CN112962169B - 一种光谱发热阻燃抗菌多功能纤维及其制备方法 - Google Patents

一种光谱发热阻燃抗菌多功能纤维及其制备方法 Download PDF

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CN112962169B
CN112962169B CN202110204345.9A CN202110204345A CN112962169B CN 112962169 B CN112962169 B CN 112962169B CN 202110204345 A CN202110204345 A CN 202110204345A CN 112962169 B CN112962169 B CN 112962169B
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李圣军
张守运
孙燕琳
刘艳丽
钱婷婷
楼梦娜
杨卫星
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Zhejiang Tongkun New Material Research Institute Co ltd
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Abstract

本发明涉及一种光谱发热阻燃抗菌多功能纤维，其特征在于：包括含水率在30‑50ppm的复合母粒占重量百分比为10‑12％；含水率25ppm‑30ppm的PET或含水率50‑70ppm的PA高聚物占重量百分比为88‑90％。该纤维及其织物具有光谱发热、阻燃、抗菌、抗病毒等多重功能性，其织物与现有的织物对比，光照5‑10min，温差高出15‑20℃，远红外发射率大于98％，辐射升温大于3.0℃，克罗值大于0.5，传热系数大于18.0W/m2k，热阻小于0.05m2k/w，对大肠杆菌、金葡萄球、白念珠菌、肺炎杆菌的抑菌率均大于99.0％，对流感以及冠状病毒等具有较好的抗病毒效果。

Description

一种光谱发热阻燃抗菌多功能纤维及其制备方法
技术领域
本发明涉及纺织技术领域，具体涉及一种光谱发热阻燃抗菌多功能纤维及其制备方法。
背景技术
涤纶和锦纶是使用量最大的服装面料原料，其织物具有很好的强度和易洗效果，在纺织服装等民用领域应用分厂广泛，但是其在军工、防护服等特殊领域的应用却相对较少，需要对其性能进行大幅度的改进才能满足需要，产品的多功能化成为行业发展的制约瓶颈，但目前产品功能化率较低，而且由于不同改性剂同时添加使用，容易相互影响或发生团聚或发生反应，功能性降低，无法发挥综合功能性，同时传统的生产方法如改性剂添加种类和数量较多，纺丝难度大，容易飘丝断头，难以成纤。
发明内容
针对现有技术存在的不足，本发明的目的在于提供一种抗病毒效果好且辐射升温高且阻燃的光谱发热阻燃抗菌多功能纤维及其制备方法。
本发明的技术方案是这样实现的：一种光谱发热阻燃抗菌多功能纤维，其特征在于：包括含水率在30-50ppm的复合母粒占重量百分比为10-12％；含水率25ppm-30ppm的PET(聚对苯二甲酸丁二醇酯)或含水率50-70ppm的PA(聚酰胺)高聚物占重量百分比为88-90％。
优选为：所述复合母粒包括：占重量百分比为40-50％的含水率23ppm-27ppm 的PBT(聚对苯二甲酸丁二醇酯)；占重量百分比为6.7-10.0％的光谱发热剂远红外发射剂纳米级氧化钼；均占重量百分比为3.3-5.0％的抗菌与抗病毒剂纳米级氧化锌和纳米级氧化亚铜；占重量百分比为6.7-10.0％％的含水率25ppm-30ppm阻燃剂三聚氰胺磷酸酯。
