯酸C1至C8烷基酯选自下组，该组由以下各项组成：(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸正己酯和(甲基)丙烯酸2-乙基己基酯；所述共聚物含有按重量计至少60％、优选按重量计至少70％、更优选按重量计至少80％的甲基丙烯酸甲酯。
优选使用聚(甲基丙烯酸甲酯)(PMMA)。
这些(甲基)丙烯酸烷基酯嵌段共聚物(iii.b)包含按重量计从10％至90％、优选按重量计从20％至80％的一个或多个包含甲基丙烯酸烷基酯单体的嵌段，和按重量计从90％至10％、优选按重量计从80％至20％的一个或多个包含丙烯酸烷基酯单体的嵌段。
优选地，包含甲基丙烯酸烷基酯的嵌段的玻璃化转变温度(根据ASTM D3418以20℃/分钟的加热梯度通过差示扫描量热法测量的)包括在70℃与110℃之间、更优选在80℃与110℃之间、并且最优选在90℃与110℃之间。包含丙烯酸烷基酯的嵌段的玻璃化转变温度包括在-70℃与-20℃之间、优选在-60℃与-30℃之间、并且更优选在-50℃与-40℃之间。
优选地，该(甲基)丙烯酸烷基酯嵌段共聚物是二嵌段共聚物，该二嵌段共聚物包括含有丙烯酸烷基酯单体的嵌段和含有甲基丙烯酸烷基酯单体的嵌段，例如像包括含有丙烯酸正丁酯单体的嵌段和含有甲基丙烯酸甲酯单体的嵌段的二嵌段共聚物。
该(甲基)丙烯酸烷基酯共聚物更优选地是三嵌段共聚物，该三嵌段共聚物包括一个含有丙烯酸烷基酯单体的嵌段和两个含有甲基丙烯酸烷基酯单体的嵌段，例如像包括一个含有丙烯酸正丁酯单体的嵌段和两个含有甲基丙烯酸甲酯单体的嵌段的三嵌段共聚物。
这些烯烃/(甲基)丙烯酸烷基酯共聚物(iii.c)包含按重量计从50％至95％的一种或多种烯烃以及按重量计从5％至50％的一种或多种(甲基)丙烯酸C1-C8烷基酯，其中该一种或多种烯烃由通式R1R2C＝CR3R4定义，其中R1、R2、R3和R4独立地是氢或含有从1至4个碳原子的烷基，并且优选选自下组，该组由乙烯、丙烯、1-丁烯、1-戊烯、1-己烯、2-甲基-1-丁烯、2,3-二甲基-1-戊烯组成；并且其中这些(甲基)丙烯酸C1-C8烷基酯选自如在(甲基)丙烯酸烷基酯(共)聚合物(iii.a)中定义的组。
优选地，该烯烃/(甲基)丙烯酸烷基酯共聚物是乙烯/丙烯酸甲酯或乙烯/丙烯酸丁酯共聚物。
这些烯烃/(甲基)丙烯酸烷基酯/一氧化碳共聚物(iii.d)包含按重量计从40％至80％的一种或多种烯烃和按重量计从5％至60％的一种或多种(甲基)丙烯酸C1-C8烷基酯以及按重量计从3％至30％的一氧化碳，其中该一种或多种烯烃和该一种或多种(甲基)丙烯酸C1-C8烷基酯选自如在(iii.c)中定义的组。
优选地，该烯烃/(甲基)丙烯酸烷基酯/一氧化碳共聚物是乙烯/丙烯酸乙酯/一氧化碳、乙烯/丙烯酸正丁酯/一氧化碳或乙烯/丙烯酸2-乙基己基酯/一氧化碳共聚物。
用于本发明的芯层的聚合物共混物中的包含链烷酸乙烯酯的聚合物(iv)选自下组，该组由以下各项组成：链烷酸乙烯酯均聚物和共聚物(iv.a)、烯烃/链烷酸乙烯酯共聚物(iv.b)、烯烃/链烷酸乙烯酯/一氧化碳共聚物(iv.c)及其混合物。
这些包含链烷酸乙烯酯的均聚物和共聚物(iv.a)包含一种或多种链烷酸乙烯酯单体，这些单体由通式RCOOCH＝CH2定义，其中R是含有从1至20个碳原子的烷基，并且优选选自下组，该组由以下各项组成：甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、辛酸乙烯酯和硬脂酸乙烯酯。
