CN1805846B - 制备层状材料的方法和层状材料 - Google Patents

制备层状材料的方法和层状材料 Download PDF

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CN1805846B
CN1805846B CN2004800164805A CN200480016480A CN1805846B CN 1805846 B CN1805846 B CN 1805846B CN 2004800164805 A CN2004800164805 A CN 2004800164805A CN 200480016480 A CN200480016480 A CN 200480016480A CN 1805846 B CN1805846 B CN 1805846B
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microsphere
swellable
thermoplastic polymer
bearing bed
heat
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CN1805846A (zh
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M·B·比索夫
A·布兰斯
M·古斯
C·B·海默尔
T·G·W·克伦克
T·特夫斯
D·A·温泽尔
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Coveright Surfaces Holding GmbH
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Abstract

提供了一种制备层状材料的方法。该方法包括以下步骤：用热固性树脂浸渍基质，并且进一步用包括有可热膨胀的微球体的分散体浸渍或者涂覆该如此浸渍的基质。

Description

制备层状材料的方法和层状材料
本发明涉及一种层状材料和一种制备层状材料的方法，并且要求了欧洲专利申请03445063.5-2124和美国专利申请60/472,783的优先权，这两项专利申请根据披露内容在此被全部引入。
公知的是，当在地板材料例如木质地板或层压地板材料的硬表面上走动时会产生烦扰的噪声。声音的产生和传输取决于地板材料的结构而改变。例如，层压的地板材料通常具有中等密度纤维板的承载层，其通常比实木层产生显著更多的噪声问题。然而还有，地板材料例如通常仅由实木层组成的镶木地板尤其在浮动而不是完全被胶粘到地面上时可能产生噪声问题。
典型的用于地板的装饰性层压材料包括附着在坚硬材料的承载层上的树脂浸渍的纸层。上层包括装饰板并且通常还有覆盖层和在装饰板下面的一个或多个树脂浸渍的纸层。通常在承载层的下侧附着一个包括有树脂浸渍的纸的平衡性背衬层，以防止层压材料的扭曲。通常通过以下方式制得装饰性层压材料：将构成层压材料的层组装并且在加热下压制该组装体，以使得被浸渍的层中的树脂固化，形成均匀的层压材料。
镶木地板材料通常包括低质木材或胶合板的承载层、高质木材的表层和低质木材的背衬板。
已经作了许多尝试以降低当在地板材料上走动时所产生的噪声：
WO02/47906 A1披露了一种其中弹性体薄片被置于承载芯层上面的装饰性层压材料。
EP1247923 A1和WO01/09461 A1披露了一种下侧含有热塑性材料、具有隔音性能的地板覆盖材料。
然而在EP1247923 A1和WO01/09461 A1中，在生产过程中当将热塑性层施加到层压地板材料的已经附着的背衬层上时则需要额外的步骤。
WO01/45940涉及一种包括了含有膨胀的热塑性微球体的保护性覆盖层的耐磨性装饰板。然而，完全没有论述声音传输的问题。
