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CN107250469A - 阻燃地板装饰材料及其制备方法 - Google Patents

阻燃地板装饰材料及其制备方法 Download PDF

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Publication number
CN107250469A
CN107250469A CN201580075993.1A CN201580075993A CN107250469A CN 107250469 A CN107250469 A CN 107250469A CN 201580075993 A CN201580075993 A CN 201580075993A CN 107250469 A CN107250469 A CN 107250469A
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CN
China
Prior art keywords
layer
ornament materials
antiflaming
materials according
vinyl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201580075993.1A
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English (en)
Inventor
权炫钟
孙锡济
成在浣
朴钟大
梁光锡
金雄吉
金俊荣
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LX Hausys Ltd
Original Assignee
LG Hausys Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LG Hausys Ltd filed Critical LG Hausys Ltd
Publication of CN107250469A publication Critical patent/CN107250469A/zh
Pending legal-status Critical Current

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Abstract

本发明涉及一种阻燃地板装饰材料，其特征在于：从下至上依次包括下层、基材层、印刷层和透明层，其中，至少一个层包含聚乙烯醇缩醛树脂。并且，本发明涉及一种阻燃地板装饰材料的制备方法，所述阻燃地板装饰材料包括下层、基材层、印刷层和透明层，所述层的顺序为从上至下，所述方法包括：(1)下层制备步骤，用于使用含有100重量份聚乙烯醇缩醛树脂和100‑400重量份填料的组合物制备下层；(2)基材层制备步骤，用于制备由浸入PVC溶胶的玻璃纤维构成的基材层；(3)印刷步骤，用于通过在基材层上印刷或将印刷有印刷图案的膜或纸层压至基材层而形成印刷层；(4)透明层制备步骤，用于制备由透明PVC膜或透明PET膜构成的透明层；和(5)层压步骤，用于层压层从而使基材层和其上形成的印刷层布置在下层和透明层之间。

Description

阻燃地板装饰材料及其制备方法
技术领域
本发明涉及一种阻燃地板装饰材料及其制备方法，具体地，涉及这样一种阻燃地板装饰材料及其制备方法：通过使构成阻燃地板装饰材料的至少一个层包含聚乙烯醇缩醛树脂，从而减少在火灾时由于树脂燃烧而发生的烟密度以及有毒气体，并且所述阻燃地板装饰材料阻燃性优异。
背景技术
近来，随着生活质量的提高，不仅对健康，而且对环保产品的关注日益增加。作为一例，和居住生活密切相关的地板装饰材料具有逐渐使用环保材料的趋势。同时，对使用在制备这样的地板装饰材料的材料等的限制日益严格。