优选地，这些包含链烷酸乙烯酯的共聚物(iv.a)包含按重量计至少60％、更优选按重量计至少70％、最优选按重量计至少80％或甚至按重量计至少90％的乙酸乙烯酯。优选地，该链烷酸乙烯酯聚合物是聚乙酸乙烯酯。
这些烯烃/链烷酸乙烯酯共聚物(iv.b)包含一种或多种烯烃和一种或多种链烷酸乙烯酯，其中该一种或多种烯烃是如在(iii.c)中定义的，并且其中该一种或多种链烷酸乙烯酯单体是如在这些链烷酸乙烯酯均聚物和共聚物(iv.a)中定义的。
优选地，该烯烃/链烷酸乙烯酯共聚物(iv.b)包含按重量计至少60％、更优选按重量计至少70％、最优选按重量计至少80％、或甚至按重量计至少85％的一种或多种链烷酸乙烯酯，以及40％或更少、优选30％或更少、更优选20％或更少、最优选15％或更少的一种或多种1-烯烃。
优选地，该烯烃/链烷酸乙烯酯共聚物是乙烯/乙酸乙烯酯共聚物，该乙烯/乙酸乙烯酯共聚物包含按重量计至少60％、优选按重量计至少70％、更优选按重量计至少80％、最优选按重量计至少85％的乙酸乙烯酯。
这些烯烃/链烷酸乙烯酯/一氧化碳共聚物(iv.c)包含按重量计40％至80％的一种或多种烯烃、按重量计5％至60％的一种或多种链烷酸乙烯酯以及按重量计3％至30％的一氧化碳，其中该一种或多种烯烃和该一种或多种链烷酸乙烯酯是如在烯烃/链烷酸乙烯酯共聚物(iv.b)中定义的。
优选地，该烯烃/链烷酸乙烯酯/一氧化碳共聚物是乙烯/乙酸乙烯酯/一氧化碳共聚物。
该芯层此外可以包含一种或多种热塑性聚氨酯(v)。
热塑性聚氨酯(v)含有分别由聚合的二异氰酸酯和多元醇组分形成的硬链段和软链段。硬链段与软链段的比率或重量％决定了该热塑性聚氨酯TPU的物理特性。
热塑性聚氨酯由二异氰酸酯化合物与至少一种能够与异氰酸酯基团反应的双官能化合物、优选至少一种双官能含有羟基基团的化合物、以及任选地扩链剂的反应来获得。
适合的扩链剂包括一种或多种脂肪族二醇诸如1,4-丁二醇或1,6-己二醇；一种或多种氨基醇诸如乙醇胺；以及脂肪族二胺诸如1,6-己二胺和异佛尔酮二胺。
二异氰酸酯化合物可以是芳香族或脂肪族的。芳香族二异氰酸酯包括例如4,4’-、2,2’-和2,4’-亚甲基联苯二异氰酸酯和甲苯二异氰酸酯；脂肪族二异氰酸酯包括例如1,6-六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯和2,2’-、4,4’-和2,4’-二环己基甲烷二异氰酸酯。可使用芳香族二异氰酸酯和脂肪族二异氰酸酯的混合物。
优选的异氰酸酯是亚甲基联苯二异氰酸酯和4,4’-二环己基甲烷二异氰酸酯。
能够与异氰酸酯基团反应的双官能化合物优选地是双官能含有羟基基团的化合物，该化合物包含选自下组的结构，该组由以下各项组成：聚酯酰胺、聚硫醚、聚碳酸酯、聚缩醛、聚烯烃、聚硅氧烷、聚酯、聚醚、聚已内酯及其混合物。
聚酯、更特别是由直链二酸和直链二元醇的缩合获得的这些聚酯；聚醚，如聚四亚烷基醚，其中亚烷基是C1至C4；以及聚己内酯是优选的。
本发明的装饰性表面覆盖物的芯层由包含以下各项的聚合物共混物获得：
-按重量计从20％至95％、优选按重量计从30％至95％、更优选按重量计从40％至95％的PVB(i)、优选再循环的PVB；
-按重量计从5％至80％、优选按重量计从5％至70％、更优选按重量计从5％至60％的PLA(ii)；
●或者
●PLA和一种或多种包含链烷酸乙烯酯的聚合物(iv)的混合物；或者
●PLA和一种或多种包含(甲基)丙烯酸酯的聚合物(iii)的混合物，或者
●PLA和一种或多种包含链烷酸乙烯酯的聚合物以及一种或多种包含(甲基)丙烯酸酯的聚合物的混合物；或者
●PLA和一种或多种热塑性聚氨酯(v)的混合物；或者