因此，需要一种可以通过对已经采用的制备方法进行小的改进而以简单的方式制备的、具有优良的隔音性能的地板材料。
                        本发明
根据本发明，已经令人惊奇地发现可以通过提供这样一种层状材料来实现上述目的，该层状材料包括用热固性树脂浸渍并且进一步用嵌入分散相中的膨胀的微球体涂覆的基质。分散体的连续相优选含有热塑性聚合物。
在一个方面中，本发明进一步涉及一种制备层状材料，优选地板材料的方法。因此，根据本发明的一个实施方案，将层状材料附着在另一层上。此后使微球体膨胀。
可通过根据本发明的方法获得的层状材料适宜地包括上侧和下侧。相对于承载层而言，上侧适宜地是包括有装饰层或者用于接受材料层的一侧，其对于层状材料的最终使用者是可见的，例如为涂料或墙纸。优选地，层状材料包括上装饰层。包括有可热膨胀的微球体的层适宜地位于承载层的下面。
在本发明的一个优选实施方案中，该方法适宜地包括：将包括有可热膨胀的微球体的层(基质)与层状材料的另一层合并在一起，由此形成组装体，将该组装体压制并且在微球体于大气压下开始膨胀的温度之上加热，和从组装体中释放出压力，由此使微球体膨胀。适宜地在已经释放出压力时直接发生微球体的主要膨胀。
在本发明的另一个优选实施方案中，该方法包括以下步骤：将包括有可热膨胀的微球体的层接合到层状材料的另一层上，接着在微球体开始膨胀的温度之上在没有明显压制的情况下将包括有可热膨胀的微球体的层加热。
根据本发明的主要方面的方法包括以下步骤：用包括有可热膨胀的微球体的组合物浸渍或者涂覆用热固性树脂浸渍的基质，由此形成包括有可热膨胀的微球体的层，该微球体分散在用热固性树脂浸渍的层的顶上的连续聚合物相中。
包括有可热膨胀的微球体的层适宜地位于层状产品的0-5层深度，优选为0-2层。最优选地，包括有可热膨胀的微球体的层是层状材料的最外层。
层状材料适宜地是地板材料。合适的地板材料的例子是：装饰性层压地板材料、镶木地板材料和弹性地板材料例如乙烯基地板。优选地，该地板材料是装饰性层压地板材料。作为选择，地板材料优选是镶木地板材料。
层状材料还可以适宜地是墙部件或者屋顶部件。
包括有可热膨胀的微球体的层适宜地包括纸。
本发明进一步包括包含有两层或多层，其中一层是承载层的层状材料。该层状材料包括上侧和下侧，相对于承载层而言，上侧是包括有装饰层或者用于接受材料层的一侧，其对于层状材料的最终使用者是可见的，例如为涂料或墙纸。优选地，层状材料包括上装饰层。包括有可热膨胀的微球体的至少一层位于承载层的下面。适宜地，层状材料的最外层包括有膨胀的热塑性微球体。
包括有膨胀的热塑性微球体的层适宜地位于层状产品的0-5层深度，优选为0-2层。最优选地，包括有膨胀的热塑性微球体的层是层状材料的最外层。适宜地，层状材料的包括有膨胀的热塑性微球体的层除了热塑性微球体之外还包括聚合物相。优选地，该聚合物相包括聚氨酯。
适宜地，层状材料是地板材料。适宜地，地板材料包括上装饰层、承载层和背衬层。优选地，层状材料是装饰性层压地板材料。适宜地，背衬层包括膨胀的热塑性微球体。作为选择，地板材料适宜地包括表层、承载层、背衬板和背衬层。
优选地，地板材料是镶木地板材料。适宜地，背衬层包括膨胀的热塑性微球体。层状材料还可以适宜地是墙部件或者屋顶部件。
可热膨胀的微球体优选分散在玻璃转化温度为约-100℃至约+10℃，优选为约-80至约-20℃的热塑性聚合物中。合适的聚合物分散体的例子是聚氨酯分散体、聚丙烯酸酯分散体、聚酯分散体、PVC分散体和塑料溶胶分散体。优选地，聚合物分散体是聚氨酯分散体。
取决于所希望的成品性能，分散体中可热膨胀的微球体的量可以在宽的范围内变化，并且适宜地为约1-约80wt％，优选为约5-约25wt％。以干物计算，可热膨胀的微球体与分散在处理组合物中的聚合物的比例适宜地为约1∶1-约1∶10，优选为约1∶3-约1∶7。
最后，本发明涉及浸渍或者涂覆的基质用作层状材料的一部分，尤其是用作平衡性背衬层的用途。
