CN106048778B - 一种多孔吸附纤维及其制备方法 - Google Patents
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Abstract
本发明一种多孔吸附纤维,多孔吸附纤维是由聚酯,金属‑有机框架材料,醋酸丁酸纤维素制备而成,其中聚酯80~99.85%、金属‑有机框架材料0.05~19.9%、醋酸丁酸纤维素0.1~5%;制备多孔吸附纤维的方法是首先将金属‑有机框架材料,醋酸丁酸纤维素混合均匀得到多孔载体材料,然后将聚酯与多孔载体材料混合均匀用纺丝机进行熔融纺丝处理,得到多孔复合纤维,将多孔复合纤维依次浸渍于丙酮溶剂与吸附溶剂中,然后漂洗、干燥,即制备得到多孔吸附纤维。该种方法制备多孔吸附纤维生产工艺简单,成本低廉,具有较大的应用前景。
Description
技术领域
本发明涉及功能纺能材料领域,尤其涉及一种多孔吸附纤维及其制备方法。
背景技术
多孔吸附纤维材料指纤维表面存在大量的孔洞结构,而具有的吸附功能型药物的纤维材料。目前制备多孔吸附纤维的主要方法有两相分离法、熔融法。金属-有机框架材料,是指金属离子与有机配体通过自组装形成周期性网络的多孔材料,具有孔隙率高、比表面积大、孔道规则、粒径可控等优点,广泛应用于医疗、吸附、催化、储能等领域。
中国发明专利(公开号105199739A,公开日为2015年12月30日),公开了一种自修复多孔纤维的制备方法,首先利用废旧棉布以及枯黄植物制备改性纤维素,其次进行发泡处理得到内部多孔的纤维体,最后利用内部多孔的纤维体制备自修复多孔纤维。该发明先在废旧棉布、枯黄植物中提取改性纤维素,然后利用气体发泡技术,将纤维素制备成多孔纤维。该制备方法存在着工艺复杂、制备出的纤维机械性能差,应用范围有限等缺点。
中国发明专利(公开号104275165A,公开日为2015年1月14日)公开了一种介孔离子式吸附无纺布的制备方法,该制备方法经过多孔硅酸钙粉体的离子改性、离子改性多孔硅酸钙粉体分散溶液的制备、聚烯烃无纺布的浸轧、浸轧无纺布的离子式吸附活化后制备出介孔离子式吸附无纺布。该制备方法工艺复杂、影响无纺布的手感、且改性硅酸钙粉体容易脱落,应用范围难以推广等缺点。
发明内容
本发明的目的就是针对上述技术的不足,提供一种工艺简单,成本低廉,制备得到多孔吸附纤维及其制备方法。
为实现上述目的,本发明采用的技术方案是:
一种多孔吸附纤维是由聚酯,金属-有机框架材料,醋酸丁酸纤维素制备而成;其中金属-有机框架材料是一种新型的有机材料,具有孔隙率高、比表面积大、孔道规则、粒径可控等优点,将金属-有机框架材料引入吸附纤维的制作中,制得的功能化载体纤维具有孔隙率大,吸附能力强的特点。本发明采用聚酯、醋酸丁酸纤维素(CAB)、金属-有机框架材料进行熔融共混纺丝的方法,制备一种多孔吸附纤维。由于CAB易溶于丙酮,当CAB与聚酯、金属-有机框架材料制备成纤维后,经过丙酮浸渍后,CAB易被丙酮提取掉,如此在纤维表面、内部就形成微米尺寸的孔,增大了纤维的比表面积;另外由于金属有机框架材料尺寸小,孔洞在微纳尺寸,对聚酯纤维的纺丝性能及力学性能不会有较大的影响。
所述多孔吸附纤维由聚酯80~99.85%、金属-有机框架材料0.05~19.9%、醋酸丁酸纤维素0.1~5%制备而成。由于选用了以上比例,聚酯含量80~99.85%,可以保证聚酯纤维的力学性能,金属-有机框架材料0.05~19.9%,醋酸丁酸纤维素0.1~5%可以保证制备出的聚酯纤维有较大的孔隙率。