通过采用上述技术方案，该纤维及其织物具有光谱发热、阻燃、抗菌、抗病毒等多重功能性，其织物与现有的织物对比，光照5-10min，温差高出15-20 ℃，远红外发射率大于98％，辐射升温大于3.0℃，克罗值大于0.5，传热系数大于18.0W/m2k，热阻小于0.05m2k/w，对大肠杆菌、金葡萄球、白念珠菌、肺炎杆菌的抑菌率均大于99.0％，对流感以及冠状病毒等具有较好的抗病毒效果，抗病毒活性值大于2.5，抗病毒活性率大于99.5％，极限氧指数大于35％，阴燃时间和续燃时间均为0，损坏长度90-100cm。
本发明同时公开了一种光谱发热阻燃抗菌多功能纤维的制备方法，其特征在于，包括如下步骤：
S1、改性剂处理：准备无机改性剂和有机改性剂，先对无机改性剂进行表面修饰；
S2、复合母粒制取：无机改性剂和有机改性剂依次通过球磨法机械搅拌，并且使用PBT(聚对苯二甲酸丁二醇酯)分别进行分层包覆处理，按照一定比例添加到母粒中熔融共混后制备出复合母粒；
S3、纤维制备：然后优化纺丝及加弹工艺制备出光谱发热阻燃抗菌多功能纤维。
优选为：所述无机改性剂包括纳米二氧化钼、纳米氧化锌、纳米氧化亚铜，有机改性剂包括三聚氰胺磷酸酯。
优选为：所述纳米二氧化钼、纳米氧化锌、纳米氧化亚铜的粉体平均粒径控制在100-400nm。
优选为：在步骤S1中，先对无机改性剂进行表面修饰是采用球磨法机械搅拌的方式对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌以及纳米氧化亚铜使用硬脂酸复配体表面修饰，对三聚氰胺磷酸酯使用旋喷等离子喷涂机进行ArC3H5低温等离子表面修饰。
优选为：在步骤S2中，无机改性剂和有机改性剂依次通过球磨法机械搅拌，并且使用PBT(聚对苯二甲酸丁二醇酯)分别进行分层包覆处理，是指采用球石研磨机分别对无机改性剂进行包覆，无机改性剂的粉体优先进行包覆且平均粒径小的无机改性剂的粉体优先包覆，有机改性剂的粉体最后包覆，有机改性剂的粉体按照热稳定性高低顺序包覆，并使无机改性剂和有机改性剂经PBT包覆后，均匀分散在PET(聚对苯二甲酸乙二醇酯)或PA6(聚己内酰胺6)熔体中，球石研磨机包覆温度265-275℃，每一改性剂加入后包覆时间30-50min，三聚氰胺磷酸酯最后加入包覆，PBT质量比占母粒总量的40-50％，各改性剂总量占母粒的20-30％，纳米二氧化钼：纳米氧化锌：纳米氧化亚铜：三聚氰胺磷酸酯为2：1：1：2。优化纺丝及加弹工艺，是指纺丝及假捻变形加工过程采用降低组件压力、生产速度、拉伸比、加热温度等以保证包覆结构的稳定性，避免不同的改性剂之间相互作用、发生反应或发生团聚等，保证各不同改性剂互不干扰，在确保多种功能性都能够满足使用要求的同时，保减少纺丝断头，提高可纺性；优化纺丝及加弹工艺，是指纺丝组件起始压力80-100kgf/cm2，纺丝和假捻变形加工速度比现有的织物降低20-30％，纺丝温度、假捻变形温度、假捻定性温度比现有的织物降低15-20℃，纺丝采用双道上油并且上油率提高40％，假捻变形加工过程上油提高10％，多重功能性复合母粒的添加量质量比占纺丝纤维总质量的10％-15％。