虽然使用橡胶(Rubber)材料的地板装饰材料的阻燃性最为优异，但由于价格昂贵而无法应用。因此，多使用阻燃性不足但价格低廉的PVC材料的地板装饰材料。
图1为表示现有的一般PVC地板装饰材料结构的截面图，从下往上依次包括下层(100)、基材层(200)、透明层(300)。
但是，现有的地板装饰材料作为下层(100)、透明层(300)等主要使用PVC材料，由于具有卤族元素，虽然火灾时火焰的传播速度慢，但产生相当多的烟雾。并且，由于包含有毒的邻苯二甲酸系增塑剂，在焚烧处理或火灾时，产生环境激素以及有毒气体(氯化氢)等，在填埋处理时，在自然环境下几乎永久残存，因此存在对环境造成很大的负担的问题。
特别是，在船舶、火车、汽车中使用PVC材料的地板装饰材料的情况下，在发生火灾时，由于发热量高、毒性气体的问题，在火灾或救火时会引起如窒息的二次灾害，因此，对制备地板装饰材料的组合物具有无毒性以及低发热性等阻燃性能要求，并在法律上进行限制以及逐渐规范化。
因此，依然非常必要对阻燃性优异的地板装饰材料等的进行开发。
作为现有PVC地板材料的实例在韩国公开专利第
10-2004-0065494号公开。
现有技术文献：
专利文献
(专利文献1)KR 10-2004-0065494A(公开日：2004年7月22)
发明内容
技术问题
本发明作为解决上述问题的方案，旨在提供这样一种阻燃地板装饰材料以其制备方法，通过使构成阻燃地板装饰材料的至少一个层包含聚乙烯醇缩醛树脂，而减少在火灾时由于树脂燃烧而发生的烟密度以及有毒气体，并且所述阻燃地板装饰材料阻燃性优异。
技术手段
为了解决上述问题，本发明提供一种阻燃地板装饰材料，其特征在于：从下至上依次包括下层、基材层、印刷层和透明层，至少一个层包含聚乙烯醇缩醛树脂。
*并且，本发明提供一种阻燃地板装饰材料的制备方法，其特征在于，所述阻燃地板装饰材料从下至上依次包括下层、基材层、印刷层和透明层，所述方法包括：
(1)下层制备步骤，用于使用含有100重量份聚乙烯醇缩醛树脂和100-400重量份填料的组合物制备下层；
(2)基材层制备步骤，用于制备以PVC溶胶浸渍处理过的玻璃纤维构成的基材层；
(3)印刷步骤，用于通过在基材层上印刷或将印刷有印刷图案的膜或纸层压至基材层而形成印刷层；
(4)透明层制备步骤，用于制备由透明PVC膜或透明PET膜构成的透明层；和
(5)层压步骤，用于层压层从而使基材层和其上形成的印刷层布置在下层和透明层之间。
有益效果
本发明的阻燃地板装饰材料具有减少在火灾时由于树脂燃烧而发生的烟密度以及有毒气体并且阻燃性优异的效果。
附图说明
图1表示现有的地板装饰材料的截面图。
图2表示本发明的一个实施方案的阻燃地板装饰材料的截面图。
图3为示出本发明的一个实施方案的阻燃地板装饰材料的制备过程的流程图。
附图标记说明
1：阻燃地板装饰材料
10：附加功能层 20：下层
30：基材层 40：印刷层
50：透明层 60：表面处理层
具体实施方式
下文中，将参照附图对本发明进行详细说明。
本发明涉及一种阻燃地板装饰材料，其特征在于：从下至上依次包括下层(20)、基材层(30)、印刷层(40)和透明层(50)，至少一个层包含聚乙烯醇缩醛树脂(参照图2)。
本发明的阻燃地板装饰材料通过使构成地板装饰材料的至少一个层包含聚乙烯醇缩醛树脂而具有赋予地板装饰材料阻燃性的效果。
聚乙烯醇缩醛树脂通过将聚乙烯醇类树脂以醛化合物进行缩醛化反应而制备。作为聚乙烯醇缩醛树脂的原料而使用的聚乙烯醇树脂例如可通过聚合乙烯基酯类单体并使聚合物进行皂化(saponification)而获得。作为聚合乙烯基酯类单体的方法可使用溶液聚合法、本体聚合法、悬浮聚合法、乳液聚合法等现有技术公知的方法。聚合引发剂根据聚合方法适当选择偶氮引发剂、过氧化物引发剂、氧化还原引发剂。皂化反应可使用现有技术公知的碱催化剂或酸催化剂催化的醇解、水解等，其中最优选最简便的是，将甲醇作为溶剂并使用烧碱催化剂的皂化反应。本发明中使用的聚乙烯醇树脂的皂化值并无特别限制，优选为95mol％以上，最优选为98mol％。
