CN1208062A - 粉状可交联织物粘合剂组合物 - Google Patents

粉状可交联织物粘合剂组合物 Download PDF

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Publication number
CN1208062A
CN1208062A CN98117115A CN98117115A CN1208062A CN 1208062 A CN1208062 A CN 1208062A CN 98117115 A CN98117115 A CN 98117115A CN 98117115 A CN98117115 A CN 98117115A CN 1208062 A CN1208062 A CN 1208062A
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polymer
weight
crosslinkable
vinyl
fibre
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CN98117115A
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CN1141350C (zh
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克劳斯·科尔哈默
里夏德·格策
赖因哈德·海尔茨舍尔
阿普杜尔马吉德·哈什姆扎德
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Wacker Chemie AG
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Wacker Chemie AG
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    • C08L101/06—Compositions of unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
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Abstract

本公开内容目的在于提供一种用于生产高聚物粘结的织物模制品或片材的粉状可交联织物粘合剂组合物,包括a)通过乳液聚合且随后干燥一种或多种选自乙烯基酯、丙烯酸酯、甲基丙烯酸酯、乙烯基芳香化合物和氯乙烯及占共聚合物总重量0.01—25重量%的一种或多种含乙烯基不饱和羧基单体的单体可获得的粉状共聚合物,其Tg或熔点高于40℃且分子量Mw为60,000—300,000,和b)至少一种含两个或多个环氧或异氰酸酯基团、其熔点为40℃—150℃的粉状化合物。

Description

粉状可交联织物粘合剂组合物
本发明涉及粉状可交联织物粘合剂组合物，并且也涉及使用该织物粘合剂组合物生产高聚物粘结的织物模制品或片材的方法。
为生产非织品而用通常的方法如气流成网、湿法成网或纺丝成网方法生产的织物片材要求粘合剂能使纤维间持久粘结且可提高抗机械应力。这些粘合剂通常是基于合成大分子化合物的，在现有技术中可以固体形式如粉末、颗粒或纤维使用，或以液体形式如水相高分子分散体或溶液使用。非织品增强的强度源自纤维间通过高聚物的粘合，高聚物粘合在纤维上，因此增强了纤维结构。
WO-A 90/14457公开了一种方法，其中粗梳玻璃纤维与热塑性粉末如聚丙烯、聚酯或聚酰胺混合，随后在升高的温度和加压下固化纤维结构。AU-B 36659/89同样描述了一种通过热塑性粉末固化玻璃纤维材料的方法。推荐使用基于聚酯或聚苯乙烯的粉末。如此粘结的纤维结构与水或溶剂接触时的低强度是不利的。
由于在高温常常超过粘合剂的玻璃化转变温度或熔融温度，所以要求粘合剂的持久化学交联以便在高温获得纤维结构的尺寸稳定性。使用自交联高聚物分散体固化由聚酯、聚酰胺或棉纤维构成的纤维材料的方法是已知的(US-A4451315)。确实获得了高强度非织品，但在干燥面使用水相粘合剂是价格过高的。此外，在纤维母体中分配粘合剂不是简单的事情。
US-A 4612224描述了基于酚醛树脂的粉状可交联共聚物的固化。该粘合剂体系的缺点是在生产和使用如此固化的纤维材料期间释放出大量甲醛。