通过采用上述技术方案，采用纳米二氧化钼、纳米氧化锌、纳米氧化亚铜、三聚氰胺磷酸酯作为改性剂，首先对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌以及纳米氧化铜使用硬脂酸复配体和ArC3H5低温等离子表面修饰，提高其分散性，然后采用球磨法机械搅拌对上述各改性剂分次使用PBT分层包覆，并按照一定比例添加到母粒中制备出具有光致发热、红外保暖、阻燃、抗菌等多种功能性复合母粒，然后采用低温、低起始压力、低拉、双道上油等纺丝及假捻变形工艺制备具有光致发热、红外保暖、阻燃、抗菌、抗病毒等多种复合功能性一体化的功能性纤维。其中纳米二氧化钼收到光照后电子运动轨道发生跃迁，从而发出热量，具有较好的光谱发热效果，同时纳米二氧化钼在常态下，还具有较好发射红外线的功能，因此还具有远红外保暖的效果，纳米氧化锌、纳米氧化亚铜均具有抗菌效果，二者的复合应用，再控制好添加比例，对冠状病毒和流感病毒具有较好的抗病毒效果，三聚氰胺磷酸酯具有很好的阻燃性能，因此采用包覆复合方法把其性能综合应用，可制得可纺性好功能性强的多重功能性复合母粒，选择并控制好纺丝工艺和假捻变形工艺，可以制备出使用性能好的光致发热、红外保暖、阻燃、抗菌等多种复合功能性纤维。本发明只需在现有设备进行生产工艺优化，无需设备改造即可生产，有利于拓展涤纶和锦纶等应用空间，丰富并优化服装面料的轻质化和防护性能，有着显著的经济效益和社会效益。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种光谱发热阻燃抗菌多功能纤维，在本发明具体实施例中，包括含水率在30-50ppm的复合母粒占重量百分比为10-12％；含水率25ppm-30ppm的 PET(聚对苯二甲酸丁二醇酯)或含水率50-70ppm的PA(聚酰胺)高聚物占重量百分比为88-90％。
在本发明具体实施例中，所述复合母粒包括：占重量百分比为40-50％的含水率23ppm-27ppm的PBT(聚对苯二甲酸丁二醇酯)；占重量百分比为6.7-10.0％的光谱发热剂远红外发射剂纳米级氧化钼；均占重量百分比为3.3-5.0％的抗菌与抗病毒剂纳米级氧化锌和纳米级氧化亚铜；占重量百分比为6.7-10.0％％的含水率25ppm-30ppm阻燃剂三聚氰胺磷酸酯。
通过采用上述技术方案，该纤维及其织物具有光谱发热、阻燃、抗菌、抗病毒等多重功能性，其织物与现有的织物对比，光照5-10min，温差高出15-20 ℃，远红外发射率大于98％，辐射升温大于3.0℃，克罗值大于0.5，传热系数大于18.0W/m2k，热阻小于0.05m2k/w，对大肠杆菌、金葡萄球、白念珠菌、肺炎杆菌的抑菌率均大于99.0％，对流感以及冠状病毒等具有较好的抗病毒效果，抗病毒活性值大于2.5，抗病毒活性率大于99.5％，极限氧指数大于35％，阴燃时间和续燃时间均为0，损坏长度90-100cm。
实施例2
本发明同时公开了一种光谱发热阻燃抗菌多功能纤维的制备方法，其特征在于，包括如下步骤：
S1、改性剂处理：准备无机改性剂和有机改性剂，先对无机改性剂进行表面修饰；
S2、复合母粒制取：无机改性剂和有机改性剂依次通过球磨法机械搅拌，并且使用PBT(聚对苯二甲酸丁二醇酯)分别进行分层包覆处理，按照一定比例添加到母粒中熔融共混后制备出复合母粒；
S3、纤维制备：然后优化纺丝及加弹工艺制备出光谱发热阻燃抗菌多功能纤维。
在本发明具体实施例中，采用纳米二氧化钼、纳米氧化锌、纳米氧化亚铜、三聚氰胺磷酸酯作为改性剂，纳米二氧化钼、纳米氧化锌、纳米氧化亚铜粉体的平均粒径均控制在200nm、100nm、100nm，先采用球磨法机械搅拌，通过真空高温振动球磨机对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌、纳米氧化铜使用硬脂酸复配体进行表面修饰，采用旋喷式等离子喷涂机，使用ArC3H5对三聚氰胺磷酸酯低温等离子表面修饰，然后采用球磨法机械搅拌分