●PLA和一种或多种包含链烷酸乙烯酯的聚合物(iv)以及一种或多种热塑性聚氨酯(v)的混合物；或者
●PLA和一种或多种包含(甲基)丙烯酸酯的聚合物(iii)以及一种或多种热塑性聚氨酯(v)的混合物；或者
●PLA和一种或多种包含链烷酸乙烯酯的聚合物和一种或多种包含(甲基)丙烯酸酯的聚合物以及一种或多种热塑性聚氨酯(v)的混合物；
其中所述混合物包含按重量计至少5％、优选按重量计至少10％、更优选按重量计至少15％、最优选按重量计至少20％的聚乳酸，并且
其中该聚合物共混物中的聚合物的总量代表按重量计100％。
根据本发明的芯层的组合物可以进一步包含多种成分，如增塑剂(优选生物增塑剂)、填充剂和颜料或染料、以及一种或多种添加剂，如改性树脂、稳定剂、发泡剂、增粘剂、分散剂、抗静电剂、热和光稳定剂、阻燃剂、或其任何组合。
可以使用能够增塑包含占多数的量的PVB和PLA和/或一种或多种丙烯酸酯聚合物的组合物的任何增塑剂。合适的增塑剂选自下组，该组由以下各项组成：环己烷二羧酸的二烷基酯；脂肪族二羧酸的二烷基酯；芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯；柠檬酸低级烷基酯；磷酸低级烷基酯、磺酸烷基酯和在常规聚氯乙烯应用中使用的其他增塑剂。
优选地，这些增塑剂包含多元羧酸的烷基酯、更优选芳香族多元羧酸的烷基酯。
优选地，这些增塑剂包含环氧化的或者以其他方式衍生的植物油，例如环氧化的大豆油如环氧化的大豆油酸C1-C10烷基酯、环氧化的亚麻籽油、环氧化的大豆油、环氧化的妥尔油等。
优选地，该增塑剂是生态友好的柠檬酸基增塑剂，其包括柠檬酸酯和衍生的植物油的共混物。
优选地，该增塑剂是乙酰化的甘油单酯，例如像蓖麻油酸的乙酰化的甘油单酯。
对于100重量份的包含聚合物(i)和(ii)以及任选地(iii)和/或(iv)和/或(v)的聚合物共混物，该增塑剂典型地以最高达100重量份、优选从2至100重量份、更优选从3至70重量份、最优选从4至55重量份或甚至从5至40重量份的量存在。
对于100重量份的包含聚合物(i)和(ii)以及任选地(iii)和/或(iv)和/或(v)的聚合物共混物，本发明的芯层的组合物进一步包含包括在50与500重量份之间、优选在75与350重量份之间、更优选在100与300重量份之间的量的一种或多种填充剂。
适用于本发明组合物的填充剂的实例可以是任何常规填充剂，尤其是传统上用于表面覆盖物中的那些类型。
填充剂可以是有机的、无机的、或两者的组合，例如具有不同的形态。实例包括但不限于粉煤灰、碳酸盐(诸如碳酸镁、碳酸钙和碳酸钙镁)、硫酸钡、炭黑、金属氧化物、无机材料、天然材料、三水合氧化铝、氢氧化镁、铝土矿、滑石、云母、白云石、重晶石、高岭土、二氧化硅、消费后玻璃或后工业玻璃(post-industrial glass)、合成纤维和天然纤维、或其任何组合。
优选地，该填充剂包含滑石、云母、碳酸钙、碳酸镁、白云石、重晶石、铝土矿、氢氧化镁、高岭土、二氧化硅、玻璃、或其任何组合。
适用于本发明组合物的颜料和染料的实例是金属氧化物(如二氧化钛、氧化铁、氧化锌以及类似物)、金属氢氧化物、金属粉末、硫化物、硫酸盐、碳酸盐、硅酸盐、铁蓝、有机红、有机紫红以及类似物。
本发明的装饰性表面覆盖物的芯层可以在一些情况下包括载体，如织造或非织造网状物或织物、或者或多或少热稳定的材料的织物如玻璃纤维毡。
该载体赋予该装饰性表面覆盖物强度和尺寸稳定性二者。
有利地，该载体包含特征为大于3000l/m2.s、优选包括在3000与15000l/m2.s之间、并且优选包括在3500与10000l/m2.s之间的透气度的玻璃纤维毡和/或非织物。