WO-A 94/20661描述了基于乙烯基酯共聚物或(甲基)丙烯酸酯共聚物作为纤维粘合剂的自交联可再分散的分散体粉末。该粘合剂体系的缺点是定形(setting)需要在纤维基体中加入相当量的水，使其干燥昂贵。
US-A 4129545描述了基于丙烯酸酯和/或乙烯基酯及还含有单或多官能团羟基羧酸的(甲基)丙烯酸酯和N-烷氧基-烷基(甲基)丙烯酰胺作为交联组分的用作粉状涂料的热固性共聚物。EP-A 721004公开了可交联水分散粉末，它包括具有至少一个官能团的成膜高聚物和在粉末于水中分散时形成共价键的反应性组分。该粉末组合物的水相分散体用于生产耐水涂料。
本发明的目的是提供一种织物粘合剂，它能避免现有粘合剂技术中诸如强度不够、高的干燥要求、不良的流动性能和粘合剂的不均匀分配的缺点。
该目的通过用来生产高聚物粘结的织物模制品或片材的粉状可交联织物粘合剂组合物得以实现，该组合物包括：
a)通过乳液聚合且随后干燥一种或多种选自由乙烯基酯、丙烯酸酯、甲基丙烯酸酯、乙烯基芳香化合物和氯乙烯及占共聚合物总重量0.01-25重量％的一种或多种含乙烯基不饱和羧基单体组成的组的单体可获得的粉状共聚合物，共聚合物的玻璃化转变温度Tg或熔点高于40℃且分子量Mw为60,000-300,000，和
b)至少一种含两个或多个环氧或异氰酸酯基团的粉状化合物，其熔点为40℃-150℃。
适宜的共聚合物为基于一种或多种选自含1-15个碳原子的未支化或支化烷基羧酸的乙烯基酯、含1-10个碳原子的醇的甲基丙烯酸酯和丙烯酸酯、乙烯基芳香化合物如苯乙烯及氯乙烯组成的组中的单体的共聚合物。优选的乙烯基酯为乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、2-乙基己酸乙烯酯、月桂酸乙烯酯、乙酸-1-甲基乙烯酯、新戊酸乙烯酯及含5或9个碳原子的α-支化单羧酸的乙烯基酯，例如VeoVa5或VeoVa9。优选的甲基丙烯酸酯或丙烯酸酯为丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸-2-乙基己酯。
选择共聚合物组合物以产生高于40℃，优选55℃-150℃的玻璃化转变温度Tg或熔点是必要的。可以用常规方法通过差示扫描量热法(DSC)测定高聚物的玻璃化转变温度Tg和熔点。Tg也可事先用Fox方程的方法估算。根据Fox T.G.在Bull.Am.Physics Soc.1，3，123页(1956)的方程：1/Tg＝x1/Tg1+x2/Tg2+…+xn/Tgn，其中xn为单体n的质量分数(％重量/100)，Tgn为单体n的均聚物的玻璃化转变温度，开尔文度。均聚物的Tg值引自Polymer Handbook第2版，J.Wiley & Sons，New York(1975)。
为了粘合剂粉末在纤维结构中的均匀分配，粘合剂粉末必须具有低的熔融粘度。粘合剂粉末的熔融粘度由共聚合物的平均分子量Mw和分子量分布Mw/Mn决定。重均分子量Mw在60,000和300,000之间。分子量和分子量分布可以在聚合期间以常规方法调节，例如通过使用调节剂物质和通过聚合温度，并且可以通过凝胶渗透色谱法(GPC)测定。
优选的共聚合物为乙酸乙烯酯/氯乙烯、乙酸乙烯酯/VeoVa5、乙酸乙烯酯/VeoVa9、甲基丙烯酸甲酯/丙烯酸丁酯和苯乙烯/丙烯酸丁酯共聚合物，每种包括0.01-25重量％的所述含羧基的单体单元，选择其组合物以便产生上述玻璃化转变温度Tg或熔点。
适宜的含乙烯基不饱和羧基的单体为乙烯基不饱和单或二元羧酸，如丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸。含羧基的共聚单体单元优选占共聚合物总重量的0.01-10重量％。
如果需要，共聚合物还可包括占共聚合物总重量的0.01-10.0重量％的辅助单体(auxiliary monomers)，它来自乙烯基不饱和酰胺(carboxamides)的组，优选丙烯酰的胺；乙烯基不饱和磺酸及其盐的组，优选乙烯基磺酸；多乙烯基不饱和共聚单体的组，例如二乙烯基己二酸酯、二烯丙基马来酸酯、烯丙基甲基丙烯酸酯或三烯丙基氰尿酸酯；和/或N-羟甲基(甲基)丙烯酰胺亦及其醚组，如异丁氧基或正丁氧基醚。
在一个优选实施方案中，共聚合物含有0.01-2重量％的每一种丙烯酸和/或丙烯酰胺。
共聚合物是用常规方法制备的，优选通过乳液聚合方法，例如在WO-A 94/20661中所描述的，其这方面的公开内容在此引入作为参考。将由此得到的高聚物分散体干燥以产生粉末。干燥可以通过喷雾干燥、冷冻干燥方法或通过分散体聚沉并随后经流化床干燥而完成。优选喷雾干燥。优选不外加保护胶体制备和干燥共聚合物。
