CN1511989A - 具有混色外观的高耐用性无纺布的制备程序以及适于该目的的装置 - Google Patents

具有混色外观的高耐用性无纺布的制备程序以及适于该目的的装置 Download PDF

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CN1511989A
CN1511989A CNA2003101246867A CN200310124686A CN1511989A CN 1511989 A CN1511989 A CN 1511989A CN A2003101246867 A CNA2003101246867 A CN A2003101246867A CN 200310124686 A CN200310124686 A CN 200310124686A CN 1511989 A CN1511989 A CN 1511989A
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nonwoven fabric
felt
fiber
polyurethane
dyeing
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S
S·马里尼
¸
O·特奥弗拉斯蒂
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Alcantara SpA
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Alcantara SpA
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    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
    • C08G18/0842—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents
    • C08G18/0847—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of solvents for the polymers
    • C08G18/0852—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of solvents for the polymers the solvents being organic
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Abstract

一种含有纤维部分和基质粘合剂的具有混色视觉外观和高耐用性的无纺布，其特征在于，粘合剂基质是聚氨酯，其特征为存在有软链段和硬链段，软链段由聚碳酸酯－多元醇和聚酯－多元醇的混合物组成，硬链段由得自于异氰酸酯和多元醇的反应的氨基甲酸乙酯基团，与得自于游离异氰酸酯基团和水之间反应的酰脲基团组成，纤维部分含有混色外观的纤维，其是具有不同染色特性的两种或多种纤维的混合物。

Description

具有混色外观的高耐用性无纺布 的制备程序以及适于该目的的装置
技术领域
本发明涉及包含纤维部分和粘接相同纤维的基质的无纺布，其特征在于混色型(混色毛纱型)的视觉外观和高耐用性；制备这种无纺布的程序/方法，和适于该目的的装置。
背景技术
“混色外观”的定义是指特殊的视觉效应，其特征在于通过同时使用下列可能性的一种或更多种而获得的颜色和/或强度交替：
1.不同染色的纤维的紧密混合物
2.使用能将染料嵌入无纺布内部的合适的“针染”技术
3.采用考虑到的最适于达到所需效果的印染技术(喷墨，辊印，筛网，蚀刻等)
“高耐用性”的定义是指材料对磨蚀剂和对材料随着时间的分解的高抵抗性，其分解主要由于紫外线的吸收和氧化剂所引起。
通过使用聚氨酯基质(粘接纤维组分)获得高耐用性能，其特征不仅在于它的高耐用性，而且还在于在高于通常被用于相似目的的聚氨酯可承受的温度，其具有被加工的性能。
公知的微纤维类的无纺布显示一种结构组织，其包括高密度纤维表面和能粘接这种微纤维结构的基质。组成这些材料的微纤维是基于聚酯和/或聚酰胺，粘接基质是聚氨酯类(这里，该术语指通常被用于该目的的所有聚氨酯-聚脲聚合物)。具有类似于天然仿麂皮织物的外观和织物组织的这类产品，被描述在例如意大利专利823055，839921，858373，873669，905222，921871和美国专利US-A-3531368和US-A-3889292中，所有的都以本申请人的名义：这些专利在这里被引述以对本说明书构成完整的基础，以用作每个感兴趣的参考。
所描述的这类微纤维无纺布现在可根据能被这样概括的程序/方法来制备：
