CN105579643B - 用于制造耐磨表面的分散体 - Google Patents

用于制造耐磨表面的分散体 Download PDF

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CN105579643B
CN105579643B CN201380079880.XA CN201380079880A CN105579643B CN 105579643 B CN105579643 B CN 105579643B CN 201380079880 A CN201380079880 A CN 201380079880A CN 105579643 B CN105579643 B CN 105579643B
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resin
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laminate
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CN105579643A (zh
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迪特尔·多林
奥利弗·哈特尔
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Lignum Technology Co ltd
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Abstract

本发明涉及用于制造树脂浸渍纸的分散体，该分散体可用于制造耐磨(微防刮)表面，诸如层压地板、家具表面或层压体(CPL、HPL)之类。本发明还涉及用于制造这样的表面的方法以及相应的制造产品。由此，分散体包含例如(按重量百分比)30％至75％的水和10％至65％的具有F400至F2000的粒径的刚玉颗粒以及其它少量的添加剂。该分散体可以被引入至液体氨基树脂混合物中以浸渍纸。

Description

用于制造耐磨表面的分散体
技术领域
本发明涉及用于制造树脂浸渍纸的分散体，该分散体可用于制造耐磨(微防刮)表面，诸如层压地板、家具表面或层压体(CPL、HPL)之类。本发明还涉及用于制造这样的表面的方法以及相应的制造产品。
背景技术
从现有技术中已知具有耐磨表面的各种材料，这些材料被用作地板罩面或家具表面。在这种情况下，相对廉价并且具有良好的耐磨表面的层压地板特别普遍。这样的层压地板通常基于由MDF材料或HDF材料制成的支撑板或支撑层，在支撑层的顶部施加一个或多个树脂浸渍纸层。所使用的树脂通常是氨基树脂，该氨基树脂在热量和压力的作用下通过压制被固化。树脂或浸渍纸也常常设置有耐磨颗粒以增加表面的耐磨性。因此，粒径通常为40μm至140μm的耐磨颗粒可以在浸渍纸之前被加入到树脂中和/或颗粒在浸渍之后被添加到尚未干燥的纸上，从而在固化之前被添加。
在EP 0732449 A1中，提出特殊的树脂混合物，该混合物由水、三聚氰胺树脂、具有预定纤维长度和数量的α纤维素以及具有约20μm至50μm的粒径的刚玉粉组成。从而，混合物中的刚玉粉应当被高度地分散开并且应当被固定至α纤维素的纤维。由此，矿物保持分散均匀并且纤维素纤维确保混合物中所含的树脂不再渗入到装饰片内，而是主要保留在表面上并形成相对厚的树脂层。
EP 2288500 B1还公开了层压体及其制造方法。本文件的基本问题是所添加的耐磨颗粒一方面引起层压体的光泽度和透明度减少并且另一方面引起用于制造层压体的压板破坏或磨损。作为解决方案，该出版物提出在第一步骤中用氨基塑料树脂浸渍纸并进行干燥。然后，由表面改性的氧化硅纳米颗粒和分散剂组成的分散体应被施加到已被浸渍的该纸上。由此，分散剂应由例如水或极性溶剂组成。表面改性的氧化硅纳米颗粒的使用将导致纳米颗粒与氨基塑料树脂基质的相容性得到改善，致使纳米颗粒在树脂基质中均匀分布并在已浸渍的纸的表面上均匀分布。由此，如此产生的表面的耐性得以显著改善应由纳米颗粒的改进的嵌入造成。如此产生的层压体应适于用作地板罩面、桌面或者通常用于制造其它家具的家具。这种方式可产生微防刮表面，但是该过程是非常昂贵的。