次进行PBT包覆复合，按照制备复合母粒总质量的40％向真空高温振动球磨机内放入PBT切片，在搅拌的状态下升温至265℃，当PBT完全熔融后，按照制备复合母粒总量的3.3％向PBT加入纳米氧化锌粉体，高温球磨，机械搅拌40min后，加入复合母粒总量的3.3％的纳米氧化亚铜粉体，高温球磨，机械搅拌30min后，加入复合母粒总量的6.7％的纳米二氧化钼，球磨30min后，加入复合母粒总量的6.7％三聚氰胺磷酸酯，球磨30min，最后加入复合母粒总量的40％的PA6切片，球磨搅拌30min后，进行拉条、聚带、水冷，切粒制得有效成分20％的多重功能性复合母粒。
在现有的纺丝设备上，以PA6切片为原料，熔融添加15％的多重功能性母粒进行共混纺丝，纺丝温度250℃，纺丝速度3800m/min，制得52dtex/24f锦纶 6光谱发热阻燃抗菌纤维POY，然后在巴马格EFK-1000V型假捻变形机进行加弹后加工制得44dtex/24f锦纶6光谱发热阻燃抗菌多功能纤维DTY，其织物与常规44dtex/24f锦纶6纤维织物相比，在光照5min时温度差高出16℃，光照 10min时，温差高出18℃，远红外发射率98.3％，辐射升温3.2℃，克罗值0.53，传热系数18.6W/m2k，热阻0.048m2k/w对大肠杆菌、金葡萄球抑菌率均99.6％，白念珠菌抑菌率均99.3％、肺炎杆菌的抑菌率99.1％，对流感病毒抗病毒活性值2.5，抗病毒活性率99.5％，极限氧指数35.1％，阴燃时间和续燃时间均为0S，损坏长度93cm。
实施例3
在本发明具体实施例中，采用纳米二氧化钼、纳米氧化锌、纳米氧化亚铜、三聚氰胺磷酸酯作为改性剂，纳米二氧化钼、纳米氧化锌、纳米氧化亚铜粉体的平均粒径均控制在100nm、200nm、400nm，先采用球磨法机械搅拌，通过真空高温振动球磨机对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌、纳米氧化铜使用硬脂酸复配体进行表面你修饰，采用旋喷式等离子喷涂机，使用ArC3H5对三聚氰胺磷酸酯低温等离子表面修饰，然后采用球磨法机械搅拌分次进行PBT包覆复合，按照制备复合母粒总质量的50％向真空高温振动球磨机内放入PBT切片，在搅拌的状态下升温至275℃，当PBT完全熔融后，按照制备复合母粒总量的10.0％向PBT加入纳米二氧化钼粉体，高温球磨，机械搅拌50min后，再加入复合母粒总量的5.0％的纳米氧化锌粉体，高温球磨，机械搅拌40min后，加入复合母粒总量的5.0％的纳米氧化亚铜，球磨40min后，加入复合母粒总量的10.0％三聚氰胺磷酸酯，球磨32min，最后加入复合母粒总量的20％的PA6切片，球磨搅拌30min后，进行拉条、聚带、水冷，切粒制得30％多重功能性复合母粒。
在现有的纺丝设备上，以PA6切片为原料，熔融添加10％的多重功能性复合母粒进行共混纺丝，纺丝温度250℃，纺丝速度3800m/min，制得52dtex/24f 锦纶6光谱发热阻燃抗菌纤维POY，然后在巴马格Efk-1000V型假捻变形机进行加弹后加工制得44dtex/24f锦纶6光谱发热阻燃抗菌多功能纤维DTY，其织物与常规44dtex/24f锦纶6纤维织物相比，在光照5min时温度差高出17℃，光照10min时，温差高出20℃，远红外发射率99.0％，辐射升温3.5℃，克罗值0.56，传热系数19.8W/m2k，热阻0.036m2k/w对大肠杆菌、金葡萄球抑菌率均99.9％，白念珠菌抑菌率均99.6％、肺炎杆菌的抑菌率99.5％，对流感病毒抗病毒活性值3.6，抗病毒活性率99.8％，极限氧指数37.8％，阴燃时间和续燃时间均为0S，损坏长度90cm。
