CN113165317B - 多孔层结构体及其制备方法 - Google Patents

多孔层结构体及其制备方法 Download PDF

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Publication number
CN113165317B
CN113165317B CN201980073548.XA CN201980073548A CN113165317B CN 113165317 B CN113165317 B CN 113165317B CN 201980073548 A CN201980073548 A CN 201980073548A CN 113165317 B CN113165317 B CN 113165317B
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porous layer
substrate
polyurethane
alkylene oxide
aqueous
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CN113165317A (zh
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铃木悠介
村川达三
佐佐木一弥
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Dainichiseika Color and Chemicals Mfg Co Ltd
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Dainichiseika Color and Chemicals Mfg Co Ltd
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    • D06N2209/103—Resistant to mechanical forces, e.g. shock, impact, puncture, flexion, shear, compression, tear

Abstract

本发明涉及多孔层结构体，所述多孔层结构体含有基材和在该基材上形成的聚氨酯多孔层，其中，根据JIS L1099 A‑1(氯化钙法)测定所述多孔层结构体得到的透湿度A为2000~10000g/(m2·24h)，由根据JIS L1099 A‑1(氯化钙法)单独测定所述基材得到的透湿度B和所述透湿度A，用规定公式得到的透湿度损失率为75%以下，并且基材和聚氨酯多孔层的接合面的剥离强度为0.7kgf/英寸以上。

Description

多孔层结构体及其制备方法
技术领域
本发明涉及多孔层结构体及其制备方法。
背景技术
聚氨酯系树脂的耐磨损性、弯曲性、挠性、柔软性、加工性、粘接性、耐化学药品性等各物性优异，并且对各种加工方法的适应性也优异。因此，被广泛用作合成人造革(人造皮革与合成皮革的总称)用材料、各种涂布剂、油墨、涂料等的粘结剂或薄膜、片材和各种成型物用材料，提出了适合于各种用途的聚氨酯系树脂。
其中，通过对树脂赋予亲水性而使其可向水中乳化分散的聚氨酯树脂水分散体通过在涂布后进行干燥，容易得到机械物性、耐久性、耐化学药品性和耐磨损性等性能优异的覆膜，被广泛用于涂料、粘接剂、纤维加工处理剂、纸处理剂和油墨等。迄今为止，在这些用途中，使用溶解于有机溶剂的溶剂系聚氨酯。但是，由于存在有机溶剂的毒性、火灾的危险性、环境污染性等问题，所以近年来正在从溶剂系聚氨酯转换为使用聚氨酯树脂水分散体。
在使用聚氨酯树脂水分散体进行加工时，为了提高加工品的手感等，广泛利用实施各种处理而得到多孔结构的方法。
例如，在专利文献1中提出了以下方法：将含有(A)含有亲水性官能团的树脂与特定量的(B)铵盐和(C)非离子性增稠剂的水性分散液涂布在基材上而形成涂膜，对该涂膜进行热致凝胶化处理而形成凝胶化膜，使凝胶化膜干燥固化而形成被膜。
现有技术文献
专利文献
专利文献1：日本特许第5706897号公报。
发明内容
发明所要解决的课题
根据专利文献1，即使提高干燥温度或风量等来提高干燥效率，也可抑制被膜表面上的裂纹等的产生，显著提高整体的生产效率，并且可不依赖于所使用的基材而形成厚的被膜。但是，由专利文献1所记载的截面照片可知，被膜(聚氨酯多孔层)中形成的气泡几乎都是独立气泡，因此从良好的柔软性或透湿性的层面出发，可以说还需要改善。
另外，可以说今后不仅需要具有如上所述的特性，而且从耐久性的层面出发，还需要耐开裂性或剥离强度良好。
因此，本发明的目的在于，提供柔软性、耐开裂性和剥离强度良好的多孔层结构体及其制备方法。
解决课题的手段
本发明人进行了锐意研究，结果发现，通过下述本发明可解决上述课题，从而完成本发明。即，本发明如下所述。
[1] 多孔层结构体，所述多孔层结构体含有基材和在该基材上形成的聚氨酯多孔层，其中，
根据JIS L1099 A-1 (氯化钙法)测定所述多孔层结构体得到的透湿度A为2000~10000g/(m2·24h)，