从EP 2397448 A1中已知制造粉末材料并在玻璃基体上施加粉末材料，该粉末材料特别适于用在涂布地板的三聚氰胺树脂等中。例如，精磨硼硅酸盐玻璃可以与蜜胺树脂一起得到良好地处理，而作为蜜胺树脂的添加剂的精磨钠石灰玻璃是不适合的，这是因为形成不均匀的、连续的膜。在该文件中，下述问题因此已被提到：并非每一个添加剂都适于与三聚氰胺树脂等一起进行处理，而是与此相反，非常难以找到合适的材料。
从WO 2007/048731 A1中己知设置有无机纳米颗粒(诸如大小为2nm至500nm的氧化硅颗粒等)的氨基树脂。
由此，纳米颗粒有助于使设置有氨基树脂的表面更耐磨。
EP 0136577 A2中描述了装饰层压地板，其包括施加在例如纤维板等的支撑板上的树脂浸渍装饰纸。大小为5nm至100nm的纳米颗粒被添加于此以增强表面的防刮性。
从现有技术中已知的方法的确可以导致令人满意的磨损值，所产生的表面不论以何种方式都包括不令人满意的耐磨性(也称为防刮性或微防刮性)和/或表面的制造复杂或昂贵。本领域技术人员理解耐磨性或微防刮性为表面对深度非常小的划痕(其往往通过用软材料本身进行清洁操作所产生)的抗性。这些微刮痕通常具有不超过约6μm的深度，具体地为表面的光学损害，并且没有那么多的功能性的损害。因此，表面可以包括良好的耐磨性-并且因此很好地承受导致深划痕(大约毫米级别)的典型的应力-并且可仍对微划痕敏感。换句话说，就防刮优化而言，对良好的耐磨性进行优化的表面通常不是必须的。
已经对用于氨基树脂的纳米颗粒的修正进行了反复的尝试，由于成本和加工困难的原因还未确立该氨基树脂。与此氨基树脂相反，在丙烯酸酯树脂中纳米颗粒的修正可以更容易，这导致改进的防刮性。现在其满足现有技术使得丙烯酸涂层表面获得非常高的微防刮性。作为示例，提及Nano-X GmbH的如果未来氨基树脂表面将比丙烯酸树脂表面有竞争力，经济上和技术上的可持续发展是必需的。
因此，本发明的目的在于提供用于制造树脂浸渍纸的特殊分散体，耐磨颗粒可以被适当地供给至分散体，使得所产生的表面具有改进的微防刮性。由此，具体而言，本发明的目的在于提供一种分散体，该分散体与树脂一起易于得到处理，并且其中，只具有约181μm至1μm(按照针对产品的FEPA标准42-2(2006)，F400至2000)的平均尺寸的非常细的耐磨颗粒可以被非常均匀地分散开。发明的目的还在于提供用于制造适于制造层压地板、家具表面等的层压材料的方法以及这样的产品，其中，该产品与较细的刚玉颗粒一起使用并且具有良好的防刮性。
通过根据权利要求1所述的分散体、根据权利要求7所述的用于制造层压材料的方法以及根据权利要求12所述的层压材料实现这些目的。
发明内容
根据本发明，提供了用于制造树脂浸渍纸的分散体。该分散体优选包含下列组分(按重量百分比)：20％至75％的水；10％至65％的具有F400至F2000粒径的刚玉颗粒；0.5％至15％的阴离子分散剂，或者0.5％至15％的阴离子分散剂和非离子表面活性剂的混合物；以及0.01％至2％的增稠剂。
优选地，该分散体包括下列组分(按重量百分比)：30％至75％的水；10％至65％的具有F400至F2000(按照FEPA标准)的粒径的刚玉颗粒；0.05％至5％的阴离子分散剂和/或0.1％至5％的非离子表面活性剂；0.05％至5％的聚丙烯酸钠以及0.01％至2％的增稠剂。
