CN107750292B - 具有用耐磨的、容易清洁的和疏水的表面整理的氨基塑料树脂膜的木质复合板的涂层 - Google Patents

具有用耐磨的、容易清洁的和疏水的表面整理的氨基塑料树脂膜的木质复合板的涂层 Download PDF

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CN107750292B
CN107750292B CN201680036076.7A CN201680036076A CN107750292B CN 107750292 B CN107750292 B CN 107750292B CN 201680036076 A CN201680036076 A CN 201680036076A CN 107750292 B CN107750292 B CN 107750292B
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R·艾斯佩
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Abstract

本发明涉及用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，所述整理用于涂覆木质复合板并且形成耐磨的、容易清洁的和疏水的表面，其特征在于，在完成树脂浸渍之后在第二施加步骤中将经浸渍的纸用溶胶‑凝胶制剂涂覆，所述溶胶‑凝胶制剂包含由金属钼和/或钨的金属二硫化物组成的富勒烯状纳米结构和纳米管以及经溶解的金属烷氧化物；和随后在干燥和最终缩合之后，将表面在液压热压机中成形。

Description

具有用耐磨的、容易清洁的和疏水的表面整理的氨基塑料树 脂膜的木质复合板的涂层
本发明涉及用于涂覆木质复合板的具有耐磨的、容易清洁的和疏水的表面的氨基塑料树脂膜的整理，其用于制造地板或应用于家具制造。
氨基塑料树脂膜被理解为三聚氰胺缩合树脂、甲醛缩合树脂或者脲与三聚氰胺的混合树脂，其在压力和温度下最终缩合或者在空间上交联。
在涂覆随后用于加工成地板镶板的HDF板(高密度纤维板)时使用三聚氰胺树脂膜。在这种情况下，利用用三聚氰胺树脂浸渍的由精制纸浆组成的经印刷的装饰纸，所述三聚氰胺树脂随后在浸渍通道的干燥区域中预缩合。通常，将装饰纸与经浸渍的20至45g/m2的贴面纸一起在液压热压机中压制。贴面层用于装饰膜和其它高要求的表面的调质处理。其由用三聚氰胺树脂浸透并且另外包含有限量的矿物填料例如刚玉的高品质的精制纸浆纸组成。
地板必须是相对耐磨的，因此将其表面用这些填料强化。在此，作为硬质材料，由于其硬度、透明性和惰性，经证实有效的是电熔刚玉、烧结刚玉、单晶刚玉和/或经煅烧或经烧结的矾土产品形式的Al2O3。
这类硬质材料的施加根据现有技术以各种方式进行。因此可以向用于纸表面涂层的三聚氰胺浸透的树脂直接掺入该硬质材料。在另一情况下，在造纸时向贴面纸直接附加原纸料的一定量的刚玉，由此在树脂浸渍时取消了刚玉混入。
在EP 0732449 A1中描述了用于制造在制造耐磨的层合体时使用的装饰纸的方法。在此，向树脂混入耐磨的矿物成分如刚玉。
DE 195 29 987 A1描述了用于制备在坚硬的载体材料上的高耐磨漆层的方法。该漆层借助合成树脂漆如丙烯酸系树脂漆、聚酯树脂漆或聚氨酯树脂漆产生，其中将耐磨损性试剂在固化之前分散到漆层上。在另一文献EP 1070688 A1中描述了具有一定硬度的经表面涂覆的硬质材料。将该硬质材料作为耐磨损性试剂提供至漆层中。
合成刚玉的制备通常在电弧炉中进行，其中使起始原料矾土或铝土矿在约2000℃熔融。产物在该过程的情况下以块的形式产生，将其在冷却之后粉碎并且随后加工成粒料。
在粉碎刚玉时，由于其脆性断裂行为而产生具有许多刃型位错、微边缘和裂纹的强烈起伏的表面。
这些刚玉微粒在热压机中的稍后的压制过程中在所使用的均压板表面上引起明显问题。
将三聚氰胺树脂膜与贴面层膜一起在具有可以结构化、消光或上光的相应均压板的所谓的液压热压机中在压力和温度下进行压制。三聚氰胺树脂膜在这种情况下最终缩合并且形成不可逆的硬表面。刚玉微粒在压制之后位于经涂覆的木质复合板的表面处。