1.“海-岛”型的双组分纤维的纺织程序，其中“岛”组分包括聚酯或聚酰胺，“海”组分包括聚合物，该聚合物与岛组分不溶混并且可溶于合适的有机或无机溶剂中。
2.通过机械针刺工序编织毡(毛毡)，该工序可在第1点中得到的微纤维之间交织。
3.用粘合剂浸渍毡，该粘合剂在“海”的消除阶段中固定“岛”。这种粘合剂一般为聚乙烯醇(PVA)的水溶液。
4.将“海”组分溶于合适的有机(一般为三氯乙烯)或无机(酸性或碱性的水溶液)溶剂或仅溶于热水。
5.在有机溶剂(二甲基甲酰胺(DMF))中，将微纤维组分浸渍于聚氨酯(PU)的溶液，乳液或水分散相。
6.除去在第3点中使用的粘合剂(如果粘合剂不是聚氨酯(PU))。
7.平行于表面横向剪裁厚度，将双组分(“岛”组分+聚氨酯(PU))片材分成两个相等的部分。
8.用砂纸作适当处理将产品表面磨光，以使其在结构上具有特有的仿麂皮外观。
9.产品的最终染色。
上面提及的用于给聚酯基无纺布染色的方法，通过将材料浸入含有“分散”型着色剂的浴中给微纤维组分染色。必须强调的是，单独使用分散染料并不包括给所有的聚氨酯基质染色，由于使用这类染料这种材料没有持久的可染色性，因而聚氨酯基质保持其原有的白色或灰色。染色工序之后，通过连二亚硫酸钠的NaOH溶液进行去色过程(stripping)，以除去存在于材料中的过量的着色剂，从而改善当被洗涤，被磨损或被暴露于光时的颜色坚牢度特性。由于未被染色的粘合剂基质所致的斑点的存在，即使在聚氨酯阶段，有时第二染色程序也是成为必要的。这样的要求，通常与特别活泼的和明亮的染色有关，其依赖于第二染色浴，和上面描述的标准浴的顺流来满足，其中所谓的“预金属化的”着色剂能被用于将聚氨酯基质染色并从而避免与在微纤维和粘合剂基质之间的着色差异有关的问题。这些工序能生产出具有特有的仿麂皮织物外观和在其微纤维组分中均匀染色的产品表面。
具有混色外观的无纺布是已经公知的，其通过使用聚氨酯基质制成，聚氨酯不产生高的耐用性(对氧化剂，紫外线，和聚合物链的水解的随时间的抵抗性)和在高温下(＞170℃)的可加工性，以及有必要地需要牺牲至少一种其他所需的特性，以使最终产品具有多孔性特征并使其产生高的柔软度。
发明内容
根据未被迄今为止已知的或商业化的其他合成产品所公开的组合，本发明涉及具有高耐用性和混色型外观的仿麂皮无纺布。
本发明的目标产品无纺布包含纤维组分和聚氨酯，聚氨酯特征在于存在“软”链段和“硬”链段；前一链段由聚碳酸酯多元醇和聚酯多元醇的混合物组成，后一链段由氨基甲酸乙酯基团(由异氰酸酯和多元醇反应得到)和酰脲(ureic)基团(由游离的异氰酸酯基团和水反应得到)组成；纤维组分包括一根具有混色外观的纤维或两根或多根具有不同染色特性的纤维。通过借助于上述三种不同的制备方法可预先得到特有的“混色”外观。
在至少两种不同类型纤维的混合物被使用的情况下，这些纤维必须具有这样的物理-化学性质以致于在染色阶段使它们具有不同性能。允许无纺布中不同纤维的均质混合物在这些情况下染色，以获得由于使用合适的染料染色而具有颜色和/或强度交替的特殊的视觉效果。
用于本发明生产的以混合物或单一形式使用的纤维可以具有0.001旦和10旦的重量：这样将“传统”旦尼尔纤维(＞1旦)和微纤维(＜1旦)同时使用是合理的。在纤维中能被使用的是天然纤维(丝，毛，棉，亚麻，大麻)，纤维素纤维(粘胶纤维，乙酸酯)和人造纤维。特别地，本发明中使用的微纤维优选由聚酯(聚对苯二甲酸乙二酯，聚对苯二甲酸乙二酯离子，聚对苯二甲酸亚丙基酯，聚对苯二甲酸亚丙基酯离子，聚对苯二甲酸丁二酯，聚对苯二甲酸丁二酯离子)制备，但它们同样可以由聚酰胺(PAd，PA66)或聚烯烃(聚乙烯，聚丙烯)得到。
用于多组分纤维精纺的微纤维生产技术，通过用粘接同样微纤维的聚合物将一种或两种聚合物(由上面所提及中的得到)同时挤出，在后续的工作阶段中，粘接同样微纤维的聚合物将被除去。在更为通常的情况下，这种聚合物粘合剂包括聚苯乙烯或改性的聚酯(TLAS)或聚羟基链烷酸酯(polyhydroxyalcanoates)族的聚合物。然而，前述的粘合剂必须和组成微纤维组分的聚合物(或其他聚合物)是不相溶混的，并且必须以重量百分比10-90％(优选15-50％)存在。“微纤维/粘合剂”体系的结构优选为“海-岛”型；精纺(海+岛)后，纤维的整个截面是环状的，并且包含于其中的环状的岛(微纤维)依次被海(粘合剂组分)包围，海固定并分离这些相同的岛。
作为现在所描述的技术的一种替换，精纺后的纤维可以具有中空的，延伸的或三叶截面。两(或三)组分的截面分布也可以是“放射”型(交替的组分“放射”于环形截面中)，“皮-核”(微纤维组分被含有粘合剂的外部针根包围)或多层(使两或三组分平行以及交替层)。
就可赋予所需的混色效果的染色程序而言，本发明所使用的纤维可以在生产程序的最后和/或在中间产品毡形成之前(纺前染色的合成/人造纤维的精纺或使用已经染色的天然短纤维)和/或在中间产品生毡(raw felt)形成之前(在这种情况下，优选使用已经提到的特殊的针染技术)和/或在中间产品生毡上(在这种情况下，优选使用已经提到的特殊的针染技术和/或被认为更合适的印染技术)用合适的染色剂染色。