已经表明，在这样的分散体中，具有仅F400到F2000的粒径(相当于约18μm至1μm的粒径)的相对较细的刚玉颗粒也可以被很均匀地分散开并且也可以长时间地保持在分散体中，即，不沉降并且不会形成团块。几乎更重要的是：该分散体与常见树脂(诸如特定的氨基树脂等)配合良好，而不会导致现有技术中所述的那些问题，例如，刚玉颗粒沉降，树脂瑕疵或者膜的形成不充分等。根据本发明的分散体允许使用具有指定小粒径的刚玉颗粒，令人吃惊地，如果被适当地使用，这导致即使在非常少的添加数量的情况下表面也具有非常良好的微防刮性(耐磨性)。
一般而言，如果应该实现高磨损值，则直径较大的颗粒通常是理想的。然而，大颗粒不会导致改进的防刮值，即，虽然大颗粒很好地免受大且重的机械冲击的影响，但是它们可能并不能防止例如通过用布进行清洁操作所形成的微划痕(多达约6μm深)的形成。
一般地，优选分散体被构建如下(按重量百分比)或者包括以下比率：35％至70％的水；20％至60％的具有F400到F2000的粒径的刚玉颗粒；0.06％至4％的阴离子分散剂；0.06％至4％的聚丙烯酸钠；0.15％至4％的非离子表面活性剂以及0.02％至2％的增稠剂。
更优选地，分散体被构造如下或者包含以下比率：40％至68％的水；30％至58％的具有F400到F2000的粒径的刚玉颗粒；0.07％至3.5％的阴离子分散剂；0.07％至3.5％的聚丙烯酸钠；0.2％到3.5％的非离子表面活性剂以及0.03％至2％的增稠剂。
增稠剂优选使用页硅酸盐(sheet cilicate)和/或多糖。
已经表明，如果所使用的刚玉颗粒被硅烷化，细颗粒可能会特别好地嵌入后面的树脂基质中。
一般地，本发明的分散体甚至允许使用具有仅F500至F2000的粒径的刚玉颗粒，并且最优选地，粒径的范围为从F600至F1000。本领域的技术人员知道术语F400、F600等用于根据FEPA标准42-2(2006)来确定粒径。本发明还涉及用于制造适于制造家具和地板的层压材料，该方法包括以下步骤。
如上所述，制造方法的起点是分散体。该分散体被引入到水性(即液体)树脂混合物(优选氨基树脂混合物)中，其中优选0.5kg至7kg的分散体被引入至100kg的树脂(涉及液体树脂混合物中的固含量)、更优选地0.5kg至5kg的树脂、并且最优选地0.6kg至3kg的树脂。在这种情况下，树脂的固含量被用作计算的基础。以水性溶液形式市售提供这些树脂，其中，固含量通常在50％至60％之间变化。由这些树脂的混合物的提供者提供或者可以由本领域的技术人员所知的方式来判定固含量。示例性地参照EN 827(2005.7.6.1)，其中规定结合剂的固含量的判定。在搅拌并且分散体在树脂混合物中均匀地分散开之后，(例如，由滚涂机)浸渍纸。然而，纸也可以经过树脂混合物的浴。然后，浸渍纸被施加到例如木材或木材材料的支撑层上，并且继而在热量和压力的作用下固化在该支撑层上。由此，优选树脂为如在制造层压地板时通常使用的氨基树脂，即，具体为蜜胺树脂和/或尿素树脂。此外，自然可以执行附加制造步骤。
例如，在层压制造中结合酚醛树脂浸渍牛皮纸，其中数量和克数取决于所期望的最终的材料强度。在牛皮纸的这些核心层上施加氨基树脂浸渍装饰纸并且罩面(overlay)用作顶层。该罩面例如用含有树脂混合物的分散体浸渍。如果不使用罩面，装饰纸也可以用含有树脂混合物的分散体浸渍。然后，在热量和压力的作用下以本领域的技术人员所公知的方式压制。
已经表明，在搅拌分散体期间(即，具体地当搅拌分散体时)、在引入到树脂混合物之前，以至少10米/秒、优选地至少12米/秒并且最优选地15米/秒的剪切速率搅拌分散体至少10分钟有利于根据本发明的分散体的制造。
包括新的和迄今未达到的性能的层压材料可以在根据本发明的分散体或者根据本发明的制造方法的帮助下来制造。虽然用本分散体或者借助于本方法制造的层压体或层压材料仅提供具有F400至F2000的粒径的非常细的耐磨颗粒并且还优选只施加非常小的质量(即，从0.3g/m2至3g/m2，优选从0.3g/m2至2g/m2，甚至更优选从0.4g/m2至1.5g/m2，并且最优选从0.4g/m2至1g/m2)，但是，它们具有良好的防刮性。