适宜的交联剂为含有两个或多个环氧或异氰酸酯基团且熔点为40℃-150℃的粉状化合物。适宜的环氧交联剂的例子为双酚A型的那些，即双酚A与表氯醇或甲基表氯醇的缩聚产物。适宜的环氧交联剂可商购，如商品名为Epicot或Eurepox。适宜的二异氰酸酯也是普通的商业产品，例如四甲基间二甲苯二异氰酸酯(m-tetramethylxylenediisocyanate，TMXDI)、亚甲基二苯基二异氰酸酯(MDI)。交联剂的比例一般占粉状共聚合物的0.1-25重量％，优选4-12重量％。
在一个优选实施方案中，可交联织物粘合剂组合物还包括交联催化剂。适宜的交联催化剂的例子为来自三苯基鏻的卤化物或季铵化合物的粉状催化剂。其实例为甲基-、乙基-、丙基-、丁基-三苯基鏻的溴化物及相应的碘化物和氯化物。也可以使用带取代烷基的三苯基鏻的卤化物，如2-羧乙基-、3-溴丙基-或甲酰甲基-三苯基鏻的溴化物。适宜的季铵化合物为四丁基铵、苯基三甲基铵、甲基三丁基铵盐。所述化合物可商购且优选用量占粉状共聚合物的0.1-5重量％。
可交联织物粘合剂组合物是通过以所述混合比例混合粉状组分来生产的。已知的混合粉末的设备可用于此目的。
本发明还提供了通过用粉状高分子粘合剂接触纤维材料，并在100℃-250℃、也可在加压下固化从纤维材料生产高聚物粘结的织物模制品或片材的方法，包括使用可交联的粉末混合物，它包括：
a)通过乳液聚合且随后干燥一种或多种选自由乙烯基酯、丙烯酸酯、甲基丙烯酸酯、乙烯基芳香化合物和氯乙烯及占共聚合物总重量0.01-25重量％的一种或多种含乙烯基不饱和羧基单体组成的组的单体可获得的粉状共聚合物，该共聚合物的玻璃化转变温度Tg或熔点高于40℃且分子量Mw为60,000-300,000，和
b)至少一种含两个或多个环氧或异氰酸酯基团、其熔点为40℃-150℃的粉状化合物。
所用纤维材料为天然或合成原料。其实例为基于成纤聚合物所制造的，例如粘胶纤维、聚酯纤维、聚酰胺纤维、聚丙烯纤维、聚乙烯纤维。也可使用玻璃纤维、陶瓷纤维，矿物纤维。天然纤维材料的实例为木纤维、纤维素纤维、羊毛纤维、棉纤维、黄麻纤维、亚麻纤维、大麻纤维、椰壳纤维、苎麻纤维和剑麻纤维。纤维也可以以编织织物、细纱或非织品形式如网或针织品使用。或者这些非织品可用机械预先固化，如针刺。
对于纤维粘合，一般粉末混合物用量占纤维重量的5-30重量％。
通过混合纤维材料和粉末混合物并在固化之前用常规的非织技术方法，如气流成网、湿法成网、直接纺丝或梳理设备的方法铺设纤维和粉末的混合物来生产模制品或片材。然后通过升高温度，也可在压力下粘结织物片材。
或者，在固化之前将纤维摊铺成片材形。为此的方法是已知的且基本依赖于所使用的固化纤维材料。纤维可以通过例如气流成网、湿法成网、直接纺丝或梳理设备的方法铺设。如果需要，可通过机械固化如通过交叉铺网、针刺或喷水固化先进行粘合剂固化。然后将粉末混合物喷洒到成网纤维材料中。为此，可将粉末面喷、点喷或以部分面积提花的模式喷入，或可通过针刺将其引入纤维材料中。然后加热也可在加压下粘结纤维材料。
粉状织物粘合剂对制造层压板也是有用的，在该情况下两层纤维层互相粘结或一层纤维层粘结到另外的基底上。这可以通过用例如气流成网法铺设一层纤维层，事先混合或铺设后喷入的粘合剂粉末，并在上面再铺一层纤维层来实现。代替第二个纤维层，可将不同的基底如塑料薄膜铺在顶层。其后进行加热下也可加压下粘结。该过程可获得例如用纤维网永久包覆的作为表面材料的再生棉绝缘材料。另一个用途是在建筑绝缘材料部分将玻璃纤维粘结到装饰罩膜或盖板上或者通过将织物或非织物粘结到皮革上生产鞋头。
粉状织物粘合剂对生产例如用作从纤维材料制备模制品的半成品或用作衬垫、缓冲、绝缘和滤器衬料的膨松非织品或衬料是特别有用的。为此目的，将粘合剂粉末喷入纤维材料并优选在模具中通过加热固化该材料。
在一个可能的实施方案中，将粉末混合物混合或喷入后用水或过热蒸汽处理纤维结构。
本发明的粉状可交联织物粘合剂组合物与水相粘合剂的不同之处在于避免了高能干燥和废水处理。与现有技术的粉状粘合剂相比，其优点是获得了纤维间粘结的耐水性和耐溶剂性而不释放出有害物质，此为酚醛树脂或只含N-羟甲基丙烯酰胺作为交联剂的粉末的情形。
下文的实施例解释了本发明。
实施例1：
生产含羧基的聚合物粉末
在容量为3升的反应器中加入838.8g去离子水和6.7g十二烷基硫酸钠，氮气下搅拌将此内含物加热到80℃。在80℃向反应器中加入引发剂溶液(6.7g过硫酸氢钾和218.4g水)并在4小时内从另外的容器向反应器中计量加入下列组合物：