在纺前染色的人造纤维的情况下，应该考虑如果所使用的着色剂不溶于聚合物，相同着色剂的粒径必须与所生产的微纤维的尺寸相适应。
与无色还是预染色的纤维被用于或者不被用于混合物中无关，在无纺布生产工序的最后，所存在的一种或多种纤维最终用合适的染色剂染色。在生产程序的最后，基于所需的美学效果，对要染色的纤维，要使用的染色技术(针体系或印染技术)，用于该目的的染色剂和所需染色浴的数量作出选择。
另一方面，作为特殊的聚氨酯基质的结果是，获得了作为发明目的的产品的高耐用性特性。
出于这种目的，根据两种类型的测试使材料经受老化来测量参数“无纺布的耐用性”：
1.“Xenotest 1200”，是在相对湿度(20±10％)，温度(100±3℃)，辐照(60W/m2)和时间(138小时)的清晰条件下，在特殊的设备(Xenotest 1200 CPS)中进行的紫外线辐射老化。
2.“Jungle test”，是测量抗水解性的老化测试，在老化试验箱(climaticchamber)中，于75±1℃的温度，90±3％的相对湿度下，进行5-7-10周。
就老化而言，根据外观的变化，耐磨性，物理-机械性能的变化和，受限于聚氨酯基质，聚合物链的平均分子量的变化来分析材料。
根据本发明存在于无纺布中的聚氨酯，其特征在于包括“硬”链段，由氨基甲酸乙酯基团和酰脲基团(得自于游离的异氰酸酯基团和水之间的反应)组成和“软”链段，由聚碳酸酯-多元醇/聚酯-多元醇的混合物组成，其比例变化于80/20-20/80。
特别地，聚氨酯的“软”链段包括多元醇/聚碳酸酯/聚酯的混合物，“硬”链段包括得自于芳族二异氰酸酯，优选地，得自于4，4′-二苯甲烷-二异氰酸酯和水反应产生的酰脲基团，使得直接在反应器中生成填充剂。用作本发明的实际生产，聚碳酸酯二醇可选自聚亚己基碳酸酯二醇(polyhexamethylene)(优选)，聚亚戊基碳酸酯二醇(polypentamethylenecarbonateglycol)，和聚亚庚基碳酸酯二醇(polyheptamethylenecarbonateglycol)，聚酯多元醇可选自聚新戊基己二酸二醇(polyneopentyladipatoglycol)(优选)，聚亚己基己二酸二醇(polyhexamethyleneadipatoglycol)，聚亚丁基己二酸二醇(polytetramethyleneadipatolycol)或聚己内酯二醇(polycarprolactonediol)。
所使用的有机二异氰酸酯是芳族的，例如2-4/2-6甲苯二异氰酸酯，以任意2-4/2-6异构体比例(如果比例为80/20更好)，或单独为4-4′二苯甲烷二异氰酸酯或其与2-4异构体的混合物，2-4′异构体按重量计，重量百分比为0.01至50％或甲苯二异氰酸酯和二苯甲烷-二异氰酸酯之间以及它们的异构体之间按任意比例的混合物。可以使用的溶剂为N，N-二甲基甲酰胺，N，N-二甲基乙酰胺，二甲基亚砜，丙酮，甲基甲酮(methylketone)，四氢呋喃和N-甲基-吡咯烷酮。
制备这些聚氨酯的方法对本领域的任何专业人员而言是公知的，所述专业人员的主张能决定采用哪一些根据本发明目的的定义中所指出的原材料。
基于先前提到的制备前提，本发明的目标产品无纺布实质上包括下列基本操作来制备：
在将具有不同染色特性(在使用纤维混合物的情况)的至少两类短纤维以不同百分比进行任一必要的混合之后，通过机械针刺法生产中间产品毡；
用聚合物基质浸渍毡以生产中间产品生毡；
任一必要的染色操作；
任一必要的后处理工序。
为了更有意义地描述在前提到的制备前提，制备步骤能被概述为下列方法：
前提“A”(使用纤维混合物)
将具有不同染色特性的至少两类短纤维以变化的百分比混合；
通过机械针刺法生产中间产品毡；
通过将毡浸渍在上面描述过的高耐用性聚氨酯基质中以生产中间产品生毡；
产品的任一必要的最终染色；
任一必要的后处理工序。
前提“B”(使用特殊的染色技术织针)
f.使用一种短纤维或以可变的百分比混合的具有不同染色特性的至少两类短纤维；
g.通过机械针刺法生产中间产品毡；
h.通过将毡浸渍在上面描述过的高耐用性聚氨酯基质中来生产中间产品生毡，接着用合适的针染技术将半成品染色。
i.任一必要的后处理工序。
前提“C”(使用被认为最合适的印染技术)
与前提A中所描述的(包括在这种情况下，即使用单一类型的短纤维得到生毡)或前提B中所描述的一样，在染色之前和/或之后，用被认为最合适的印染技术对中间产品生毡进行不同的处理。
在中间产品生毡的生产中，如果有必要，则可采用第二“暂时”粘合剂进行浸渍，在得到中间产品生毡本身之前除去该粘合剂。