所述聚酯为聚对苯二甲酸乙二醇酯,聚对苯二甲酸丙二醇酯,聚对苯二甲酸丁二醇酯中的一种;所述金属-有机框架材料为粉末状,粒径目数为2000~10000目,该粒径的金属-有机框架材料符合纺丝要求;所述金属-有机框架材料的结构为类沸石咪唑骨架型(ZIFs),莱瓦希尔骨架型(MILs),孔、通道式骨架型(PCNs)中的一种。
一种多孔吸附纤维的制备方法,包括以下步骤:
a)多孔复合纤维的制备
按重量百分比计,将金属-有机框架材料0.05~19.9%,醋酸丁酸纤维素0.1~5%混合均匀得到多孔载体材料,将聚酯80~99.85%与多孔载体材料混合均匀投入纺丝机中进行熔融纺丝处理,得到多孔复合纤维。
b)多孔吸附纤维的制备
将多孔复合纤维依次浸渍于丙酮与功能型吸附溶剂中,然后置于清水中,漂洗、干燥,即制备得到多孔吸附纤维;
本发明优选的多孔吸附纤维的制备方法,包括以下步骤:
a)多孔复合纤维的制备
按重量百分比计,称量原料金属-有机框架材料0.05~19.9%,醋酸丁酸纤维素(CAB)0.1~5%,混合均匀得到多孔载体材料,称量聚酯80~99.85%,聚酯与多孔载体材料混合均匀投入纺丝机中进行熔融纺丝处理,得到多孔复合纤维,所述的熔融纺丝的喷丝板为中空性、单组份圆形、三角形、六角形中的一种;
b)多孔吸附纤维的制备
将多孔复合纤维浸渍于丙酮溶剂,浸渍时间为30~60min,浸渍温度为20~50℃,洗净丙酮,干燥后,再将纤维置于功能型吸附溶剂中进行吸附,吸附时间为20~60min,吸附温度为20~50℃,然后置于清水中,漂洗、干燥,即制备得到多孔吸附纤维;
所述功能型吸附溶剂为:银离子溶剂,卤胺类溶液,超疏水整理剂,超亲水整理剂,阻燃整理剂中的一种。
所述聚酯为聚对苯二甲酸乙二醇酯(PET),聚对苯二甲酸丙二醇酯(PBT),聚对苯二甲酸丁二醇酯(PTT)中的一种;所述金属-有机框架材料为粉末状,粒径目数为2000~10000目;所述金属-有机框架材料的结构为类沸石咪唑骨架型(ZIFs),莱瓦希尔骨架型(MILs),孔、通道式骨架型(PCNs)中的一种。
本发明的有益效果:本发明采用聚酯、金属-有机框架材料、醋酸丁酸纤维素(CAB),共混纺丝,然后进过浸渍处理,制备得到多孔吸附纤维。用该方法制备出来的多孔吸附纤维具有孔洞呈现微纳尺寸结构特点,孔隙率大、吸附能力强;根据对这种较好的吸附效果,可制备得到抗菌纤维、抗静电纤维、超疏水纤维等功能化纤维;且生产工艺简单、机械性能优异,适合大规模应用。
具体实施方式
实施例1制备多孔吸附纤维A
a)多孔复合纤维的制备
按重量百分比计,称量粒径为2000目的MILs型的金属-有机框架材料0.05%,醋酸丁酸纤维素(CAB)0.1%,混合均匀得到多孔载体材料,称量聚酯99.85%,聚酯PET与多孔载体材料混合均匀,在纺丝机上进行熔融纺丝,纺丝组件为单组份圆形,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)多孔吸附纤维的制备
将多孔复合纤维浸渍于丙酮溶剂中浸渍60min,浸渍温度为20℃,然后置于清水中,漂洗、干燥,即制备得到多孔吸附纤维A。
实施例2制备抗菌型多孔吸附纤维B
a)多孔复合纤维的制备
按重量百分比计,称量粒径为4000目的ZIFs型的金属-有机框架材料0.6%,醋酸丁酸纤维素(CAB)0.4%,混合均匀得到多孔载体材料,称量聚酯PBT99%,聚酯PBT与多孔载体材料混合均匀,在纺丝机上进行熔融纺丝,纺丝组件为中空型,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)抗菌型多孔吸附纤维的制备