根据本发明方法的包括有可热膨胀的微球体的层可以包括任意种类的可浸渍的基质，这些基质包括纸以及织造和非织造的织物。适宜地，包括有可热膨胀的微球体的层包括纸。适宜地，纸的重量为约20-约250g/m2，优选约50-约140g/m2。纸适宜地是牛皮纸/再生纸。
适宜地用一种或多种可固化树脂浸渍基质。合适的用于浸渍根据本发明的基质的可固化树脂是热固性树脂例如蜜胺树脂，如蜜胺-甲醛，脲树脂例如脲-甲醛，酚醛树脂例如苯酚-甲醛，或其混合物。优选地，将蜜胺-甲醛树脂用于浸渍背衬层。适宜地，用数量为约40-约300g/m2，优选约80-约150g/m2的可固化树脂浸渍基质。
可以通过多种涂覆树脂组合物的常规技术，例如浴、辊子、刮刀、气刀、计量辊、刮胶棒等而用一种或多种可固化树脂浸渍基质。可以在涂覆阶段之间伴随着干燥和/或部分固化而以一个或多个步骤涂覆树脂组合物。
适宜地在用一种或多种树脂组合物浸渍之后进行用可热膨胀的微球体浸渍或者涂覆基质。适宜地，通过用包括有可热膨胀的微球体的处理组合物涂覆或者浸渍基质来进行用可热膨胀的微球体浸渍或者涂覆基质。
适用于本发明的可热膨胀的微球体具有密封了推进剂的热塑性聚合物壳。该热塑性聚合物壳可由选自以下物质的单体的共聚物组成：丙烯腈、甲基丙烯腈、α-乙氧基丙烯腈、α-氯丙烯腈、富马腈、偏二氯乙烯、氯乙烯、甲基丙烯酸酯、丙烯酸酯、苯乙烯、乙酸乙烯酯、丁二烯、neoprene和其混合物。热塑性微球体可以常规的方式，例如US3,615,972中所述的那样制得，该专利在此结合作为参考。推进剂通常是沸点温度不高于热塑性聚合物壳的软化温度的液体。也被称作吹泡剂、膨胀剂或者发泡剂的推进剂可以是烃，例如正戊烷、异戊烷、新戊烷、丁烷、异丁烷、己烷、异己烷、新己烷、庚烷、异庚烷、辛烷和异辛烷，或其混合物。除了它们之外，还可以使用其他的烃类，例如石油醚和氯代或氟代烃，例如氯甲烷、二氯甲烷、二氯乙烷、二氯乙烯、三氯乙烷、三氯乙烯、三氯氟代甲烷等。推进剂适宜地占微球体的5-40wt％。在加热时，推进剂在壳软化的同时蒸发以提高内压，导致了微球体的显著膨胀，通常为它们的直径的约2-约5倍。膨胀开始的温度被称作T开始，而实现最大膨胀的温度被称作T最大，这两者在温度提升速率为20℃/每分钟下测量。用于本发明的可热膨胀的微球体的T开始适宜地为约40-约200℃，优选为约50-约150℃，最优选约70-约130℃，而T最大适宜地为约60-约250℃，优选为约80-约210℃，最优选约100-约200℃。可膨胀的微球体的粒径可以在宽的范围内变化，并且相对于所希望的成品性能来加以选择。可膨胀的微球体的粒度的合适例子可以是1-1000μm，优选为2-500μm，最优选为5-50μm。
根据本发明的承载层适宜地为坚硬的，并且可由任何合适的材料例如基于木质的材料或者基于聚合物的材料制成。适宜地，承载层由基于木质的材料例如实木、胶合板、碎木板、纤维板和刨花板制成。优选地，承载层由碎木板或者纤维板制成。
层压材料适宜地在约100-约250℃，优选约125-约200℃的温度下，在约0.1-约10MPa，优选约2-约4MPa的压力下压制。
在本发明的优选实施方案中，在第一步骤中用蜜胺树脂浸渍牛皮纸/再生纸，干燥并且随后用包括有约5-约25wt％可热膨胀的微球体的浆液和聚氨酯的分散体浸渍，其中以干物计算，可热膨胀的微球体与分散在浆液中的聚合物的比例为约1∶3-约1∶7。此后，将所浸渍的纸干燥并且组装，在约2-约4MPa的压力下压制到MDF的承载层上。在释放出压力后，微球体膨胀并且形成平滑的层。
现在将连同以下实施例进一步描述本发明，然而这些实施例不应该被认为限制了本发明的范围。
实施例1
将再生纸(120g/m2重量/单位面积)用作基质并且采用标准方法浸渍(即，用蜜胺树脂填充纸基质并且将纸涂覆)。然后在浮动的网式干燥机中将所浸渍的纸干燥至挥发性物质的残余含量为6.5％。所浸渍和涂覆的再生纸的最终重量为250g/m2。