除该芯层之外，本发明的装饰性多层表面覆盖物还包含背衬层、印刷层和耐磨层，各自具有顶部表面和底部表面，其中该背衬层的顶部表面被粘接到该芯层的底部表面上，其中该芯层的顶部表面被粘接到该印刷层的底部表面上；其中该印刷层的顶部表面被粘接到该耐磨层的底层上，并且其中该耐磨层的顶部表面覆盖有保护性顶涂层。
优选地，该背衬层、该印刷层和该耐磨层中的至少一个包含PVB和/或PLA和/或一种或多种包含(甲基)丙烯酸酯的聚合物和/或包含链烷酸乙烯酯的聚合物。
该背衬层、该印刷层和该耐磨层可以进一步包含一种或多种选自下组的聚合物，该组由含有极性基团的聚烯烃以及包含一种或多种乙烯基芳香族单体的序列和一种或多种烯烃(alkylene)的序列的热塑性弹性体组成。
优选地，该背衬层、该印刷层和该耐磨层中的至少一个不含聚氯乙烯。
该耐磨层可以在其顶部表面上包含保护性顶涂层。
用于在该耐磨层的顶部表面上使用、接触该印刷层的顶涂层配制品可以选自常规用于涂覆聚氯乙烯表面覆盖物的标准聚氨酯配制品。
所述标准配制品的实例是二组分溶剂基、水基或无溶剂的聚氨酯配制品，溶剂基空气干燥或可湿固化的单组分配制品和水性聚氨酯分散体，其中干燥和/或交联最后与强制空气条件组合在室温或更高温度下进行。
该印刷层可以在其表面中的至少一个上包含一个或多个印刷物。
该一个或多个印刷物优选获得自干燥和/或固化选自下组的油墨组合物，该组由以下各项组成：水性油墨组合物、可辐射固化的油墨组合物、可辐射固化的水性油墨组合物、PVC塑料溶胶和聚(甲基)丙烯酸酯塑料溶胶。
本发明提供了一种用于制备所述装饰性表面覆盖物的方法。
总体上，使用压延方法，其中以这样的方式将熔融聚合物共混物进料到一系列的两个或更多个加热辊以便产生具有均匀厚度的聚合物层。
通过以下方式制备用于制备该芯层的热聚合物共混物：在适合的加热的混合器中(例如在双螺杆挤出机或单螺杆挤出机、具有加热的夹套的混料罐、班伯里密炼机、连续混合器、螺条混合器或其任何组合中)在包括在150℃与240℃之间、优选在170℃与220℃之间、更优选在180℃与210℃之间的内部温度下将PVB、优选再循环的PVB和PLA以及任选地一种或多种包含(甲基)丙烯酸酯的聚合物和/或一种或多种包含链烷酸乙烯酯的聚合物和/或一种或多种热塑性聚氨酯与一种或多种填充剂、一种或多种增塑剂(优选生物增塑剂)、以及任选地一种或多种添加剂(如稳定剂、阻燃剂和抗静电剂)一起混配以形成共混物。
该共混物的特征为在200℃下并且在100/s的剪切速率下包括在500与10000Pa.s之间、优选在800与7000Pa.s之间并且更优选在1000与2500Pa.s之间的动态粘度。
内部温度意指不含PVC糊料的实际温度并且不是用于制备并且加工所述不含PVC糊料的设备的设定温度。
然后将该均匀的热物质排放到一个或多个加工机器中，该一个或多个加工机器包含一系列的两个或更多个加热的辊以产生具有均匀厚度的聚合物层。
压延辊的设定温度包括在120℃与200℃之间、优选在150℃与180℃之间。
在本发明的方法的优选实施例中，该芯层包含玻璃纤维毡，其中优选地进行多次压延以保证玻璃纤维毡的完全浸渍。
该背衬层、印刷层和耐磨层由熔融混合和熔融压延相应的聚合物共混物、一种或多种增塑剂和任选的颜料、填充剂和添加剂来制备。
该印刷层可以提供有一个或多个印刷物。该一个或多个印刷物可以在该聚合物层的顶部表面上或底部表面上提供。另外一个或多个印刷物可以在所述层的两个表面上提供。
用于本发明中的油墨组合物是可干燥和/或可固化的，并且是含溶剂的、水基的或无溶剂的油墨。对于可固化的油墨组合物，本发明是指在热量的影响下或在光化辐射的影响下交联。