将多孔复合纤维先浸渍于丙酮溶剂,浸渍时间为30min,浸渍温度为50℃,洗净丙酮,干燥后,再将纤维置于质量百分浓度为5%的银离子溶剂中分别浸渍20min,浸渍温度为30℃,然后置于清水中,漂洗、干燥,即制备得到抗菌型多孔吸附纤维B。
实施例3制备抗菌型多孔吸附纤维C
a)多孔复合纤维的制备
按重量百分比计,称量粒径为6000目的PCNs型的金属-有机框架材料3.5%,醋酸丁酸纤维素(CAB)1.5%,混合均匀得到多孔载体材料,称量聚酯PTT95%,聚酯PTT与多孔载体材料混合均匀,在纺丝机上进行熔融纺丝,纺丝组件为三角形,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)抗菌型多孔吸附纤维的制备
将多孔复合纤维先浸渍于丙酮溶剂,浸渍时间为40min,浸渍温度为40℃,洗净丙酮,干燥后,再将纤维置于活性氯的含量为10000ppm氯胺类溶液中分别浸渍30min,浸渍温度为40℃,然后置于清水中,漂洗、干燥,即制备得到抗菌型多孔吸附纤维C。
实施例4制备疏水型多孔吸附纤维D
a)多孔复合纤维的制备
按重量百分比计,称量粒径为8000目的PCNs型的金属-有机框架材料5%,醋酸丁酸纤维素(CAB)5%,混合均匀得到多孔载体材料,称量聚酯PTT90%,聚酯PTT与多孔载体材料混合均匀,在纺丝机上进行熔融纺丝,纺丝组件为六角形,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)超疏水型多孔吸附纤维的制备
将多孔复合纤维先浸渍于丙酮溶剂,浸渍时间为50min,浸渍温度为50℃,洗净丙酮,干燥后,再将纤维置于生态无氟超疏水整理剂中分别浸渍50min,浸渍温度为50℃,然后置于清水中,漂洗、干燥,即制备超疏水型多孔吸附纤维D。
实施例5制备亲水型多孔吸附纤维E
a)多孔复合纤维的制备
按重量百分比计,称量粒径为10000目的PCNs型金属-有机框架材料19.9%,醋酸丁酸纤维素(CAB)0.1%,混合均匀得到多孔载体材料,称量聚酯PTT80%,聚酯PTT与多孔载体材料混合均匀,在纺丝机上进行熔融纺丝,纺丝组件为六角形,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)亲水型多孔吸附纤维的制备
将多孔复合纤维先浸渍于丙酮溶剂,浸渍时间为60min,浸渍温度为50℃,洗净丙酮,干燥后,再将纤维置于聚丙烯酸钠类亲水整理剂中分别浸渍60min,浸渍温度为50℃,然后置于清水中,漂洗、干燥,即制备亲水型多孔吸附纤维E。
实施例6制备阻燃型多孔吸附纤维F
a)多孔复合纤维的制备
按重量百分比计,称量粒径为10000目的PCNs型金属-有机框架材料19.9%,醋酸丁酸纤维素(CAB)0.1%,混合均匀得到多孔载体材料,称量聚酯PTT80%,聚酯PTT与多孔载体材料,在纺丝机上进行熔融纺丝,纺丝组件为六角形,纺丝温度为280℃,进行卷绕收集,得到多孔复合纤维;
b)燃型多孔吸附纤维的制备
将多孔复合纤维先浸渍于丙酮溶剂,浸渍时间为60min,浸渍温度为50℃,洗净丙酮,干燥后,再将纤维置于含磷阻燃整理剂中分别浸渍60min,浸渍温度为50℃,然后置于清水中,漂洗、干燥,即制备阻燃型多孔吸附纤维E。