在相同的机器运行中，用含有10％(以重量计)的未膨胀的微球体(粒度：28-38μm)，T开始＝116-126℃，T最大＝190-202℃和90％或78％(以重量计)的含水聚氨酯分散体(固含量＝40wt％)的含水的、多相的并且稳定的混合物涂覆到纸的一侧并且干燥。聚氨酯分散体的玻璃转化温度(TG)为-32℃。如此浸渍和涂覆的纸的最终重量为330g/m2，挥发性物质的残余含量为6.5％。
为了制备装饰性层压材料，将8mm中等密度纤维板(MDF)在上面与装饰层(蜜胺树脂浸渍、印刷的装饰纸；最终重量250g/m2；纸重120g/m2)组装并且在下面与如上所述的浸渍的纸组装。在160℃下在2.0MPa的压力下将该组装体压制30秒。
在从所涂覆的MDF上加热剥离(stripping)时，背面上的微球体膨胀。嵌入聚氨酯基质中的膨胀的微球体提供了带有密闭孔的隔音层，其深深地并且牢固地连接和粘附到蜜胺树脂上(根据切格测试)。
如根据实施例5的方法所研究的那样，由此提供的层压材料具有产生12个宋单位的隔音性能，而没有表现出背衬纸的平衡性的任意退化。该层压材料在4周的检验周期内没有表现出任何明显的扭曲。
实施例2
将泡碱牛皮纸(80g/m2重量/单位面积)用作承载层并且根据标准方法用可商购获得的蜜胺树脂浸渍，然后在浮动的网式干燥机中干燥至挥发性物质的残余含量为7.0％。所浸渍和涂覆的牛皮纸的最终重量为200g/m2。
在相同的程序步骤期间，用含有15％(以重量计)的未膨胀的微球体(粒度：35-45μm)，T开始＝112-120℃，T最大＝180-188℃，和85％(以重量计)的含水聚氨酯分散体(固含量＝45wt％)的含水的、多相的并且稳定的混合物涂覆到纸的一侧并且干燥。聚氨酯分散体的玻璃转化温度(TG)为-55℃。如此浸渍和涂覆的纸的最终重量为275g/m2，挥发性物质的残余含量为6.9％。
根据实施例1中所述的方法，采用最终重量为200g/m2(纸重80g/m2)的装饰纸制备装饰性层压材料。
在从所涂覆的MDF上加热剥离时，背面上的微球体膨胀。嵌入聚氨酯基质中的膨胀的微球体提供了带有密闭孔的隔音层，其深深地并且牢固地连接和粘附到蜜胺树脂上(根据切格测试)。
在4周的检验周期期间，该层压材料的平整度保持不变。背衬层的平衡性没有受到施加了隔音层的负面影响。根据实施例5测量的隔音性能，即声音衰减为8个宋单位。
实施例3
用如实施例1中所述的标准蜜胺树脂浸渍再生纸(120g/m2重量/单位面积)，然后在浮动的网式干燥机中干燥至挥发性物质的残余含量为6.2％。该浸渍物的最终重量为260g/m2。
在相同的程序步骤期间，用含有8％(以重量计)的未膨胀的微球体(粒度：18-24μm)，T开始＝116-124℃，T最大＝171-181℃，和92％(重量/重量)的50％的含水丁二烯-苯乙烯共聚物阴离子分散体(TG＝-66℃)的含水的、多相的并且稳定的混合物涂覆到该浸渍物的一侧。如此浸渍的纸的最终重量为340g/m2，挥发性物质的残余含量为6.1％。
根据实施例1中所述的方法，采用最终重量为255g/m2(纸重120g/m2)的装饰纸制备装饰性层压材料。
在从所涂覆的MDF上加热剥离时，背面上的微球体膨胀。嵌入丁二烯-苯乙烯共聚物中的膨胀的微球体提供了带有密闭孔的隔音层，其深深地并且牢固地连接和粘附到蜜胺树脂上(根据切格测试)。
在6周的检验周期期间，该层压材料的平整度保持不变。背衬层的平衡性没有受到施加了隔音层的负面影响。根据实施例5测量的隔音性能，即声音衰减为10个宋单位。
实施例4
根据实施例1，用标准蜜胺树脂浸渍再生纸(120g/m2重量/单位面积)并且干燥至挥发性物质的残余含量为6.8％。所浸渍的纸的最终重量为255g/m2。
在相同的程序步骤期间，用含有10％(以重量计)的未膨胀的微球体(粒度：28-38μm)，T开始＝116-126℃，T最大＝190-202℃，和90％(以重量计)的42％的含水聚氯乙烯(PVC)糊料(TG＝-15℃)的含水的、多相的并且稳定的混合物涂覆到该浸渍物的一侧。如此浸渍的纸的最终重量为335g/m2，挥发性物质的残余含量为6.6％。