所使用的均压板通常由硬度为38&ndash；42HRC的来源AISI 410、AISI 630的硬质铬钢组成。但也可以使用硬度为130HB的黄铜板MS 64。为了改进金属表面相对三聚氰胺树脂的分离性质和保护表面免受划痕，金属板表面配备有铬镀层，这以电化学方式在铬酸浴中用Cr(VI)化合物进行。铬镀层应当具有功能性质，因此力求达到超过20μm的硬铬层。
尽管镀铬的金属板表面具有1000至最高1200HV的硬度，仍然产生金属板表面的过早磨损，其中铬层的光泽度改变。这由于大的硬度差异而发生，刚玉具有1800至2000HV的维氏硬度。在压制过程期间由于在加热板相向运动(Zufahren)之后的金属板膨胀而发生运动。均压板经受温度突变，因为其与加热板紧密接触。在另一侧上，三聚氰胺树脂的逐渐缩合导致表面的收缩，由此在高压下产生强烈摩擦，所述摩擦引起金属板表面的过早磨损。因此必须将金属板表面相对快地再次加工和重新镀铬。
本发明的任务在于，如此整理经氨基塑料树脂浸渍的装饰纸和贴面层，从而防止镀铬的均压板表面的过早磨损，最终缩合的氨基塑料树脂表面是耐磨的和形成额外的容易清洁的和疏水的表面。
所述任务根据本发明的建议由此解决，装饰纸和/或贴面纸在完成用氨基塑料树脂的浸渍之后获得额外的溶胶-凝胶涂层，所述溶胶-凝胶涂层富集有纳米结构化的二硫化钨或二硫化钼，其中金属二硫化物的纳米结构以富勒烯状纳米颗粒和纳米管的形式形成。
例如二硫化钨的富勒烯状纳米颗粒在溶胶-凝胶混合物中的额外的富集在膜固化之后赋予表面额外的高分离效果和滑动效果。因此防止了均压板表面处的磨损并且改进了复合材料层的摩擦性质。由溶胶-凝胶法产生的例如由Al2O3、TiO2或SiO2组成的表面层产生稍后涂覆的木质复合板的表面的硬度，其中产生额外的容易清洁的和疏水的表面。
溶胶-凝胶法是用于制备陶瓷以及杂合有机-无机材料的湿化学方法。可以通过溶胶-凝胶过程制备薄的层以及小的颗粒和纤维、气溶胶和干凝胶，还有整料材料。基本上溶胶-凝胶法描述了贯穿每个产品的两个典型阶段。首先制备溶胶，其由在液体中的约1nm至100nm尺寸的细分散的胶态颗粒组成或由经分散的低聚物组成，所述低聚物由支化的大分子组成。为了产生溶胶，使用所谓的前体，其为溶于水中或另一液体中的金属烷氧化物或金属盐。如果要例如将来自醇溶液的可水解的多价金属离子(M＝Ti、Si或Al)的醇盐施加至表面上，则在H2O存在下即使在低温的情况下也已经在溶剂蒸发时形成金属氢氧化物网络。那么这包含大量MOH基团并且因此是亲水性的和抗静电的。
因为水解反应和缩合反应，出现颗粒的生长和增强的聚合，直至最后在液相内已形成牢固的网络，所述网络之后被称为凝胶。通过蒸发溶剂，由凝胶产生干凝胶，所述干凝胶通过另外的温度控制转变成牢固和致密的形式。其通过H2O消去而变成金属氧化物基团并且表面是坚硬和防刮的。
在经浸渍的装饰纸或贴面纸(在另外的描述中也称为基材)上沉积或施加薄的层可以借助于多种涂覆方法进行。因此可使用浸涂(dip-coating)、旋涂(spin-coating)，但是合适的是，对于单侧表面施加而言经证实有效的是借助刮刀涂覆或用涂抹辊施涂。通常，将基材用液态溶胶涂覆。在施加之后，然后是蒸发溶剂，在这种情况下颗粒的浓度急剧升高，这此时通过使颗粒彼此结合导致凝胶的形成和因此导致牢固但是还多孔的层。所述层也被称为干凝胶，还包含轻微份额的溶剂。只有通过在浸渍通道的随后的干燥区域中发生的退火才已由溶胶-凝胶过程形成金属氧化物的牢固的固相，并且在热压机中在压力和温度下的浸渍树脂的最终缩合的另外的进程中形成金属氧化物的整个硬的层。
取决于期望的表面硬度作出对金属氧化物的选择。作为合适的金属化合物，经证实有效的是金属铝、锆、钛和硅。借助于其氧化性化合物能够实现非常好的溶胶-凝胶层。在另外的进程中，描述了两个溶胶-凝胶层，其为Al2O3和SiO2。
制备Al2O3的起始原料可以例如为Yoldas溶胶。方法的第一步骤为铝烷氧化物的水解，取名例如三仲丁氧基铝Al(OCH(CH3)C2H5)3并且在大大过量的水中在约85℃水解。这产生氢氧化铝悬浮液，接着将其通过添加少量硝酸HNO3转变成清澈的溶胶或者转变成胶态溶液。