作为聚乙烯醇类树脂可举例的有甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、新戊酸乙烯酯、叔碳酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、乙烯基月桂酸乙烯酯、棕榈酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯以及苯甲酸乙烯酯等，特别地，优选乙酸乙烯酯。
并且，在聚合所述乙烯基酯类单体的情况下，在不破坏本发明树脂的范围内，能够与不同单体进行共聚。作为不同单体，可列举的实例有：α-烯烃，如乙烯、丙烯、正丁烯、异丁烯等；丙烯酸或其酯，如丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯、丙烯酸异丙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸叔丁酯、丙烯酸2-乙基己酯、丙烯酸十二烷基酯、丙烯酸十八烷基酯等；甲基丙烯酸及其酯，如甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸十二烷基酯、甲基丙烯酸十八烷基酯等；丙烯酰胺，N-甲基丙烯酰胺、N-乙基丙烯酰胺、N,N-二甲基丙烯酰胺、双丙酮丙烯酰胺；丙烯酰胺丙磺酸及其酯；甲基丙烯酰胺，如二甲基胺基丙基丙烯酰胺或其酯或其4级盐；丙烯酰胺衍生物，如N-羟甲基丙烯酰胺及其衍生物；甲基丙烯酰胺，如N-甲基甲基丙烯酰胺、N-乙基甲基丙烯酰胺；甲基丙烯酰胺丙磺酸及其盐；甲基丙烯酰胺衍生物，如二甲氨基丙基甲基丙烯酰胺或其盐或其4级盐、N-羟甲基甲基丙烯酰胺及其衍生物等；乙烯基醚，如甲基乙烯基醚、乙基乙烯基醚、正丙基乙烯基醚、异丙基乙烯基醚、正丁基乙烯基醚、异丁基乙烯基醚、叔丁基乙烯基醚、十二烷基乙烯基醚、十八烷基乙烯基醚；腈类，如丙烯腈、甲基丙烯腈等；卤代乙烯，如氯乙烯、氟乙烯等；亚乙烯基卤化物，如偏二氯乙烯、偏二氟乙烯等；烯丙基化合物，如乙酸烯丙酯、烯丙基氯等；马来酸及其盐或其酯或其酐；乙烯基硅烷，如三甲氧基硅烷等；乙酸异丙烯酯等。这些单体单元相对于通常的乙烯基酯类单体以不足20mol％，更优选不足10mol％的比率使用。
在聚合乙烯基酯类单体时，可在存在有巯基乙酸、巯基丙酸等巯基化合物或除此之外的链转移剂的情况下进行。
对用于制备聚乙烯醇缩醛树脂的溶剂没有特别的限制，在工业上大量制造时，优选使用水，并在进行反应之前，优选将聚乙烯醇类树脂在高温下，例如在90℃以上的温度下充分地进行溶解。并且，水溶液的浓度优选5～40质量％，更优选5～20质量％，特别优选8～15质量％。浓度过低生产率低，浓度过高会使反应中的搅拌变得困难，并且，会产生由于聚乙烯醇树脂的分子间氢键引起的凝胶化，而使反应变得不均匀，因此不优选。
可通过在聚乙烯醇类树脂水溶液中添加醛化合物并在酸性条件下进行反应，而获得聚乙烯醇缩醛树脂。在本文中，醛类化合物可使用例如甲醛、乙醛、丙醛、丁醛、己醛、苯甲醛等。优选碳原子数1～12的醛化合物，更优选碳原子数1～6的饱和烷基醛化合物，特别优选碳原子数1～4的饱和烷基醛化合物，其中，在地板装饰材料的阻燃性等的物性观点上，优选丁醛。并且，可使用单一醛类化合物，也可并用两种以上。并且，可在全部醛类化合物的20质量％以下的范围内少量使用多官能醛类化合物或其他具有官能基的醛类化合物等。作为在聚乙烯醇类树脂水溶液中反应醛类化合物的催化剂，不特别受限制，能够使用任意有机酸及无机酸，例如乙酸、对甲苯磺酸、硝酸、硫酸、盐酸、碳酸等。其中优选无机酸，特别地，考虑到可获得充分的反应速度以及反应后容易清洗，优选盐酸、硫酸、硝酸。在反应中使用的酸的浓度根据使用的酸的种类而不同，但在盐酸、硫酸、硝酸的情况下，优选0.01～5mol/l，更优选0.0～2mol/l。如果酸的浓度过低，会使反应速度变慢，达到目标缩醛化度、获得目标物性的聚乙烯醇缩醛树脂需要的时间不那么长。如果酸的浓度过高，将很难控制反应，与此同时容易生成醛的三聚体。