因此，本发明还涉及包括木材、木材材料或层压地板的支撑层的层压材料，其中在优选的顶层中的支撑层的主面包括氨基树脂浸渍纸，该浸渍纸包括具有从F400至F2000的粒径的刚玉颗粒。根据ENl6094：2012-04，这样的压制表面的微刮伤性为至少MSR-A2、优选MSR-A1并且抗性级别为至少MSR-B2和甚至优选地MSR-B1。层压体可以通过使用上述方法浸渍纸获得，即，使用根据本发明的按限定比例引入至液体树脂中的分散体。如果根据本发明的层压材料例如用作地板罩面，或者用于制造地板罩面，可以根据已知方法额外地施加具有40μm至140μm的粒径的刚玉来获得该附加的高耐磨值。
支撑板或支撑层优选由具有4mm至40mm板厚的MDF或HDF板构成，并且所使用的树脂依次优选为氨基树脂，具体地为蜜胺树脂和/或尿素树脂。
下面，将参照若干示例性实施例更详细地描述本发明：
示例1：微刚玉分散体的制造
提交40kg水、4kg低脂肪醇聚氧乙烯醚(low ethoxylated fatty alcohol)(例如，来自BASF的Lutensol TO3)、4kg琥珀酸二辛酯钠(例如，来自BASF的Lutensit A-BO)、4kg聚丙烯酸钠(例如，Lopon LF；BK Giulini)。在室温下搅拌该混合物5分钟。接着，在搅拌的同时加入具有F1000的粒径的47.5kg的刚玉。此后，加入0.5kg页硅酸盐(对应于增稠剂)(Betone EW；Elementis)。现在以15米/分钟的剪切速率使其分散10分钟。也可以代替页硅酸盐加入相同比率的多糖类(阿拉伯树胶或角豆粉)。也可以提交阿拉伯胶和Betone EW的组合物。
示例2：浸渍树脂混合物的制造
来自示例1的微刚玉分散体以及具有60％的固含量的90kg的市售蜜胺甲醛浸渍树脂用作起点。用0.37kg合适的三聚氰胺树脂固化剂、0.21kg润湿剂、0.45kg脱模剂和8.15kg水对其进行处理。混浊时间范围应为从5：00至5：30分钟。在搅拌的同时，加入示例1中所述的0.82kg微刚玉分散体(因此，这对应于浸渍树脂的固含量为每100kg具有1.52kg的分散体)。这样制造的树脂放入至市售浸渍通道的浸渍浴中。
示例3：具有微防刮表面的复合地板的制造
用示例2的树脂混合物浸渍具有60g/m2的克重的含刚玉罩面纸。因此，设定280％的树脂施加，即浸渍体的克数为228g/m2。本领域的技术人员理解浸渍体为干燥后但在树脂固化前的浸渍纸。因此，在浸渍纸干燥后进行测量。这具有实际的原因，由于在工厂中干燥器直接跟在浸渍浴或浸渍通道后面，使得用于测量树脂含量的采样通常在干燥之后才是可行的或者有意义的。然后，采集的样本切成100cm2的片材并被称重。原纸(这里是60g/m2)的重量与称重值之间的差大致对应于树脂的施加量(干燥后不可避免的残留水分中的任何差异是非常低的并且可忽略不计)。在本示例中，浸渍体含有约168g/m2的树脂添加(60g/m2的280％)。然后，浸渍体被进一步处理如下：在厚度为8mm的HDF支撑板的下侧设置有常规浸渍中和纸，并且在支撑板的上侧设置常规浸渍装饰纸。然后，浸渍罩面被布置在该装饰纸上作为最上层。该夹层复合材料进入到短周期压缩机并且在185℃下被压制15秒。在冷却并沉积由此获得的涂布层压材料板之后，分割并将己知的轮廓切割成地板。按照EN 13329，由此生产的地板达到耐磨级别AC5，并且按照16094，地板达到最高微防刮水平MSR-A1和MSR-B1。
示例4：具有微防刮表面的层压地板的制造
用如示例2所述的树脂混合物浸渍具有25g/m2的克重的罩面。设定300％的树脂施加，使得浸渍体的克数为约100g/m2。然后，双带压机(诸如可从Hymmen公司获得)从底部到顶部组装如下：羊皮纸50g/m2、每一者都具有278g/m2的克重的两个酚树脂浸渍芯层、三聚氰胺树脂和所述罩面。该夹层复合材料在180℃的表面温度下并且以12米/分钟的速度经过双带压机。由此获得的层压材料或层压地板背部被研磨并且粘到38mm厚的硬纸板上。以这种方式，按照EN 16094，获得具有最高微防刮等级MSR-A1和MSR-B1的厨房操作台(kitchenworktop)。在具有常规的蜜胺树脂表面的对比试验中，仅获得等级MSR-A3和MSR-B4。