然后在随后的压延步骤中接触并且粘接该背衬层、芯层、印刷层和耐磨层。
压延在以下条件下进行：
-包括在130℃与220℃之间、优选在150℃与210℃之间、更优选在170℃与200℃之间的温度；
-包括在2与100m/min之间、优选在10与50m/min之间、更优选在10与20m/min之间的速度。
优选将保护性顶涂层施用于该耐磨层的顶部表面上。该保护性顶涂层优选地是交联的，更优选通过光化照射交联。
将可辐射固化的组合物、优选可辐射固化的水性聚氨酯分散体均匀地施用在该装饰性基材的顶部表面上，在包括在25℃与60℃之间、优选在30℃与50℃之间的温度下静置。
该保护性顶涂层可以通过本领域普通技术人员已知的任何合适的涂覆方法施用，例如通过直接凹版涂布、反向凹版涂布、胶版凹版涂布(offset gravure coating)、光辊涂布、幕式涂布、喷涂及其组合。直接凹版涂布和光辊涂布是优选的。
对于水性聚氨酯分散体的特定情况，将水蒸发，优选在约100℃的对流烘箱中，于是将包括聚氨酯顶层的装饰性基材任选地加热到包括在100℃与200℃之间的温度，并且随后在交联之前进行机械压花。
对于其中可固化的组合物不是基于水的例如像100％固体组合物或近似100％固体组合物的特定情况，优选将所述组合物施用到装饰性基材上并在压花步骤之后进行交联。
机械压花是通过将纹理压制到在顶部包括聚氨酯层的装饰性表面覆盖物中进行的。压花是在包括在10与25kg.cm-2之间的压力和包括在100℃与200℃之间、优选在130℃与200℃之间的表面温度下进行的。
用于对基材进行机械压花的装置通常包括冷却的压花辊和可操作地放置在该压花辊内的支承辊，使得在该支承辊与该压花辊之间形成辊隙，由此基材可以穿过辊隙并且接合该压花辊用于赋予机械压花图案。该装置进一步包括能够在对基材进行压花时量化机械压花图案的轮廓仪。
通常，从机械压花获得的纹理的特征为包括在约10至100μm之间的深度、包括在约125至400μm之间的宽度、包括在约5至40度之间的壁角度(相对于表面的角度)和每cm约4至20个特征的频率。
已经观察到，在一方面在该芯层与该背衬层之间以及在另一方面在该芯层与该印刷层之间的结合强度与当前聚氯乙烯表面覆盖物的两个或更多个层之间的结合强度相当。
在本发明的层之间的结合的特征为根据ISO 24345:12(弹性地板覆盖物-耐剥离性的确定(Resilient floor coverings-determination of peel resistance))的超过50N/5cm的剥离强度。在该印刷层与该耐磨层之间测量了剥离强度的类似值。
实例
以下说明性实例仅仅旨在举例说明本发明，而并非意欲限制或以其他方式限定本发明的范围。
表1和2说明了根据本发明(实例1至22)连同对比实例1的芯层的组成、加工能力和粘附性能。
在表1和2中，该聚合物共混物的热塑性聚合物的总和等于100份。
在所有实例和对比实例中使用的聚乙烯醇缩丁醛是包含约27％的增塑剂的再循环的聚乙烯醇缩丁醛。如在这些表中给出的值代表存在于该再循环的聚乙烯醇缩丁醛中的聚乙烯醇缩丁醛的量。
增塑剂、填充剂、抗氧化剂和润滑剂的量以对于100份的聚合物共混物的份数表示。
该填充剂是来自欧米亚公司(Omya)的白垩VS35(CaCO3)；该抗氧化剂是来自巴斯夫公司(BASF)的Irganox 1010、Irganox 1076或二者的1/1混合物；该润滑剂是来自欧林公司(Olean)的444(硬脂酸类型)。
聚乳酸是来自萘琪沃克公司(NatureWorks)的IngeoTM(4043D或4060D)。
表1.
