CN106739319A - 一种热塑性聚氨酯发泡革的制备方法 - Google Patents

一种热塑性聚氨酯发泡革的制备方法 Download PDF

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CN106739319A
CN106739319A CN201611002653.9A CN201611002653A CN106739319A CN 106739319 A CN106739319 A CN 106739319A CN 201611002653 A CN201611002653 A CN 201611002653A CN 106739319 A CN106739319 A CN 106739319A
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胡华
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ZHEJIANG HUANLONG NEW MATERIAL SCIENCE & TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种热塑性聚氨酯发泡革的制备方法，1）将TPU树脂、扩链剂、气体阻隔剂、相容剂、成核剂进行干混；2）将混合物加入挤出机的料筒中，经挤出机加热得到TPU熔体，将超临界N2以1～30毫升/分钟的速度注入到TPU熔体中，将TPU熔体与超临界N2混合均匀，混合后熔体经热交换器逐渐降低温度至155℃，再将混合后溶体经过狭缝口模挤出得到膨胀的TPU薄膜，挤出过程中所述挤出机的口模温度为140～160℃，挤出机口模的压力为5～25MPa；3) TPU薄膜经过温度为130～160℃的单轴拉伸设备进行牵伸变薄，拉伸时间不超过15秒，制得TPU发泡薄膜，再将TPU发泡薄膜与布高温贴合，得到TPU发泡革。采用上述技术方案，避免了TPU发泡革中TPU发泡薄膜密度较大、泡孔较大的缺陷。

Description

一种热塑性聚氨酯发泡革的制备方法
技术领域
本发明涉及一种热塑性聚氨酯（TPU）发泡革的制备方法，尤其涉及一种超临界流体物理发泡连续制备TPU发泡革的方法。
背景技术
人造革如聚氨酯（PU）发泡革、聚氯乙烯（PVC）等发泡革作为天然皮革的替代材料，在我国发展迅速。不过，人造革在生产加工过程中不可避免的使用大量有毒有害的溶剂和增塑剂。近年来，随着人们环保意识的提高，人造革在使用时存在的可挥发性有机物（VOC）问题已经引起社会各界和人造革行业的重视。目前，欧美、日本、中国都已先后出台VOC的检测法规。
TPU具有优异的耐磨性、耐化学腐蚀性、耐油、耐水、高弹性、抗疲劳等诸多优点，是一种性能优异、有价格竞争力的环保材料。TPU树脂制备成发泡膜后，还具有轻质、柔软、高回弹等优点，可作为代替传统PU、PVC人造革的新型环保人造革。
中国专利文献CN104861642A公开了一种以化学发泡剂偶氮二甲酰胺（AC）结合碳酸氢钠为复合发泡剂，制备人造革用的TPU发泡膜的方法，先将反应原料高速混合后，进入螺杆挤出机进行反应挤出制成TPU母粒，再将TPU母粒与发泡剂在双辊开炼机下开练成片进行发泡。此方法所使用的AC发泡剂还导致VOC的问题, 还存在效率低的问题。
采用化学发泡剂连续挤出TPU发泡薄膜的研究也曾有研究者涉及。不过，TPU树脂熔体强度低，采用化学发泡法制备的TPU发泡材料泡孔尺寸高达200～500微米，难以制备厚度仅为0.2～0.5毫米的薄膜来说。
高压流体如高压N2、CO2流体是一种价格低廉，并且无色、无毒、无臭、无害的物理发泡剂。根据需求，高压流体可以为高压气体流体、高压液体流体和超临界流体。高压流体能轻易从产物中脱除，完全省去了使用传统溶剂带来的复杂的后处理工序，因而仅有低VOC的特征。
中国专利文献 CN103951965A公开了以高压流体或者超临界流体为发泡剂制备TPU 发泡片材的方法。由于高压流体在TPU基体中扩散速度极快，该方法难以制备厚度仅为0.1～0.5毫米的人造革用发泡薄膜材料，而只能制备厚度较大的鞋垫等材料。另外，该方法为间歇方法，存在加工效率低的问题。
中国专利文献CN104385479A公开了超临界流体挤出发泡TPU树脂的方法，该方法采用超临界CO2为发泡剂，经连续挤出和水下切粒制备了TPU发泡珠粒，不过该方法不适于制备TPU发泡薄膜和TPU发泡革。
发明内容
因此，本发明的目的在于克服现有技术中的缺陷，提供一种热塑性聚氨酯发泡革的制备方法。
为了实现上述目的，本发明的一种热塑性聚氨酯发泡革的制备方法，使用以下重量份数的原料：
TPU树脂100份；
扩链剂1～3份；
气体阻隔剂为5～10份；
相容剂为1～3份；
成核剂为1～5份；
包括以下步骤：
1）按照上述质量份数将TPU树脂、扩链剂、气体阻隔剂、相容剂、成核剂进行干混；
2）将步骤1中的到的混合物加入挤出机的料筒中，经挤出机加热得到TPU熔体，将超临界N2以1～30毫升/分钟的速度注入到TPU熔体中，将TPU熔体与超临界N2混合均匀，混合后熔体经热交换器逐渐降低温度至155℃，再将混合后溶体经过狭缝口模挤出得到膨胀的TPU薄膜，挤出过程中所述挤出机的口模温度为140～160℃，挤出机口模的压力为5～25MPa；
3) TPU薄膜经过温度为130～160℃的单轴拉伸设备进行牵伸变薄，拉伸时间不超过15秒，制得TPU发泡薄膜，再将TPU发泡薄膜与布高温贴合，得到TPU发泡革。
所述步骤1中TPU树脂在190℃下的熔指为2.0～5.0g/10min。
所述步骤1中气体阻隔剂包括聚乙烯醇、聚偏氟乙烯中的至少一种；所述相容剂包括氢化热塑性丁苯橡胶-聚氨酯接枝物、氢化热塑性丁苯橡胶-热塑性聚氨酯共聚物、热塑性丁苯橡胶-甲基丙烯酸甲酯接枝物中的至少一种；所述扩链剂包括1，4-丁二醇；所述成核剂包括三氧化二氯、二氧化硅中的至少一种。
所述步骤2中所述挤出机的口模直径为0.3～0.8毫米。
所述步骤2中膨胀的TPU薄膜的厚度为0.5～1.2毫米。
所述步骤3中单轴拉伸设备有1组以上牵伸辊，牵伸辊的牵伸比为1.2～2.0。
所述步骤3中TPU发泡革中TPU发泡薄膜的厚度为0.3～0.8毫米。
所述步骤3中TPU发泡革中TPU发泡薄膜的密度为0.4～0.6g/cm3。
所述步骤3中TPU发泡革中TPU发泡薄膜的泡孔尺寸为50～150微米。
采用上述技术方案，本发明的热塑性聚氨酯发泡革的制备方法，选用清洁、廉价、环境友好的超临界流体为物理发泡剂，经过物理发泡和后牵伸定型等关键步骤，能够制备厚度为0.3～0.8毫米，密度为0.4～0.6g/cm3，泡孔尺寸为50～150微米的TPU微发泡薄膜材料，并且避免了TPU发泡革中TPU发泡薄膜密度较大、泡孔较大的缺陷。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明。
实施例1：
将100份熔指为3 g/10min的TPU树脂，2份扩链剂，6份包含有聚乙烯醇的阻隔剂母料，2份相容剂，2份成核剂在搅拌器中干混，将混合物加入挤出机的料筒中，经挤出机加热得到TPU熔体，将超临界N2以5毫升/分钟的速度注入到TPU熔体中，使TPU熔体与超临界N2混合均匀，混合熔体经热交换器逐渐降低温度至155度，混合熔体经过尺寸为0.4毫米的狭缝口模挤出得到膨胀的TPU薄膜混合料经挤出流延机的熔融挤出得到厚度为0.7～0.8毫米的TPU发泡薄膜；将TPU发泡薄膜经过温度为150度的单轴拉伸系统，经2组牵伸拉伸，贴布，裁边，得到厚度均匀的，膨胀程度均匀的TPU发泡革材料。测试表明，TPU发泡革中TPU发泡薄膜的厚度为0.4毫米，密度为0.45g/cm3，平均泡孔尺寸为120微米。
显然，上述实施例仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (9)