由根据JIS L1099 A-1 (氯化钙法)单独测定所述基材得到的透湿度B和所述透湿度A，用下述公式得到的透湿度损失率为75%以下，并且基材与聚氨酯多孔层的接合面的剥离强度为0.7kgf/英寸以上：
公式) 透湿度损失率(%)=(1-(透湿度A/透湿度B))×100 。
[2] [1]所述的多孔层结构体，其中，所述聚氨酯多孔层的厚度为0.1~1.0mm，并且所述聚氨酯多孔层的密度为0.10~0.90g/cm3。
[3] 多孔层结构体的制备方法，所述方法是[1]或[2]所述的多孔层结构体的制备方法，其包括：
(1) 含水基材制作工序，其是将含有多孔层形成助剂A的基材处理用水溶液涂布在基材上而制成含水基材的工序，所述多孔层形成助剂A含有至少一种以上的盐，
(2) 涂膜结构体制作工序，其是将对含有多孔层形成助剂B、稳泡剂、水溶性树脂和聚氨酯树脂水分散体的调配液进行发泡处理而成的发泡组合物涂布在所述含水基材上而制成涂膜结构体的工序，所述多孔层形成助剂B含有至少一种以上的盐，
(3) 第1干燥工序，其是对所述涂膜结构体实施干燥处理的工序，
(4) 清洗工序，其是在第1干燥工序后进行清洗的工序，和
(5) 第2干燥工序，其是在清洗工序后实施干燥处理的工序；
所述聚氨酯树脂水分散体中的聚氨酯树脂粒子含有多元醇成分、异氰酸酯成分和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，所述亲水性氧化烯烃成分相对于聚氨酯树脂粒子的含量为1~25质量%。
[4] [3]所述的多孔层结构体的制备方法，其中，在所述含水基材制作工序、所述涂膜结构体制作工序和所述清洗工序中，实质上不使用有机溶剂。
[5] [4]或[5]所述的多孔层结构体的制备方法，其中，所述发泡处理为机械发泡。
发明的效果
根据本发明，可提供柔软性、耐开裂性和剥离强度良好的多孔层结构体及其制备方法。
附图说明
[图1] 说明本发明的一个实施方式所涉及的多孔层结构体的制备过程的概略说明图。
[图2] 表示本发明的一个实施方式所涉及的多孔层结构体的推测的截面结构的示意性的概略截面图。
具体实施方式
以下，对本发明进行详细说明。需说明的是，在本发明中，聚氨酯树脂是聚氨酯树脂和聚氨酯-尿素树脂的总称。
[1. 多孔层结构体]
本发明的多孔层结构体含有基材和在该基材上形成的聚氨酯多孔层，根据JISL1099 A-1 (氯化钙法)测定该多孔层结构体得到的透湿度A为2000~10000g/(m2·24h)。
在这里，透湿度是根据JIS L1099 A-1 (氯化钙法)测定的值，是将透过纤维制品(多孔层结构体或基材)的水蒸气的质量换算成每1m2的该纤维制品且每24小时的值，在本发明的情况下将其用作多孔层中的水蒸气的易通过性的指标。
即，在透湿度A大到超过10000g/(m2·24h)的情况下，推测多孔层中形成的气泡为连续气泡，并且形成与厚度方向平行的连续气泡。其结果是，若产生局部的剥离力，则树脂层容易被破坏，不耐用。另一方面，如本发明那样，若透湿度A为2000~10000g/(m2·24h)，则推测具有例如直径大的气泡彼此共有形成于其中的小孔而构成连续气泡这样的复杂形态。其结果是，即使产生局部的剥离力，也可发挥比形成与厚度方向平行的连续气泡的情况高的耐久性(剥离强度)。另外，当然也具有透湿性，而且也可良好地维持柔软性。需说明的是，若透湿度A低于2000g/(m2·24h)，则作为透湿性能变得不充分。
该透湿度A优选为2200~10000g/(m2·24h)，更优选为2500~10000g/(m2·24h)。
另外，由根据JIS L1099 A-1 (氯化钙法)单独测定多孔结构体的基材得到的透湿度B和透湿度A，用下述公式得到的透湿度损失率为75%以下：
公式) 透湿度损失率(%)=(1-(透湿度A/透湿度B))×100 。
透湿度损失率表示相对于基材单独的透湿度，因在基材上形成树脂层(多孔层)等而损失的透湿度的程度，若其超过75%，则作为结构体，透湿度显著受损。透湿度损失率优选为60%以下，更优选为50%以下。
基材和聚氨酯多孔层的接合面的剥离强度为0.7kgf/英寸以上，优选为0.75kgf/英寸以上，进一步优选为0.80kgf/英寸以上。若剥离强度低于0.7kgf/英寸，则无法得到充分的耐久性。推测本发明中的0.7kgf/英寸以上的剥离强度是由于直径大的气泡彼此共有形成于其中的小孔而构成连续气泡这样的复杂形态所引起的。
从良好的剥离强度与柔软性的并存的观点出发，聚氨酯多孔层的厚度优选为0.1~1.0mm，更优选为0.2~0.8mm。
多孔结构体中的聚氨酯多孔层的密度优选为0.10~0.90g/cm3，更优选为0.3~0.9g/cm3，进一步优选为0.4~0.8g/cm3。通过聚氨酯多孔层的密度为0.10g/cm3以上，可得到良好的剥离强度，通过为0.90g/cm3以下，可使得到的结构体的柔软性良好。
作为基材，可列举出使用如下所述的树脂的薄膜、织布、无纺布、合成皮革等。另外，基材也可以是发泡基材。