表2.
该包含(甲基)丙烯酸酯的聚合物是：
-用于实例1、3和19的来自钟渊公司(Kaneka)的Kane(甲基)丙烯酸酯均聚物或无规(共)聚合物；
-用于实例4、6、16和20的来自LG化学公司(LG Chemicals)的PA 910(聚甲基丙烯酸甲酯)；
-用于实例9和12的来自杜邦公司(Dupont)的D(烯烃/(甲基)丙烯酸酯共聚物)；
-用于实例7、21和对比实例1的来自杜邦公司的441HP(烯烃/(甲基)丙烯酸酯/一氧化碳共聚物)。
该包含链烷酸乙烯酯的聚合物是：
-用于实例4、5、11、20和21的来自瓦克公司(Wacker)的2510(包含按重量计至少60％的乙酸乙烯酯的链烷酸乙烯酯聚合物)。
-用于实例2、10、16和19的来自朗盛公司(Lanxess)的900(烯烃/链烷酸乙烯酯共聚物)。
-用于实例1、8、9、13、14和15的来自杜邦公司的742(烯烃/链烷酸乙烯酯/一氧化碳共聚物)。
引入这些聚合物共混物中的增塑剂是用于实例1、4、10和对比实例2的来自丹尼斯克公司(Danisco)的Soft-N-Safe(乙酰化的甘油单酯)；用于实例6、12和14的来自永本兹劳尔公司(Jungbunzlauer)的AII(乙酰柠檬酸C1-C8烷基酯)；用于实例3、5和对比实例1的来自永本兹劳尔公司的BII(乙酰柠檬酸C1-C8烷基酯)和来自伊士曼公司(Eastman)的EastmanTM TOTM增塑剂(芳香族三羧酸的三烷基酯)的1/1混合物；用于实例7、8和15的AII和EastmanTM TOTM增塑剂的1/1混合物；用于实例11和17的Soft-N-Safe和来自朗盛公司的DPO(磷酸低级烷基芳基酯)的3/1混合物；用于实例9、13和20的来自巴斯夫公司的DOA(芳香族二羧酸的二烷基酯)和来自加拉塔化工公司(Galata Chemical)的3.2(环氧化的植物油)的1/1混合物；用于实例18和21的3.2；以及用于实例2、16和19的DOA和来自加拉塔化工公司的6.8(环氧化的植物油)的1/1混合物。
这些聚合物共混物通过使用再循环的聚乙烯醇缩丁醛进一步包含附加的增稠剂，一般是三乙二醇二-2-乙基己酸酯。
对于100份的聚合物共混物的附加的增塑剂的量是对于实例1和19的10份，对于实例2的16.5份、对于实例3的20份，对于实例4的23份，对于实例5的26份，对于实例6的30份，对于实例7至15的25份，对于对比实例1和实例16至18的31份，对于实例20的8.3份以及对于实例21的6.5份。
通过在挤出机中在170℃的温度下熔融混合并在辊磨机中在170℃的温度下压延来制备厚度为1.25mm的芯层。
在热压/冷压步骤中在160℃下在大约4巴的压力下将包括包含按重量计20％的聚乳酸、按重量计30％的聚乙烯醇缩丁醛和按重量计50％的包含(甲基)丙烯酸酯的聚合物的聚合物共混物的(0.5mm的)背衬层以及包括包含按重量计30％的聚乳酸、按重量计30％的聚乙烯醇缩丁醛、按重量计20％的包含(甲基)丙烯酸酯的聚合物和按重量计20％的包含链烷酸乙烯酯的聚合物的聚合物共混物的(0.25mm的)的印刷层分别粘合到该芯层的底部表面和顶部表面上，随后冷却至25℃。
向该印刷层的顶部表面上层压包括包含按重量计70％的包含(甲基)丙烯酸酯的聚合物以及按重量计30％的PLA的聚合物共混物的(0.5mm的)耐磨层。层压时间是约60秒。
如从以上实例中呈现的，根据本发明的组合物(实例1至21)使得能够使用常规加工条件在现有设备上加工，并且特征为如通过至少40N/50mm、总体上至少50N/50mm的剥离强度表示的对该背衬层以及对该印刷层的粘附性。
对比实例的组合物的特征为抑制良好的箔压延的过高的熔体强度，并且特征为如通过最多40N/50mm的剥离强度表示的对该背衬层以及对该印刷层的粘附性。
Claims (16)
1.一种包含芯层的装饰性多层表面覆盖物，所述芯层包含聚合物共混物，所述聚合物共混物包含：
-按重量计从20％至95％、优选按重量计30％至95％、更优选按重量计40％至95％的聚乙烯醇缩丁醛(i)；以及