计量加入的单体1：
甲基丙烯酸                       67.3g
丙烯酸丁酯                       403.7g
苯乙烯                           861.3g
十二烷硫醇                       6.7g
计量加入的单体2：
水                               67.3g
丙烯酰胺(30％)                   44.9g
计量加入的引发剂：
水                          217.6g
过硫酸氢钾                  6.7g
计量加入完成后，继续在80℃聚合约2小时。冷却后用氨调节pH至8，喷雾干燥分散体。此产品的玻璃化转变温度为59℃。
实施例2：
生产含羧基的聚合物粉末
在容量为3升的反应器中加入855g去离子水和6.7g十二烷基硫酸钠，氮气下搅拌将此内含物加热到80℃。在80℃向反应器中加入引发剂溶液(6.7g过硫酸氢钾和217.4g水)，并在4小时内从另外的容器向反应器中计量加入下列组合物：
计量加入的单体1：
甲基丙烯酸                    67.2g
丙烯酸丁酯                    403.4g
苯乙烯                        860.5g
十二烷硫醇                    6.7g
计量加入的单体2：
水                            67.3g
N-羟甲基丙烯酰胺(48％)        28.0g
计量加入的引发剂：
水                            217.4g
过硫酸氢钾                    6.6g
计量加入完成后，继续在80℃聚合约2小时。冷却后用氨调节pH至8，喷雾干燥分散体。此产品的玻璃化转变温度为59℃。
实施例3：
制备粉末混合物
在粉末混合机中将98g实施例1的含羧基聚合物粉末与2g粉状多官能团环氧化合物及0.5g三苯乙基鏻的溴化物TEP混合。
实施例4：
制备粉末混合物
在粉末混合机中将98g实施例2的含羧基聚合物粉末与2g粉状多官能团环氧化合物及0.5g三苯乙基鏻的溴化物TEP混合。
实施例5：
根据由WO-A 94/20661代表的现有技术制备基于可再分散自交联分散体粉末的粘合剂粉末。通过聚乙烯醇稳定该聚合物粉末并让其含有N-羟甲基基团作为可交联基团。分子量(GPC)约为700,000g/mol。
制备纤维模制品(用水)：
为了生产压塑样板，将115g再生棉与13.2g实施例1-5之一的粘合剂粉末混合并分散成24×24cm的面积。另外用喷入的约40g水将纤维/粉末混合物润湿，其后立即在约180℃压塑5分钟以生成2mm厚的硬质样板或10mm厚的软质样板，每种基重约为2200g/m2，密度分别约为1115kg/m3或223kg/m3。
制备纤维模制品(干法)：
为了生产压塑样板，将115g再生棉与13.2g实施例之一的粘合剂粉末混合并分散成24×24cm的面积。其后立即将纤维/粉末混合物在约180℃压塑5分钟以生成2mm厚的硬质样板或10mm厚的软质样板，每种基重约为2200g/m2，密度分别约为1115kg/m3或223kg/m3。
应用试验：
极限拉伸强度UTS：
于室温在与DIN 53857相似的Zwick拉伸试验机上测试之前将纤维压塑模制品冲压形成10×100mm的试验样条。
水回潮率：
为了测定水回潮率，将干燥的纤维模制品(尺寸：50×20mm)浸泡在水中1h或24h，重量分析法测定由于水膨胀引起的重量增加。
耐热性：
为了测定耐热性，切成长为240×20mm的样条。将这些样条水平固定在平面基底上使样条悬挂在基底边缘100mm处。在硬质模制品(2mm厚样板)的情形下附加40g的重物，而对软质模制品(样板厚度：10mm)只承受其本身重量的重力。通过测量在T＝120℃一小时后的挠度d来测定耐热性。
将应用试验结果总结于表1和表2中。
本发明的织物粘合剂粉末(实施例3和4)与未交联体系(实施例1和2)相比显示了明显更高的UTS和改进了的耐热性(＝加热下挠度减小)。
此外，两个表显示出发明实施例3和4与现有技术(实施例5)相比室温下的极限拉伸强度提高了。实际上，2mm厚硬质高压纤维模制品的耐热性在实验误差范围内相等是必须考虑的。在“类衬料”的软质纤维模制品的情形下，本发明的粘合剂粉末(实施例3和4)的耐热性比现有技术(实施例5)的得到了显著改善。