能被使用的这类短纤维与前面所描述的一致。另外，在对获得混色产品来说是必要的纤维混合物的生产(按照上面已报告的指示生产这些微纤维的步骤)中，优选使用至少一种微纤维类的短纤维，但不是绝对必要的。不同类型纤维的任一必要的混合通常在短纤维的生产后进行，但是，在可能的情况下，纤维也可以在连续丝的切断前被混合。混合物的每一纤维组分能以1-99％的百分比使用，以得到所需的混色效果。
中间产品毡的生产紧接在短纤维的均质混合之后，并通过纤维混合物的机械梳理和针刺制备而成。这样获得的毡具有2-5mm的厚度和0.1-0.6g/cm3的密度。
中间产品生毡的生产可由不同的程序而实现，取决于存在于毡中纤维的类型和上面描述的作业前提“A”或“B”或“C”。为了更好地然而并不限定其范围地阐述发明，以下的例子将详细的举例说明：
前提“A”为与常规纤维混合的至少一种类型的微纤维(优选情况)。
这种情况的特征在于，需要在制备生毡的过程中溶解组分，该组分用在精纺过程中固定和分离微纤维(本段开始提到的一般例子中的聚苯乙烯或改性聚酯或聚羟基链烷酸酯族聚合物)。
出于这个原因，有必要提供用第二粘合剂浸渍毡的第一阶段，除去在精纺期间使用过的粘合剂之后，第二粘合剂依次地固定微纤维。通常，使用的第二粘合剂是聚乙烯醇或前面描述过的相同的高耐用性聚氨酯的溶液(在合适的浓度下)。最好在该阶段之后复合，在干燥后，用溶剂处理以溶解第一粘合剂并再次干燥。在这种粘合剂为聚苯乙烯时，氯化的溶剂例如三氯乙烯或全氯乙烯适合于所陈述的目的；在这种粘合剂是改性的聚酯(TLAS)或聚羟基链烷酸酯时，溶解在酸或碱的水溶液，或热水中进行。这样获得的中间产品被浸渍在高耐用性的聚氨酯溶液中，聚氨酯具有之前已广泛描述过的特性。在先前使用的第二粘合剂包括同样的聚氨酯时，第二浸渍仅仅优化了材料中聚氨酯(PU)的含量，以及最大化了粘合剂在微纤维上的作用。随着聚氨酯在水中的凝聚(在温度为20-50℃)和第二粘合剂的除去，中间产品生毡的生产继续进行：一般情况是，当这样的粘合剂是聚乙烯醇，浸渍在约80℃的水中，足以得到令人满意的溶解。干燥这样制得的复合物产生层压制品，然后通过在平行于两个表面的截面上剪裁(分割)将该制品分成两半。通过金刚砂抛光工序完成中间产品生毡的制备，该抛光工序使用合适的砂纸从聚氨酯基质中部分地抽取不同种类的纤维(打磨程序)。
前提“A”仅用于传统的旦尼尔纤维。
第二种情况与前面的情况区别在于，不存在微纤维，因此也不存在有关的“海”组分。这种情况简化了中间产品生毡的生产，既不需要用第二暂时粘合剂浸渍，也不需要在精纺中使用粘合剂溶液。因而程序被限于将毡浸渍于高耐用性的聚氨酯溶液中，干燥毡，并进行上述的分割和打磨工序。
前提“B”用于至少一种微纤维或仅用于传统的旦尼尔纤维或两者的混合物。
第三种情况与前面的情况区别在于，正如前面所述，在分裂工序之前或在中间产品生毡上使用特殊的“针染”技术。产品染色技术特征在于使用合适的“织针”机，“织针”机能将一种或多种染料同时注射到包括纤维组分和高耐用性聚氨酯基质的半成品中。因而，根据所需的混色效果，这样制得的中间产品生毡已经被染色。
前提“C”：重复前提“B”所描述的程序，不同仅在于，使用被认为是最合适的印刷技术代替“针染”技术，以获得所需的混色效果。
在通过纤维和至少一种还未被染色的那些纤维的混合物而获得混色效果的情况下；或者，在通过在包括单纤维或预先已被染色的纤维混合物的基质上的“织针”技术和/或印染(如前提“B”和“C”分别描述的)而获得混色效果的情况下，生毡的最终染色变得必要。
在前所描述的针织设备具有十分全面的价值，远远超过本专利申请的上下文所描述的范围。
本发明的另一个目的是装有空针的针刺机，空针连接于供给一种或多种染料的分配系统。
附图说明
图1示出了本发明的分配系统。
上述机器的非限定说明在图1中显示，这里：
1.连接于染料分配系统的复式接头，其分支为数个分配单独染料的小管；
2.与空针相连接的小孔管；
3.具有一个或多个孔的针；
4.针的细部；
5.放置待染色产品的工作台。
即使在一根或多根纤维已经被染色的情况下，可以进行包含产品的纤维的最终染色工序。在多数纤维在生产工序的最终阶段被染色的情况下，可以通过在单一的染色浴中不同类染料的混合物或者通过使用连续的浴来完成相同的染色。
这样得到的混色无纺布能够承受另外的加工工序，例如与其他基质连接，旨在赋予阻燃性，抗菌性等性质的后处理。
具体实施方式
本发明现将就作为举例说明的附加实施例作进一步描述。
该表显示被用于实施例中的缩写以确认原材料。
缩写 原材料
PET 聚对苯二甲酸乙二醇酯(Polyethyleneterdftalato)
PET阳离子 含有得自于间苯二酸-5-磺酸钠酸(isophthalic-5-solfonato sodico acid)的离子基团的聚对苯二甲酸乙二醇酯(Polyethylenetereftalato)
PS 聚苯乙烯
PA6 尼龙6
PA66 尼龙66
PVA 聚乙烯醇
DMF 二甲基甲酰胺