本发明中用测试各实施例中纤维的比表面积来反应纤维的吸附性,比表面积采用Rise-1030全自动比表面积机孔隙度分析仪进行分析;接触角反应纤维的疏水与亲水性,采用Dataphysics OCA50AF接触角测试仪进行检测;极限氧指数反应纤维燃烧的难易程度,极限氧指数的测试方法为:将试样竖直地固定在玻璃燃烧筒中,其底座与可产生氮氧混合气流的装置相连,点燃试样的顶端,混合气流中的氧浓度将会持续下降,直至火焰熄灭,记录混合气流中点燃后能使其维持稳定的烛焰形燃烧时氧气的最低体积分数即为极限氧指数;抗菌率反应纤维的抗菌性能,其测量方法:将各样品的抗菌纤维与细菌接触,采用细菌计数测定法(AATCC 100-1988)进行测定,计数接触前的细菌数(m),接触60min后再采用上述的细菌计数测定法计数接触后的细菌数(n),计算杀菌率(m-n)/(m)×100%。
测试的结果如下表1所示。
对比例是采用常规的纤维,常规的纤维是使用纯的PET,在纺丝机上进行熔融纺丝,纺丝组件为六角形,纺丝温度为280℃,进行卷绕收集,并在丙酮中浸渍、清水漂洗得到聚酯常规纤维,得到为对比例中的常规纤维。
表1
从表1中可以看出,用本申请案制备出的多孔吸附纤维A、B、C、D、E、F与对比样相比,功能性有较大的提高。其中,多孔吸附纤维A的比表面积为对比样的3倍,抗菌型多孔纤维B、C都具有良好的杀菌效果,通过吸附疏水整理剂和亲水整理剂的多孔纤维D和E,与空白相比,有很好的亲疏水效果。阻燃型多孔纤维F的极限氧指数比空白对比样也有较大的提高,达到了阻燃纤维的要求。
Claims (3)
1.一种多孔吸附纤维,其特征在于:按重量百分比计,多孔吸附纤维由聚酯80~99.85%、金属-有机框架材料0.05~19.9%、醋酸丁酸纤维素0.1~5%制备而成;
所述聚酯为聚对苯二甲酸乙二醇酯,聚对苯二甲酸丙二醇酯,聚对苯二甲酸丁二醇酯中的一种;所述金属-有机框架材料的粒径目数为2000~10000目;所述金属-有机框架材料的结构为类沸石咪唑骨架型,莱瓦希尔骨架型,孔、通道式骨架型中的一种。
2.一种多孔吸附纤维的制备方法,包括以下步骤:
a)多孔复合纤维的制备:
按重量百分比计,将金属-有机框架材料0.05~19.9%、醋酸丁酸纤维素0.1~5%混合均匀得到多孔载体材料,将聚酯80~99.85%与多孔载体材料混合均匀放入纺丝机中进行熔融纺丝处理,得到多孔复合纤维;
b)多孔吸附纤维的制备:
将多孔复合纤维依次浸渍于丙酮与功能型吸附溶剂中,然后进行漂洗、干燥,即制备得到多功能载体纤维;
所述聚酯为聚对苯二甲酸乙二醇酯,聚对苯二甲酸丙二醇酯,聚对苯二甲酸丁二醇酯中的一种;所述金属-有机框架材料的粒径目数为2000~10000目;所述金属-有机框架材料的结构为类沸石咪唑骨架型,莱瓦希尔骨架型,孔、通道式骨架型中的一种;所述功能型吸附溶剂为银离子溶剂,卤胺类溶液,超疏水整理剂,超亲水整理剂、阻燃整理剂中的一种。
3.根据权利要求2所述的一种多孔吸附纤维的制备方法,具体包括以下步骤:
a)多孔复合纤维的制备:
按重量百分比计,称量原料:金属-有机框架材料0.05~19.9%,醋酸丁酸纤维素0.1~5%,混合均匀得到多孔载体材料,称量聚酯80~99.85%,聚酯与多孔载体材料混合均匀放入纺丝机中进行熔融纺丝处理,得到多孔复合纤维,所述熔融纺丝的喷丝板为中空性、单组份圆形、三角形、六角形中的一种;
b)多孔吸附纤维的制备:
将多孔复合纤维浸渍于丙酮溶剂中,浸渍时间为30~60min,浸渍温度为20~50℃,洗净丙酮,干燥后,再将纤维置于功能型吸附溶剂中进行吸附,吸附时间为20~60min,吸附温度为20~50℃,然后置于清水中,漂洗、干燥,即制备得到多孔吸附纤维。
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