-按重量计从5％至80％、优选按重量计从5％至70％、更优选按重量计从5％至60％的聚乳酸(ii)或聚乳酸和一种或多种包含链烷酸乙烯酯的聚合物(iv)和/或一种或多种包含(甲基)丙烯酸烷基酯的聚合物(iii)和/或一种或多种热塑性聚氨酯(v)的混合物，其中所述混合物包含按重量计至少5％的聚乳酸；
该聚合物共混物中的聚合物的总量代表按重量计100％。
2.根据权利要求1所述的装饰性多层表面覆盖物，其中聚乙烯醇缩丁醛是再循环的聚乙烯醇缩丁醛。
3.根据权利要求1或2所述的装饰性多层表面覆盖物，其中聚乙烯醇缩丁醛是包含按重量计从约5％至约50％的一种或多种选自下组的增塑剂的再循环的聚乙烯醇缩丁醛，该组由以下各项组成：聚乙二醇的烷基酯，脂肪族二羧酸的二烷基酯，脂肪族二羧酸的烷基芳基酯，芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯，芳香族二羧酸、三羧酸或四羧酸的烷基芳基酯，磷酸酯和蓖麻油酸酯。
4.根据权利要求1至3所述的装饰性多层表面覆盖物，其中该聚合物共混物包含一种或多种包含(甲基)丙烯酸烷基酯的聚合物(iii)，并且其中该一种或多种包含(甲基)丙烯酸烷基酯的聚合物(iii)选自以下各项的组：
-(iii.a)包含按重量计至少60％、优选按重量计至少70％、更优选至少80重量份的(甲基)丙烯酸甲酯的(甲基)丙烯酸烷基酯均聚物或无规(共)聚合物；
-(iii.b)该(甲基)丙烯酸烷基酯共聚物是嵌段共聚物，该嵌段共聚物包含甲基丙烯酸酯单元的一个或多个嵌段和丙烯酸酯单元的一个或多个嵌段；
-(iii.c)包含按重量计从50％至95％的一种或多种烯烃以及按重量计从5％至50％的一种或多种(甲基)丙烯酸C1-C8烷基酯的烯烃/(甲基)丙烯酸烷基酯共聚物；
-(iii.d)包含按重量计从40％至80％的一种或多种烯烃和按重量计从5％至60％的一种或多种(甲基)丙烯酸C1-C8烷基酯以及按重量计3％至30％的一氧化碳的烯烃/(甲基)丙烯酸烷基酯/一氧化碳共聚物；以及
-(iii.a)、(iii.b)、(iii.c)和(iii.d)的混合物。
5.根据权利要求1至4所述的装饰性多层表面覆盖物，其中该聚合物共混物包括包含链烷酸乙烯酯的聚合物(iv)，并且其中该一种或多种包含链烷酸乙烯酯的聚合物(iv)选自下组，该组由以下各项组成：
-(iv.a)包含按重量计60％或更多、优选70％或更多、更优选80％或更多、最优选90％或更多的乙酸乙烯酯的链烷酸乙烯酯均聚物或共聚物；
-(iv.b)包含按重量计60％或更多、优选70％或更多、更优选80％或更多、最优选85％或更多的链烷酸乙烯酯的烯烃/链烷酸乙烯酯共聚物；
-(iv.c)包含按重量计40％至80％的一种或多种烯烃、按重量计5％至60％的一种或多种链烷酸乙烯酯以及按重量计3％至30％的一氧化碳的烯烃/链烷酸乙烯酯/一氧化碳共聚物；以及
-(iv.a)、(iv.b)和(iv.c)的混合物。
6.根据权利要求1至5中任一项所述的装饰性表面覆盖物，进一步包含对于100重量份的聚合物共混物从2至100重量份、优选从3至70重量份、更优选从4至55重量份并且最优选从5至40重量份的一种或多种选自下组的增塑剂，该组由以下各项组成：环己烷二羧酸的二烷基酯；脂肪族二羧酸的二烷基酯；芳香族单羧酸、二羧酸、三羧酸或四羧酸的烷基酯；磷酸低级烷基酯；磷酸低级烷基芳基酯；磺酸烷基酯和生物增塑剂。
7.根据权利要求1至6中任一项所述的装饰性表面覆盖物，其中该芯层包含一种或多种选自下组的生物增塑剂，该组由乙酰化的甘油单酯、柠檬酸C1-C8烷基酯、乙酰柠檬酸C1-C8烷基酯和环氧化的植物油组成。
8.根据权利要求1至7中任一项所述的装饰性表面覆盖物，其中该芯层包含对于100重量份的聚合物共混物从50至500重量份、优选从75至350重量份、更优选从100至300重量份的一种或多种选自下组的填充剂，该组由滑石、云母、碳酸钙、碳酸镁、白云石、重晶石、铝土矿、氢氧化镁、高岭土、二氧化硅和玻璃组成。