实施例4
采用纳米二氧化钼、纳米氧化锌、纳米氧化亚铜、三聚氰胺磷酸酯作为改性剂，纳米二氧化钼、纳米氧化锌、纳米氧化亚铜粉体的平均粒径均控制在 100nm、300nm、200nm，先采用球磨法机械搅拌，通过真空高温振动球磨机对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌、纳米氧化铜使用硬脂酸复配体进行表面你修饰，采用旋喷式等离子喷涂机，使用 ArC3H5对三聚氰胺磷酸酯低温等离子表面修饰，然后采用球磨法机械搅拌分次进行PBT包覆复合，按照制备复合母粒总质量的45％向真空高温振动球磨机内放入PBT切片，在搅拌的状态下升温至269℃，当PBT完全熔融后，按照制备复合母粒总量的8.0％向PBT加入纳米二氧化钼粉体，高温球磨，机械搅拌36min 后，加入复合母粒总量的4.0％的纳米氧化亚铜粉体，高温球磨，机械搅拌33min 后，加入复合母粒总量4.0％的氧化锌，球磨39min后，加入复合母粒总量的8.0％三聚氰胺磷酸酯，球磨33min,最后加入复合母粒总量的31％的PET切片，球磨搅拌37min后，进行拉条、聚带、水冷，切粒制得有效成份24％多重功能性复合母粒。
在现有的纺丝设备上，以PET切片为原料，熔融添加13％的多重功能性复合母粒进行共混纺丝，纺丝温度275℃，纺丝速度2500m/min，制得265dtex/48f 涤纶光谱发热阻燃抗菌纤维POY，然后在巴马格EFK-1000V型假捻变形机进行加弹后加工制得167dtex/48f涤纶光谱发热阻燃抗菌多功能纤维DTY，其织物与常规167dtex/48f涤纶纤维织物相比，在光照5min时温度差高出18℃，光照10min 时，温差高出20℃，远红外发射率99.0％，辐射升温3.5℃，克罗值0.55，传热系数18.9W/m2k，热阻小于0.037m2k/w对大肠杆菌、金葡萄球抑菌率均99.8％，白念珠菌抑菌率均99.5％、肺炎杆菌的抑菌率99.4％，对流感病毒抗病毒活性值3.9，抗病毒活性率99.7％，极限氧指数35.7％，阴燃时间和续燃时间均为0，损坏长度91cm。
实施例5
采用纳米二氧化钼、纳米氧化锌、纳米氧化亚铜、三聚氰胺磷酸酯作为改性剂，纳米二氧化钼、纳米氧化锌、纳米氧化亚铜粉体的平均粒径均控制在 150nm、200nm、270nm，先采用球磨法机械搅拌，通过真空高温振动球磨机对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米二氧化锌、纳米氧化铜使用硬脂酸复配体进行表面你修饰，采用旋喷式等离子喷涂机，使用 ArC3H5对三聚氰胺磷酸酯低温等离子表面修饰，然后采用球磨法机械搅拌分次进行PBT包覆复合，按照制备复合母粒总质量的28％向真空高温振动球磨机内放入PBT切片，在搅拌的状态下升温至272℃，当PBT完全熔融后，按照制备复合母粒总量的9.0％向PBT加入纳米二氧化钼粉体，高温球磨，机械搅拌40min 后，加入复合母粒总量的4.5％的纳米二氧化锌粉体，高温球磨，机械搅拌30min 后，再加入复合母粒总量的4.5％的纳米氧化亚铜，球磨34min后，加入复合母粒总量的9.0％三聚氰胺磷酸酯，球磨36min，最后加入复合母粒总量的28％的 PET切片，球磨搅拌38min后，进行拉条、聚带、水冷，切粒制得27％多重功能性复合母粒。