作为树脂，可列举出聚氯乙烯树脂、聚乙烯系树脂、聚丙烯系树脂、热塑性聚烯烃等烯烃系树脂、乙烯丙烯二烯系树脂、苯乙烯丙烯腈系树脂、聚砜系树脂、聚苯醚系树脂、丙烯酸系树脂、硅酮系树脂、氟系树脂、聚酯系树脂、聚酰胺系树脂、聚酰亚胺系树脂、聚苯乙烯系树脂、聚氨酯系树脂、聚碳酸酯系树脂、降冰片烯系树脂、纤维素系树脂、聚乙烯醇系树脂、聚乙烯醇缩甲醛系树脂、聚乙烯醇缩丁醛系树脂、聚乙烯基吡咯烷酮系树脂、聚乙烯醇缩乙醛系树脂、聚醋酸乙烯酯系树脂、工程塑料、生物降解性塑料等。
特别是作为汽车用的内装材料用树脂，可列举出聚氯乙烯树脂、热塑性聚烯烃、聚氨酯、聚丙烯等。
另外，在基材为发泡基材的情况下，可使用如氯乙烯树脂这样的基材。
基材的厚度优选为0.2~1.5mm，在基材为发泡基材、并使其发泡的情况下的发泡后的厚度优选为0.3~4.5mm。
[2. 多孔层结构体的制备方法]
本发明的多孔层结构体的制备方法为本发明的多孔层结构体的制备方法，包括：
(1) 含水基材制作工序，其是将含有多孔层形成助剂A的基材处理用水溶液涂布在基材上而制成含水基材的工序，所述多孔层形成助剂A含有至少一种以上的盐；
(2) 涂膜结构体制作工序，其是将对含有多孔层形成助剂B、稳泡剂、水溶性树脂和聚氨酯树脂水分散体的调配液进行发泡处理而成的发泡组合物涂布在所述含水基材上而制成涂膜结构体的工序，所述多孔层形成助剂B含有至少一种以上的盐；
(3) 第1干燥工序，其是对所述涂膜结构体实施干燥处理的工序；
(4) 清洗工序，其是在第1干燥工序后进行清洗的工序；和
(5) 第2干燥工序，其是在清洗工序后实施干燥处理的工序。
以下，一面参照图1，一面对各工序进行说明。
(含水基材制作工序)
在含水基材制作工序中，如图1所示，制成辊状的基材10被从辊12A抽出，一面由辊12B、12C、12D架设，一面在辊12C的位置通过含水处理槽14的基材处理用水溶液14A中。由此，将基材处理用水溶液14A浸渍涂布于基材10。需说明的是，基材10的详细情况如上所述。
在基材处理用水溶液14A中含有多孔层形成助剂A，所述多孔层形成助剂A含有至少一种以上的盐。
作为多孔层形成助剂A中的盐，可列举出铵、镁、钙等的硫酸盐或氯化物等。它们优选在水溶液中含有5~40质量%。通过含有5~40质量%，可促进调配液的固化。
含水量可通过浸渍于基材处理用水溶液14A的时间和/或含水量调整辊(辊12E)等进行调整。虽然也取决于基材10的种类，但含水量例如相对于基材10优选设为200~400质量%左右。
基材处理用水溶液14A的温度无特殊限定，但优选设为10~40℃左右。需说明的是，作为向基材的涂布方法，不限于浸渍涂布，可应用喷雾涂布、辊涂、刷涂之类的涂布方法，但若考虑实用性，则优选浸渍涂布。
在浸渍涂布后，将抽出的基材10例如用一对含水量调整辊(辊12E)压缩成规定的含水量，进行脱水而制成含水基材10A。
(涂膜结构体制作工序)
含水基材10A是用刮浆板17以规定厚度涂布规定的发泡组合物16而形成涂膜结构体10B。
发泡组合物16是在发泡槽18内对含有多孔层形成助剂B、稳泡剂、水溶性树脂和聚氨酯树脂水分散体的调配液进行发泡处理而成，所述多孔层形成助剂B含有至少一种以上的盐。
在这里，多孔层形成助剂B的至少一种以上的盐可示例出与多孔层形成助剂A中的至少一种以上的盐相同的盐，多孔层形成助剂B可设为与多孔层形成助剂A相同组成，也可设为不同的组成。至少一种以上的盐在调配液中优选为5~40质量%。
另外，作为调配液中含有的稳泡剂，可列举出硅酮系稳泡剂、非离子系稳泡剂、金属盐系稳泡剂等。从保持泡沫的观点出发，调配液中的稳泡剂相对于聚氨酯树脂优选为0.1~3质量%。
作为水溶性树脂，可列举出聚乙烯醇、甲基纤维素、黄原胶等多糖类、水溶性聚氨酯树脂、水溶性丙烯酸树脂等。从保持泡沫和辅助成膜的观点出发，调配液中的水溶性树脂优选为5~40质量%。
对于调配液中的聚氨酯树脂水分散体，调整其量以达到所期望的聚氨酯多孔层的厚度。
发泡处理的方法无特殊限定，但优选为机械搅拌原料而使空气渗入，从而使其发泡的机械发泡。
作为将发泡组合物16涂布在含水基材10A上的方法，可应用刮刀涂布机、刮板涂布机、MB反向涂布机等之类的涂布方法，但无特殊限定，可根据作为目标的涂布厚度选择最合适的涂布方法。
从确保发泡性的观点出发，涂布后的涂膜厚度优选为200~2000μm，更优选为600~1000μm。
通过利用含水基材制作工序进行的基材的含水处理和利用涂膜结构体制作工序进行的发泡组合物的涂布处理这两者的处理，可进一步提高基材与聚氨酯多孔层的密合性。
(第1干燥工序)
涂膜结构体10B被抽出至干燥装置19，实施干燥处理。干燥温度例如优选设为100~150℃。通过干燥处理，在涂膜结构体的涂膜凝固的同时，因发泡而产生的气泡彼此在其一部分中合并，共有直径比气泡直径小的孔，得到形成有连续气泡的多孔结构体10C。
需说明的是，由于该状态下的多孔结构体10C附着有未反应物或无用物，所以实施清洗处理。
(清洗工序)
上述多孔结构体10C被抽出至清洗槽20，通过清洗槽20内的清洗水20A中而被实施清洗处理。在图1所示的实例中，一面由辊12E、辊12F、一对辊12G、辊12H、一对辊12J架设一面被抽出，在辊12F、辊12H的位置通过清洗槽20内的清洗水20A中。清洗例如可在清洗水20的温度为40~50℃左右下进行，或增加辊的数量而增加浸渍的次数，或延长浸渍时间来进行调整。由此，充分进行清洗，送至第2干燥工序。