作为在聚乙烯醇类树脂水溶液中反应的醛类化合物的顺序，可使用公知的方法，例如在聚乙烯醇类树脂水溶液中添加催化剂之后添加醛类化合物的方法、事先添加醛类化合物之后添加酸催化剂的方法。并且，可使用将添加的醛化合物或酸催化剂一次性添加或依次添加、分批添加的方法或在包含酸催化剂或醛化合物的溶液中添加聚乙烯醇类树脂水溶液和醛化合物或酸催化剂混合溶液的方法。
反应温度不特别受限制，优选0～80℃，但为了获得本发明的阻燃地板装饰材料中使用的层，优选反应后容易洗净的多孔状的聚乙烯醇缩醛树脂，并在反应过程中，在析出聚乙烯醇缩醛颗粒之前在0～40℃、优选在5～20℃的较低温度下进行反应。之后，为了加快反应，优选升高反应温度，例如50～80℃，特别是考虑到生产率优选65～75℃。
通过这样的反应而获得的聚乙烯醇缩醛树脂的颗粒为了有效地去除残存的酸或醛化合物，优选多孔状。为了获得多孔状聚乙烯醇缩醛树脂，有必要调整反应液的粘度、搅拌速度、搅拌叶的形状、反应容器的形状、反应温度、反应速度、催化剂及醛类的添加方法。例如，如果反应温度过高，由于聚乙烯醇缩醛类树脂熔融，因此很难形成多孔状。
*在反应之后去除残存醛化合物及残存酸催化剂的方法可使用公知的方法。聚乙烯醇缩醛树脂在水的存在下由酸分解而产生醛类化合物，因此优选进行使碱性滴度值成为正值的调整。在本文中，碱性滴度定义为将100g的聚乙烯醇缩醛树脂滴定为碱性所需要的0.01mol/l盐酸的量(ml)。即，通过反应而获得的聚乙烯醇缩醛树脂由碱性化合物中和，但为了获得本发明的阻燃地板装饰材料，优选在碱性中和之前，尽可能去除树脂中残存的醛类化合物，并且以下方法比较有用：以醛化合物的反应率增加的条件快速反应的方法、或以水或水/醇混合溶剂等充分洗净的方法、化学性地处理醛化合物的方法。作为在碱性中和中使用的碱性化合物，例如有氢氧化钠、氢氧化钾等的碱金属氢氧化物或氨、三乙胺、吡啶等的胺类化合物，但在着色的观点上优选无机金属的氢氧化物，特别优选很难影响与玻璃的粘合性的碱金属氢氧化物。并且，碱性洗净后的聚乙烯醇缩醛树脂的碱性滴度值优选为0.1～30，更优选1～20。如果碱性滴度值过低会使耐水解性变差，相反，如果碱性滴度值过高，在制备地板装饰材料用层时，容易引起着色。
本发明中使用的聚乙烯醇缩醛树脂的平均聚合度优选为800～4000，更优选为1000～3000。并且，聚乙烯醇缩醛树脂的根据JIS K6728:1977的规定检测的平均缩醛化度(乙烯基缩醛单元的含量)优选为50～90mol％，更优选55～88mol％，特别优选60～85mol％。
本发明中使用的聚乙烯醇缩醛树脂的根据JIS K6728:1977的规定检测的乙烯醇单元的量优选为10～50mol％，更优选为12～45mol％，最优选15～40mol％。当乙烯醇单元的量超过50mol％时，会使吸湿性变高，并且吸收的水有可能成为引起腐蚀或绝缘性变低、使用聚乙烯醇缩醛树脂的层从其他层剥离的原因。另外，当乙烯醇单元的量不足10mol％时，在热压的情况下，有可能产生力学强度变低、粘接性不良等问题。
本发明中使用的聚乙烯醇缩醛树脂的根据JIS K6728:1977的规定检测的乙烯基酯单元的量优选为4mol％以下，更优选为2mol％以下，最优选为1mol％以下。当乙酸乙烯酯单元的量超过4mol％时，由于热分解以及由于水分的水解会产生腐蚀性物质的乙酸。并且，根据由于乙酸的脱离而产生的烯烃，使聚乙烯醇缩醛树脂容易着色。并且，缩醛度、乙烯醇单元的量及乙烯基酯单元的量的值为相对于缩醛度(乙烯基缩醛单元的量)、乙烯醇单元的量及乙烯基酯单元的量的总量的值。
在制备本发明的阻燃地板装饰材料中使用的聚乙烯醇缩醛类树脂中，在所获得的地板装饰材料不损伤本发明的效果的范围内，根据所需可添加填料、增塑剂、抗氧化剂、紫外线吸收剂、粘合性控制剂、防粘连剂、颜料、染料、功能性无机化合物等添加剂。
另外，在本发明的地板装饰材料中，优选使厚度及重量相对于其他层的厚度和重量更重更厚的下层(20)包含聚乙烯醇缩醛树脂，除此之外的基材层(30)、印刷层(40)、透明层(50)等可选择性地使用其他和合成树脂来制备(参照图2)。