示例5：用于家具表面的直接涂布纸板的制造
用来自示例2的浸渍树脂混合物浸渍具有橡木复制品和70g/m2的克重的装饰纸。树脂施加为135％，即浸渍体的克重为约164.5g/m2(即，70g/m2纸加上94.5g/m2的树脂施加)。厚度为18mm的纸板在两侧结合有装饰浸渍体并且在185℃下在短周期压机中被压制18秒。由此获得的层压材料的表面具有最高微防刮等级MSR-A1和MSR-B1。
这些实施例示出可以通过所述过程使用非常少的微刚玉添加剂完全令人惊讶地实现最高微防刮等级。在示例5中，微刚玉含量例如为0.7g/m2。由此，该处理是鲁棒的，在浸渍浴中产品(Absatzerscheinungen)没有分离，甚至经过较长的生产时间段也不会分离。微刚玉的浓度极低的另一个优势当然也是这样的事实：将不会不利地影响处理操作，并且表面保持高度透明并且添加剂不能使其变浑浊。
附图说明
下面，将参照附图更加详细地解释本发明，其中
图1是示出了根据本发明的方法的框图。
具体实施方式
在图1中，根据本发明的方法被示例性地示出。本领域的技术人员将会理解，所图示的方法的步骤S1至S7中不一定必须按给定的顺序发生，也可以以任何逻辑顺序发生。具体而言，例如步骤S1和S2是否在S3和S4之前发生是不重要的。在示例性方法的第一步骤S1中，提供MDF的支撑层，诸如约6mm厚的MDF板之类。在步骤S2中，提供纸，诸如装饰纸之类，即，带有装饰图案的印色纸。然后，在步骤S3，继而根据上述指示制备根据本发明的分散体并且在步骤S4中将分散体引入至蜜胺树脂的液态树脂混合物并且引入到常用的添加剂中并被搅拌。在步骤S5中，这种树脂分散体混合物供应给纸，并且该纸浸渍有混合物。这样的浸渍纸中间是干燥的并且继而施加在MDF的支撑层上。然后，这样的浸渍纸在热量和压力的作用下被固化在支撑层上，从而形成层压材料，该层压材料具有良好的微防刮性并且能够被进一步加工成例如地板或家具板。

Claims (31)

1.一种用于制造浸渍有树脂的纸的分散体，所述分散体按重量百分比计包括下列组分：
30％至75％的水；
10％至65％的具有F400至F2000的粒径的刚玉颗粒；
0.05％至5％的阴离子分散剂；
0.05％至5％的聚丙烯酸钠；
0.1％至5％的非离子表面活性剂；
0.01％至2％的增稠剂。
2.根据权利要求1所述的分散体，其特征在于，所述组分按重量百分比计为如下：
35％至70％的水；
20％至60％的具有F400至F2000的粒径的刚玉颗粒；
0.06％至4％的阴离子分散剂；
0.06％至4％的聚丙烯酸钠；
0.15％至4％的非离子表面活性剂；
0.02％至2％的增稠剂。
3.根据权利要求2所述的分散体，其特征在于，所述组分按重量百分比计为如下：
40％至68％的水；
30％至58％的具有F400至F2000的粒径的刚玉颗粒；
0.07％至3.5％的阴离子分散剂；
0.07％至3.5％的聚丙烯酸钠；
0.2％至3.5％的非离子表面活性剂；
0.03％至2％的增稠剂。
4.根据权利要求1-3中任一项所述的分散体，其特征在于，所述增稠剂包括页硅酸盐或多糖。
5.根据权利要求1-3中任一项所述的分散体，其特征在于，所述增稠剂是页硅酸盐或多糖。
6.根据权利要求1所述的分散体，其特征在于，所述刚玉颗粒被硅烷化。
7.根据权利要求1所述的分散体，其特征在于，所述刚玉颗粒的粒径从F500至F2000。
8.根据权利要求1所述的分散体，其特征在于，所述刚玉颗粒的粒径从F600到F1000。
9.一种用于制造层压材料的方法，所述方法包括以下步骤：
a)提供支撑层；
b)提供纸；
c)提供分散体，所述分散体按重量百分比计包括以下组分：
30％至75％的水；
10％至65％的具有F400至F2000的粒径的刚玉颗粒；
0.05％至5％的阴离子分散剂；
0.05％至5％的聚丙烯酸钠；
