CN111485325A - 一种耐高温的抗菌纳米纤维无纺布及其制备方法和用途 - Google Patents
一种耐高温的抗菌纳米纤维无纺布及其制备方法和用途 Download PDFInfo
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Abstract
一种耐高温的抗菌纳米纤维无纺布及其制备方法和用途。无纺布由51%~98.5wt.%的丁烯聚合物,0.05%~5wt.%的抑菌剂,0.05%~5wt.%的防老剂,0.05%~5wt.%的抗静电剂,0%~2wt.%的染色剂,0%~2wt.%的表面活性剂,0%~30wt.%的无机填料组成。无纺布由直径100~1000nm的超细纤维多层无序排列组成,厚度为5μm~1cm,无纺布对真菌、细菌、病毒有抑制和消杀作用,除菌率达到99.99%,病毒抑制率达到99.99%。该无纺布采用熔融静电纺丝制备。
Description
技术领域
本发明属于聚合物超细纤维无纺布领域,涉及静电纺丝制备技术,具体涉及一种丁烯聚合物纳米纤维无纺布及其制备方法和用途。
背景技术
高等规聚丁烯是一种半结晶性聚烯烃材料,具有突出的耐热蠕变、耐应力开裂、高的耐热温度、高韧性等特点。以高等规聚丁烯为主的聚烯烃合金(釜内合金和物理共混物)不仅兼具聚丁烯的优点,同时也具备另外一种聚烯烃的特点。聚丁烯主要用于管材,也可以应用于薄膜材料领域。
静电纺丝技术是目前制备纳米纤维最为简单有效的方法,其制得的纤维直径可在10nm~1000nm之间。在静电纺丝(电纺)工艺过程中,外界高压电场作用于聚合物熔体或液体,带电的聚合物液滴或熔滴在电场力的作用下克服表面张力形成带有电荷的喷射细流。聚合物喷射细流在空中由于拉伸作用形成多种形式的不稳定流动,进而被高倍拉伸,并在接收装置上形成聚合物纤维。相对于一般方法制得的纤维,电纺纤维具有极大的比表面积和空隙率,相同体积下具有极轻的体积,特别适合作为药物载体、过滤分离材料、催化剂负载载体、导电、导热和隔离材料使用,有广泛的应用前景。到目前为止,已有超过200种高分子材料通过静电纺丝制成纤维产品。
美国专利US20030215624和US20040013873、中国发明专利201010505164.1和201010130867.0公开了多种聚合物包括:聚乙烯、聚丙烯、聚乙烯醇、聚苯乙烯、聚砜、聚碳酸酯、聚氨酯、聚甲基丙烯酸甲酯、聚氯乙烯、聚酰胺、聚乙烯吡咯烷酮、聚氧化乙烯等的电纺纤维。中国发明专利CN 105926156A报道了一种多孔结构的反式橡胶超细纤维无纺布的制备,得到不同形貌的超细纤维组成的多孔无纺布,可以应用于分离过滤、催化剂载体、保温和防护等领域。但二烯烃类的反式橡胶由于双键的存在,其耐溶剂性、耐老化性能和使用寿命有限制。虽然中国发明专利CN 103741230A报道了将反式橡胶纤维硫化,可以提高其耐溶剂性,但橡胶纤维中仍会存在大量易老化的双键。
现有静电纺丝纤维及无纺布主要集中在形貌控制、过滤材料、保温和光电材料制备等领域,尚未见有报道除菌抑病毒超细纤维无纺布。同时大部分材料的耐热温度较低,不适用于高温消毒操作。为了克服和解决上述提及的超细微纳米纤维存在的问题,本发明提供一种丁烯聚合物纳米纤维无纺布及其制备方法和应用。通过该方法制备的多孔的丁烯聚合物纳米纤维无纺布,具有较大的孔隙率和比表面积,较高的耐热温度,同时载有抗菌抑病毒填充剂,预计可以在医疗卫生、家居装饰、过滤材料、包装场合,具有过滤和抑菌作用。
发明内容
本发明的目的之一是提供一种丁烯聚合物为基体的具有较高耐热温度的纳米纤维无纺布,可适用于较高温度的消毒操作。
本发明的目的之二是提供一种具有抗菌抑病毒作用的纳米纤维无纺布,可以在医疗卫生、家居装饰、过滤材料、包装场合使用。