在现有的纺丝设备上，以PET切片为原料，熔融添加12％的多重功能性复合母粒进行共混纺丝，纺丝温度280℃，纺丝速度2700m/min，制得125dtex/772F 涤纶光谱发热阻燃抗菌纤维POY，然后在巴马格EFK-1000V型假捻变形机进行加弹后加工制得83dtex/72F涤纶光谱发热阻燃抗菌多功能纤维DTY，其织物与常规83dtex/72f涤纶纤维织物相比，在光照5min时温度差高出16℃，光照10min 时，温差高出19℃，远红外发射率98.6％，辐射升温3.3℃，克罗值0.55，传热系数18.9W/m2k，热阻小于0.042m2k/w对大肠杆菌、金葡萄球抑菌率均99.9％，白念珠菌抑菌率均99.5％、肺炎杆菌的抑菌率99.3％，对流感病毒抗病毒活性值2.9，抗病毒活性率99.4％，极限氧指数36.8％，阴燃时间和续燃时间均为0S，损坏长度96cm。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (4)

1.一种光谱发热阻燃抗菌多功能纤维，其特征在于：包括含水率在30-50ppm的复合母粒占重量百分比为10-12%；含水率25ppm-30ppm的聚对苯二甲酸丁二醇酯或含水率50-70ppm的聚酰胺高聚物占重量百分比为88-90%，所述复合母粒包括：占重量百分比为40-50%的含水率23ppm-27ppm的聚对苯二甲酸丁二醇酯；占重量百分比为6.7-10.0%的光谱发热剂远红外发射剂纳米级氧化钼；均占重量百分比为3.3-5.0%的抗菌与抗病毒剂纳米级氧化锌和纳米级氧化亚铜；占重量百分比为6.7-10.0%%的含水率25ppm-30ppm阻燃剂三聚氰胺磷酸酯；所述纳米二氧化钼是采用十二烷基苯磺酸表面活性剂进行表面修饰的，所述纳米氧化锌和纳米氧化亚铜是采用硬脂酸复配体进行表面修饰的，所述三聚氰胺磷酸酯是使用旋喷等离子喷涂机进行ArC3H5低温等离子进行表面修饰的。
2.一种适于上述权利要求1所述光谱发热阻燃抗菌多功能纤维的制备方法，其特征在于，包括如下步骤：
S1、改性剂处理：准备无机改性剂和有机改性剂，所述无机改性剂包括纳米二氧化钼、纳米氧化锌、纳米氧化亚铜，有机改性剂包括三聚氰胺磷酸酯，先对无机改性剂进行表面修饰；
S2、复合母粒制取：无机改性剂和有机改性剂依次通过球磨法机械搅拌，并且使用聚对苯二甲酸丁二醇酯分别进行分层包覆处理，是指采用球石研磨机分别对无机改性剂进行包覆，无机改性剂的粉体优先进行包覆且平均粒径小的无机改性剂的粉体优先包覆，有机改性剂的粉体最后包覆，有机改性剂的粉体按照热稳定性高低顺序包覆，并使无机改性剂和有机改性剂经聚对苯二甲酸丁二醇酯包覆后，均匀分散在聚对苯二甲酸乙二醇酯或聚己内酰胺6熔体中，球石研磨机包覆温度265-275℃，每一改性剂加入后包覆时间30-50min，三聚氰胺磷酸酯最后加入包覆，聚对苯二甲酸丁二醇酯质量比占母粒总量的40-50%，各改性剂总量占母粒的20-30%，纳米二氧化钼：纳米氧化锌：纳米氧化亚铜：三聚氰胺磷酸酯为2：1：1：2；
S3、纤维制备：然后优化纺丝及加弹工艺制备出光谱发热阻燃抗菌多功能纤维。
3.根据权利要求2所述的一种光谱发热阻燃抗菌多功能纤维的制备方法，其特征在于：所述纳米二氧化钼、纳米氧化锌、纳米氧化亚铜的粉体平均粒径控制在100-400nm。
4.根据权利要求2或3所述的一种光谱发热阻燃抗菌多功能纤维的制备方法，其特征在于：在步骤S1中，先对无机改性剂进行表面修饰是采用球磨法机械搅拌的方式对纳米二氧化钼使用十二烷基苯磺酸表面活性剂表面修饰，对纳米氧化锌以及纳米氧化亚铜使用硬脂酸复配体表面修饰，对三聚氰胺磷酸酯使用旋喷等离子喷涂机进行ArC3H5低温等离子表面修饰。
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