作为清洗水，通常使用蒸馏水。
(第2干燥工序)
清洗工序后的多孔结构体10C被抽出至干燥装置22，实施干燥处理。干燥温度只要是可将在清洗时含有的水充分干燥的温度即可，但例如优选设为120~150℃。
在第2干燥工序后，利用辊12J卷绕成辊状，制备本发明的被净化的多孔结构体10C。
在所述含水基材制作工序、所述涂膜结构体制作工序和所述清洗工序中，优选实质上不使用有机溶剂，更优选完全不使用有机溶剂。
在这里，作为涂膜结构体制作工序的调配液中调配的聚氨酯树脂水分散体的聚氨酯树脂粒子，使用含有多元醇成分、异氰酸酯成分和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，亲水性氧化烯烃成分相对于聚氨酯树脂粒子的含量为1~25质量%的聚氨酯树脂粒子。
以下，对聚氨酯树脂水分散体进行说明。
[聚氨酯树脂水分散体]
本发明所涉及的聚氨酯树脂水分散体是聚氨酯树脂粒子分散在水中而成的聚氨酯树脂水分散体，如上所述，聚氨酯树脂粒子含有多元醇成分、异氰酸酯成分和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，亲水性氧化烯烃成分相对于聚氨酯树脂粒子的含量为1~25质量%。通过使用这样的聚氨酯树脂粒子，容易将透湿度A、透湿度损失率和剥离强度调整至所期望的范围。另外，聚氨酯树脂水分散体优选含有40质量%以上的不挥发成分。此外，聚氨酯树脂粒子的体积平均粒径优选为0.3~5μm。
在本发明中，作为聚氨酯树脂粒子的构成成分，通过含有具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分(以下有时简称为“亲水性氧化烯烃成分”)，即使聚氨酯树脂粒子的体积平均粒径为0.3~5μm这样的较大的粒径，也可满足分散稳定性和成膜性。另外，由于体积平均粒径为0.3~5μm，所以容易使不挥发成分为40质量%以上，由于不挥发成分为40质量%以上，所以可以说具有比迄今为止的聚氨酯树脂水分散体更高的生产能力。
在这里，推测亲水性氧化烯烃成分在树脂粒子的表面发挥由该氧化烯烃产生的立体位阻效果，即使大粒径的树脂粒子沉降，也可因氧化烯烃引起的粒子彼此的排斥来防止凝聚。其结果是，即使为了使不挥发成分为40质量%以上而使体积平均粒径为0.3~5μm，也可得到良好的分散稳定性。
需说明的是，本发明中的“不挥发成分”是指下述聚氨酯树脂粒子或不挥发性的添加剂等，具体而言，是指将2g的聚氨酯树脂水分散体在120℃下干燥2小时的情况下得到的固体成分。
以下，对构成聚氨酯树脂水分散体中含有的聚氨酯树脂粒子的各成分进行更详细说明。
<聚氨酯树脂粒子>
构成本发明所涉及的聚氨酯树脂粒子的聚氨酯树脂主要含有多元醇成分、异氰酸酯成分和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分。
[多元醇成分]
作为构成本发明中的多元醇成分的多元醇，可示例出以下(1)~(6)。
(1) 聚碳酸酯多元醇
作为聚碳酸酯多元醇，可列举出聚碳酸四亚甲基二醇酯二醇、聚碳酸五亚甲基二醇酯二醇、聚碳酸新戊二醇酯二醇、聚碳酸六亚甲基二醇酯二醇、聚(碳酸-1,4-环己烷二亚甲基二醇酯)二醇等聚碳酸酯二醇及其无规/嵌段共聚物等。
(2) 聚醚多元醇
作为聚醚多元醇，可列举出将氧化烯烃(氧化乙烯、氧化丙烯、氧化丁烯等)和杂环式醚(四氢呋喃等)中的任一种聚合或共聚而得到的物质。具体而言，可列举出聚丙二醇、聚乙二醇-聚四亚甲基二醇(嵌段或无规)、聚四亚甲基醚二醇和聚六亚甲基二醇等。
需说明的是，聚醚多元醇中的氧化乙烯(EO)含有率设为低于50质量%。
(3) 聚酯多元醇
作为聚酯多元醇，可列举出将脂族系二羧酸(例如琥珀酸、己二酸、癸二酸、戊二酸和壬二酸等)和芳族系二羧酸(例如间苯二甲酸和对苯二甲酸等)中的至少任一种与低分子量二醇类(例如乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-六亚甲基二醇、新戊二醇和1,4-双羟基甲基环己烷等)缩聚得到的物质。
具体而言，可列举出聚己二酸乙二醇酯二醇、聚己二酸丁二醇酯二醇、聚己二酸六亚甲基二醇酯二醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇/丁二醇酯二醇、聚己二酸新戊二醇/己二醇酯二醇、聚己二酸-3-甲基戊二醇酯二醇和聚间苯二甲酸丁二醇酯二醇等。
(4) 聚内酯多元醇
作为聚内酯多元醇，可列举出聚己内酯二醇和聚-3-甲基戊内酯二醇等。
(5) 聚烯烃多元醇
作为聚烯烃多元醇，可列举出聚丁二烯二醇和聚异戊二烯二醇、或其氢化物等。
(6) 聚甲基丙烯酸酯二醇
作为聚甲基丙烯酸酯二醇，可列举出α,ω-聚甲基丙烯酸甲酯二醇和α,ω-聚甲基丙烯酸丁酯二醇等。
多元醇的数均分子量若为500以上，则无特殊限制，但优选500~4,000左右，进一步优选为1000~3000左右。这些多元醇可单独使用或组合使用2种以上，但从长期耐久性的观点出发，优选含有聚碳酸酯二醇。