本发明的目的之三是提供一种超轻、高孔隙率、高吸附能力的纳米纤维无纺布,可以提高吸附能力,降低单位体积的产品质量。
本发明的目的之四是提供这种耐高温的抗菌纳米纤维无纺布的制备方法。
本发明的耐高温的抗菌纳米纤维无纺布,按重量百分比计,无纺布中丁烯聚合物占51~98.5%,抑菌剂占0.05~5%,防老剂占0.05~5%,抗静电剂占0.05~5%,染色剂占0~2%,表面活性剂占0~2%,无机填料占0~30%。
本发明提供的耐高温的抗菌纳米纤维无纺布,其中,超细纤维无纺布的厚度为5μm~1cm,无纺布为多孔结构,孔隙率45%~65%,比表面积320~480m2/g,无纺布由直径100~1000nm的纳米纤维多层无序排列组成。本发明提供的耐高温的抗菌纳米纤维无纺布,丁烯聚合物的熔融指数0.01~120g/10min(190℃,2.16kg),选自聚丁烯、聚丁烯/聚丙烯釜内合金,聚丁烯/聚乙烯釜内合金,聚丁烯/聚苯乙烯釜内合金,聚丁烯/聚丙烯物理共混物,聚丁烯/聚乙烯物理共混物、聚丁烯/聚苯乙烯物理共混物中的一种。在以上的丁烯聚合物中,丁烯单体单元含量为80~100wt.%,聚丁烯、聚丙烯的等规度为85~99wt.%,聚苯乙烯为无规聚苯乙烯。
本发明提供的耐高温的抗菌纳米纤维无纺布,通过加入消毒抑菌剂,如纳米银、金属氧化物、金属氧酸盐中的一种或两种以上,其中金属氧化物为氧化锌、氧化银、氧化钛、氧化汞、氧化铜、氧化亚铜、氧化镍、氧化钴、氧化铁中的一种或两种以上,金属氧酸盐为单金属氧酸盐、双金属氧酸盐、多金属氧酸盐中的一种或两种以上。
本发明的无纺布中,添加的防老剂为2,6-二叔丁基对甲酚、三(3,5-二叔丁基-4-羟基苄基)异氰酸酯、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、十八烷基-3,5-双(1,1-二甲基乙基)-4-羟基苯丙酸酯、N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮、亚磷酸三(2,4-二叔丁基苯基)酯、双(2,4-二叔丁基苯酚)季戊四醇二亚磷酸酯、3,9-二(2,4-二枯基苯氧基)-2,4,8,10-四氧杂-3,9-二磷杂螺[5.5]十一烷、硫代二丙酸双十八醇酯、硫代二丙酸双十四醇酯、硫代二丙酸双十三醇酯中的一种或两种以上。
本发明中所述的抗静电剂为季铵盐、磷酸盐、磺酸盐、脂肪酸、多元醇酯、聚氧化乙烯、丙胺酸盐、聚丙烯酸及其衍生物中的一种或两种以上;所述的染色剂为氧化钛、苏木精、洋红、刚果红、品红、甲基蓝、固绿、苏丹红、结晶紫、龙胆紫、美蓝、甲基绿、硫酸铜中的一种或两种以上;所述的表面活性剂为碱金属皂、碱土金属皂、有机胺皂、烷基硫酸钠、烷基磺酸钠、季铵盐、聚氧乙烯-聚氧丙烯共聚物、聚氧乙烯及其衍生物、吐温、司盘、脂肪酸甘油酯中的一种或两种以上;所述的无机填料为碳酸钙、碳酸镁、磷酸钙、磷酸镁、磷氢酸钙、氢氧化镁、氢氧化钙、二氧化硅、陶土、滑石粉、云母粉、蒙脱土、高岭土、海泡石、羟基磷灰石中的一种或两种以上。
本发明的一种耐高温的抗菌纳米纤维无纺布的制备方法,包括以下步骤:
(1)将丁烯聚合物、抑菌剂、防老剂、抗静电剂、染色剂、表面活性剂及无机填料在双螺杆挤出机中熔融共混,造粒,制成无纺布专用料;
(2)将步骤(1)的无纺布专用料加入静电纺丝设备料筒内,控制料筒温度为180~240℃,设置静电纺丝设备两极间距离为5~50cm,两极间施加电压为10~60kV,纺丝液推进速度为10~200μL/h;纺丝环境温度为20~60℃,纺丝环境湿度为10~80%,纺丝0.1~48h,得到由超细纤维组成的无纺布;