如果根据Yoldas过程采用较低的化学计量水含量加工，则例如将三仲丁氧基铝与绝对乙醇和乙酸以三仲丁氧基铝:C2H5OH:H2O(DI)＝1:16:0.6的比例混合并且在约50分钟的持续搅拌下升温至约65℃。原始的浑浊混合物在开始水解之后缓慢变清澈。将清澈的溶胶混合物冷却至室温。在第二步骤中，通过添加甲醇CH3和H2O产生凝胶，其中重量比可以为大约溶胶:CH3:H2O＝1g:0.2g:0.003g，为此还提供少量乙酸。
另一种溶胶可以由商业上可得的勃姆石粉末制备。
在制备SiO2凝胶时，可以使用硅酸酯，例如使用原硅酸四乙酯TEOS作为前体。由有机改性的氧化硅组成的这样的杂合有机-无机层的名称也经常被称为有机改性硅酸盐(Ormosile)。为了制备有机改性硅酸盐层，可以使用不同的材料，尤其是从不同的硅烷出发。溶胶-凝胶层的稍后的机械行为依赖于化学结构及其在溶胶中的浓度。例如可以使用式(OC2H5)3Si-(CH2)3-CH(O)CH2的硅烷、3-缩水甘油氧基丙基三甲氧基硅烷，也已知其商标名
Figure BDA0001515310870000041
或GLYMO。如果要提高层的硬度，则可以引入由SiO2或Al2O3组成的额外的纳米颗粒。位于胶态无定形SiO2颗粒表面上的OH基团在这种情况下可以与所使用的硅烷反应并且因此将颗粒纳入层基质中。还可以由具有亲水的或疏水的或防污的效果的有机改性的SiO2制备层。
在制备为涂层提供的溶胶之后，随后进行无机富勒烯状二硫化钨颗粒的制备，将两个制剂合并在一起。
无机富勒烯状纳米颗粒和纳米管具有10至25nm的粒径。纳米管具有10至25nm的直径和200至300nm的长度。在薄的层中观察到由二硫化钨或二硫化钼组成的第一无机富勒烯状颗粒，它们通过在还原性气氛下硫化WO3层或者MoO3层产生。无机富勒烯在1990年在以色列首次制备，所使用的材料为二硫化钨(WS2)和二硫化钼(MoS2)。在另一进程中制备了大量其它无机富勒烯状材料，例如TiS2、硒化物、溴化物和氯化物如NiBr2、NiCl2，还有各种氧化物例如V2O5以及氮化硼。对于根据本发明的应用，选择二硫化钨，还有二硫化钼。富勒烯状纳米颗粒和纳米管形式的二硫化钨因为其物理性质和晶体学形态极佳地适合于各种应用目的。在溶胶-凝胶制剂中，已证实富勒烯状二硫化钨极其有效并且因此避免了在稍后的使用中经涂覆的木质复合板上的磨损。同样防止了在压制过程期间均压板上的磨损。二硫化钨和二硫化钼在摩擦接触中的润滑效果主要是由于形成WS2或者MoS2的薄的膜，其在摩擦体的表面上的接触区域中形成。该所谓的摩擦膜(Tribofilm)使得彼此低摩擦滑动表面成为可能并且因此减少摩擦体的磨损。因此相对于作用在镀铬的均压板表面上的摩擦力，该效果扩大得相当积极。
在商业上，主要的无机富勒烯状二硫化钨颗粒以干燥的粉末形式提供。然而颗粒由于生产过程而部分地共同生长(聚集)和凝聚，并且因此形成具有数微米直径的次级颗粒。如果将如此形成的粉末直接加至水和乙醇中或含水溶胶中，则二硫化钨由于高的质量沉淀出来。因此必须将二硫化钨颗粒在溶胶-凝胶过程中制备之前解聚，并且作为单独的颗粒在溶胶中稳定化。使用分散剂已被证实是有利的。因此将WS2粉末与Sigma-Aldrich公司的鲸蜡基三甲基溴化铵一起或与Pretoctol(BASF公司)一起借助超声技术分散。
富勒烯状二硫化钨WS2在溶胶中的份额根据经涂覆的木质复合板的期望的表面规格和所使用的均压板的脱模性质来调整，并且可以为1至50％，基于固体份额计。
随后将因此制成的具有经分散的WS2颗粒的溶胶-凝胶制剂施加至所使用的经树脂浸渍的装饰纸或帖面层纸上，如前文所述。
溶胶-凝胶涂布可以在已知的和根据现有技术整理的用于热固性塑料树脂浸渍的浸渍-干燥设备中进行。在此例如将贴面纸首先用相应的液态含水氨基塑料树脂浸渍并且在经加热的干燥区域中干燥至一定的水分含量，其中同时发生预缩合。然后在第二施加区域中施加具有富勒烯状WS2微粒的制备的溶胶，并且随后穿过经加热的干燥通道。速度和通道温度根据由使用者预先设定的各种树脂参数来调整。