需说明的是，数均分子量是换算成聚苯乙烯的数均分子量，通常可通过测定凝胶渗透色谱(GPC)来求得。
[异氰酸酯成分]
作为构成本发明中的异氰酸酯成分的异氰酸酯，无特殊限定，但优选脂族二异氰酸酯、脂环族二异氰酸酯、芳族二异氰酸酯等双官能团的多异氰酸酯。
作为多异氰酸酯的具体例，有甲苯二异氰酸酯、4-甲氧基-1,3-亚苯基二异氰酸酯、4-异丙基-1,3-亚苯基二异氰酸酯、4-氯-1,3-亚苯基二异氰酸酯、4-丁氧基-1,3-亚苯基二异氰酸酯、2,4-二异氰酸酯-二苯醚、均三甲苯二异氰酸酯、4,4’-二苯基甲烷二异氰酸酯、亚杜基二异氰酸酯(durylene diisocyanate)、1,5-萘二异氰酸酯、联苯胺二异氰酸酯、邻硝基联苯胺二异氰酸酯、4,4-二苄基二异氰酸酯、1,4-四亚甲基二异氰酸酯、1,5-五亚甲基二异氰酸酯、1,6-六亚甲基二异氰酸酯、1,10-十亚甲基二异氰酸酯、1,4-亚环己基二异氰酸酯、二甲苯二异氰酸酯、4,4’-亚甲基双(环己基异氰酸酯)、1,5-四氢萘二异氰酸酯、异佛尔酮二异氰酸酯、二环己基甲烷4,4’-二异氰酸酯等。其中，优选至少含有二环己基甲烷4,4’-二异氰酸酯。
需说明的是，在如车辆用途或浅色系用途等这样需要柔软性、机械物性和耐变色性的情况下，优选与4,4’-二苯基甲烷二异氰酸酯一起并用脂族二异氰酸酯或脂环族二异氰酸酯。
多异氰酸酯成分的异氰酸酯基当量与所有成分的羟基当量之比优选为1.1~2.2，更优选为1.2~1.9。若NCO/OH为1.2~1.9，则柔软性和耐久性均变得更好。
[具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分]
具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分赋予聚氨酯树脂粒子以水分散性。虽然水分散性变好的理由尚不明确，但推测是通过氧化烯烃以从聚氨酯树脂粒子的表面伸长的方式向水中突出，从而其发挥阻碍其它的聚氨酯树脂粒子接近的立体位阻效果。
在亲水性氧化烯烃成分中，活性氢是与异氰酸酯的异氰酸酯基反应的氢原子，可列举出羟基、巯基、氨基等中的氢原子，其中优选羟基的氢原子。
另外，氧化烯烃成为显示亲水性的亲水性基团，有助于聚氨酯树脂粒子的水分散性。该氧化烯烃的碳原子数例如优选2~12，具体而言，可列举出氧化乙烯、1,2-或1,3-氧化丙烯、1,2-、2,3-或1,3-氧化丁烯、四氢呋喃、3-甲基四氢呋喃、α-氧化烯烃、氧化苯乙烯和表卤醇(表氯醇等)等。其中，作为氧化烯烃，优选含有氧化乙烯。
氧化乙烯的重复单元在具有氧化烯烃的亲水成分中优选至少含有50质量%以上，更优选含有70质量%以上，进一步优选氧化烯烃为氧化乙烯。
作为构成亲水性氧化烯烃成分的化合物，可列举出聚乙二醇、聚氧乙烯-聚氧丙烯共聚物二醇、聚氧乙烯-聚氧丁烯共聚物二醇、聚氧乙烯-聚氧化烯共聚物二醇，和它们的甲基醚、乙基醚、丁基醚等单烷基醚类，对这些单烷基醚类加成如1,3-二醇这样的二醇得到的聚亚烷基二醇单烷基醚的二醇加成物。
其中，优选聚乙二醇，如聚乙二醇单甲基醚和聚乙二醇单乙基醚等这样的聚乙二醇单烷基醚，对聚乙二醇单烷基醚加成如1,3-二醇这样的二醇得到的聚乙二醇单烷基醚的二醇加成物等。
特别是从不仅进一步提高分散稳定性，而且使再分散性也良好，发挥优异的耐热性的观点出发，更优选聚乙二醇单烷基醚和聚乙二醇单烷基醚的二醇加成物，进一步优选聚乙二醇单烷基醚的二醇加成物。
推测它们在聚氨酯树脂粒子中保持适合于发挥分散性和热稳定性的形态。
构成亲水性氧化烯烃成分的化合物的数均分子量优选为500~3000，更优选为700~2000。
作为聚乙二醇的市售品，例如可列举出日油株式会社制的“PEG#200”、“PEG#300”、“PEG#400”、“PEG#600”、“PEG#1000”、“PEG#1500”、“PEG#1540”、“PEG#2000”等。
作为聚乙二醇单甲基醚的市售品，例如可列举出日油株式会社制的“Uniox M-400”、“Uniox M-550”、 “Uniox M-1000”、“Uniox M-2000”等。
作为聚乙二醇单烷基醚的二醇加成物的市售品，例如可列举出Evonic公司制的“TEGOMER D3403”等。
以上是优选的成分的示例，本发明并不限定于此。因此，不仅上述示例，其它现在市售的、能够容易从市场上获取的化合物均可使用。
亲水性氧化烯烃成分相对于聚氨酯树脂粒子的含量为1~25质量%，优选为3~20质量%，更优选为5~10质量%。若含量低于1质量%，则分散稳定性降低，或成膜性降低而产生裂纹。若超过25质量%，则有机械物性降低、水分散体增稠的可能性，导致作业性降低或不挥发成分降低。
另外，通过含有1~20质量%的亲水性氧化烯烃成分，可减缓成膜时的干燥(水分的蒸发)速度，抑制裂纹产生。
[聚氨酯树脂粒子的体积平均粒径]
本发明的聚氨酯树脂粒子的体积平均粒径为0.3~5μm。若聚氨酯树脂粒子的体积平均粒径低于0.3μm，则水分散体的粘度上升，产生不挥发成分降低的必要性。另一方面，若体积平均粒径超过5μm，则粒子变得容易沉降。