作为具体实例，使下层(20)包含聚乙烯醇缩醛树脂，并使基材层(30)、透明层(50)等使用如PVC树脂的其他合成树脂。
为了提高强度、阻燃性及耐久性并减少费用，下层(20)可包含填料。所述填料可包含选自碳酸钙、滑石、粉煤灰、高炉矿渣及以这些组合组成的组中的一个以上。所述填料可为光学各向同性，在该情况下，可通过考虑经济效果及物性提高的效果而选择使用适当大小的颗粒。具体地，填料可包括碳酸钙，由于在价格以及多功能性上有利，并能够提高阻燃性及耐久性，因此优选。下层相对于100重量份的聚乙烯醇缩醛树脂可包含100-400重量份的填料，优选包含130-350重量份。当填料少于100重量份时，地板装饰材料的价格会上升并降低阻燃性等物性，当使用超过400重量份时，会降低地板装饰材料的加工性，因此优选上述范围内的量。下层(20)的厚度可为1-2mm。
基材层(30)起到补强地板装饰材料尺寸稳定性的作用。这样的基材层(30)优选以PVC溶胶浸渍处理过的玻璃纤维(优选玻璃纤维无纺布)构成。此情况下，以PVC溶胶浸渍处理可理解为为了固定玻璃纤维且同时利于与下层(20)胶合。在这里，PVC溶胶可优选包含：100重量份的聚合度为1000至1700的聚氯乙烯；50至100重量份的作为增塑剂的对苯二甲酸二辛酯(dioctylterephthalate:DOTP)或邻苯二甲酸二辛酯(Dioctylphthalate，DOP)；1至3重量份的环氧大豆油；2至6重量份的钡-锌热稳定剂；10至80重量份的碳酸钙；5至50重量份的作为白色颜料的二氧化钛。基材层(30)厚度可为0.30至0.40mm。
印刷层(40)起到赋予所获得的地板装饰材料多种多样的印刷图案的作用。此情况下，印刷层(40)可在所基材层(30)上通过转印印刷、凹版印刷或丝网印刷而形成，优选转印印刷。或者，选择性地将形成有印刷图案的膜或纸等和基材层进行层压而形成。这样的印刷层(40)通过印刷而赋予图案，起到赋予具有美感的外观和设计效果的作用。
透明层(50)可为以选自聚氯乙烯(poly vinyl chloride,PVC)、聚对苯二甲酸乙二醇酯(polyethylene terephthalate,PET)、聚对苯二酸丁二醇酯(polybutyleneterephthalate,PBT)、聚丙烯(polypropylene,PP)、聚乙烯(polyethylene,PE)、聚甲基丙烯酸甲酯(poly methyl methacrylate,PMMA)、丙烯腈-丁二烯-苯乙烯(acrylonitrile-butadiene-styrene,ABS)、聚碳酸酯(polycarbonate,PC)、苯乙烯-丙烯腈共聚物(styrene-acrylonitrile copolymer,SAN)中的一种树脂制备的膜。优选使用透明性优异的透明聚氯乙烯或透明聚对苯二甲酸乙二醇酯。透明层的厚度可为0.1至0.7mm。
另外，本发明的阻燃地板装饰材料可进一步选择性地在最上部层形成表面处理层(60)。
也就是说，表面处理层(60)可形成在透明层的上部，并在地板装饰材料表面上起到初期防污染的作用，即起到防止污染物的附着并提高抗划伤性及耐磨性的作用。表面处理层通常可通过涂布热固性或光固性化合物溶解在溶剂中的涂布液而形成。但是，在热固性化合物的情况下，为了形成表面处理层而进行加热时，由于热量有可能改变位于其下部的其他层、特别是弹性层的物性，因此优选使用光固性化合物。此时，作为固化化合物可使用具有1个以上能够进行交联反应的不饱和键的官能团的单体或低聚物，其可使用聚氨酯丙烯酸酯、环氧丙烯酸酯、聚醚丙烯酸酯、聚酯丙烯酸酯、二季戊四醇五丙烯酸酯、二季戊四醇四丙烯酸酯、二季戊四醇六丙烯酸酯、二季戊四醇五丙烯酸酯等，但这些仅为例示，本发明不限于此。本发明中可以将其单独或两中以上进行混合作为光固化性化合物来使用。在包含光固化化合物的涂布液中通常除了光固化性化合物和溶剂以外也包含光引发剂，根据所需可包含光稳定剂、流平剂等不改变硬涂布层的物性的的多种添加剂。表面处理层根据铅笔硬度测量的表面硬度可为7H以上，并显示出优异的塑料膜表面的表面硬度，更优选调节到7H至8H范围内。构成表面处理层(60)的光固化性化合物优选为通常的光固化型聚氨酯丙烯酸酯。表面处理层(60)的厚度可为5至40μm。