PHC 聚亚己基碳酸酯二醇(Polyhexamethylenecarbonateglycol)
PNA 聚新戊基己二酸二醇(Polineopentiladipatoglycol)
MDI 4-4′二苯甲烷二异氰酸酯(4，4′Difenilmetanodiisocianato)
DBA 二丁胺
PTHF 聚四亚甲基醚二醇(Polyoxytetramethyleneglycol)
PPG 聚氧丙二醇(Polyoxypropilenglycol)
实施例1(PET+具有D-PU的PET阳离子)
用短纤维制备纤维，在PS基质中包含PET的微纤维(0.13到0.15旦尼尔)，具有：
旦尼尔：3.8旦
长度：51毫米
卷曲：大约4-5/cm
特别地，纤维由57重量份的PET和43重量份的PS组成。如果在截面上测量，纤维显示出被嵌入PS基质中的16根PET微纤维的存在。接着，由聚苯乙烯基质中的阳离子PET的微纤维制备短纤维，具有下列特征：
旦尼尔：3.8旦
长度：51毫米
卷曲：大约4-5/cm
纤维由57重量份的PET阳离子和43重量份的PS组成。如果在截面上测量，纤维显示出被嵌入PS基质中的16根PET微纤维的存在。
将所得到的两类短纤维以最合适的比例均质地混合，以获得所需的混色效果。PET的含量通常为85-40％，阳离子PET的含量通常为15-60％。通过混合两种短纤维(fibers in staple)，生毡的制备是使生毡经受针刺，以形成具有特有的密度为0.160-0.220g/cm3之间的针刺毡。针刺毡被浸渍于20wt％的聚乙烯醇水溶液中，然后被干燥。这样处理过的针刺毡接着被浸渍于三氯乙烯中，直到聚苯乙烯纤维基质被完全溶解，结果形成了与阳离子PET微纤维相混合的PET微纤维无纺布。然后干燥无纺布，得到称为D1毡的中间产品。
以溶液的形式在N，N-二甲基甲酰胺中独立地制备聚氨酯弹性体。在第一步(预聚合)中，分子量均为2,000的PHC和PNA，在65℃的温度以及搅拌下，与MDI在摩尔比为2.9∶1的异氰酸酯/二醇中反应。反应3小时后，这样得到的预聚物被冷却到45℃并用含水量为0.03％的DMF稀释，直到得到游离NCO含量为1.46％的25％预聚物溶液。
然后，将温度保持在45℃，在5分钟的时间内将溶于DMF的DBA和水缓慢加入，以生成计算分子量为43,000的聚氨酯-聚脲。然后将温度升高到65℃，使反应器保持搅拌另外的8小时，最后，产生聚氨酯聚脲溶液，其随着时间而稳定，且在20℃时具有的粘度为24,000Pa*sec。所制备的弹性体溶液用含有Irganox1098和Tinuvin350的N，N二甲基甲酰胺稀释，以形成14wt％的溶液。通过在水中凝聚这种溶液的薄层，得到具有高孔隙率的聚合物。
如上述制备的D1毡，被浸渍于聚氨酯弹性体溶液中，从而被浸渍的无纺布经过一对辊子首先被拧出，并接着将无纺布浸渍于水浴中于40℃下恒温1小时。将这样制得的凝聚片材经过被加热到80℃的水浴中，以除去残余的溶剂和聚乙烯醇。干燥后，得到的复合微纤维片材被剪裁成具有厚度通常定制为0.9-1.2mm的片材，使得到的片材经受金刚砂抛光以增加毛度：结果是，被称为E1生毡的合成微纤维无纺布典一般具有在0.7-1.0mm之间变化的厚度。
实施例2(阳离子PET+具有传统的低耐用性PU的PET)
该实施例重复实施例1的工序，不同在于其使用了特征在于耐用性较劣的“传统”型的聚氨酯。与根据实施例1所描述的步骤而制备的毡D2相平行，聚氨酯弹生体的制备是通过使PTHF和PPG于65℃的温度在搅拌下(分子量均为2000)，在摩尔比为2.9∶1的异氰酸酯/二醇中反应。反应3小时后，这样得到的预聚物被冷却到45℃并用含水量为0.03％的DMF稀释，直到得到游离NCO含量为1.46％的25％预聚物溶液。将温度保持在45℃，在5分钟的时间内将溶于DMF的DBA和水缓慢加入，以生成计算分子量为43,000的聚氨酯-聚脲。然后将温度升高到65℃，使反应器保持搅拌另外的8小时，最后，产生聚氨酯聚脲溶液，其随着时间而稳定，且在20℃时具有的粘度为25,000Pa*sec。
所制备的弹性体溶液用含有Irganox1098和Tinuvin350的N，N二甲基甲酰胺稀释，以形成14wt％的溶液。通过在水中凝聚这种溶液的薄层，得到具有高孔隙率的聚合物。
然后将D2毡浸渍于聚氨酯溶液中，直至根据实施例1所提到的相同工序生成E2中间产品生毡。
实施例3(变化：阳离子PET+具有PET/PS＝80/20的PET)
该实施例重复实施例1的工序，不同在于，由阳离子PET(和/或PET)制备的微纤维不同于由80重量份阳离子PET和20重量份PS(和/或80重量份PET和20重量份PS)所制备的微纤维。如果在截面上测量，纤维显示出被嵌入PS基质中的16根PET微纤维的存在。无纺布生毡的生产按照实施例1所描述的工序。实施例4(变化：尼龙-6或尼龙-66代替阳离子PET)