从这样的观点出发，聚氨酯树脂粒子的体积平均粒径优选0.3~5.0μm，更优选0.3~3.0μm，进一步优选0.3~1.5μm。
[聚氨酯树脂水分散体的粘度]
聚氨酯树脂水分散体在25℃下的粘度优选为3000mPa·s以下，更优选为2000mPa·s以下。通过粘度为2000mPa·s以下，在制备时容易实施异物除去(过滤等)，可提高生产效率。
[聚氨酯树脂水分散体的制备方法]
作为本发明中的聚氨酯树脂水分散体的制备方法，例如可列举出以下方法：(1)所述方法经历使多元醇、构成亲水性氧化烯烃成分的化合物、异氰酸酯反应的反应工序，和在反应后添加表面活性剂等，添加离子交换水和二胺等的混合液，边乳化边高分子化的乳化和高分子量化工序，其中，将在乳化和高分子量化工序中的添加表面活性剂等时的搅拌设为100~300rpm左右的缓慢搅拌，将添加离子交换水和二胺等的混合液时的搅拌设为4000~6000rpm左右的强搅拌；和(2)所述方法在具有槽内循环用的搅拌桨和用于赋予剪切力的搅拌桨的搅拌槽中，至少使多元醇、异氰酸酯和构成亲水性氧化烯烃成分的化合物反应并乳化。
通过该制备方法，可有效地以上述高不挥发性成分浓度制备具有上述体积平均粒径的聚氨酯树脂粒子。另外，可制成所期望的粘度。
对于(2)的方法，具体而言，可通过在具备能够应对可实现均匀化的超高粘度液体的搅拌桨的反应容器(上述搅拌槽)中，使多元醇、根据需要添加的短链二醇、异氰酸酯和构成亲水性氧化烯烃成分的化合物反应，然后，加入短链二胺等扩链剂或扩链终止剂、表面活性剂、作为分散介质的离子交换水，边乳化边反应来制备。
需说明的是，短链二醇或短链二胺等扩链剂或扩链终止剂等在(1)的方法中也可适当添加。
另外，作为上述搅拌槽，例如可列举出在搅拌槽内具有2个以上的搅拌桨，例如具有2个以槽内循环为目的的搅拌桨、1个以对槽内赋予高剪切力为目的的用于赋予剪切力的搅拌桨的搅拌装置，其中，优选在反应容器内的上部、底部和上部与底部的中间部这3个部位具有搅拌桨的搅拌装置。具体而言，可列举出高粘度高剪切复合搅拌装置(商品名：NANOVisK，Sumitomo Heavy Industries Process Equipment Co., Ltd.制)或真空乳化搅拌装置(Mizuho Industrial Co., Ltd.制)。
在上述(1)和(2)的制备方法中，若需要，则也可使用有机溶剂进行反应，接着通过减压来除去有机溶剂，从而制备聚氨酯树脂水分散体。
作为有机溶剂，例如可列举出酮系溶剂(丙酮、甲乙酮、甲基异丁基酮、环己酮等)、芳族系烃溶剂(甲苯、二甲苯、SWASOLVE (Cosmo Oil Co., Ltd.制的芳族系烃溶剂)、Solvesso (Exxon Chemical Co., Ltd.制的芳族系烃溶剂)等)、脂族系烃溶剂(正己烷等)。其中，从操作性的观点出发，优选甲乙酮、丙酮和四氢呋喃等。
作为表面活性剂，可列举出非反应性的非离子性表面活性剂。
作为上述非离子性表面活性剂，例如可列举出聚氧乙烯烷基醚等二醇醚和乙炔二醇等。
作为短链二胺，可列举出乙二胺、三亚甲基二胺、六亚甲基二胺和八亚甲基二胺等脂族二胺化合物，苯二胺、3,3’-二氯-4,4’-二氨基二苯基甲烷、4,4’-亚甲基双(苯胺)、4,4’-二氨基二苯醚和4,4’-二氨基二苯砜等芳族二胺化合物，环戊二胺、环己二胺、4,4-二氨基二环己基甲烷、1,4-二氨基环己烷和异佛尔酮二胺等脂环式二胺化合物，肼、碳二酰肼、己二酸二酰肼、癸二酸二酰肼、邻苯二甲酸二酰肼等肼类等。其中，更优选肼(水合肼)。
短链二醇是数均分子量低于500的化合物，可列举出乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇和新戊二醇等脂族二醇类及其氧化烯烃低摩尔加成物(数均分子量低于500)、二甘醇、三甘醇、一缩二丙二醇等亚烷基醚二醇，1,4-双羟基甲基环己烷和2-甲基-1,1-环己烷二甲醇等脂环系二醇类及其氧化烯烃低摩尔加成物(数均分子量低于500)、苯二甲醇等芳族二醇类及其氧化烯烃低摩尔加成物(数均分子量低于500)、双酚A、硫代双酚和磺基双酚等双酚类及其氧化烯烃低摩尔加成物(数均分子量低于500)，和C1~C18的烷基二乙醇胺等烷基二链烷醇胺类等化合物。其中，优选脂族二醇类。
<聚氨酯树脂水分散体中的不挥发成分的量>
在本发明中，由于聚氨酯树脂水分散体中的不挥发成分为40质量%以上，所以通过在干燥工序中使其挥发而向体系外排出的挥发成分的量少，可削减干燥所需要的能量。
在本发明中，从削减在干燥工序中使用的能量的观点出发，聚氨酯树脂水分散体中的不挥发成分的量优选41质量%以上，更优选45质量%以上。上限值无特殊限定，但例如为70质量%左右。
如上所述，由于本发明的聚氨酯树脂水分散体的挥发成分的量少，所以与以往相比可容易地除去挥发成分，通过经过干燥工序，聚氨酯树脂粒子可熔融而薄膜化。这里所谓的薄膜化是指例如在脱模纸上涂布本发明的聚氨酯树脂水分散体使得薄膜厚度为40μm，在120℃下干燥5分钟后，可从剥离纸上保持薄膜形态而剥离。
<添加剂>