另外，本发明的阻燃地板装饰材料可进一步选择性地在最下层形成附加功能层(10)。
附加功能层(10)可为通常的机织织物、编织织物或无纺布，机织织物、编织织物或无纺布可为将天然纤维或合成纤维或将其混纺的混纤丝织造的织布或编织织物，或通过针刺等公知的加工方法制造的无纺布；附加功能层(10)起到如下作用：将地板装饰材料的外观、特别是将地板装饰材料的背面(底面)的外观变得美观而使产品变得高档，且提高市场价值的同时提高地板装饰材料和地板的贴附力而使地板装饰材料的设置变得容易。附加功能层(10)的厚度可为0.1至1.0mm。
并且，本发明提供一种阻燃地板装饰材料的制备方法，其特征在于：
所述阻燃地板装饰材料从下至上依次包括下层、基材层、印刷层和透明层，所述方法包括：
(1)下层制备步骤，用于使用含有100重量份聚乙烯醇缩醛树脂和100-400重量份填料的组合物制备下层；
(2)基材层制备步骤，用于制备以PVC溶胶浸渍处理过的玻璃纤维构成的基材层；
(3)印刷步骤，用于通过在基材层上印刷或将印刷有印刷图案的膜或纸层压至基材层而形成印刷层；
(4)透明层制备步骤，用于制备由透明PVC膜或透明PET膜构成的透明层；和
(5)层压步骤，用于层压层从而使基材层和其上形成的印刷层布置在下层和透明层之间。
在下层制备步骤中，将聚乙烯醇缩醛树脂通过将聚乙烯醇类树脂以醛化合物进行缩醛化反应而制备作为特征。对于在本发明中使用的聚乙烯醇缩醛树脂在上文中进行了详细说明，因此省略重复的说明。
基材层制备步骤为将以PVC溶胶浸渍处理过的玻璃纤维进行凝胶的步骤。所述玻璃纤维优选以玻璃纤维无纺布构成。
印刷步骤为在基材层上通过凹版印刷、丝网印刷或转印印刷赋予图案而形成印刷层或将印刷有印刷图案的膜或纸进行层压的步骤。
透明层制备步骤为制备由透明合成树脂组合物制备的透明膜、优选制备透明PVC膜或透明PET膜的步骤。
层压步骤为在下层和透明层之间布置形成有印刷层的基材层的方式进行层压的层压步骤。
在层压步骤之后可进一步包括表面处理步骤：在透明层上部涂布光固化组合物，并通过紫外线照射光固化组合物进行固化而形成表面处理层。
并且，可选择性地在层压步骤之前，制备以机织织物、编织织物或无纺布构成的附加功能层，并预先和下层进行层压。
下文中，将概括说明如上所述的本发明的阻燃地板装饰材料的制备方法(参照图3)。
本发明的形成阻燃地板装饰材料的各层除了表面处理层、印刷层及基材层、附加功能层之外的下层和透明层可通过使用压延成型、铸造成型、吹塑成型或挤出成型制备。
压延成型为在相互向相反方向旋转的两个以上的辊之间压延原料而连续制备板或膜的成型方法；铸造成型为在容易剥离的耐热性优异的离型纸上多层涂布合成树脂溶胶之后进行层压的成型方法；吹塑成型为这样的成型方法：将热塑性塑料加热并熔融，之后从挤出机连续挤出成管状型坯，其挂在一个或两个以上模具上，关闭将其上下密封，之后当从顶杆向型坯吹气使其膨胀，型坯贴附在其模具内壁上而制备中空容器制品；挤出成型为在基材的表面上使用挤出机将热可塑性塑料进行加热熔融而成为流动状态之后在T型模头上以膜状挤出的同时连续压缩的成型方法。
优选压延成型，相对于其他制备方法，由于能够自由控制添加剂等成分的含量，因此可提供具有优异柔韧性、耐冲击性、机械强度、加工性、稳定性及熔融效率的地板装饰材料，并加上能够减少原材料费用，因此优选使用压延成型进行制备。
将各自制备的多个层，首先从下往上将附加功能层(可选择性使用)层压到下层的下面(一次层压)。
同时，将玻璃纤维无纺布浸渍到PVC溶胶中，并准备完成凝胶化而形成基材层。
之后，在基材层上通过通常的印刷方法，例如凹版印刷、丝网印刷或转印印刷赋予图案而形成印刷层或将印刷有印刷图案的膜或纸层压而形成印刷层。
之后，在形成印刷层的基材层上层压透明层(二次层压)。
像这样各自独立地层压构成地板装饰材料的上层和下层之后，将下层上面对接到基材层的底面后层压成一体(三次层压)。