该实施例重复实施例1-3的工序，不同在于，用PA6或PA66代替阳离子PET，生成被称为D3毡的中间产品无纺布。按如实施例1中所描述的一直进行下去，随后得到被称为生毡E3的合成微纤维无纺布。用传统的聚氨酯代替高耐用性聚氨酯的不同，包括与那些存在于中间产品E1和E2之间非常相似的耐用性的不同，在本实施例中不予明确地考虑。
实施例5(变化：纺前染色的PET代替阳离子PET)
本实施例重复实施例1-3的工序，不同在于，用纺前染色的PET代替阳离子PET，生成被称为D4毡的中间产品无纺布。纺前染色的PET包含可溶于聚合物的染料和/或不溶于聚合物的颜料(有机和/或无机类)。按如实施例1中所描述的一直进行下去，随后得到被称为生毡E4的合成微纤维无纺布，其具有染色-非染色-染色型的双色混色效果。用传统的聚氨酯代替高耐用性的聚氨酯的不同，包括与那些存在于中间产品E1和E2之间非常相似的耐用性的不同，在本实施例中不予明确地考虑。
实施例6(变化：纺前染色的尼-6或尼-66代替阳离子PET)
本实施例重复实施例1-3的工序，不同在于，用纺前染色的PA6或PA66代替阳离子PET，得到被称为D5毡的中间无纺布。按如实施例1中所描述的一直进行下去，随后得到被称为生毡E5的合成微纤维无纺布，其具有染色-非染色-染色型的双色混色效果。
用传统的聚氨酯代替高耐用性的聚氨酯的不同，包括与那些存在于中间产品E1和E2之间非常相似的耐用性的不同，在本实施例中不予明确地考虑。
实施例7(变化：纺前染色的阳离子PET代替阳离子PET)
本实施例重复实施例1-3的工序，不同在于，使用纺前染色的阳离子PET代替阳离子PET，得到被称作D6毡的中间产品无纺布。按如实施例1中所描述的一直进行下去，随后得到被称为生毡E6的合成微纤维无纺布，其具有染色-非染色-染色型的双色混色效果。
用传统的聚氨酯代替高耐用性的聚氨酯的不同，包括与那些存在于中间产品E1和E2之间非常相似的耐用性的不同，在本实施例中不予明确地考虑。
实施例8(变化：TLAS)
在实施例1，4，5，6，7中分别被称为D1，D3，D4，D5，D6毡的无纺布，也可以通过本实施例中所述的步骤得到，不同在于，其使用了海组分为改性聚酯(TLAS)的纤维。如果在截面上测量，纤维显示出被嵌入TLAS基质中的16根微纤维的存在。生毡由短纤维制备；使其经受针刺以形成具有密度为0.160-0.220g/cm3的针刺毡。针刺毡在90℃的热水中收缩，被浸渍于12％的高度皂化的温度约为70℃的聚乙烯醇(H.S.PVA)溶液中，并且在烘箱中于150℃下热固化30分钟。用PVA浸渍过的工件被浸渍于温度为60℃的10％的NaOH溶液中，以溶解“海”组分。
实施例9(变化：双重浸渍)
在实施例1，4，5，6，7中分别称作作D1，D3，D4，D5，D6毡的无纺布，也可以按照本实施例中所述的步骤得到，不同在于，针刺毡不直接被浸渍在聚乙烯醇水溶液中，而是浸渍在浓度更合适的聚氨酯溶液中。经干燥的材料随后浸渍在三氯乙烯中，直到聚苯乙烯纤维基质被完全溶解，结果形成混有阳离子PET微纤维的PET微纤维无纺布。然后干燥无纺布，如实施例1所述，在聚氨酯溶液中准备第二道浸渍。第二道浸渍对于最大化PU的粘合剂的作用以及最优化所制备的无纺布中PU是必需的。对于与实施例1中所描述的相似的中间产品生毡E1的生产，随后的工序阶段是必要的。
实施例10(变化：在齿杆或裁剪机中混合的毡)
在实施例1，4，5，6，7，8中分别被称为D1，D3，D4，D5，D6，D7毡的无纺布，也可以通过在剪裁连续纱线(形成短纤维)之前而不是之后，混合不同类型的纤维而得到。在这种情况下，被剪裁的纤维将导致已经含有纤维混合物的短纤维形成。
实施例11(PET+经纱羊毛(wool staple))
按照实施例1-3或实施例8-9中描述的步骤制备由PET的微纤维形成的短纤维。
将所述的微纤维以被认为是最合适的比例与经纱羊毛混合，以得到所需的最终混色效果。按照如实施例1中所描述的进行，得到被称为D10毡的无纺布，随后得到被称作E10生毡的中间产品无纺布。用传统的聚氨酯代替高耐用性的聚氨酯的不同，包括与那些存在于中间产品E1和E2之间非常相似的耐用性的不同，在本实施例中不予明确地考虑。
实施例12(PET+丝短纤维)
该实施例重复实施例11所述的工序，不同在于，其用丝短纤维代替羊毛，得到被称为D11毡的中间产品无纺布和被称为生毡E11的无纺布。
实施例13(PET+棉短纤维)
该实施例重复实施例11所述的工序，不同在于，其用棉短纤维代替羊毛，得到被称作D12毡的中间产品无纺布，以及随后得到的被称作生毡E12的无纺布。
实施例14(PET+麻短纤维)
该实施例重复实施例11所述的工序，不同在于，其用麻短纤维代替羊毛，得到被称为D13毡的中间无纺布，以及随后得到的被称为生毡E13的无纺布。
实施例15(粘性PET+短纤维的)
该实施例重复实施例11所述的工序，不同在于，其用短纤维代替羊毛，得到被称为D14毡的中间产品无纺布，以及随后得到的被称为生毡E14的无纺布。