9.根据权利要求1至8中任一项所述的装饰性多层表面覆盖物，其中该芯层不含聚氯乙烯。
10.根据权利要求1至9中任一项所述的装饰性多层表面覆盖物，其中包含这些聚合物、一种或多种增塑剂和一种或多种填充剂的该共混物的特征为在200℃下并且在100/s的剪切速率下根据标准ISO 11443:2014测量的包括在500与10000Pa.s之间、优选在800与7000Pa.s之间并且更优选在1000与2500Pa.s之间的动态粘度。
11.根据权利要求1至10中任一项所述的装饰性表面覆盖物，其包含
-与该芯层的底部表面接触的背衬层，
-与该芯层的顶部表面接触的印刷层，
-与该印刷层的顶部表面接触的耐磨层，
其中所述背衬层、印刷层和耐磨层中的至少一个包含聚乳酸和/或聚乙烯醇缩丁醛和/或包含(甲基)丙烯酸酯的聚合物和/或包含链烷酸乙烯酯的聚合物。
12.根据权利要求1至11中任一项所述的装饰性多层表面覆盖物，其中该背衬层、该印刷层和该耐磨层中的至少一个不含聚氯乙烯。
13.根据权利要求1至12中任一项所述的印刷的装饰性表面覆盖物，其中该芯层包含载体，其中所述载体包含玻璃纤维毡和/或非织物，该玻璃纤维毡和/或非织物的特征为根据标准DIN EN ISO 9237:1995测量的大于3000l/m2.s、优选包括在3000与15000l/m2.s之间、并且优选包括在3500与10000l/m2.s之间的透气度。
14.一种用于制备根据权利要求1至13所述的装饰性多层表面覆盖物的方法，该方法包括以下步骤：
a)在包括在150℃与240℃之间的温度下熔融混合这些芯层成分以形成芯糊料；
b)在包括在120℃与200℃之间的温度下使用压延法将步骤a)的该芯糊料转化成该芯层；
c)将步骤b)的该芯层与一种或多种糊料接触并且粘接，其中所述糊料中的至少一种包含聚乳酸和/或聚乙烯醇缩丁醛，所述接触和粘接通过压延法在包括在130℃与220℃之间的温度下进行，以形成装饰性多层堆叠体。
15.根据权利要求14所述的方法，其中该聚乙烯醇缩丁醛至少部分地从再循环过程获得。
16.根据权利要求14所述的方法，包括在步骤b)的压延中用步骤a)的该芯糊料浸渍非织物或玻璃纤维毡。
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| EP15190123.8 | 2015-10-16 | ||
| PCT/EP2016/074735 WO2017064260A1 (en) | 2015-10-16 | 2016-10-14 | Decorative multi-layer surface covering comprising polyvinyl butyral |
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| WO2020131021A1 (en) | 2018-12-18 | 2020-06-25 | Hewlett-Packard Development Company, L.P. | Fabric print media |
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| NL2025762B1 (en) * | 2020-06-04 | 2022-01-28 | I4F Licensing Nv | Decorative panel, and decorative floor covering consisting of said panels |
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| US20180298620A1 (en) | 2018-10-18 |
| WO2017064260A1 (en) | 2017-04-20 |
| EP3362281A1 (en) | 2018-08-22 |
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