(3)步骤(2)得到的超细纤维无纺布在真空干燥箱中20~40℃真空干燥至恒重。
本发明的耐高温的抗菌纳米纤维无纺布,也可以采用以下步骤制备:
(1)将丁烯聚合物、抑菌剂、防老剂、抗静电剂、染色剂、表面活性剂及无机填料在高速搅拌机中混合均匀,得到匀混物,混合温度为0~40℃,搅拌机转速为100~1000rpm,混合时间为5~10min;然后共混挤出造粒,得到无纺布专用料;
(2)将步骤(1)得到的专用料置于静电纺丝设备的熔融腔,熔融10~50min,熔融温度为128℃~210℃;设置静电纺丝设备两极间距离为5~50cm,两极间施加电压为10~60kV,纺丝熔融液供料推进速度为10~200μL/h;纺丝环境温度为20~60℃,纺丝环境湿度为10~80%;纺丝0.1~48h得到由超细纤维组成的无纺布;
(3)步骤(2)得到的超细纤维无纺布在真空干燥箱中20~40℃真空干燥至恒重。
采用本发明提供的方法制备的耐高温的抗菌纳米纤维无纺布,所述的金属氧化物和/或金属氧酸盐加入到无纺布中,对真菌、细菌、病毒有抑制和消杀作用,除菌率达到99.99%,病毒抑制率达到99.99%。
本发明所述的丁烯聚合物作为无纺布的基体材料,具有高的热变形温度,可适用于更高温度的消毒操作。采用本发明提供的方法制备的耐高温的抗菌纳米纤维无纺布,孔隙率高,透气性高;比表面积大,有利于静电吸附尘埃,阻隔细菌和病毒;质量轻,节省成本;应用于医疗卫生、家居装饰、过滤材料、包装等领域,具有过滤和抑菌作用;特别是用于制作口罩、隔离服,起到透气、阻隔和吸附病毒及细菌的作用。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
除菌率和病毒抑制率:除菌率采用金黄色葡萄球菌菌落计数法表征,病毒抑制率采用流感病毒MTT测试。实施例中采用的聚合物具体参数如下:
聚丁烯:乙醚抽提等规度98wt.%,熔融指数25.2g/10min(190℃,2.16kg);
聚丁烯/聚丙烯釜内合金:熔融指数15.3g/10min,丁烯单体单元含量为95wt.%,乙醚抽提等规度97wt.%;聚丁烯/聚乙烯釜内合金:熔融指数20.1g/10min,丁烯单体单元含量为80wt.%,乙醚抽提等规度96wt.%;聚丁烯/聚苯乙烯物理共混物:其中聚丁烯的乙醚抽提等规度98wt.%,聚丁烯含量为85wt.%,熔融指数10.2g/10min(190℃,2.16kg);聚苯乙烯为无规聚苯乙烯,熔融指数22.5g/10min。
实施例1
1)将聚丁烯、纳米银(抑菌剂)、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(防老剂1)、亚磷酸三(2,4-二叔丁基苯基)酯(防老剂2)、硬脂酸(抗静电剂)、氧化钛(染色剂)、十二烷基苯磺酸钠(表面活性剂)、碳酸钙(填料)按照表1的配方在双螺杆挤出机中共混,造粒,制成无纺布专用料;
2)将上述无纺布专用料加入到静电纺丝设备料筒内,控制料筒温度200℃,设置静电纺丝设备两极间距离为20cm,两极间施加电压为60kV,纺丝液推进速度为200μL/h;纺丝环境温度为40℃,纺丝环境湿度为40%,纺丝0.5h,得到由聚丁烯超细纤维组成的无纺布;置于真空干燥箱中40℃干燥至恒重。
对制备的聚丁烯超细纤维无纺布进行测试,结果列于表1。
对比例1
除了未使用抑菌剂,其他同实施例1。对制备的超细纤维无纺布进行测试,结果列于表1。
实施例2
将聚丁烯/聚丙烯釜内合金、Na7PMo11MnO40(抑菌剂)、十八烷基-3,5-双(1,1-二甲基乙基)-4-羟基苯丙酸酯(防老剂1)、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(防老剂2)、十二烷基三甲基氯化铵(抗静电剂)、甲基蓝(染色剂)、十八烷基硫酸钠(表面活性剂)、二氧化硅(填料)按照表1的配方在双螺杆挤出机中共混,造粒,制成无纺布专用料。