实施例16(PET+纤维素乙酸酯短纤维)
该实施例重复实施例11所述的工序，不同在于，其用纤维素乙酸酯短纤维代替羊毛，得到被称为D15毡的中间无纺布，以及随后得到的被称为生毡E15的无纺布。
实施例17(PET+亚麻短纤维)
该实施例重复实施例11所述的工序，不同在于，其用亚麻短纤维代替羊毛，得到被称为D16毡的中间产品无纺布，以及随后得到的被称为生毡E16的无纺布。
实施例18(阳离子PET/PET混染-单染色周期)
根据实施例1-3-8-9-10和实施例2中所描述的步骤分别得到的被称为生毡E1和E2的合成微纤维无纺布，在装配有“文氏管”的“JET”设备中被染色。特别地，使合成的微纤维无纺布生毡在“文氏管”穿过1小时，操作进行是于125℃下在含有分散染料Yellow Dianix SE-G和阳离子染料Blue Astrazon FBL的单独的含水染浴中进行，染料的量分别为合成无纺布微纤维生毡的2wt％和1wt％。在处理结束时得到了具有双色混色效果的两种合成仿麂皮织物样品。根据表I所列的测试，将由高耐用性聚氨酯和传统聚氨酯得到的样品相比较，实现耐用性结果的评价。
实施例19(阳离子PET/PET混染-双染色周期)
根据实施例1-3-8-9-10和实施例2中所描述的步骤，而分别得到的被称为生毡E1和E2的合成微纤维无纺布，在装配有“文氏管”的“JET”设备中被染色。特别地，使合成的微纤维无纺布生毡在“文氏管”中穿过1小时，操作于125℃下在含有分散的染料Yellow Dianix SE-G的含水染浴中进行，该染料的量为合成无纺布微纤维生毡的2wt％。使这样得到的染色产品再在“文氏管”穿过1小时，操作于100℃下在含有阳离子染料Blue Astrazon FBL的含水染浴中进行，该染料的量为合成无纺布微纤维生毡的1wt％。在处理结束时得到了具有双色混色效果的的两种合成仿麂皮织物样品。参见表1可知对根据本实施例获得的产品的耐用性能的评价。许多特征与实施例18中生产的无纺布的特征相似。
实施例20(阳离子PET/PET染色混色-仅染色-非染色-染色阳离子染料的使用)
根据实施例1-3-8-9-10和实施例2中所描述的步骤而分别得到的被称为生毡E1和E2的合成微纤维无纺布，在装配有“文氏管”的“JET”设备中被染色。特别地，使合成的微纤维无纺布生毡穿过“文氏管”1小时，操作于100℃下在含有阳离子染料Blue Astrazon FBL的含水染浴中进行，该染料的量为合成无纺布微纤维生毡的1wt％。在处理结束时，得到了具有染色-非染色-染色型双色混色效果的两种合成仿麂皮织物样品。对根据本实施例获得的产品的耐用性能的评价在表中示出，表明有多少特征与实施例18中生产的无纺布的特征相似。
实施例21(微PET染色/尼龙)
按照实施例4或实施例8，或实施例9，或实施例10所描述的程序得到的被称为生毡E3的合成微纤维无纺布，在如实施例19或实施例20所述的“JET”设备中染色，仅有的不同是，用Blue Telon GGL染料代替Blue Astrazon FBL染料。
实施例22(微PET染色/纺前的所有染色)
分别在实施例6，7，8中得到的被称为生毡E4，E5，E6的合成微纤维无纺布，或者，两者择一地，在实施例9或实施例10中得到的无纺布，在装配有“文氏管”的“JET”设备中被染色。特别地，使上述每种合成的微纤维无纺布生毡穿过“文氏管”1小时，操作于125℃下，在含有分散染料Yellow Dianix SE-G的含水染浴中进行，该染料的量为合成无纺布微纤维生毡的2wt％。在处理结束时，得到了具有双色混色效果的合成仿麂皮织物样品。
实施例23(微PET染色/羊毛-丝短纤维)
分别按照实施例11和12所描述的步骤所得到的被称为E10，E11的无纺布生毡，一般按照实施例18，或实施例19，或实施例20中所描述的进行染色操作，但考虑到羊毛和丝超出了用阳离子染料着色的范围，也可以用其他类的染料例如酸，金属化的，直接的，活性的来染色。
实施例24(微PET染色/棉，麻，亚麻，粘胶短纤维)
分别按照实施例13，14，15和17所描述的步骤所得到的被称为E12，E13，E14和E16的无纺布生毡，一般如实施例18，或实施例19，或实施例20中所描述的进行染色操作，但考虑到棉，麻，亚麻，超出了用阳离子染料染色的范围，也可以用其他类的染料例如直接的，活性的来染色(水溶性的或非水溶性的)。
实施例25(“针染”系统)
正如实施例1至17和实施例21至24中所描述的，D和E类的半成品生毡和在工序步骤中得到的其他合理的中间产品类型，其中工序步骤提供将中间产品类型由一类转变成另一类的途径，也包括正如实施例18或19或20中所述的含有100％单一类型纤维的相应中间体，在染色之前或之后，都可以通过下面被称作“针染”的处理过程进行染色，其中装配有空针的专用针刺机与供应合适染料的分配系统相连接，将染料沉积在产品的结构里。