0.1％至5％的非离子表面活性剂；
0.01％至2％的增稠剂；
d)将所述分散体引入至液态树脂混合物中，其中，0.5至7kg的分散体引入到100kg的树脂；之后
e)用树脂分散体混合物浸渍所述纸；
f)将浸渍纸施加到所述支撑层上；以及
g)将所述浸渍纸固化在支撑层上。
10.根据权利要求9所述的用于制造层压材料的方法，其中，0.5至5kg的分散体引入到100kg的树脂。
11.根据权利要求9所述的用于制造层压材料的方法，其中，0.6至3kg的分散体引入到100kg的树脂。
12.根据权利要求9所述的用于制造层压材料的方法，其特征在于，所述树脂为氨基树脂。
13.根据权利要求9所述的用于制造层压材料的方法，其特征在于，所述树脂是蜜胺树脂和/或尿素树脂。
14.根据权利要求9-13中任一项所述的制造层压材料的方法，其特征在于，固化所述浸渍纸的步骤是在热量和/或压力下执行的。
15.根据权利要求9-13中任一项所述的制造层压材料的方法，其特征在于，固化所述浸渍纸的步骤是在压力机中执行。
16.根据权利要求9所述的用于制造层压材料的方法，其特征在于，在所述步骤d)之前，以至少10米/秒的剪切速率混合所述分散体至少10分钟。
17.根据权利要求9所述的用于制造层压材料的方法，其特征在于，在所述步骤d)之前，以至少12米/秒的剪切速率混合所述分散体至少10分钟。
18.根据权利要求9所述的用于制造层压材料的方法，其特征在于，在所述步骤d)之前，以至少15米/秒的剪切速率混合所述分散体至少10分钟。
19.根据权利要求9所述的用于制造层压材料的方法，其特征在于，所述支撑层由木材、木质材料或层压体组成。
20.一种层压材料，其包括木材、木质材料或层压体的支撑层，
-其中，至少在所述支撑层的一个主侧设置树脂浸渍纸，所述树脂浸渍纸包括：
-具有F400至F2000的粒径的刚玉颗粒；其中
-按照EN 16094:2012-04，所述层压体包括至少MSR-A2的微防刮性，以及至少MSR-B2的抗性级别；并且所述层压体是通过使用以下方法浸渍所述纸而获得的：
a)提供分散体，所述分散体按重量百分比计包括以下组分：
30％至75％的水；
10％至65％的具有F400至F2000的粒径的刚玉颗粒；
0.05％至5％的阴离子分散剂；
0.05％至5％的聚丙烯酸钠；
0.1％至5％的非离子表面活性剂；
0.01％至2％的增稠剂；
b)将所述分散体引入至液态树脂混合物中，其中，0.5至6kg的分散体引入到100kg的树脂；之后
c)用树脂分散体混合物浸渍所述纸。
21.根据权利要求20所述的层压材料，其特征在于，按照EN 16094:2012-04，所述层压体包括至少MSR-A1的微防刮性。
22.根据权利要求20所述的层压材料，其特征在于，所述层压体包括至少MSR-B1的抗性级别。
23.根据权利要求20所述的层压材料，其特征在于，0.5至5kg分散体引入到100kg的树脂。
24.根据权利要求20所述的层压材料，其特征在于，0.6至4kg的分散体引入到100kg的树脂。
25.根据权利要求20-24中任一项所述的层压材料，其特征在于，所述树脂是氨基树脂。
26.根据权利要求20-24中任一项所述的层压材料，其特征在于，所述树脂是蜜胺树脂和/或尿素树脂。
27.根据权利要求20所述的层压材料，其特征在于，所述支撑层是具有4mm至40mm的板厚度的MDF板或HDF板。
28.根据权利要求20所述的层压材料，其特征在于，所述树脂浸渍纸包括0.3至3g/m2的刚玉含量。
29.根据权利要求20所述的层压材料，其特征在于，所述树脂浸渍纸包括0.3至2g/m2的刚玉含量。
30.根据权利要求20所述的层压材料，其特征在于，所述树脂浸渍纸包括0.4至1.5g/m2的刚玉含量。
31.根据权利要求20所述的层压材料，其特征在于，所述树脂浸渍纸包括0.4至1g/m2的刚玉含量。
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