本发明的聚氨酯树脂水分散体也可根据需要含有添加剂。作为添加剂，例如可列举出消光剂、抗氧化剂(受阻酚系、亚磷酸酯系、硫醚系等)、光稳定剂(受阻胺系等)、紫外线吸收剂(二苯甲酮系、苯并三唑系等)、气体变色稳定剂(肼系等)、金属钝化剂等。
作为消光剂，可列举出树脂粒子、二氧化硅粒子、滑石粉、氢氧化铝、硫酸钙、硅酸钙、碳酸钙、碳酸镁、碳酸钡、硅酸铝、分子筛、高岭土、云母和云母等。在本发明的聚氨酯树脂水分散体含有消光剂的情况下，可使构成表皮材料的覆膜消光。
如上所述的本发明的多孔层结构体，若用电子显微镜观察其截面，则如图2所示，是基材4上的聚氨酯多孔层1中因发泡而产生的气泡2彼此在其一部分中合并，共有直径比气泡直径小的孔3，形成连续气泡而成。通过这样的结构，成为柔软性、耐开裂性和剥离强度良好的多孔层结构体。
本发明的多孔层结构体可优选应用于天然皮革、合成人造革、人造皮革等人造革、塑料片状物、各种薄膜、塑料成型物、橡胶成型物等。
实施例
以下列举实施例和比较例来更具体地说明本发明，但本发明并不限定于此。另外，以下的“份”表示质量份，“%”表示质量%。
<作为聚氨酯树脂水分散体的PUD1~12和比较PUD1~8的制作>
[含有末端NCO基的聚氨酯预聚物合成工序]
在用氮气置换具备搅拌器、回流冷却管、温度计、氮吹入管和探孔的反应容器后，以表1和表2所记载的配比，投入多元醇、扩链剂、构成作为亲水成分的亲水性氧化烯烃成分的化合物、异氰酸酯，边搅拌边升温，在95℃下使其反应，由此得到在末端具有NCO基的聚氨酯预聚物。
需说明的是，多异氰酸酯成分的异氰酸酯基当量与所有成分的羟基当量之比(NCO/OH)设为1.5。
[乳化和高分子量化反应]
将得到的含有末端NCO基的聚氨酯预聚物转移至不锈钢容器中，使用安装有直径为50mm的分散桨的T.K.均质分散器(特殊机化工工业社制)以100~300rpm缓慢搅拌5分钟。接着，以表1和2所记载的配比，添加表面活性剂，在比较PUD7、8的情况下还添加中和剂，搅拌至均匀。在确认体系内均匀后，边以4000~6000rpm强搅拌10分钟，边以表1和2所记载的配比添加离子交换水(分散剂)和二胺的混合液，边乳化边高分子量化，由此得到作为聚氨酯树脂水分散体的PUD1~12和比较PUD1~8。
<聚氨酯原料>
·多元醇A：宇部兴产(株)制的UH-100 (聚碳酸酯二醇，数均分子量为1000)
·构成亲水性氧化烯烃成分的化合物B：宇部兴产(株)制的PEG1000 (聚乙二醇，数均分子量为1000)
·构成亲水性氧化烯烃成分的化合物C：Evonic公司制的TEGOMER D 3403 (聚乙二醇单甲基醚-1,3-二醇，数均分子量为1000)
·构成亲水性氧化烯烃成分的化合物D：日油(株)制的Uniox M-1000 (聚氧乙烯单甲基醚，数均分子量为1000)
·亲水成分E：Bis-MPA (二羟甲基丙酸)
·扩链剂F：1,4-丁二醇
·异氰酸酯G：Sumika Covestro Urethane Co., Ltd.制的Desmodur W (二环己基甲烷4,4’-二异氰酸酯)
·二胺H：60%水合肼
·表面活性剂I：日本乳化剂(株)制的Newcol 2306-Y (聚氧化烯烷基醚，EOPO非离子系表面活性剂)
·中和剂J：三乙胺
·分散介质K：离子交换水。
(不挥发成分的测定)
用电子天平测量不锈钢容器的重量(g0)，称量2g的得到的各聚氨酯水分散体至不锈钢容器中(g1)。接着，将称量过聚氨酯水分散体的不锈钢容器在120℃下干燥2小时，测量干燥后的重量(g2)。根据得到的各重量和以下式(1)，测定不挥发成分：
不挥发成分(质量%)=(g2-g0)/(g1-g0)×100 式(1)。
(酸值)
比较PUD7、8的酸值根据亲水成分等的调配量作为计算值计算。
Figure DEST_PATH_IMAGE001
需说明的是，表1、2中的配比的数值为质量份。
Figure DEST_PATH_IMAGE002
<多孔层结构体的制作>
作为基布含浸用多孔层形成助剂(多孔层形成助剂A)，使用20质量%的硫酸铵水溶液或20质量%的氯化镁水溶液，在该水溶液中浸渍涂布在基材(聚酯圆编的基布，厚度为1mm)上而制成含水基材(含水基材制作工序)。需说明的是，含水率设为200~400质量%。
制备以表3和表4所表示的比例含有多孔层形成助剂B (20质量%的硫酸铵水溶液或20质量%的氯化镁水溶液)、硅酮系添加剂(Shin-Etsu Silicone公司制的硅酮稳泡剂)、水溶性树脂(15质量%的聚乙烯醇水溶液)、聚氨酯系增稠剂(大日精化工业社制，RESAMINED-870T)和聚氨酯树脂水分散体的调配液。将调配液用分散桨以3000rpm搅拌2分钟，由此通过机械发泡进行发泡处理，制成发泡组合物。将其涂布在含水基材上使得涂布厚度为1000μm，制成涂膜结构体(涂膜结构体制作工序)。
然后，在150℃下以5~10分钟的条件对涂膜结构体进行干燥处理(第1干燥工序)。
在干燥结束后，用45℃的热水浴对残留的多孔层形成助剂等进行清洗(清洗工序)。
在确认已充分清洗后，除去多余的水分，在120℃下以5~10分钟的条件进行干燥处理(第2干燥工序)，得到实施例1~24、比较例1~20的多孔层结构体(合成人造革)。