紧接着的热处理确保了染料的固着。在这种情况下，得到具有混色效果的产品，基于所选择的组合并与供给针系统的染料种类有关，其可以是双色的或多色的。
实施例26(印染技术)
按照如实施例25中所描述的进行，仅有的不同在于，“针”系统被那些已知技术中公知的印刷技术所取代，允许将得到所需的混色效果。
表1
混色样品 染色后的生毡E1 (实施例.18) 染色后的生毡E2  (实施例.19)
所使用的聚氨酯类型 D-PU(高耐用性) 传统的
老化后的无纺布
与未老化值相比的数均分子量“Mn”的保持率(％)
Xenotest1200(1) 93  50
Jungle test(2)5周 85  70
Jungle test(2)7周 75  65
Jungle test(2)10周 65  55
在马丁代尔(Martindale)上进行20,000转的摩擦后的外观。负载＝12Kpa(等级1-5)  0
Xenotest1200(1) 4  1
Jungle test(2)5周 4-5  4-5
Jungle test(2)7周 4-5  4
Jungle test(2)10周 4  2-3
与非老化相比的断裂破坏应变保持率％
Xenotext1200(1) 95  60
Jungle test(2)5周 90  90
Jungle test(2)7周 90  90
Jungle test(2)10周 80  80
Xenotest1200(1)
紫外线老化，T＝100±3℃；相对湿度＝20±10％；辐射能＝60W/m3；持续时间＝138小时。
Jungle test(2)
在人工气候室中老化；T＝75±1℃；相对湿度＝90±3％。

Claims (18)

1.一种无纺布，该无纺布具有混色视觉外观和高耐用性并含有纤维部分和基质粘合剂，其特征在于，粘合剂基质是聚氨酯，该聚氨酯的特征为存在有软链段和硬链段，软链段包括聚碳酸酯-多元醇和聚酯-多元醇的混合物，硬链段包括得自于异氰酸酯和多元醇反应的氨基甲酸乙酯基团，和得自于游离异氰酸酯基团和水之间反应的酰脲基团，以及纤维部分含有混色外观的纤维，或具有不同染色特性的两种或多种纤维的混合物。
2.根据前述权利要求的无纺布，其含有被浸渍在聚氨酯中的毡，所述毡含有具有不同染色特性的两种或多种纤维。
3.如前述权利要求的无纺布，其特征在于所述形成软链段的聚氨酯部分由聚碳酸酯二醇的混合物组成，聚碳酸酯二醇选自聚亚戊基碳酸酯二醇、聚亚己基碳酸酯二醇和聚亚庚基碳酸酯二醇，以及所述聚酯多元醇选自聚亚己基己二酸二醇、聚新戊基己二酸二醇、聚亚丁基己二酸二醇或聚己内酯二醇。
4.如前述权利要求的无纺布，其特征在于，在多元醇混合物中，聚碳酸酯-多元醇和聚酯多元醇的重量比为80/20至20/80。
5.根据权利要求1和2的无纺布，其特征在于，异氰酸酯基团得自于选自于下述的异氰酸酯：2-4(2-6)甲苯二异氰酸酯，4-4′-二苯甲烷-二异氰酸酯，3-异氰酸酯甲基3-5-5三甲基酸己基异氰酸酯(3-5-5 trimethlacidohexylisocyanate)，和它们混合物。
6.根据权利要求1和2的无纺布，其特征在于，含有重量为0.001-10旦尼尔的纤维。
7.根据前述权利要求的无纺布，其中纤维选自天然纤维，纤维素纤维和人造纤维。
8.根据前述权利要求的无纺布，其中存在的至少一种纤维优选自微纤维。
9.根据权利要求1或2的无纺布，其中在毡形成之前一种或多种纤维已经被染色。
10.根据权利要求1的无纺布，其中纤维部分含有其混色外观是通过使用装配有空针的针织机而获得的纤维。
11.根据权利要求1的无纺布，其中纤维部分含有其混色外观是通过使用印染技术而获得的纤维。
12.根据权利要求1定义的无纺布的制备程序，包括下列操作：
-通过机械针刺法生产中间产品毡，接着将具有不同染色特性的至少两种短纤维以不同的百分比进行任一必要的混合；
-通过将毡浸渍于上述高耐用性的聚氨酯基质中，以生产中间产品生毡；
-任一必要的产品最终染色；
-任一必要的后处理程序。
13.根据前述权利要求的无纺布的制备程序，其中中间产品生毡的生产，是通过采用将其浸渍于第二粘合剂中而实现，所述第二粘合剂过后被除去。
14.根据权利要求12的无纺布的制备程序，其中在将毡浸渍于聚氨酯基质中的阶段后，继之以用针染技术对半成品染色。
15.根据前述权利要求的无纺布的制备程序，其中通过使用连接于用于分散染料的系统上的装配有空针的针刺机，实现对半成品的染色。
16.根据权利要求12-15中的一项或多项的无纺布的制备程序，其中中间产品生毡在染色之前和/或之后，被印染技术处理。
17.一种针刺机，装配有与供给一种或多种染料的分配系统相连接的空针系统。
18.根据前述权利要求的针刺机基本上由图1示出。
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