Claims (8)

1.用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，所述整理用于涂覆木质复合板并且形成耐磨的、容易清洁的和疏水的表面，其特征在于，在完成树脂浸渍之后在第二施加步骤中将经浸渍的纸用溶胶-凝胶制剂涂覆，所述溶胶-凝胶制剂包含由金属钼和/或钨的金属二硫化物组成的富勒烯状纳米结构以及经溶解的金属烷氧化物；和随后在干燥和最终缩合之后，将表面在液压热压机中成形。
2.根据权利要求1所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其中所述纳米结构为纳米管。
3.根据权利要求1所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，所述金属烷氧化物由金属铝、钛、硅或锆组成。
4.根据权利要求1所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，额外用于提高耐刮性的具有溶解的金属烷氧化物的所述溶胶-凝胶制剂分散有少量纳米尺度的金属氧化物。
5.根据权利要求4所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，所述金属氧化物为SiO2、Al2O3、TiO2、ZrO2。
6.根据权利要求1至5任一项所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，将富勒烯状二硫化钨颗粒和/或二硫化钼颗粒用阳离子型表面活性剂鲸蜡基三甲基溴化铵分散。
7.根据权利要求1至5任一项所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，溶胶-凝胶制剂包含3-缩水甘油氧基丙基三甲氧基硅烷的有机改性硅酸盐配方。
8.根据权利要求1至5任一项所述的用氨基塑料树脂浸渍的装饰纸和/或贴面层纸的整理，其特征在于，溶胶-凝胶制剂包含Al(OCH(CH3)C2H5)3的Yoldas溶胶配方。
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