<聚氨酯多孔层的密度>
将制作的多孔层结构体切取10cm×10cm见方，用下述公式计算聚氨酯多孔层的密度。
(1) 多孔层结构体的重量测定和计算
根据多孔层结构体整体的重量：A、涂布基材的重量：B，由下述公式求得聚氨酯多孔层的重量：C。
C=A-B(g)
(2) 多孔层结构体的厚度测定和计算
根据多孔层结构体整体的厚度：D、涂布基材的厚度：E，由下述公式求得聚氨酯多孔层的厚度：F。
F=D-E(cm)
(3) 聚氨酯多孔层的密度计算
利用下述公式求得聚氨酯多孔层的密度。
聚氨酯多孔层密度=C÷(F×10×10)(g/cm3)
<评价方法>
(表面裂纹评价方法)
通过目视确认在所制作的多孔层结构体的中央部分10cm×10cm的范围内是否存在长度为1mm以上的裂纹，并进行评价。
〇：无裂纹，×：有裂纹
(剥离评价)
将6000号Polycotape(奥田产业社制)热压接在所制作的多孔层结构体的树脂涂布面上，用自动绘图仪(岛津制作所社制)测定T型剥离强度。
(透湿度)
从所制作的多孔层结构体上切出试验片，依据JIS L1099 A-1 (氯化钙法)，评价多孔层结构体的透湿度A。
(透湿度损失率)
测定所制作的多孔层结构体的透湿度A和结构体中使用的基材的透湿度B，利用下述公式计算透湿度损失率。
透湿度损失率(%)=(1-(多孔层结构体透湿度A/基材透湿度B))×100
需说明的是，对于基材的透湿度B，切出在多孔层结构体的制作中使用的基材，依据JIS L1099 A-1 (氯化钙法)，评价透湿度。
Figure DEST_PATH_IMAGE004
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Figure 257408DEST_PATH_IMAGE008
所有实施例的耐开裂性、剥离强度均良好。需说明的是，无法测定的比较例的原因是由于产生表面裂纹所引起的无法测定正常值(比较例1、3、5、7、8、9、11、13、15、16、20)或由于基材多孔层间的水侵入所引起的无法测定正常值(比较例17、18)。
标记说明
10 基材
10A 含水基材
10B 涂膜结构体
10C 多孔结构体
12A~12H 辊
14 含水处理槽
14A 基材处理用水溶液
16 发泡组合物
17 刮浆板
18 发泡槽
19 干燥装置
20、22 清洗槽
20A 清洗水。

Claims (5)

1.多孔层结构体，所述多孔层结构体含有基材和在该基材上形成的聚氨酯多孔层，其中，构成所述聚氨酯多孔层的聚氨酯含有多元醇成分、异氰酸酯成分、和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，含有1～25质量％的所述亲水性氧化烯烃成分，
所述聚氨酯多孔层的厚度为0.1～1.0mm，并且所述聚氨酯多孔层的密度为0.10～0.90g/cm3，根据JISL1099A-1(氯化钙法)测定所述多孔层结构体得到的透湿度A为2000～10000g/(m2·24h)，
由根据JISL1099A-1(氯化钙法)单独测定所述基材得到的透湿度B和所述透湿度A，用下述公式得到的透湿度损失率为75％以下，并且基材与聚氨酯多孔层的接合面的剥离强度为0.7kgf/英寸以上：
公式)透湿度损失率(％)＝(1-(透湿度A/透湿度B))×100。
2.权利要求1所述的多孔层结构体，其中，构成所述聚氨酯多孔层的聚氨酯含有聚碳酸酯多元醇、选自脂族二异氰酸酯、脂环族二异氰酸酯和芳族二异氰酸酯中的至少一种的2官能的多异氰酸酯、和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，含有1～25质量％的所述亲水性氧化烯烃成分。
3.多孔层结构体的制备方法，所述方法是权利要求1或2所述的多孔层结构体的制备方法，其包括：
(1)含水基材制作工序，其是将含有多孔层形成助剂A的基材处理用水溶液涂布在基材上而制成含水基材的工序，所述多孔层形成助剂A含有至少一种以上的盐，
(2)涂膜结构体制作工序，其是将对含有多孔层形成助剂B、稳泡剂、水溶性树脂和聚氨酯树脂水分散体的调配液进行发泡处理而成的发泡组合物涂布在所述含水基材上而制成涂膜结构体的工序，所述多孔层形成助剂B含有至少一种以上的盐，
(3)第1干燥工序，其是对所述涂膜结构体实施干燥处理的工序，
(4)清洗工序，其是在第1干燥工序后进行清洗的工序，和
(5)第2干燥工序，其是在清洗工序后实施干燥处理的工序；
所述聚氨酯树脂水分散体中的聚氨酯树脂粒子含有多元醇成分、异氰酸酯成分和具有1个以上的活性氢基、并且具有氧化烯烃的亲水性氧化烯烃成分，所述亲水性氧化烯烃成分相对于聚氨酯树脂粒子的含量为1～25质量％。
4.权利要求3所述的多孔层结构体的制备方法，其中，在所述含水基材制作工序、所述涂膜结构体制作工序和所述清洗工序中，实质上不使用有机溶剂。
5.权利要求3或4所述的多孔层结构体的制备方法，其中，所述发泡处理为机械发泡。
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