一次、二次、三次层压方法可通过粘合剂涂布以及/或热压方法来进行。
多个层层压为一体之后，将其冷却的同时，选择性地在透明层上面以涂布机涂布涂布液(优选光固化化合物溶解在溶剂中的涂布液)，并照射紫外线进行固化，而形成表面处理层而获得作为最终产品的阻燃地板装饰材料。
下文中，为了方便理解本发明而提供优选实施例，但下述实施例仅为本发明的示例，在本发明的范围及技术构思范围内可进行多种改变及修改，这对于本领域技术人员来明显的，并且这样的改变及修改落在权利要求范围内。
[实施例]
实施例1
以包含PVC树脂的组合物通过压延成型制备0.2mm厚度的透明层。
并且，将包含100重量份作为聚乙烯醇缩醛树脂的聚乙烯醇缩丁醛和包含150重量份的作为填料的碳酸钙的组合物通过压延成型，从而制备制备1.5mm厚度的下层。
通过添加100重量份聚合度1000的聚氯乙烯、60重量份对苯二甲酸二辛酯、100重量份碳酸钙、2重量份钡-锌热稳定剂形成的PVC溶胶浸渍玻璃纤维板(30g/m2)，干燥制备基材层，并在其上部通过凹版印刷方法赋予印刷图案而形成印刷层。
之后，在将形成有印刷层的基材层和透明层进行热压之后，将基材层的底面和下层的上面以对接的方式进行热压。之后，将有光泽的聚氨酯丙烯酸酯类紫外线固化型树脂通过滚涂方法全面涂布后，照射紫外线而制备形成有表面处理层的阻燃地板装饰材料。
实施例2
在实施例1中如下改变下层的组成并进行制备。
将包含100重量份作为聚乙烯醇缩醛树脂的聚乙烯醇缩丁醛和300重量份作为填料的碳酸钙的组合物通过压延成型制备1.5mm厚度的下层。除此之外，其他层的组分及加工方法和实施例1相同。
比较例1
在所述实施例1中如下改变下层的组成并进行制备。
将在100重量份的PVC中添加100重量份的碳酸钙、40重量份的对苯二甲酸二辛酯、2重量份的钡-锌热稳定剂的组合物通过压延成型制备1.5mm的下层。除此之外，其他层的组分及加工方法和实施例1相同。
比较例2
在所述实施例1中如下改变下层的组成并进行制备。
将在100重量份的PVC中添加300重量份的碳酸钙、55重量份的对苯二甲酸二辛酯、2重量份的钡-锌热稳定剂的组合物通过压延成型制备1.5mm的下层。除此之外，其他层的组分及加工方法和实施例1相同。
实验例1
测量实施例1、2及比较例1、2的地板装饰材料的烟密度、有毒气体及火焰传播性，并将其结果示于下记表1中。
烟密度及有毒气体的测量方法根据ISO 5659-2燃烧室测试方法进行。
表1
如表1中所示，本发明的地板装饰材料(实施例1、2)相对于比较例，烟密度显示出最高约1/3程度的减少、有毒气体中氯化氢也显示出最高约1/3程度的减少、一氧化碳显示出最高约1/5程度的减少。并且，维持了和现有PVC地板装饰材料相同水准的火焰传播性。
因此，证实本发明的阻燃地板装饰材料具有减少在火灾时由于树脂燃烧而发生的烟密度以及有毒气体的安全并且阻燃性优异的效果。

Claims (23)

1.一种阻燃地板装饰材料，其特征在于：
从下至上依次包括下层、基材层、印刷层和透明层，
至少一个层包含聚乙烯醇缩醛树脂。
2.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
聚乙烯醇缩醛树脂通过将聚乙烯醇类树脂以醛化合物进行缩醛化反应而制备。
3.根据权利要求2所述的阻燃地板装饰材料，其特征在于：
聚乙烯醇类树脂通过将乙烯基酯类单体聚合后进行皂化而制备，所述乙烯基酯类单体选自甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、异丁酸乙烯酯、新戊酸乙烯酯、叔碳酸乙烯酯、己酸乙烯酯、辛酸乙烯酯、乙烯基月桂酸乙烯酯、棕榈酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯以及苯甲酸乙烯酯的乙烯基酯类单体中的一种或一种以上。
4.根据权利要求3所述的阻燃地板装饰材料，其特征在于：
乙烯基酯类单体为乙醋酸乙烯酯。
5.根据权利要求所述2的阻燃地板装饰材料，其特征在于：