根据实施例1中所述的方法，采用最终重量为250g/m2(纸重120g/m2)的装饰纸制备装饰性层压材料。
在从所涂覆的MDF上加热剥离时，背面上的微球体膨胀。嵌入PVC中的膨胀的微球体提供了带有密闭孔的均匀的隔音层。
在4周的检验周期期间，该层压材料的平整度保持不变。背衬层的平衡性没有受到施加了隔音层的负面影响。根据实施例5测量的隔音性能，即声音衰减为2个宋单位。
实施例5
为了评价根据本发明制备的层压材料的隔音性能，根据方案EPLF(欧洲的层压地板制造商)标准021029-1“层压地板覆盖物-测量通过撞击机产生的鼓声”(得自于2002年10月29日，修改状态2003年11月)来检验该层压材料。该方案标准可由EPLF获得。
根据该方案标准，通过采用标准的撞击机来提供激感。声音环境中的点测(stationary measurement)类似于消声室(free-fieldroom)。信号根据ISO 532B评价特定的响度和总的响度。
特定响度的量纲是“宋”。0-15个宋单位的宋减少值被认为与隔音相关。

Claims (22)

1.一种制备包括承载层的装饰性层压材料的方法，其中该方法包括以下步骤：
-用热固性树脂浸渍基质，并且进一步用包括有可热膨胀的微球体的分散体浸渍或涂覆该用热固性树脂浸渍的基质，由此形成层状材料；
-通过使包括有可热膨胀的微球体的层状材料位于承载层的下面和装饰层位于承载层的上面，将层压材料组装。
2.根据权利要求1的方法，其中装饰层用蜜胺树脂浸渍。
3.根据权利要求1的方法，其中包括有可热膨胀的微球体的层状材料形成装饰性层压材料下侧上的最外层。
4.根据权利要求1的方法，其中该方法还包括使微球体膨胀。
5.根据权利要求1的方法，其还包括：在微球体开始膨胀的温度之上在没有压制的情况下至少将包括有可热膨胀的微球体的层状材料加热。
6.根据权利要求1的方法，其中包括有可热膨胀的微球体的层状材料还包括纸。
7.根据权利要求1的方法，其中层压材料是装饰性地板材料。
8.根据权利要求1的方法，其中层压材料是镶木地板材料。
9.根据权利要求1的方法，其中可热膨胀的微球体分散在热塑性聚合物中。
10.根据权利要求9的方法，其中热塑性聚合物的玻璃转化温度为-100℃至+10℃。
11.一种材料，包括有承载层、装饰层和层状材料，其中该层状材料包括一个用热固性树脂浸渍并进一步地用包括有可热膨胀的微球体的分散体浸渍或涂覆的基质，和其中所述层状材料位于承载层的下面和装饰层位于承载层的上面。
12.根据权利要求11的材料，其中微球体分散在热塑性聚合物中。
13.根据权利要求12的材料，其中热塑性聚合物的玻璃转化温度为-100℃至+10℃。
14.一种可通过包括以下步骤的方法获得的层状地板材料：用热固性树脂浸渍基质，进一步用可热膨胀的微球体涂覆或者浸渍该如此浸渍的基质，和通过如此浸渍的基质位于承载层的上面和装饰层位于承载层的下面，组装层状地板材料。
15.根据权利要求14的层状地板材料，其中可热膨胀的微球体分散在包括有热塑性聚合物的连续相中。
16.根据权利要求14的层状地板材料，其中用于获得层状地板材料的方法还包括在压力下进行加热。
17.根据权利要求11的材料，其中分散体包括聚氨酯。
18.根据权利要求11的材料，其中基质包括纸。
19.根据权利要求10的方法，其中热塑性聚合物的玻璃转化温度为-80℃至-20℃。
20.根据权利要求13的材料，其中热塑性聚合物的玻璃转化温度为-80℃至-20℃。
21.根据权利要求15的层状地板材料，其中热塑性聚合物的玻璃转化温度为-100℃至+10℃。
22.根据权利要求21的层状地板材料，其中热塑性聚合物的玻璃转化温度为-80至-20℃。
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