1.一种热塑性聚氨酯发泡革的制备方法，其特征在于，使用以下重量份数的原料：
TPU树脂100份；
扩链剂1～3份；
气体阻隔剂为5～10份；
相容剂为1～3份；
成核剂为1～5份；
包括以下步骤：
1）按照上述质量份数将TPU树脂、扩链剂、气体阻隔剂、相容剂、成核剂进行干混；
2）将步骤1中的到的混合物加入挤出机的料筒中，经挤出机加热得到TPU熔体，将超临界N2以1～30毫升/分钟的速度注入到TPU熔体中，将TPU熔体与超临界N2混合均匀，混合后熔体经热交换器逐渐降低温度至155℃，再将混合后溶体经过狭缝口模挤出得到膨胀的TPU薄膜，挤出过程中所述挤出机的口模温度为140～160℃，挤出机口模的压力为5～25MPa；
3) TPU薄膜经过温度为130～160℃的单轴拉伸设备进行牵伸变薄，拉伸时间不超过15秒，制得TPU发泡薄膜，再将TPU发泡薄膜与布高温贴合，得到TPU发泡革。
2.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于： 所述步骤1中TPU树脂在190℃下的熔指为2.0～5.0g/10min。
3.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤1中气体阻隔剂包括聚乙烯醇、聚偏氟乙烯中的至少一种；所述相容剂包括氢化热塑性丁苯橡胶-聚氨酯接枝物、氢化热塑性丁苯橡胶-热塑性聚氨酯共聚物、热塑性丁苯橡胶-甲基丙烯酸甲酯接枝物中的至少一种；所述成核剂包括三氧化二氯、二氧化硅中的至少一种；所述扩链剂包括1，4-丁二醇。
4.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤2中所述挤出机的口模直径为0.3～0.8毫米。
5.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤2中膨胀的TPU薄膜的厚度为0.5～1.2毫米。
6.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤3中单轴拉伸设备有1组以上牵伸辊，牵伸辊的牵伸比为1.2～2.0。
7.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤3中TPU发泡革中TPU发泡薄膜的厚度为0.3～0.8毫米。
8.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤3中TPU发泡革中TPU发泡薄膜的密度为0.4～0.6g/cm3。
9.如权利要求1所述的热塑性聚氨酯发泡革的制备方法，其特征在于：所述步骤3中TPU发泡革中TPU发泡薄膜的泡孔尺寸为50～150微米。
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