醛化合物为选自甲醛、乙醛、丙醛、丁醛、己醛、苯甲醛中的一种或一种以上的醛化合物。
6.根据权利要求5所述的阻燃地板装饰材料，其特征在于：
醛化合物为丁醛。
7.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
聚乙烯醇缩醛树脂的平均聚合度为800～4000。
8.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
聚乙烯醇缩醛树脂的乙烯醇单元的量为10～50mol％。
9.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
聚乙烯醇缩醛树脂的乙烯基酯单元的量为4mol％以下。
10.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
在聚乙烯醇缩醛树脂中添加添加剂，所述添加剂选自填料、增塑剂、抗氧化剂、紫外线吸收剂、粘合性控制剂、防粘连剂、颜料、染料、包含功能性无机化合物的添加剂中的一种或一种以上。
11.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
下层在100重量份的聚乙烯醇缩醛树脂中包含100～400重量份的填料。
12.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
下层的厚度为1-2mm。
13.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
基材层为以PVC溶胶浸渍处理过的玻璃纤维。
14.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
印刷层为以转印印刷、凹版印刷以及丝网印刷形成的墨层或印刷有印刷图案的膜或纸。
15.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
透明层为透明PVC膜或透明PET膜。
16.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
阻燃地板装饰材料进一步包含形成在透明层上的表面处理层。
17.根据权利要求16所述的阻燃地板装饰材料，其特征在于：
表面处理层通过涂布热固化或光固化化合物溶解在溶剂中的涂布液而形成。
18.根据权利要求1所述的阻燃地板装饰材料，其特征在于：
阻燃地板装饰材料进一步包含形成在下层下部的附加功能层。
19.根据权利要求18所述的阻燃地板装饰材料，其特征在于：
附加功能层以机织织物、编织织物或无纺布形成。
20.一种阻燃地板装饰材料的制备方法，其特征在于：
所述阻燃地板装饰材料从下至上依次包括下层、基材层、印刷层和透明层，所述方法包括：
(1)下层制备步骤，用于使用含有100重量份聚乙烯醇缩醛树脂和100-400重量份填料的组合物制备下层；
(2)基材层制备步骤，用于制备以PVC溶胶浸渍处理过的玻璃纤维构成的基材层；
(3)印刷步骤，用于通过在基材层上印刷或将印刷有印刷图案的膜或纸层压至基材层而形成印刷层；
(4)透明层制备步骤，用于制备由透明PVC膜或透明PET膜构成的透明层；和
(5)层压步骤，用于层压层从而使基材层和其上形成的印刷层布置在下层和透明层之间。
21.根据权利要求20所述的阻燃地板装饰材料的制备方法，其特征在于：
聚乙烯醇缩醛树脂通过将聚乙烯醇类树脂以醛化合物进行缩醛化反应而制备。
22.根据权利要求20所述的阻燃地板装饰材料的制备方法，其特征在于：
所述方法进一步包括：表面处理步骤，在层压步骤之后，在透明层上部涂布光固化组合物，并通过紫外线照射将光固化组合物固化而形成表面处理层。
23.根据权利要求20所述的阻燃地板装饰材料的制备方法，其特征在于：
在层压步骤之前，单独制备以机织织物、编织织物或无纺布构成的附加功能层，并先与下层层压。
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