其他同实施例1。对制备的超细纤维无纺布进行测试,结果列于表1。
实施例3
除了使用的丁烯聚合物为聚丁烯/聚乙烯釜内合金,纺丝时间为4h外,其他同实施例2。
对制备的超细纤维无纺布进行测试,结果列于表1。
实施例4
1)将聚丁烯/聚苯乙烯物理共混物、Na7PMo11MnO40(抑菌剂)、十八烷基-3,5-双(1,1-二甲基乙基)-4-羟基苯丙酸酯(防老剂1)、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(防老剂2)、十二烷基三甲基氯化铵(抗静电剂),按照表1的配方在双螺杆挤出机中共混,造粒,制成无纺布专用料;
2)将上述无纺布专用料加入到静电纺丝设备熔融腔,在210℃下熔融50min,设置静电纺丝设备两极间距离为50cm,两极间施加电压为40kV,纺丝液推进速度为100μL/h;纺丝环境温度为40℃,纺丝环境湿度为60%,纺丝10h,得到由超细纤维组成的无纺布;置于真空干燥箱中40℃干燥至恒重。
对制备的超细纤维无纺布进行测试,结果列于表1。
实施例5
除了纺丝时纺丝电压为60kV外,其他同实施例1。对制备的超细纤维无纺布进行测试,结果列于表1。
实施例6
除了抑菌剂纳米银的含量为3%外,其他同实施例1。对制备的超细纤维无纺布进行测试,结果列于表1。
表1实施例和对比例的配方及性能
Claims (10)
1.一种耐高温的抗菌纳米纤维无纺布,其特征在于,无纺布中丁烯聚合物占51wt.%~98.5wt.%,抑菌剂占0.05wt.%~5wt.%,防老剂占0.05wt.%~5wt.%,抗静电剂占0.05wt.%~5wt.%,染色剂占0wt.%~2wt.%,表面活性剂占0wt.%~2wt.%,无机填料占0wt.%~30wt.%。
2.根据权利要求1所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的无纺布由直径100~1000nm的超细纤维多层无序排列组成,无纺布的厚度为5μm~1cm。
3.根据权利要求1和2任一所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的丁烯聚合物在190℃,2.16kg下测试的熔融指数0.01~120g/10min,选自聚丁烯、聚丁烯/聚丙烯釜内合金,聚丁烯/聚乙烯釜内合金,聚丁烯/聚苯乙烯釜内合金,聚丁烯/聚丙烯物理共混物,聚丁烯/聚乙烯物理共混物、聚丁烯/聚苯乙烯物理共混物中的一种。
4.根据权利要求1和3任一所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的丁烯聚合物中丁烯单体单元含量为80~100wt.%,聚丁烯、聚丙烯的等规度为85~99wt.%,聚苯乙烯为无规聚苯乙烯。
5.根据权利要求1所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的抑菌剂为纳米银、金属氧化物、金属氧酸盐中的一种或两种以上,其中金属氧化物为氧化锌、氧化银、氧化钛、氧化汞、氧化铜、氧化亚铜、氧化镍、氧化钴、氧化铁中的一种或两种以上,金属氧酸盐为单金属氧酸盐、双金属氧酸盐、多金属氧酸盐中的一种或两种以上;所述的防老剂为2,6-二叔丁基对甲酚、三(3,5-二叔丁基-4-羟基苄基)异氰酸酯、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、十八烷基-3,5-双(1,1-