当在压塑期间不外加水而制备纤维模制品时，在所有情况下观察到水膨胀比现有技术有显著改进(＝减少)。
表1：
硬质模制品试验(基重：2200kg/m2，密度：115kg/m3)
实施例          湿压模塑         干压模塑
  UTS[N] 耐热性[mm] 水回潮率1h/24h[重量％]   UTS[N] 耐热性[mm] 水回潮率1h/24h[重量％]
实施例1   390   70   72/83   282   70  214/238
实施例2   440   66   67/83   310   66  198/225
实施例3   948   21   48/57   560   22  139/161
实施例4   926   19   51/60   526   20  159/180
实施例5   326   20   68/79   165   41  253/284
表2：
软质模制品试验(基重：2200kg/m2，密度：223kg/m3)
实施例           湿压模塑            干压模塑
  UTS[N]   耐热性[mm] 水回潮率1h/24h[重量％]   UTS[N]   耐热性[mm] 水回潮率1h/24h[重量％]
实施例1   15.2     16  602/621   15.4     15  728/739
实施例2   16.3     14  509/550   16.2     14  730/741
实施例3   18.8     8  441/447   18.3     11  758/774
实施例4   17.9     7  423/439   18.8     8  721/752
实施例5   11.9     14  589/662   7.9     39  987/994

Claims (10)

1.一种用于生产高聚物粘结的织物模制品或片材的粉状可交联织物粘合剂组合物，包括
a)通过乳液聚合且随后干燥一种或多种选自由乙烯基酯、丙烯酸酯、甲基丙烯酸酯、乙烯基芳香化合物和氯乙烯及占共聚合物总重量0.01-25重量％的一种或多种含乙烯基不饱和羧基单体组成的组的单体可获得的粉状共聚合物，该共聚合物的玻璃化转变温度Tg或熔点高于40℃且分子量Mw为60,000-300,000，和
b)至少一种含两个或多个环氧或异氰酸酯基团、其熔点为40℃-150℃的粉状化合物。
2.如权利要求1的粉状可交联织物粘合剂组合物，进一步包括占粉状共聚合物0.1-5重量％的粉状可交联催化剂。
3.如权利要求1或2的粉状可交联织物粘合剂组合物，其中，所用共聚合物为选自由乙酸乙烯酯/氯乙烯共聚合物、乙酸乙烯酯/VeoVa5共聚合物、乙酸乙烯酯/VeoVa9共聚合物、甲基丙烯酸甲酯/丙烯酸丁酯共聚合物和苯乙烯/丙烯酸丁酯共聚合物组成的组的共聚合物，每种包含0.01-25重量％的所述含羧基单体的单元。
4.如权利要求1-3中任一项的粉状可交联织物粘合剂组合物，其中，含羧基的单体单元选自由丙烯酸、甲基丙烯酸、马来酸、富马酸和衣康酸组成的组。
5.如权利要求1-4中任一项的粉状可交联织物粘合剂组合物，其中，共聚合物进一步包含占共聚合物总重量0.01-10.0重量％的一种或多种来自由乙烯基不饱和酰胺的组、乙烯基不饱和磺酸及其盐的组、多乙烯基不饱和共聚单体的组、和N-羟甲基(甲基)丙烯酰胺亦及其醚的组，如异丁氧基或正丁氧基醚的单体。
6.如权利要求1-5中任一项的粉状可交联织物粘合剂组合物，包括每种量为0.01-2重量％的丙烯酸和/或丙烯酰胺。
7.一种通过用粉状高分子粘合剂接触纤维材料并在100℃-250℃也可在加压下固化而从纤维材料生产高聚物粘结的织物模制品或片材的方法，包括使用如权利要求1-6的任一项所要求的可交联粉末混合物作为粘合剂。
8.如权利要求7的方法，其中，所用纤维材料包括一种或多种选自由以编织织物形式、以细纱形式或以非织品如网或针织品形式的粘胶纤维、聚酯纤维、聚酰胺纤维、聚丙烯纤维、聚乙烯纤维、玻璃纤维、陶瓷纤维，矿物纤维、木纤维、纤维素纤维、羊毛纤维、棉纤维、黄麻纤维、亚麻纤维、大麻纤维、椰壳纤维、苎麻纤维和剑麻纤维组成的组。
9.如权利要求7或8的方法，其中，可交联粉末混合物的用量占纤维重量的5-30重量％。
10.如权利要求7-9中任一项的方法，其中，在将粉末混合物混合或喷入后，用水或过热蒸汽处理含有纤维的结构。
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