二甲基乙基)-4-羟基苯丙酸酯、N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)-1,3,5-三嗪-2,4,6-(1H,3H,5H)-三酮、亚磷酸三(2,4-二叔丁基苯基)酯、双(2,4-二叔丁基苯酚)季戊四醇二亚磷酸酯、3,9-二(2,4-二枯基苯氧基)-2,4,8,10-四氧杂-3,9-二磷杂螺[5.5]十一烷、硫代二丙酸双十八醇酯、硫代二丙酸双十四醇酯、硫代二丙酸双十三醇酯中的一种或两种以上;所述的抗静电剂为季铵盐、磷酸盐、磺酸盐、脂肪酸、多元醇酯、聚氧化乙烯、丙胺酸盐、聚丙烯酸及其衍生物中的一种或两种以上;所述的染色剂为氧化钛、苏木精、洋红、刚果红、品红、甲基蓝、固绿、苏丹红、结晶紫、龙胆紫、美蓝、甲基绿、硫酸铜中的一种或两种以上;所述的表面活性剂为碱金属皂、碱土金属皂、有机胺皂、烷基硫酸钠、烷基磺酸钠、季铵盐、聚氧乙烯-聚氧丙烯共聚物、聚氧乙烯及其衍生物、吐温、司盘、脂肪酸甘油酯中的一种或两种以上;所述的无机填料为碳酸钙、碳酸镁、磷酸钙、磷酸镁、磷氢酸钙、氢氧化镁、氢氧化钙、二氧化硅、陶土、滑石粉、云母粉、蒙脱土、高岭土、海泡石、羟基磷灰石中的一种或两种以上。
6.一种耐高温的抗菌纳米纤维无纺布的制备方法,包括以下步骤:
(1)将丁烯聚合物、抑菌剂、防老剂、抗静电剂、染色剂、表面活性剂及无机填料在双螺杆挤出机中熔融共混,造粒,制成无纺布专用料;
(2)将步骤(1)的无纺布专用料加入静电纺丝设备料筒内,控制料筒温度为180~240℃,设置静电纺丝设备两极间距离为5~50cm,两极间施加电压为10~60kV,纺丝液推进速度为10~200μL/h;纺丝环境温度为20~60℃,纺丝环境湿度为10~80%,纺丝0.1~48h,得到由超细纤维组成的无纺布;
(3)步骤(2)得到的超细纤维无纺布在真空干燥箱中20~40℃真空干燥至恒重。
7.一种耐高温的抗菌纳米纤维无纺布的制备方法,包括以下步骤:
(1)将丁烯聚合物、抑菌剂、防老剂、抗静电剂、染色剂、表面活性剂及无机填料在高速搅拌机中混合均匀,得到匀混物,混合温度为0~40℃,搅拌机转速为100~1000rpm,混合时间为5~10min;然后共混挤出造粒,得到无纺布专用料;
(2)将步骤(1)得到的专用料置于静电纺丝设备的熔融腔,熔融10~50min,熔融温度为128℃~210℃;设置静电纺丝设备两极间距离为5~50cm,两极间施加电压为10~60kV,纺丝熔融液供料推进速度为10~200μL/h;纺丝环境温度为20~60℃,纺丝环境湿度为10~80%;纺丝0.1~48h得到由超细纤维组成的无纺布;
(3)步骤(2)得到的超细纤维无纺布在真空干燥箱中20~40℃真空干燥至恒重。
8.根据权利要求1、5任一所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的抑菌剂加入到无纺布中,对真菌、细菌、病毒有抑制和消杀作用,除菌率达到99.99%,病毒抑制率达到99.99%。
9.根据权利要求1、2任一所述的一种耐高温的抗菌纳米纤维无纺布,其特征在于,所述的丁烯聚合物作为无纺布的基体材料,具有高的热变形温度,可适用于更高温度的消毒操作。
10.根据权利要求1、2、5任一所述的耐高温的抗菌纳米纤维无纺布,其特征在于,孔隙率高,透气性高;比表面积大,有利于静电吸附尘埃,阻隔细菌和病毒;质量轻,节省成本;应用于医疗卫生、家居装饰、过滤材料、包装等领域,具有过滤和抑菌作用;特别是用于制作口罩、隔离服,起到透气、阻隔和吸附病毒及细菌的作用。
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